# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email agapie@caltech.edu _publ_contact_author_name 'Theodor Agapie' loop_ _publ_author_name P.Kelley M.Radlauer A.Yanez-McKay M.Day T.Agapie data_mrr06 _database_code_depnum_ccdc_archive 'CCDC 861065' #TrackingRef '- mrr06.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H72 Al2 N8 O8 Pd, 6(C4 H8 O)' _chemical_formula_sum 'C92 H120 Al2 N8 O14 Pd' _chemical_formula_weight 1722.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9146(3) _cell_length_b 16.3913(5) _cell_length_c 24.2331(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.8030(10) _cell_angle_gamma 90.00 _cell_volume 4243.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7654 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 22.92 _exptl_crystal_description Fragment _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.309 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9638 _exptl_absorpt_correction_T_max 0.9908 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 6 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35112 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.38 _reflns_number_total 7335 _reflns_number_gt 4833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.68A' _computing_data_reduction 'Bruker SAINT-Plus v7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7335 _refine_ls_number_parameters 531 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 2.000 _refine_ls_restrained_S_all 1.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.0000 0.5000 0.01993(14) Uani 1 2 d S . . Al2 Al 0.64070(10) 0.01324(8) 0.37887(5) 0.0209(3) Uani 1 1 d . . . O1 O 0.6703(2) 0.09169(16) 0.43757(11) 0.0197(7) Uani 1 1 d . . . O2 O 0.53592(19) 0.00014(18) 0.62609(9) 0.0207(6) Uani 1 1 d . . . O3 O 0.6044(2) 0.09452(16) 0.32763(11) 0.0213(7) Uani 1 1 d . . . O4 O 0.6805(2) -0.06608(16) 0.43128(11) 0.0211(7) Uani 1 1 d . . . N1 N 0.6427(3) 0.07228(18) 0.48679(14) 0.0182(8) Uani 1 1 d . . . N2 N 0.5729(3) 0.02734(18) 0.58033(13) 0.0198(8) Uani 1 1 d . . . N3 N 0.6364(3) -0.07602(19) 0.31590(14) 0.0196(9) Uani 1 1 d . . . N4 N 0.8390(3) 0.02019(18) 0.37356(12) 0.0202(9) Uani 1 1 d . . . C1 C 0.7054(4) 0.1020(2) 0.53381(17) 0.0180(10) Uani 1 1 d . . . C2 C 0.6707(4) 0.0749(2) 0.58620(16) 0.0187(10) Uani 1 1 d . . . C3 C 0.8114(4) 0.1581(2) 0.54895(17) 0.0186(11) Uani 1 1 d . . . C4 C 0.8811(3) 0.2057(2) 0.51983(18) 0.0253(11) Uani 1 1 d . . . H4 H 0.8641 0.2064 0.4798 0.030 Uiso 1 1 calc R . . C5 C 0.9793(4) 0.2536(2) 0.55174(18) 0.0255(11) Uani 1 1 d . . . H5 H 1.0269 0.2873 0.5321 0.031 Uiso 1 1 calc R . . C6 C 1.0080(4) 0.2533(2) 0.60895(19) 0.0273(11) Uani 1 1 d . . . H6 H 1.0757 0.2855 0.6282 0.033 Uiso 1 1 calc R . . C7 C 0.9377(4) 0.2052(2) 0.64038(18) 0.0223(10) Uani 1 1 d . . . C8 C 0.9565(4) 0.1964(2) 0.69947(18) 0.0285(11) Uani 1 1 d . . . H8 H 1.0216 0.2264 0.7229 0.034 Uiso 1 1 calc R . . C9 C 0.8833(4) 0.1458(3) 0.72370(18) 0.0251(11) Uani 1 1 d . . . H9 H 0.8998 0.1405 0.7636 0.030 Uiso 1 1 calc R . . C10 C 0.7828(4) 0.1007(2) 0.69081(18) 0.0234(11) Uani 1 1 d . . . H10 H 0.7326 0.0659 0.7084 0.028 Uiso 1 1 calc R . . C11 C 0.7600(3) 0.1087(2) 0.63349(18) 0.0205(10) Uani 1 1 d . . . C12 C 0.8402(3) 0.1593(2) 0.60858(17) 0.0187(10) Uani 1 1 d . . . C13 C 0.7670(3) -0.0973(2) 0.31170(17) 0.0244(11) Uani 1 1 d . . . H13A H 0.7669 -0.1205 0.2740 0.029 Uiso 1 1 calc R . . H13B H 0.8000 -0.1394 0.3402 0.029 Uiso 1 1 calc R . . C14 C 0.8511(3) -0.0231(2) 0.32098(16) 0.0235(11) Uani 1 1 d . . . H14A H 0.9391 -0.0402 0.3236 0.028 Uiso 1 1 calc R . . H14B H 0.8283 0.0143 0.2885 0.028 Uiso 1 1 calc R . . C15 C 0.8843(3) 0.1053(2) 0.36997(17) 0.0274(11) Uani 1 1 d . . . H15A H 0.8733 0.1359 0.4034 0.041 Uiso 1 1 calc R . . H15B H 0.8362 0.1315 0.3360 0.041 Uiso 1 1 calc R . . H15C H 0.9731 0.1044 0.3681 0.041 Uiso 1 1 calc R . . C16 C 0.9220(3) -0.0177(2) 0.42282(15) 0.0263(11) Uani 1 1 d . . . H16A H 1.0095 -0.0099 0.4200 0.039 Uiso 1 1 calc R . . H16B H 0.9038 -0.0762 0.4236 0.039 Uiso 1 1 calc R . . H16C H 0.9076 0.0079 0.4575 0.039 Uiso 1 1 calc R . . C17 C 0.5633(4) -0.0469(2) 0.26048(16) 0.0244(11) Uani 1 1 d . . . H17A H 0.4749 -0.0401 0.2638 0.029 Uiso 1 1 calc R . . H17B H 0.5654 -0.0900 0.2321 0.029 Uiso 1 1 calc R . . C18 C 0.6062(3) 0.0313(2) 0.23884(17) 0.0202(10) Uani 1 1 d . . . C19 C 0.6277(3) 0.0384(3) 0.18435(17) 0.0257(11) Uani 1 1 d . . . H19 H 0.6204 -0.0085 0.1609 0.031 Uiso 1 1 calc R . . C20 C 0.6591(4) 0.1118(3) 0.16365(17) 0.0246(11) Uani 1 1 d . . . C21 C 0.6651(3) 0.1798(3) 0.19738(17) 0.0237(11) Uani 1 1 d . . . H21 H 0.6837 0.2310 0.1828 0.028 Uiso 1 1 calc R . . C22 C 0.6448(3) 0.1761(2) 0.25227(16) 0.0187(10) Uani 1 1 d . . . C23 C 0.6176(3) 0.0996(2) 0.27376(17) 0.0186(10) Uani 1 1 d . . . C24 C 0.6796(4) 0.1206(3) 0.10358(16) 0.0383(13) Uani 1 1 d . . . H24A H 0.6668 0.0676 0.0845 0.058 Uiso 1 1 calc R . . H24B H 0.7653 0.1394 0.1045 0.058 Uiso 1 1 calc R . . H24C H 0.6201 0.1603 0.0832 0.058 Uiso 1 1 calc R . . C25 C 0.6484(3) 0.2505(2) 0.28905(16) 0.0277(11) Uani 1 1 d . . . H25A H 0.5655 0.2596 0.2976 0.042 Uiso 1 1 calc R . . H25B H 0.6724 0.2982 0.2692 0.042 Uiso 1 1 calc R . . H25C H 0.7097 0.2423 0.3242 0.042 Uiso 1 1 calc R . . C26 C 0.5726(4) -0.1525(2) 0.32967(16) 0.0236(11) Uani 1 1 d . . . H26A H 0.4846 -0.1390 0.3305 0.028 Uiso 1 1 calc R . . H26B H 0.5713 -0.1921 0.2987 0.028 Uiso 1 1 calc R . . C27 C 0.6301(4) -0.1932(2) 0.38410(18) 0.0227(10) Uani 1 1 d . . . C28 C 0.6309(4) -0.2776(3) 0.38733(18) 0.0273(11) Uani 1 1 d . . . H28 H 0.5992 -0.3082 0.3542 0.033 Uiso 1 1 calc R . . C29 C 0.6758(4) -0.3188(3) 0.4366(2) 0.0292(11) Uani 1 1 d . . . C30 C 0.7248(3) -0.2726(3) 0.48353(18) 0.0247(11) Uani 1 1 d . . . H30 H 0.7575 -0.2999 0.5179 0.030 Uiso 1 1 calc R . . C31 C 0.7284(3) -0.1883(3) 0.48276(17) 0.0226(11) Uani 1 1 d . . . C32 C 0.6795(4) -0.1473(3) 0.43221(18) 0.0201(10) Uani 1 1 d . . . C33 C 0.6739(4) -0.4110(3) 0.43958(19) 0.0450(13) Uani 1 1 d . . . H33A H 0.7540 -0.4326 0.4337 0.068 Uiso 1 1 calc R . . H33B H 0.6059 -0.4321 0.4102 0.068 Uiso 1 1 calc R . . H33C H 0.6606 -0.4280 0.4767 0.068 Uiso 1 1 calc R . . C34 C 0.7835(4) -0.1397(3) 0.53419(18) 0.0336(13) Uani 1 1 d . . . H34A H 0.8171 -0.1769 0.5653 0.050 Uiso 1 1 calc R . . H34B H 0.7185 -0.1054 0.5448 0.050 Uiso 1 1 calc R . . H34C H 0.8510 -0.1051 0.5262 0.050 Uiso 1 1 calc R . . O1C O -0.0313(5) 0.3335(4) 0.3928(3) 0.198(3) Uani 1 1 d D . . C1C C 0.0607(5) 0.3490(3) 0.36059(19) 0.0586(16) Uani 1 1 d D . . H1C1 H 0.0247 0.3404 0.3201 0.070 Uiso 1 1 calc R . . H1C2 H 0.1318 0.3110 0.3719 0.070 Uiso 1 1 calc R . . C2C C 0.1039(7) 0.4328(4) 0.3700(4) 0.154(4) Uani 1 1 d D . . H2C1 H 0.0817 0.4649 0.3347 0.185 Uiso 1 1 calc R . . H2C2 H 0.1959 0.4345 0.3834 0.185 Uiso 1 1 calc R . . C3C C 0.0382(8) 0.4667(5) 0.4145(4) 0.225(7) Uani 1 1 d D . . H3C1 H 0.0923 0.4633 0.4526 0.270 Uiso 1 1 calc R . . H3C2 H 0.0125 0.5241 0.4065 0.270 Uiso 1 1 calc R . . C4C C -0.0662(8) 0.4150(5) 0.4096(4) 0.222(7) Uani 1 1 d D . . H4C1 H -0.1365 0.4368 0.3810 0.267 Uiso 1 1 calc R . . H4C2 H -0.0933 0.4119 0.4461 0.267 Uiso 1 1 calc R . . O1D O 0.1434(7) 0.0683(5) 0.2089(3) 0.219(4) Uani 1 1 d . . . C1D C 0.2596(7) 0.0916(4) 0.2176(3) 0.106(3) Uani 1 1 d . . . H1D H 0.2771 0.1176 0.1832 0.127 Uiso 1 1 calc R . . H1E H 0.3155 0.0438 0.2267 0.127 Uiso 1 1 calc R . . C2D C 0.2829(5) 0.1492(5) 0.2640(3) 0.093(2) Uani 1 1 d . . . H2D1 H 0.2810 0.2058 0.2496 0.112 Uiso 1 1 calc R . . H2D2 H 0.3658 0.1390 0.2885 0.112 Uiso 1 1 calc R . . C3D C 0.1822(7) 0.1367(4) 0.2959(3) 0.092(2) Uani 1 1 d . . . H3D1 H 0.1488 0.1891 0.3067 0.110 Uiso 1 1 calc R . . H3D2 H 0.2109 0.1030 0.3300 0.110 Uiso 1 1 calc R . . C4D C 0.0851(5) 0.0910(4) 0.2513(3) 0.085(2) Uani 1 1 d . . . H4D1 H 0.0539 0.0423 0.2682 0.102 Uiso 1 1 calc R . . H4D2 H 0.0131 0.1270 0.2364 0.102 Uiso 1 1 calc R . . O1E O 0.3794(7) 0.3020(4) 0.3788(3) 0.139(3) Uiso 0.614(5) 1 d PD A 1 C1E C 0.4665(5) 0.2444(3) 0.4073(2) 0.0138(17) Uiso 0.614(5) 1 d PD A 1 H1E1 H 0.5073 0.2158 0.3799 0.017 Uiso 0.614(5) 1 calc PR A 1 H1E2 H 0.4227 0.2034 0.4262 0.017 Uiso 0.614(5) 1 calc PR A 1 C2E C 0.5603(6) 0.2865(4) 0.4489(3) 0.043(3) Uiso 0.614(5) 1 d PD A 1 H2E1 H 0.6457 0.2724 0.4440 0.051 Uiso 0.614(5) 1 calc PR A 1 H2E2 H 0.5524 0.2714 0.4876 0.051 Uiso 0.614(5) 1 calc PR A 1 C3E C 0.5347(7) 0.3768(5) 0.4385(3) 0.074(3) Uiso 0.614(5) 1 d PD A 1 H3E1 H 0.5499 0.4079 0.4742 0.089 Uiso 0.614(5) 1 calc PR A 1 H3E2 H 0.5867 0.3998 0.4132 0.089 Uiso 0.614(5) 1 calc PR A 1 C4E C 0.4070(5) 0.3768(3) 0.4125(2) 0.0127(17) Uiso 0.614(5) 1 d PD A 1 H4E1 H 0.3874 0.4253 0.3880 0.015 Uiso 0.614(5) 1 calc PR A 1 H4E2 H 0.3551 0.3789 0.4415 0.015 Uiso 0.614(5) 1 calc PR A 1 O1F O 0.4651(7) 0.3366(5) 0.3674(3) 0.040(3) Uiso 0.386(5) 1 d PD A 2 C1F C 0.5718(9) 0.3814(5) 0.3938(4) 0.042(4) Uiso 0.386(5) 1 d PD A 2 H1F1 H 0.5467 0.4371 0.4027 0.050 Uiso 0.386(5) 1 calc PR A 2 H1F2 H 0.6312 0.3860 0.3681 0.050 Uiso 0.386(5) 1 calc PR A 2 C2F C 0.6316(10) 0.3399(8) 0.4454(4) 0.076(5) Uiso 0.386(5) 1 d PD A 2 H2F1 H 0.6239 0.3727 0.4789 0.092 Uiso 0.386(5) 1 calc PR A 2 H2F2 H 0.7215 0.3307 0.4460 0.092 Uiso 0.386(5) 1 calc PR A 2 C3F C 0.5631(19) 0.2593(10) 0.4451(7) 0.28(2) Uiso 0.386(5) 1 d PD A 2 H3F1 H 0.6069 0.2150 0.4291 0.336 Uiso 0.386(5) 1 calc PR A 2 H3F2 H 0.5537 0.2437 0.4835 0.336 Uiso 0.386(5) 1 calc PR A 2 C4F C 0.4466(15) 0.2768(11) 0.4101(7) 0.41(3) Uiso 0.386(5) 1 d PD A 2 H4F1 H 0.3888 0.2991 0.4329 0.496 Uiso 0.386(5) 1 calc PR A 2 H4F2 H 0.4093 0.2262 0.3915 0.496 Uiso 0.386(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0171(2) 0.0221(3) 0.0213(3) -0.0003(3) 0.0056(2) -0.0041(3) Al2 0.0162(7) 0.0251(8) 0.0221(7) 0.0001(7) 0.0052(5) -0.0017(7) O1 0.0180(17) 0.0229(18) 0.0195(18) 0.0033(14) 0.0070(14) -0.0043(14) O2 0.0189(14) 0.0256(15) 0.0188(15) 0.0032(16) 0.0070(11) -0.0020(17) O3 0.0174(17) 0.0254(18) 0.0214(19) 0.0026(14) 0.0045(14) -0.0024(14) O4 0.0187(17) 0.0220(18) 0.0227(18) 0.0018(14) 0.0049(14) -0.0028(13) N1 0.0129(19) 0.020(2) 0.023(2) 0.0028(17) 0.0062(17) -0.0010(16) N2 0.021(2) 0.021(2) 0.019(2) 0.0051(15) 0.0060(16) 0.0019(16) N3 0.015(2) 0.025(2) 0.018(2) 0.0017(17) 0.0021(17) -0.0013(17) N4 0.0172(18) 0.022(2) 0.022(2) -0.0010(16) 0.0043(16) -0.0008(16) C1 0.014(2) 0.017(2) 0.022(3) 0.000(2) 0.003(2) -0.001(2) C2 0.016(2) 0.019(3) 0.021(3) -0.001(2) 0.004(2) 0.002(2) C3 0.016(3) 0.015(2) 0.025(3) 0.001(2) 0.007(2) 0.004(2) C4 0.020(3) 0.027(3) 0.030(3) -0.001(2) 0.007(2) 0.000(2) C5 0.019(3) 0.022(3) 0.037(3) -0.002(2) 0.009(2) -0.004(2) C6 0.017(3) 0.024(3) 0.039(3) -0.005(2) 0.002(2) -0.004(2) C7 0.017(3) 0.025(3) 0.025(3) -0.005(2) 0.004(2) 0.004(2) C8 0.016(3) 0.028(3) 0.039(3) -0.014(2) 0.001(2) 0.001(2) C9 0.025(3) 0.029(3) 0.017(3) 0.001(2) -0.005(2) 0.010(2) C10 0.022(3) 0.024(3) 0.027(3) 0.002(2) 0.011(2) 0.002(2) C11 0.016(2) 0.022(3) 0.022(3) -0.002(2) 0.000(2) 0.006(2) C12 0.014(2) 0.019(2) 0.024(3) -0.006(2) 0.004(2) 0.004(2) C13 0.019(3) 0.024(3) 0.031(3) -0.005(2) 0.009(2) 0.001(2) C14 0.015(2) 0.027(3) 0.030(3) -0.003(2) 0.009(2) 0.004(2) C15 0.022(3) 0.022(3) 0.039(3) 0.001(2) 0.007(2) -0.003(2) C16 0.017(2) 0.031(3) 0.029(3) -0.001(2) -0.0011(19) -0.001(2) C17 0.022(3) 0.029(3) 0.021(3) -0.004(2) 0.002(2) 0.000(2) C18 0.013(2) 0.024(3) 0.023(3) -0.001(2) 0.002(2) -0.0001(19) C19 0.017(3) 0.031(3) 0.028(3) -0.004(2) 0.002(2) 0.001(2) C20 0.022(3) 0.033(3) 0.019(3) 0.002(2) 0.004(2) 0.004(2) C21 0.018(2) 0.028(3) 0.027(3) 0.008(2) 0.007(2) -0.001(2) C22 0.009(2) 0.025(3) 0.020(3) -0.001(2) -0.0025(19) 0.0024(19) C23 0.007(2) 0.025(3) 0.023(3) 0.004(2) 0.001(2) 0.000(2) C24 0.046(3) 0.044(3) 0.029(3) 0.002(2) 0.018(3) -0.004(3) C25 0.023(3) 0.028(3) 0.032(3) 0.007(2) 0.005(2) -0.003(2) C26 0.023(3) 0.018(3) 0.032(3) -0.005(2) 0.011(2) -0.005(2) C27 0.018(2) 0.021(3) 0.030(3) 0.004(2) 0.008(2) 0.000(2) C28 0.024(3) 0.023(3) 0.035(3) -0.006(2) 0.008(2) -0.004(2) C29 0.028(3) 0.022(3) 0.038(3) 0.006(2) 0.008(2) -0.001(2) C30 0.020(3) 0.025(3) 0.028(3) 0.008(2) 0.003(2) 0.003(2) C31 0.016(3) 0.029(3) 0.024(3) 0.004(2) 0.005(2) 0.001(2) C32 0.017(2) 0.018(3) 0.027(3) -0.003(2) 0.009(2) -0.003(2) C33 0.045(3) 0.029(3) 0.055(4) 0.009(3) -0.001(3) -0.001(3) C34 0.035(3) 0.034(3) 0.032(3) 0.007(2) 0.007(2) -0.003(2) O1C 0.135(6) 0.278(10) 0.172(6) 0.049(7) 0.009(5) -0.067(6) C1C 0.067(4) 0.079(5) 0.021(3) 0.011(3) -0.012(3) -0.004(4) C2C 0.105(7) 0.127(8) 0.240(11) 0.060(7) 0.056(7) -0.047(6) C3C 0.079(7) 0.293(17) 0.274(14) 0.041(12) -0.031(7) -0.101(9) C4C 0.249(15) 0.104(9) 0.344(17) 0.032(9) 0.130(12) 0.105(10) O1D 0.203(7) 0.336(10) 0.140(6) -0.088(6) 0.084(5) -0.161(7) C1D 0.102(7) 0.074(5) 0.156(9) 0.035(5) 0.059(6) -0.002(5) C2D 0.043(4) 0.107(6) 0.129(7) -0.035(5) 0.016(4) -0.018(4) C3D 0.151(7) 0.083(5) 0.051(5) 0.002(4) 0.043(5) 0.009(5) C4D 0.065(5) 0.082(5) 0.125(7) 0.045(5) 0.055(5) 0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 1.997(3) . yes Pd1 N2 1.997(3) 3_656 yes Pd1 N1 2.034(3) 3_656 yes Pd1 N1 2.034(3) . yes Al2 O4 1.807(3) . ? Al2 O3 1.809(3) . ? Al2 O1 1.896(3) . ? Al2 O2 1.919(2) 3_656 ? Al2 N3 2.108(3) . ? Al2 N4 2.197(3) . ? O1 N1 1.327(3) . ? O2 N2 1.332(3) . ? O2 Al2 1.919(2) 3_656 ? O3 C23 1.345(4) . ? O4 C32 1.332(4) . ? N1 C1 1.298(5) . ? N2 C2 1.307(4) . ? N3 C13 1.491(4) . ? N3 C17 1.493(5) . ? N3 C26 1.504(4) . ? N4 C16 1.479(4) . ? N4 C15 1.488(4) . ? N4 C14 1.488(4) . ? C1 C2 1.466(5) . ? C1 C3 1.465(5) . ? C2 C11 1.453(5) . ? C3 C4 1.380(5) . ? C3 C12 1.415(5) . ? C4 C5 1.422(5) . ? C5 C6 1.358(5) . ? C6 C7 1.425(5) . ? C7 C12 1.399(5) . ? C7 C8 1.412(5) . ? C8 C9 1.366(5) . ? C9 C10 1.423(5) . ? C10 C11 1.367(5) . ? C11 C12 1.426(5) . ? C13 C14 1.513(5) . ? C17 C18 1.496(5) . ? C18 C19 1.392(5) . ? C18 C23 1.394(5) . ? C19 C20 1.373(5) . ? C20 C21 1.376(5) . ? C20 C24 1.524(5) . ? C21 C22 1.394(5) . ? C22 C23 1.412(5) . ? C22 C25 1.507(5) . ? C26 C27 1.496(5) . ? C27 C28 1.387(5) . ? C27 C32 1.399(5) . ? C28 C29 1.371(5) . ? C29 C30 1.380(5) . ? C29 C33 1.514(6) . ? C30 C31 1.382(5) . ? C31 C32 1.403(5) . ? C31 C34 1.497(5) . ? O1C C1C 1.415(5) . ? O1C C4C 1.470(6) . ? C1C C2C 1.455(6) . ? C2C C3C 1.518(7) . ? C3C C4C 1.406(7) . ? O1D C1D 1.299(7) . ? O1D C4D 1.365(7) . ? C1D C2D 1.450(8) . ? C2D C3D 1.482(7) . ? C3D C4D 1.544(8) . ? O1E C1E 1.415(5) . ? O1E C4E 1.469(6) . ? C1E C2E 1.455(6) . ? C2E C3E 1.518(7) . ? C3E C4E 1.407(7) . ? O1F C1F 1.415(5) . ? O1F C4F 1.469(6) . ? C1F C2F 1.455(6) . ? C2F C3F 1.518(7) . ? C3F C4F 1.406(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N2 180.0 . 3_656 yes N2 Pd1 N1 98.19(13) . 3_656 yes N2 Pd1 N1 81.81(13) 3_656 3_656 yes N2 Pd1 N1 81.81(13) . . yes N2 Pd1 N1 98.19(13) 3_656 . yes N1 Pd1 N1 180.0 3_656 . yes O4 Al2 O3 178.30(14) . . ? O4 Al2 O1 88.92(11) . . ? O3 Al2 O1 89.73(13) . . ? O4 Al2 O2 93.22(12) . 3_656 ? O3 Al2 O2 87.99(12) . 3_656 ? O1 Al2 O2 98.03(11) . 3_656 ? O4 Al2 N3 88.62(13) . . ? O3 Al2 N3 92.57(13) . . ? O1 Al2 N3 171.61(12) . . ? O2 Al2 N3 90.12(12) 3_656 . ? O4 Al2 N4 88.86(12) . . ? O3 Al2 N4 90.10(12) . . ? O1 Al2 N4 89.42(12) . . ? O2 Al2 N4 172.30(12) 3_656 . ? N3 Al2 N4 82.52(12) . . ? N1 O1 Al2 118.5(2) . . ? N2 O2 Al2 117.21(19) . 3_656 ? C23 O3 Al2 131.3(2) . . ? C32 O4 Al2 136.8(3) . . ? C1 N1 O1 121.5(3) . . ? C1 N1 Pd1 111.3(3) . . ? O1 N1 Pd1 127.1(2) . . ? C2 N2 O2 119.3(3) . . ? C2 N2 Pd1 113.2(2) . . ? O2 N2 Pd1 127.5(2) . . ? C13 N3 C17 110.9(3) . . ? C13 N3 C26 108.2(3) . . ? C17 N3 C26 106.2(3) . . ? C13 N3 Al2 109.4(2) . . ? C17 N3 Al2 111.0(2) . . ? C26 N3 Al2 111.1(2) . . ? C16 N4 C15 106.6(3) . . ? C16 N4 C14 110.1(3) . . ? C15 N4 C14 108.0(3) . . ? C16 N4 Al2 112.3(2) . . ? C15 N4 Al2 113.2(2) . . ? C14 N4 Al2 106.6(2) . . ? N1 C1 C2 117.6(4) . . ? N1 C1 C3 134.7(4) . . ? C2 C1 C3 107.7(4) . . ? N2 C2 C11 135.6(4) . . ? N2 C2 C1 115.9(4) . . ? C11 C2 C1 108.5(3) . . ? C4 C3 C12 119.0(4) . . ? C4 C3 C1 135.8(4) . . ? C12 C3 C1 105.3(3) . . ? C3 C4 C5 117.8(4) . . ? C6 C5 C4 123.0(4) . . ? C5 C6 C7 120.7(4) . . ? C12 C7 C8 116.1(4) . . ? C12 C7 C6 115.8(4) . . ? C8 C7 C6 128.0(4) . . ? C9 C8 C7 121.4(4) . . ? C8 C9 C10 121.8(4) . . ? C11 C10 C9 118.6(4) . . ? C10 C11 C12 119.1(4) . . ? C10 C11 C2 135.9(4) . . ? C12 C11 C2 105.0(3) . . ? C7 C12 C3 123.7(4) . . ? C7 C12 C11 122.9(4) . . ? C3 C12 C11 113.4(4) . . ? N3 C13 C14 111.2(3) . . ? N4 C14 C13 110.7(3) . . ? N3 C17 C18 116.2(3) . . ? C19 C18 C23 119.8(4) . . ? C19 C18 C17 122.0(3) . . ? C23 C18 C17 118.1(3) . . ? C20 C19 C18 121.6(4) . . ? C19 C20 C21 118.5(4) . . ? C19 C20 C24 121.9(4) . . ? C21 C20 C24 119.5(4) . . ? C20 C21 C22 122.3(4) . . ? C21 C22 C23 118.5(4) . . ? C21 C22 C25 122.6(4) . . ? C23 C22 C25 118.9(3) . . ? O3 C23 C18 121.7(4) . . ? O3 C23 C22 119.0(4) . . ? C18 C23 C22 119.3(4) . . ? C27 C26 N3 115.9(3) . . ? C28 C27 C32 119.5(4) . . ? C28 C27 C26 119.4(4) . . ? C32 C27 C26 121.0(4) . . ? C29 C28 C27 122.5(4) . . ? C28 C29 C30 117.2(4) . . ? C28 C29 C33 121.8(4) . . ? C30 C29 C33 121.0(4) . . ? C29 C30 C31 123.0(4) . . ? C30 C31 C32 118.9(4) . . ? C30 C31 C34 121.9(4) . . ? C32 C31 C34 119.3(4) . . ? O4 C32 C27 121.7(4) . . ? O4 C32 C31 119.3(4) . . ? C27 C32 C31 118.9(4) . . ? C1C O1C C4C 104.0(4) . . ? O1C C1C C2C 109.1(4) . . ? C1C C2C C3C 105.8(4) . . ? C4C C3C C2C 102.2(6) . . ? C3C C4C O1C 108.7(5) . . ? C1D O1D C4D 112.8(7) . . ? O1D C1D C2D 109.1(6) . . ? C1D C2D C3D 106.5(6) . . ? C2D C3D C4D 100.2(5) . . ? O1D C4D C3D 107.5(5) . . ? C1E O1E C4E 104.2(4) . . ? O1E C1E C2E 109.2(4) . . ? C1E C2E C3E 105.5(4) . . ? C4E C3E C2E 101.9(6) . . ? C3E C4E O1E 108.6(5) . . ? C1F O1F C4F 104.3(4) . . ? O1F C1F C2F 109.2(4) . . ? C1F C2F C3F 105.6(5) . . ? C4F C3F C2F 102.1(6) . . ? C3F C4F O1F 108.8(5) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.941 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.088 # Attachment '- mrr11.cif' data_mrr11 _database_code_depnum_ccdc_archive 'CCDC 861066' #TrackingRef '- mrr11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H120 Al2 N8 O8, 4(C4 H8 O)' _chemical_formula_sum 'C108 H152 Al2 N8 O12' _chemical_formula_weight 1808.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9403(6) _cell_length_b 12.7271(7) _cell_length_c 17.7934(9) _cell_angle_alpha 98.660(2) _cell_angle_beta 103.176(2) _cell_angle_gamma 106.624(2) _cell_volume 2454.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9551 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.61 _exptl_crystal_description Plate _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 978 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9756 _exptl_absorpt_correction_T_max 0.9962 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 13 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10751 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.71 _reflns_number_total 10751 _reflns_number_gt 8322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.68A' _computing_data_reduction 'Bruker SAINT-Plus v7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10751 _refine_ls_number_parameters 601 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 3.445 _refine_ls_restrained_S_all 3.445 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.25186(6) 0.74258(6) 0.64938(5) 0.01205(18) Uani 1 1 d . . . O1 O 0.25110(13) 0.67875(13) 0.54774(9) 0.0131(4) Uani 1 1 d . . . O2 O -0.16738(13) 0.39285(13) 0.32141(10) 0.0143(4) Uani 1 1 d . . . O3 O 0.39416(12) 0.71901(13) 0.68486(9) 0.0130(4) Uani 1 1 d . . . O4 O 0.10496(13) 0.76134(13) 0.60989(9) 0.0130(4) Uani 1 1 d . . . N1 N 0.14330(16) 0.60930(16) 0.49691(12) 0.0122(5) Uani 1 1 d . . . N2 N -0.06360(16) 0.45770(15) 0.37766(12) 0.0127(5) Uani 1 1 d . . . N3 N 0.27504(16) 0.83732(16) 0.76308(12) 0.0123(5) Uani 1 1 d . . . N4 N 0.34625(16) 0.91029(16) 0.63429(12) 0.0144(5) Uani 1 1 d . . . C1 C 0.1413(2) 0.59346(19) 0.42309(15) 0.0113(6) Uani 1 1 d . . . C2 C 0.0289(2) 0.52164(19) 0.36019(14) 0.0121(6) Uani 1 1 d . . . C3 C 0.2325(2) 0.63906(19) 0.38242(15) 0.0128(6) Uani 1 1 d . . . C4 C 0.3547(2) 0.70121(19) 0.40662(15) 0.0150(6) Uani 1 1 d . . . H4 H 0.3981 0.7275 0.4614 0.018 Uiso 1 1 calc R . . C5 C 0.4141(2) 0.7249(2) 0.34779(15) 0.0157(6) Uani 1 1 d . . . H5 H 0.4986 0.7674 0.3642 0.019 Uiso 1 1 calc R . . C6 C 0.3552(2) 0.6893(2) 0.26826(16) 0.0178(6) Uani 1 1 d . . . H6 H 0.3991 0.7077 0.2311 0.021 Uiso 1 1 calc R . . C7 C 0.2288(2) 0.6249(2) 0.24076(15) 0.0152(6) Uani 1 1 d . . . C8 C 0.1540(2) 0.5789(2) 0.16139(16) 0.0196(7) Uani 1 1 d . . . H8 H 0.1877 0.5928 0.1189 0.024 Uiso 1 1 calc R . . C9 C 0.0328(2) 0.5141(2) 0.14491(16) 0.0209(7) Uani 1 1 d . . . H9 H -0.0154 0.4856 0.0912 0.025 Uiso 1 1 calc R . . C10 C -0.0210(2) 0.4892(2) 0.20566(15) 0.0181(6) Uani 1 1 d . . . H10 H -0.1041 0.4433 0.1930 0.022 Uiso 1 1 calc R . . C11 C 0.0480(2) 0.5320(2) 0.28323(15) 0.0125(6) Uani 1 1 d . . . C12 C 0.1720(2) 0.60156(19) 0.29991(15) 0.0115(6) Uani 1 1 d . . . C13 C 0.3505(2) 0.95696(19) 0.77353(15) 0.0163(6) Uani 1 1 d . . . H13A H 0.4378 0.9661 0.7942 0.020 Uiso 1 1 calc R . . H13B H 0.3293 1.0061 0.8127 0.020 Uiso 1 1 calc R . . C14 C 0.3290(2) 0.9923(2) 0.69524(15) 0.0187(6) Uani 1 1 d . . . H14A H 0.2451 0.9951 0.6786 0.022 Uiso 1 1 calc R . . H14B H 0.3870 1.0685 0.7014 0.022 Uiso 1 1 calc R . . C15 C 0.3359(2) 0.7900(2) 0.82558(15) 0.0149(6) Uani 1 1 d . . . H15A H 0.2812 0.7131 0.8213 0.018 Uiso 1 1 calc R . . H15B H 0.3444 0.8362 0.8779 0.018 Uiso 1 1 calc R . . C16 C 0.4596(2) 0.7831(2) 0.82465(15) 0.0140(6) Uani 1 1 d . . . C17 C 0.5482(2) 0.80521(19) 0.89696(15) 0.0149(6) Uani 1 1 d . . . H17 H 0.5351 0.8382 0.9443 0.018 Uiso 1 1 calc R . . C18 C 0.6549(2) 0.7802(2) 0.90130(15) 0.0151(6) Uani 1 1 d . . . C19 C 0.6693(2) 0.73221(19) 0.82984(15) 0.0150(6) Uani 1 1 d . . . H19 H 0.7417 0.7143 0.8319 0.018 Uiso 1 1 calc R . . C20 C 0.5852(2) 0.7086(2) 0.75549(15) 0.0136(6) Uani 1 1 d . . . C21 C 0.4773(2) 0.73778(19) 0.75326(15) 0.0135(6) Uani 1 1 d . . . C22 C 0.7520(2) 0.7993(2) 0.97980(15) 0.0184(6) Uani 1 1 d . . . C23 C 0.7666(2) 0.6866(2) 0.99145(16) 0.0295(7) Uani 1 1 d . . . H23A H 0.7869 0.6512 0.9459 0.044 Uiso 1 1 calc R . . H23B H 0.6901 0.6367 0.9960 0.044 Uiso 1 1 calc R . . H23C H 0.8322 0.6996 1.0400 0.044 Uiso 1 1 calc R . . C24 C 0.7197(2) 0.8518(2) 1.05028(15) 0.0259(7) Uani 1 1 d . . . H24A H 0.7855 0.8653 1.0988 0.039 Uiso 1 1 calc R . . H24B H 0.6438 0.8006 1.0546 0.039 Uiso 1 1 calc R . . H24C H 0.7088 0.9235 1.0432 0.039 Uiso 1 1 calc R . . C25 C 0.8754(2) 0.8777(2) 0.97799(16) 0.0303(8) Uani 1 1 d . . . H25A H 0.8686 0.9511 0.9720 0.045 Uiso 1 1 calc R . . H25B H 0.8989 0.8444 0.9332 0.045 Uiso 1 1 calc R . . H25C H 0.9375 0.8876 1.0276 0.045 Uiso 1 1 calc R . . C26 C 0.6017(2) 0.6462(2) 0.68049(15) 0.0165(6) Uani 1 1 d . . . C27 C 0.7277(2) 0.6305(2) 0.69620(16) 0.0247(7) Uani 1 1 d . . . H27A H 0.7354 0.5911 0.6469 0.037 Uiso 1 1 calc R . . H27B H 0.7359 0.5861 0.7363 0.037 Uiso 1 1 calc R . . H27C H 0.7918 0.7045 0.7154 0.037 Uiso 1 1 calc R . . C28 C 0.5905(2) 0.7078(2) 0.61274(15) 0.0203(7) Uani 1 1 d . . . H28A H 0.6030 0.6650 0.5666 0.030 Uiso 1 1 calc R . . H28B H 0.6523 0.7831 0.6301 0.030 Uiso 1 1 calc R . . H28C H 0.5091 0.7148 0.5983 0.030 Uiso 1 1 calc R . . C29 C 0.5025(2) 0.5291(2) 0.65203(16) 0.0249(7) Uani 1 1 d . . . H29A H 0.4218 0.5378 0.6422 0.037 Uiso 1 1 calc R . . H29B H 0.5125 0.4860 0.6929 0.037 Uiso 1 1 calc R . . H29C H 0.5099 0.4889 0.6029 0.037 Uiso 1 1 calc R . . C30 C 0.15292(19) 0.8296(2) 0.77526(14) 0.0141(6) Uani 1 1 d . . . H30A H 0.1088 0.7498 0.7727 0.017 Uiso 1 1 calc R . . H30B H 0.1665 0.8730 0.8295 0.017 Uiso 1 1 calc R . . C31 C 0.07209(19) 0.8706(2) 0.71839(14) 0.0118(6) Uani 1 1 d . . . C32 C 0.0178(2) 0.94542(19) 0.74600(15) 0.0151(6) Uani 1 1 d . . . H32 H 0.0405 0.9772 0.8013 0.018 Uiso 1 1 calc R . . C33 C -0.0688(2) 0.97535(19) 0.69524(15) 0.0119(6) Uani 1 1 d . . . C34 C -0.10469(19) 0.92033(19) 0.61528(15) 0.0131(6) Uani 1 1 d . . . H34 H -0.1664 0.9371 0.5800 0.016 Uiso 1 1 calc R . . C35 C -0.0560(2) 0.8422(2) 0.58360(15) 0.0125(6) Uani 1 1 d . . . C36 C 0.0420(2) 0.82293(19) 0.63597(15) 0.0135(6) Uani 1 1 d . . . C37 C -0.1227(2) 1.0615(2) 0.72720(15) 0.0154(6) Uani 1 1 d . . . C38 C -0.0209(2) 1.1729(2) 0.77038(15) 0.0216(7) Uani 1 1 d . . . H38A H 0.0356 1.1607 0.8149 0.032 Uiso 1 1 calc R . . H38B H -0.0563 1.2280 0.7904 0.032 Uiso 1 1 calc R . . H38C H 0.0233 1.2015 0.7335 0.032 Uiso 1 1 calc R . . C39 C -0.1903(2) 1.0177(2) 0.78584(15) 0.0232(7) Uani 1 1 d . . . H39A H -0.1326 1.0075 0.8307 0.035 Uiso 1 1 calc R . . H39B H -0.2545 0.9453 0.7591 0.035 Uiso 1 1 calc R . . H39C H -0.2268 1.0722 0.8052 0.035 Uiso 1 1 calc R . . C40 C -0.2112(2) 1.0857(2) 0.66114(15) 0.0196(7) Uani 1 1 d . . . H40A H -0.2440 1.1410 0.6841 0.029 Uiso 1 1 calc R . . H40B H -0.2783 1.0158 0.6328 0.029 Uiso 1 1 calc R . . H40C H -0.1683 1.1158 0.6241 0.029 Uiso 1 1 calc R . . C41 C -0.1122(2) 0.7736(2) 0.49708(15) 0.0145(6) Uani 1 1 d . . . C42 C -0.0221(2) 0.7980(2) 0.44790(14) 0.0189(6) Uani 1 1 d . . . H42A H -0.0626 0.7559 0.3928 0.028 Uiso 1 1 calc R . . H42B H 0.0477 0.7747 0.4696 0.028 Uiso 1 1 calc R . . H42C H 0.0063 0.8789 0.4499 0.028 Uiso 1 1 calc R . . C43 C -0.1526(2) 0.64755(19) 0.49595(15) 0.0174(6) Uani 1 1 d . . . H43A H -0.1910 0.6037 0.4411 0.026 Uiso 1 1 calc R . . H43B H -0.2112 0.6311 0.5268 0.026 Uiso 1 1 calc R . . H43C H -0.0814 0.6272 0.5193 0.026 Uiso 1 1 calc R . . C44 C -0.2253(2) 0.8006(2) 0.45501(15) 0.0219(7) Uani 1 1 d . . . H44A H -0.2009 0.8800 0.4522 0.033 Uiso 1 1 calc R . . H44B H -0.2854 0.7866 0.4849 0.033 Uiso 1 1 calc R . . H44C H -0.2613 0.7525 0.4012 0.033 Uiso 1 1 calc R . . C45 C 0.47784(19) 0.9333(2) 0.64375(15) 0.0196(7) Uani 1 1 d . . . H45A H 0.5152 1.0110 0.6401 0.029 Uiso 1 1 calc R . . H45B H 0.4887 0.8811 0.6018 0.029 Uiso 1 1 calc R . . H45C H 0.5169 0.9232 0.6956 0.029 Uiso 1 1 calc R . . C46 C 0.2942(2) 0.9287(2) 0.55507(15) 0.0210(7) Uani 1 1 d . . . H46A H 0.2085 0.9223 0.5481 0.031 Uiso 1 1 calc R . . H46B H 0.2997 0.8719 0.5136 0.031 Uiso 1 1 calc R . . H46C H 0.3400 1.0040 0.5513 0.031 Uiso 1 1 calc R . . O1C O 0.56829(16) 0.67502(17) 0.15767(13) 0.0379(6) Uani 1 1 d . . . C1C C 0.5235(3) 0.5566(2) 0.12794(18) 0.0423(9) Uani 1 1 d . . . H1C1 H 0.4907 0.5380 0.0694 0.051 Uiso 1 1 calc R . . H1C2 H 0.4573 0.5216 0.1504 0.051 Uiso 1 1 calc R . . C2C C 0.6277(3) 0.5133(2) 0.15158(19) 0.0454(9) Uani 1 1 d . . . H2C1 H 0.6643 0.5028 0.1076 0.055 Uiso 1 1 calc R . . H2C2 H 0.6001 0.4405 0.1667 0.055 Uiso 1 1 calc R . . C3C C 0.7174(2) 0.6025(2) 0.2211(2) 0.0474(10) Uani 1 1 d . . . H3C1 H 0.8001 0.6243 0.2139 0.057 Uiso 1 1 calc R . . H3C2 H 0.7205 0.5762 0.2709 0.057 Uiso 1 1 calc R . . C4C C 0.6695(3) 0.6991(2) 0.22243(18) 0.0421(9) Uani 1 1 d . . . H4C1 H 0.6467 0.7144 0.2721 0.051 Uiso 1 1 calc R . . H4C2 H 0.7340 0.7675 0.2213 0.051 Uiso 1 1 calc R . . O1D O 0.20451(17) 0.68081(18) -0.01210(13) 0.0529(7) Uani 1 1 d . . . C1D C 0.1706(3) 0.7773(3) 0.0080(2) 0.0636(12) Uani 1 1 d . . . H1D1 H 0.1280 0.7695 0.0496 0.076 Uiso 1 1 calc R . . H1D2 H 0.1156 0.7874 -0.0392 0.076 Uiso 1 1 calc R . . C2D C 0.2869(4) 0.8755(3) 0.0378(2) 0.0647(12) Uani 1 1 d . . . H2D1 H 0.3121 0.9051 -0.0063 0.078 Uiso 1 1 calc R . . H2D2 H 0.2798 0.9370 0.0757 0.078 Uiso 1 1 calc R . . C3D C 0.3722(3) 0.8225(3) 0.07750(19) 0.0469(10) Uani 1 1 d . . . H3D1 H 0.3665 0.8194 0.1318 0.056 Uiso 1 1 calc R . . H3D2 H 0.4575 0.8644 0.0804 0.056 Uiso 1 1 calc R . . C4D C 0.3295(2) 0.7057(2) 0.02479(18) 0.0335(8) Uani 1 1 d . . . H4D1 H 0.3747 0.7039 -0.0154 0.040 Uiso 1 1 calc R . . H4D2 H 0.3423 0.6505 0.0566 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0110(4) 0.0134(4) 0.0107(5) 0.0007(4) 0.0020(3) 0.0043(3) O1 0.0093(8) 0.0149(10) 0.0097(10) -0.0019(8) -0.0018(8) 0.0021(7) O2 0.0078(8) 0.0157(10) 0.0146(11) 0.0013(8) -0.0002(8) 0.0006(7) O3 0.0093(9) 0.0182(10) 0.0108(10) 0.0019(8) 0.0015(8) 0.0053(7) O4 0.0082(8) 0.0168(10) 0.0135(10) 0.0003(8) 0.0020(8) 0.0062(7) N1 0.0108(11) 0.0093(11) 0.0127(13) -0.0017(10) -0.0007(10) 0.0032(9) N2 0.0048(10) 0.0089(11) 0.0201(13) -0.0016(10) 0.0017(10) -0.0001(9) N3 0.0096(11) 0.0141(12) 0.0132(13) 0.0025(10) 0.0029(10) 0.0043(9) N4 0.0103(11) 0.0172(12) 0.0159(13) 0.0026(10) 0.0039(10) 0.0055(9) C1 0.0110(13) 0.0107(14) 0.0122(16) 0.0020(12) 0.0029(12) 0.0042(10) C2 0.0130(13) 0.0123(14) 0.0119(15) 0.0013(12) 0.0033(12) 0.0065(11) C3 0.0165(14) 0.0136(14) 0.0137(16) 0.0054(12) 0.0080(12) 0.0088(11) C4 0.0144(14) 0.0163(15) 0.0131(16) 0.0018(12) 0.0023(12) 0.0052(11) C5 0.0100(13) 0.0149(15) 0.0220(17) 0.0041(13) 0.0049(13) 0.0036(11) C6 0.0174(14) 0.0180(15) 0.0253(18) 0.0094(13) 0.0144(14) 0.0080(12) C7 0.0183(14) 0.0126(14) 0.0174(16) 0.0050(12) 0.0066(13) 0.0072(11) C8 0.0258(15) 0.0195(16) 0.0181(17) 0.0068(13) 0.0140(14) 0.0068(12) C9 0.0256(15) 0.0214(16) 0.0115(16) 0.0010(13) 0.0039(13) 0.0040(12) C10 0.0123(13) 0.0164(15) 0.0212(17) 0.0040(13) 0.0035(13) -0.0003(11) C11 0.0131(13) 0.0142(14) 0.0103(15) 0.0016(12) 0.0028(12) 0.0055(11) C12 0.0149(13) 0.0107(14) 0.0114(15) 0.0039(12) 0.0052(12) 0.0061(11) C13 0.0132(13) 0.0146(14) 0.0174(16) -0.0008(12) 0.0023(12) 0.0029(11) C14 0.0163(14) 0.0138(15) 0.0239(18) 0.0003(13) 0.0044(13) 0.0048(11) C15 0.0146(13) 0.0189(15) 0.0121(15) 0.0035(12) 0.0029(12) 0.0075(11) C16 0.0104(13) 0.0139(14) 0.0174(16) 0.0038(12) 0.0047(12) 0.0029(11) C17 0.0153(13) 0.0139(14) 0.0124(16) 0.0009(12) 0.0027(12) 0.0022(11) C18 0.0103(13) 0.0170(15) 0.0172(17) 0.0048(12) 0.0038(12) 0.0033(11) C19 0.0088(13) 0.0188(15) 0.0211(17) 0.0076(13) 0.0070(13) 0.0062(11) C20 0.0098(13) 0.0144(14) 0.0163(16) 0.0050(12) 0.0052(12) 0.0017(11) C21 0.0103(13) 0.0116(14) 0.0165(16) 0.0057(12) 0.0022(12) 0.0006(11) C22 0.0145(14) 0.0249(16) 0.0130(16) 0.0035(13) -0.0015(12) 0.0069(12) C23 0.0299(16) 0.0339(18) 0.0222(18) 0.0071(15) -0.0026(14) 0.0147(14) C24 0.0191(15) 0.0348(18) 0.0173(17) 0.0025(14) -0.0037(13) 0.0078(13) C25 0.0146(15) 0.043(2) 0.0234(18) 0.0088(15) -0.0036(13) 0.0013(13) C26 0.0133(13) 0.0204(15) 0.0178(17) 0.0040(13) 0.0050(12) 0.0083(11) C27 0.0263(15) 0.0331(18) 0.0233(18) 0.0065(14) 0.0106(14) 0.0199(13) C28 0.0201(14) 0.0271(17) 0.0156(17) 0.0025(13) 0.0084(13) 0.0094(12) C29 0.0288(16) 0.0202(16) 0.0266(18) 0.0013(13) 0.0101(14) 0.0099(13) C30 0.0111(13) 0.0199(15) 0.0118(15) 0.0021(12) 0.0044(12) 0.0058(11) C31 0.0078(12) 0.0162(15) 0.0098(15) 0.0023(12) 0.0029(12) 0.0020(11) C32 0.0142(14) 0.0161(15) 0.0111(15) -0.0007(12) 0.0036(12) 0.0011(11) C33 0.0107(13) 0.0107(14) 0.0126(15) 0.0012(11) 0.0041(12) 0.0014(10) C34 0.0090(13) 0.0154(14) 0.0160(16) 0.0057(12) 0.0044(12) 0.0039(11) C35 0.0102(13) 0.0138(14) 0.0138(16) 0.0053(12) 0.0057(12) 0.0016(11) C36 0.0109(13) 0.0111(14) 0.0169(16) 0.0031(12) 0.0058(12) 0.0002(11) C37 0.0145(13) 0.0188(15) 0.0151(16) 0.0039(12) 0.0048(12) 0.0083(11) C38 0.0225(14) 0.0238(16) 0.0174(17) -0.0007(13) 0.0020(13) 0.0117(12) C39 0.0266(15) 0.0273(17) 0.0241(18) 0.0095(14) 0.0115(14) 0.0165(13) C40 0.0167(14) 0.0240(16) 0.0219(17) 0.0038(13) 0.0079(13) 0.0114(12) C41 0.0135(13) 0.0180(15) 0.0104(15) -0.0002(12) 0.0010(12) 0.0065(11) C42 0.0185(14) 0.0241(16) 0.0121(16) 0.0020(13) 0.0041(13) 0.0054(12) C43 0.0143(14) 0.0178(15) 0.0173(16) -0.0006(12) 0.0036(12) 0.0040(11) C44 0.0205(15) 0.0277(17) 0.0144(16) -0.0011(13) -0.0007(13) 0.0107(12) C45 0.0158(14) 0.0188(16) 0.0249(18) 0.0055(13) 0.0077(13) 0.0051(11) C46 0.0193(14) 0.0225(16) 0.0193(17) 0.0059(13) 0.0033(13) 0.0054(12) O1C 0.0284(12) 0.0371(14) 0.0493(16) 0.0142(11) 0.0082(11) 0.0128(10) C1C 0.042(2) 0.040(2) 0.028(2) 0.0021(17) 0.0041(17) -0.0037(16) C2C 0.069(2) 0.0228(19) 0.051(2) 0.0103(17) 0.025(2) 0.0177(17) C3C 0.0301(18) 0.032(2) 0.075(3) 0.0058(19) 0.0100(19) 0.0113(15) C4C 0.054(2) 0.038(2) 0.028(2) -0.0019(17) -0.0026(18) 0.0219(17) O1D 0.0296(12) 0.0524(16) 0.0552(17) -0.0166(13) -0.0034(12) 0.0087(11) C1D 0.057(2) 0.091(3) 0.048(3) 0.006(2) -0.002(2) 0.052(2) C2D 0.141(4) 0.036(2) 0.051(3) 0.021(2) 0.065(3) 0.044(2) C3D 0.039(2) 0.049(2) 0.038(2) -0.0144(18) 0.0138(18) 0.0019(17) C4D 0.0324(18) 0.036(2) 0.036(2) 0.0123(16) 0.0181(16) 0.0086(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O3 1.7988(16) . ? Al1 O4 1.8318(16) . ? Al1 O1 1.8646(17) . ? Al1 O2 1.9423(17) 2_566 ? Al1 N3 2.108(2) . ? Al1 N4 2.198(2) . ? O1 N1 1.354(2) . ? O2 N2 1.349(2) . ? O2 Al1 1.9423(17) 2_566 ? O3 C21 1.323(3) . ? O4 C36 1.334(3) . ? N1 C1 1.292(3) . ? N2 C2 1.303(3) . ? N3 C15 1.487(3) . ? N3 C13 1.489(3) . ? N3 C30 1.501(3) . ? N4 C45 1.478(3) . ? N4 C14 1.481(3) . ? N4 C46 1.487(3) . ? C1 C2 1.481(3) . ? C1 C3 1.474(3) . ? C2 C11 1.457(3) . ? C3 C4 1.375(3) . ? C3 C12 1.419(3) . ? C4 C5 1.414(3) . ? C5 C6 1.369(3) . ? C6 C7 1.422(3) . ? C7 C12 1.400(3) . ? C7 C8 1.418(3) . ? C8 C9 1.382(3) . ? C9 C10 1.409(3) . ? C10 C11 1.371(3) . ? C11 C12 1.427(3) . ? C13 C14 1.517(3) . ? C15 C16 1.508(3) . ? C16 C17 1.398(3) . ? C16 C21 1.401(3) . ? C17 C18 1.387(3) . ? C18 C19 1.395(3) . ? C18 C22 1.534(3) . ? C19 C20 1.397(3) . ? C20 C21 1.433(3) . ? C20 C26 1.530(3) . ? C22 C24 1.512(3) . ? C22 C25 1.535(3) . ? C22 C23 1.532(3) . ? C26 C28 1.536(3) . ? C26 C27 1.542(3) . ? C26 C29 1.540(3) . ? C30 C31 1.493(3) . ? C31 C32 1.388(3) . ? C31 C36 1.420(3) . ? C32 C33 1.390(3) . ? C33 C34 1.396(3) . ? C33 C37 1.525(3) . ? C34 C35 1.398(3) . ? C35 C36 1.427(3) . ? C35 C41 1.540(3) . ? C37 C40 1.524(3) . ? C37 C38 1.529(3) . ? C37 C39 1.534(3) . ? C41 C42 1.529(3) . ? C41 C43 1.532(3) . ? C41 C44 1.544(3) . ? O1C C4C 1.389(3) . ? O1C C1C 1.416(3) . ? C1C C2C 1.501(4) . ? C2C C3C 1.498(4) . ? C3C C4C 1.496(4) . ? O1D C4D 1.407(3) . ? O1D C1D 1.421(3) . ? C1D C2D 1.498(4) . ? C2D C3D 1.483(4) . ? C3D C4D 1.509(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Al1 O4 177.61(9) . . ? O3 Al1 O1 86.96(8) . . ? O4 Al1 O1 91.00(8) . . ? O3 Al1 O2 89.77(7) . 2_566 ? O4 Al1 O2 89.32(7) . 2_566 ? O1 Al1 O2 99.38(7) . 2_566 ? O3 Al1 N3 90.35(8) . . ? O4 Al1 N3 91.86(8) . . ? O1 Al1 N3 170.78(8) . . ? O2 Al1 N3 89.42(8) 2_566 . ? O3 Al1 N4 91.58(7) . . ? O4 Al1 N4 89.66(8) . . ? O1 Al1 N4 89.70(8) . . ? O2 Al1 N4 170.88(8) 2_566 . ? N3 Al1 N4 81.56(8) . . ? N1 O1 Al1 117.86(13) . . ? N2 O2 Al1 113.03(13) . 2_566 ? C21 O3 Al1 138.11(16) . . ? C36 O4 Al1 135.89(15) . . ? C1 N1 O1 114.44(18) . . ? C2 N2 O2 122.0(2) . . ? C15 N3 C13 108.82(18) . . ? C15 N3 C30 106.17(17) . . ? C13 N3 C30 110.74(18) . . ? C15 N3 Al1 110.50(14) . . ? C13 N3 Al1 110.62(14) . . ? C30 N3 Al1 109.90(14) . . ? C45 N4 C14 109.82(18) . . ? C45 N4 C46 106.22(18) . . ? C14 N4 C46 108.15(18) . . ? C45 N4 Al1 113.75(14) . . ? C14 N4 Al1 105.99(14) . . ? C46 N4 Al1 112.82(14) . . ? N1 C1 C2 120.8(2) . . ? N1 C1 C3 132.6(2) . . ? C2 C1 C3 106.5(2) . . ? N2 C2 C11 130.2(2) . . ? N2 C2 C1 121.1(2) . . ? C11 C2 C1 108.6(2) . . ? C4 C3 C12 118.7(2) . . ? C4 C3 C1 134.9(2) . . ? C12 C3 C1 106.34(19) . . ? C3 C4 C5 118.2(2) . . ? C6 C5 C4 122.9(2) . . ? C5 C6 C7 120.6(2) . . ? C12 C7 C8 116.0(2) . . ? C12 C7 C6 115.5(2) . . ? C8 C7 C6 128.4(2) . . ? C9 C8 C7 121.0(2) . . ? C8 C9 C10 121.8(2) . . ? C11 C10 C9 119.1(2) . . ? C10 C11 C12 118.8(2) . . ? C10 C11 C2 135.6(2) . . ? C12 C11 C2 105.6(2) . . ? C7 C12 C3 124.0(2) . . ? C7 C12 C11 123.2(2) . . ? C3 C12 C11 112.7(2) . . ? N3 C13 C14 110.59(19) . . ? N4 C14 C13 109.3(2) . . ? N3 C15 C16 117.1(2) . . ? C17 C16 C21 120.9(2) . . ? C17 C16 C15 118.7(2) . . ? C21 C16 C15 119.6(2) . . ? C18 C17 C16 121.6(2) . . ? C17 C18 C19 116.6(2) . . ? C17 C18 C22 123.1(2) . . ? C19 C18 C22 120.2(2) . . ? C20 C19 C18 124.9(2) . . ? C19 C20 C21 116.9(2) . . ? C19 C20 C26 122.0(2) . . ? C21 C20 C26 121.0(2) . . ? O3 C21 C16 120.6(2) . . ? O3 C21 C20 120.3(2) . . ? C16 C21 C20 119.0(2) . . ? C24 C22 C25 108.2(2) . . ? C24 C22 C23 108.6(2) . . ? C25 C22 C23 108.1(2) . . ? C24 C22 C18 112.2(2) . . ? C25 C22 C18 110.0(2) . . ? C23 C22 C18 109.7(2) . . ? C28 C26 C20 112.8(2) . . ? C28 C26 C27 106.9(2) . . ? C20 C26 C27 111.7(2) . . ? C28 C26 C29 108.3(2) . . ? C20 C26 C29 108.4(2) . . ? C27 C26 C29 108.6(2) . . ? C31 C30 N3 116.71(19) . . ? C32 C31 C36 120.6(2) . . ? C32 C31 C30 120.5(2) . . ? C36 C31 C30 118.7(2) . . ? C31 C32 C33 122.1(2) . . ? C34 C33 C32 116.5(2) . . ? C34 C33 C37 122.8(2) . . ? C32 C33 C37 120.7(2) . . ? C35 C34 C33 124.4(2) . . ? C34 C35 C36 117.4(2) . . ? C34 C35 C41 121.1(2) . . ? C36 C35 C41 121.3(2) . . ? O4 C36 C31 119.6(2) . . ? O4 C36 C35 122.1(2) . . ? C31 C36 C35 118.3(2) . . ? C40 C37 C38 107.6(2) . . ? C40 C37 C33 112.0(2) . . ? C38 C37 C33 109.96(19) . . ? C40 C37 C39 108.83(19) . . ? C38 C37 C39 108.8(2) . . ? C33 C37 C39 109.6(2) . . ? C42 C41 C43 109.0(2) . . ? C42 C41 C44 106.8(2) . . ? C43 C41 C44 107.89(18) . . ? C42 C41 C35 112.01(18) . . ? C43 C41 C35 109.3(2) . . ? C44 C41 C35 111.7(2) . . ? C4C O1C C1C 107.1(2) . . ? O1C C1C C2C 107.8(2) . . ? C1C C2C C3C 104.6(3) . . ? C2C C3C C4C 104.1(3) . . ? O1C C4C C3C 110.6(2) . . ? C4D O1D C1D 109.5(2) . . ? O1D C1D C2D 106.0(3) . . ? C3D C2D C1D 101.1(3) . . ? C2D C3D C4D 103.4(3) . . ? O1D C4D C3D 105.9(2) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.649 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.072 # Attachment '- p7k03.cif' data_p7k03 _database_code_depnum_ccdc_archive 'CCDC 861067' #TrackingRef '- p7k03.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H80 Al2 Fe N8 O8' _chemical_formula_sum 'C72 H80 Al2 Fe N8 O8' _chemical_formula_weight 1295.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.511(4) _cell_length_b 10.8586(19) _cell_length_c 28.663(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.657(2) _cell_angle_gamma 90.00 _cell_volume 6598(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2147 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 19.40 _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5816 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'TWINABS v2009/1, Bruker-AXS, Madison' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 7 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7969 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7969 _reflns_number_gt 5571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.68A' _computing_data_reduction 'Bruker SAINT-Plus v7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7969 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.423 _refine_ls_restrained_S_all 1.423 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 0.20740(4) 0.2500 0.01355(11) Uani 1 2 d S . . Al1 Al 0.11418(3) 0.21043(6) 0.36101(2) 0.01610(15) Uani 1 1 d . . . O1 O 0.04513(7) 0.12277(13) 0.36318(5) 0.0201(4) Uani 1 1 d . . . O2 O -0.13194(7) 0.12756(13) 0.18951(4) 0.0181(3) Uani 1 1 d . . . O3 O 0.16878(7) 0.10611(14) 0.40353(5) 0.0235(4) Uani 1 1 d . . . O4 O 0.05677(7) 0.31728(12) 0.31346(4) 0.0154(3) Uani 1 1 d . . . N1 N -0.00073(8) 0.10737(16) 0.31826(6) 0.0166(4) Uani 1 1 d . . . N2 N -0.09299(8) 0.13479(16) 0.23685(6) 0.0152(4) Uani 1 1 d . . . N3 N 0.19002(9) 0.33428(17) 0.36857(6) 0.0206(4) Uani 1 1 d . A . N4 N 0.11229(8) 0.30790(17) 0.42726(6) 0.0200(4) Uani 1 1 d . . . C1 C -0.05483(10) 0.07068(19) 0.31898(7) 0.0169(5) Uani 1 1 d . . . C2 C -0.10401(10) 0.06073(19) 0.26903(7) 0.0162(5) Uani 1 1 d . . . C3 C -0.07205(11) 0.0522(2) 0.36457(7) 0.0204(5) Uani 1 1 d . . . C4 C -0.03786(12) -0.0245(2) 0.40288(8) 0.0321(6) Uani 1 1 d . . . H4 H -0.0013 -0.0655 0.4012 0.038 Uiso 1 1 calc R . . C5 C -0.05707(13) -0.0413(3) 0.44344(8) 0.0402(7) Uani 1 1 d . . . H5 H -0.0344 -0.0963 0.4690 0.048 Uiso 1 1 calc R . . C6 C -0.10862(13) 0.0207(3) 0.44729(8) 0.0385(7) Uani 1 1 d . . . H6 H -0.1210 0.0099 0.4756 0.046 Uiso 1 1 calc R . . C7 C -0.14200(13) 0.0983(2) 0.40971(8) 0.0338(6) Uani 1 1 d . . . H7 H -0.1772 0.1426 0.4122 0.041 Uiso 1 1 calc R . . C8 C -0.12431(11) 0.1119(2) 0.36834(8) 0.0251(6) Uani 1 1 d . . . H8 H -0.1486 0.1633 0.3420 0.030 Uiso 1 1 calc R . . C9 C -0.15335(10) -0.0355(2) 0.25778(7) 0.0175(5) Uani 1 1 d . . . C10 C -0.13956(10) -0.1459(2) 0.28427(7) 0.0193(5) Uani 1 1 d . . . H10 H -0.1004 -0.1545 0.3104 0.023 Uiso 1 1 calc R . . C11 C -0.18170(11) -0.2428(2) 0.27331(8) 0.0230(5) Uani 1 1 d . . . H11 H -0.1709 -0.3177 0.2913 0.028 Uiso 1 1 calc R . . C12 C -0.23993(11) -0.2312(2) 0.23600(8) 0.0256(6) Uani 1 1 d . . . H12 H -0.2692 -0.2975 0.2285 0.031 Uiso 1 1 calc R . . C13 C -0.25465(11) -0.1216(2) 0.20986(7) 0.0256(6) Uani 1 1 d . . . H13 H -0.2944 -0.1128 0.1845 0.031 Uiso 1 1 calc R . . C14 C -0.21233(11) -0.0250(2) 0.22017(7) 0.0212(5) Uani 1 1 d . . . H14 H -0.2232 0.0492 0.2017 0.025 Uiso 1 1 calc R . . C15 C 0.24600(11) 0.2677(2) 0.36392(8) 0.0283(6) Uani 1 1 d . . . H15A H 0.2816 0.3266 0.3718 0.034 Uiso 1 1 calc R . . H15B H 0.2359 0.2434 0.3288 0.034 Uiso 1 1 calc R . . C16 C 0.26854(11) 0.1541(2) 0.39549(8) 0.0304(6) Uani 1 1 d . . . C17 C 0.33172(12) 0.1191(3) 0.40507(9) 0.0427(8) Uani 1 1 d . . . H17 H 0.3591 0.1720 0.3953 0.051 Uiso 1 1 calc R . . C18 C 0.35497(14) 0.0080(3) 0.42865(9) 0.0493(9) Uani 1 1 d . . . C19 C 0.31439(15) -0.0666(3) 0.44284(9) 0.0495(9) Uani 1 1 d . . . H19 H 0.3297 -0.1426 0.4588 0.059 Uiso 1 1 calc R . . C20 C 0.25211(13) -0.0345(2) 0.43469(8) 0.0366(7) Uani 1 1 d . . . C21 C 0.22832(12) 0.0777(2) 0.41025(7) 0.0273(6) Uani 1 1 d . . . C22 C 0.42288(14) -0.0292(3) 0.43744(10) 0.0725(12) Uani 1 1 d . . . H22A H 0.4427 -0.0549 0.4720 0.109 Uiso 1 1 calc R . . H22B H 0.4460 0.0410 0.4306 0.109 Uiso 1 1 calc R . . H22C H 0.4238 -0.0977 0.4154 0.109 Uiso 1 1 calc R . . C23 C 0.20869(15) -0.1165(3) 0.45056(9) 0.0498(8) Uani 1 1 d . . . H23A H 0.2284 -0.1974 0.4599 0.075 Uiso 1 1 calc R . . H23B H 0.1688 -0.1259 0.4231 0.075 Uiso 1 1 calc R . . H23C H 0.2006 -0.0796 0.4790 0.075 Uiso 1 1 calc R . . C24 C 0.17302(11) 0.4289(2) 0.32760(8) 0.0246(5) Uani 1 1 d . . . H24A H 0.2093 0.4853 0.3331 0.029 Uiso 1 1 calc R . . H24B H 0.1663 0.3860 0.2957 0.029 Uiso 1 1 calc R . . C25 C 0.11588(11) 0.5038(2) 0.32314(7) 0.0210(5) Uani 1 1 d . . . C26 C 0.11795(12) 0.6321(2) 0.32517(7) 0.0270(6) Uani 1 1 d . . . H26 H 0.1570 0.6730 0.3306 0.032 Uiso 1 1 calc R . . C27 C 0.06419(13) 0.7011(2) 0.31945(7) 0.0298(6) Uani 1 1 d . . . C28 C 0.00781(13) 0.6379(2) 0.31223(7) 0.0271(6) Uani 1 1 d . . . H28 H -0.0292 0.6844 0.3087 0.032 Uiso 1 1 calc R . . C29 C 0.00334(11) 0.5099(2) 0.31001(7) 0.0191(5) Uani 1 1 d . . . C30 C 0.05840(11) 0.44250(19) 0.31516(7) 0.0178(5) Uani 1 1 d . . . C31 C 0.06651(15) 0.8400(2) 0.32045(9) 0.0444(8) Uani 1 1 d . . . H31A H 0.1096 0.8675 0.3250 0.067 Uiso 1 1 calc R . . H31B H 0.0538 0.8704 0.3479 0.067 Uiso 1 1 calc R . . H31C H 0.0377 0.8724 0.2891 0.067 Uiso 1 1 calc R . . C32 C -0.05804(11) 0.4445(2) 0.30298(8) 0.0239(5) Uani 1 1 d . . . H32A H -0.0911 0.5053 0.3006 0.036 Uiso 1 1 calc R . . H32B H -0.0532 0.3900 0.3313 0.036 Uiso 1 1 calc R . . H32C H -0.0697 0.3956 0.2725 0.036 Uiso 1 1 calc R . . C33 C 0.20833(11) 0.3956(2) 0.41805(7) 0.0284(6) Uani 1 1 d . . . H33A H 0.2390 0.3429 0.4429 0.034 Uiso 0.619(5) 1 calc PR A 1 H33B H 0.2293 0.4749 0.4165 0.034 Uiso 0.619(5) 1 calc PR A 1 H33C H 0.2549 0.3953 0.4328 0.034 Uiso 0.381(5) 1 calc PR A 2 H33D H 0.1945 0.4826 0.4132 0.034 Uiso 0.381(5) 1 calc PR A 2 C34A C 0.15320(19) 0.4187(4) 0.43400(14) 0.0259(12) Uani 0.619(5) 1 d P A 1 H34A H 0.1681 0.4430 0.4693 0.031 Uiso 0.619(5) 1 calc PR A 1 H34B H 0.1282 0.4878 0.4145 0.031 Uiso 0.619(5) 1 calc PR A 1 C35A C 0.1329(3) 0.2271(5) 0.47068(15) 0.0301(13) Uani 0.619(5) 1 d P A 1 H35A H 0.1275 0.2695 0.4992 0.045 Uiso 0.619(5) 1 calc PR A 1 H35B H 0.1775 0.2062 0.4781 0.045 Uiso 0.619(5) 1 calc PR A 1 H35C H 0.1076 0.1516 0.4638 0.045 Uiso 0.619(5) 1 calc PR A 1 C36A C 0.0473(2) 0.3502(5) 0.42287(13) 0.0229(11) Uani 0.619(5) 1 d P A 1 H36A H 0.0317 0.4071 0.3949 0.034 Uiso 0.619(5) 1 calc PR A 1 H36B H 0.0486 0.3922 0.4534 0.034 Uiso 0.619(5) 1 calc PR A 1 H36C H 0.0191 0.2788 0.4174 0.034 Uiso 0.619(5) 1 calc PR A 1 C34B C 0.1820(3) 0.3386(7) 0.4536(2) 0.026(2) Uani 0.381(5) 1 d P A 2 H34C H 0.1862 0.3960 0.4814 0.031 Uiso 0.381(5) 1 calc PR A 2 H34D H 0.2056 0.2624 0.4673 0.031 Uiso 0.381(5) 1 calc PR A 2 C35B C 0.0965(4) 0.2172(9) 0.4620(3) 0.032(2) Uani 0.381(5) 1 d P A 2 H35D H 0.1074 0.2537 0.4951 0.047 Uiso 0.381(5) 1 calc PR A 2 H35E H 0.1207 0.1412 0.4639 0.047 Uiso 0.381(5) 1 calc PR A 2 H35F H 0.0513 0.1983 0.4493 0.047 Uiso 0.381(5) 1 calc PR A 2 C36B C 0.0744(4) 0.4162(8) 0.4255(2) 0.0276(19) Uani 0.381(5) 1 d P A 2 H36D H 0.0906 0.4847 0.4111 0.041 Uiso 0.381(5) 1 calc PR A 2 H36E H 0.0762 0.4380 0.4591 0.041 Uiso 0.381(5) 1 calc PR A 2 H36F H 0.0305 0.3993 0.4051 0.041 Uiso 0.381(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0099(2) 0.0145(3) 0.0148(2) 0.000 0.00236(16) 0.000 Al1 0.0119(3) 0.0187(4) 0.0155(3) -0.0024(3) 0.0016(2) 0.0020(3) O1 0.0163(8) 0.0240(9) 0.0147(7) 0.0022(6) -0.0017(6) -0.0043(7) O2 0.0141(8) 0.0219(9) 0.0138(7) 0.0037(6) -0.0011(6) -0.0021(7) O3 0.0172(9) 0.0276(10) 0.0207(8) -0.0009(6) -0.0001(6) 0.0080(7) O4 0.0137(8) 0.0129(8) 0.0189(8) -0.0022(6) 0.0047(6) -0.0005(7) N1 0.0123(10) 0.0175(10) 0.0158(9) -0.0009(7) -0.0007(7) -0.0013(8) N2 0.0134(10) 0.0154(10) 0.0144(9) 0.0030(7) 0.0013(7) -0.0002(8) N3 0.0172(10) 0.0271(12) 0.0181(9) -0.0084(7) 0.0066(8) -0.0013(9) N4 0.0153(10) 0.0255(12) 0.0179(9) -0.0017(8) 0.0041(7) 0.0013(9) C1 0.0173(12) 0.0166(12) 0.0155(10) 0.0046(8) 0.0036(9) -0.0019(10) C2 0.0129(12) 0.0175(12) 0.0172(10) 0.0021(9) 0.0036(8) -0.0013(10) C3 0.0182(13) 0.0232(14) 0.0185(11) 0.0016(9) 0.0043(9) -0.0071(11) C4 0.0265(15) 0.0432(17) 0.0248(13) 0.0110(11) 0.0063(11) 0.0046(13) C5 0.0410(18) 0.055(2) 0.0248(13) 0.0176(12) 0.0117(12) 0.0018(16) C6 0.0428(18) 0.053(2) 0.0246(14) 0.0036(12) 0.0180(12) -0.0077(15) C7 0.0339(16) 0.0380(17) 0.0352(14) -0.0034(12) 0.0189(12) -0.0033(13) C8 0.0248(14) 0.0261(15) 0.0242(12) 0.0031(10) 0.0080(10) 0.0000(12) C9 0.0152(12) 0.0214(13) 0.0167(10) 0.0018(9) 0.0065(9) -0.0015(10) C10 0.0156(12) 0.0214(13) 0.0205(11) 0.0031(9) 0.0056(9) -0.0015(10) C11 0.0240(13) 0.0204(13) 0.0272(12) 0.0053(9) 0.0118(10) -0.0020(11) C12 0.0229(13) 0.0225(14) 0.0304(13) 0.0015(10) 0.0077(10) -0.0105(11) C13 0.0157(12) 0.0323(15) 0.0241(12) 0.0040(10) 0.0006(9) -0.0105(11) C14 0.0199(13) 0.0219(13) 0.0212(11) 0.0041(9) 0.0063(9) -0.0017(11) C15 0.0116(12) 0.0444(17) 0.0296(13) -0.0170(11) 0.0080(10) -0.0056(11) C16 0.0164(13) 0.0475(18) 0.0207(12) -0.0145(11) -0.0023(10) 0.0098(12) C17 0.0192(14) 0.073(2) 0.0308(14) -0.0256(14) 0.0016(11) 0.0084(15) C18 0.0263(16) 0.079(3) 0.0288(15) -0.0252(14) -0.0087(12) 0.0313(17) C19 0.047(2) 0.062(2) 0.0265(14) -0.0134(13) -0.0048(13) 0.0363(18) C20 0.0386(17) 0.0431(18) 0.0177(12) -0.0096(11) -0.0044(11) 0.0222(14) C21 0.0218(14) 0.0370(16) 0.0162(11) -0.0111(10) -0.0028(9) 0.0120(12) C22 0.0323(19) 0.124(3) 0.0469(18) -0.0320(18) -0.0053(14) 0.042(2) C23 0.067(2) 0.0383(19) 0.0355(15) 0.0118(12) 0.0055(14) 0.0237(17) C24 0.0213(13) 0.0285(15) 0.0256(12) -0.0050(10) 0.0102(10) -0.0100(11) C25 0.0257(14) 0.0192(13) 0.0202(11) -0.0049(9) 0.0104(10) -0.0036(11) C26 0.0380(16) 0.0207(14) 0.0241(12) -0.0061(10) 0.0127(11) -0.0102(12) C27 0.0499(17) 0.0173(13) 0.0235(12) -0.0038(10) 0.0144(11) -0.0001(14) C28 0.0395(16) 0.0214(14) 0.0228(12) 0.0011(10) 0.0137(11) 0.0097(13) C29 0.0231(13) 0.0198(13) 0.0159(11) 0.0002(9) 0.0085(9) 0.0047(11) C30 0.0228(13) 0.0150(12) 0.0165(11) -0.0009(8) 0.0079(9) -0.0007(11) C31 0.079(2) 0.0167(14) 0.0405(15) -0.0027(11) 0.0247(15) -0.0045(15) C32 0.0217(13) 0.0261(14) 0.0247(12) 0.0025(10) 0.0090(10) 0.0093(11) C33 0.0222(14) 0.0385(17) 0.0220(12) -0.0144(10) 0.0043(10) -0.0083(12) C34A 0.020(2) 0.033(3) 0.022(2) -0.0123(18) 0.0028(16) -0.001(2) C35A 0.034(3) 0.041(3) 0.014(2) -0.0010(18) 0.006(2) 0.011(3) C36A 0.019(2) 0.037(3) 0.0159(19) -0.0031(18) 0.0091(16) 0.006(2) C34B 0.023(4) 0.037(5) 0.013(3) -0.012(3) -0.001(3) -0.005(3) C35B 0.034(5) 0.047(5) 0.017(4) 0.006(3) 0.012(4) 0.000(5) C36B 0.020(4) 0.039(5) 0.023(3) -0.006(3) 0.007(3) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.1481(18) . yes Fe1 N2 2.1481(18) 2 yes Fe1 O4 2.1913(13) . yes Fe1 O4 2.1914(13) 2 yes Fe1 N1 2.2427(16) 2 yes Fe1 N1 2.2427(16) . yes Al1 O3 1.8086(16) . yes Al1 O1 1.8415(16) . yes Al1 O2 1.8590(15) 2 yes Al1 O4 1.9206(15) . yes Al1 N3 2.1263(19) . yes Al1 N4 2.1868(18) . yes O1 N1 1.363(2) . ? O2 N2 1.3476(19) . ? O2 Al1 1.8589(15) 2 ? O3 C21 1.325(3) . ? O4 C30 1.361(2) . ? N1 C1 1.288(3) . ? N2 C2 1.309(2) . ? N3 C15 1.497(3) . ? N3 C24 1.509(3) . ? N3 C33 1.494(2) . ? N4 C36B 1.444(7) . ? N4 C35A 1.465(5) . ? N4 C34A 1.487(4) . ? N4 C36A 1.497(4) . ? N4 C34B 1.532(6) . ? N4 C35B 1.525(8) . ? C1 C2 1.490(3) . ? C1 C3 1.496(3) . ? C2 C9 1.480(3) . ? C3 C8 1.379(3) . ? C3 C4 1.387(3) . ? C4 C5 1.382(3) . ? C5 C6 1.378(4) . ? C6 C7 1.376(3) . ? C7 C8 1.380(3) . ? C9 C10 1.397(3) . ? C9 C14 1.406(3) . ? C10 C11 1.380(3) . ? C11 C12 1.391(3) . ? C12 C13 1.386(3) . ? C13 C14 1.381(3) . ? C15 C16 1.512(3) . ? C16 C21 1.395(3) . ? C16 C17 1.407(3) . ? C17 C18 1.396(4) . ? C18 C19 1.380(4) . ? C18 C22 1.518(4) . ? C19 C20 1.386(4) . ? C20 C21 1.418(3) . ? C20 C23 1.501(4) . ? C24 C25 1.490(3) . ? C25 C26 1.395(3) . ? C25 C30 1.404(3) . ? C26 C27 1.385(3) . ? C27 C28 1.395(3) . ? C27 C31 1.510(3) . ? C28 C29 1.394(3) . ? C29 C30 1.404(3) . ? C29 C32 1.506(3) . ? C33 C34B 1.476(6) . ? C33 C34A 1.481(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 136.93(9) . 2 yes N2 Fe1 O4 127.39(5) . . yes N2 Fe1 O4 78.02(6) 2 . yes N2 Fe1 O4 78.03(6) . 2 yes N2 Fe1 O4 127.39(5) 2 2 yes O4 Fe1 O4 114.02(7) . 2 yes N2 Fe1 N1 87.81(6) . 2 yes N2 Fe1 N1 71.50(6) 2 2 yes O4 Fe1 N1 144.55(6) . 2 yes O4 Fe1 N1 73.31(6) 2 2 yes N2 Fe1 N1 71.50(6) . . yes N2 Fe1 N1 87.81(6) 2 . yes O4 Fe1 N1 73.31(6) . . yes O4 Fe1 N1 144.55(6) 2 . yes N1 Fe1 N1 122.06(9) 2 . yes O3 Al1 O1 92.49(7) . . yes O3 Al1 O2 86.92(7) . 2 yes O1 Al1 O2 100.44(7) . 2 yes O3 Al1 O4 177.45(7) . . yes O1 Al1 O4 87.83(7) . . yes O2 Al1 O4 90.53(6) 2 . yes O3 Al1 N3 89.27(7) . . yes O1 Al1 N3 168.93(7) . . yes O2 Al1 N3 90.56(7) 2 . yes O4 Al1 N3 90.90(7) . . yes O3 Al1 N4 85.72(7) . . yes O1 Al1 N4 87.57(7) . . yes O2 Al1 N4 169.35(7) 2 . yes O4 Al1 N4 96.82(7) . . yes N3 Al1 N4 81.66(7) . . yes N1 O1 Al1 114.28(11) . . ? N2 O2 Al1 121.25(12) . 2 ? C21 O3 Al1 131.97(15) . . ? C30 O4 Al1 125.08(12) . . ? C30 O4 Fe1 125.09(11) . . ? Al1 O4 Fe1 108.99(6) . . ? C1 N1 O1 116.26(16) . . ? C1 N1 Fe1 116.63(13) . . ? O1 N1 Fe1 122.64(12) . . ? C2 N2 O2 117.42(17) . . ? C2 N2 Fe1 120.43(13) . . ? O2 N2 Fe1 117.61(11) . . ? C15 N3 C24 105.09(16) . . ? C15 N3 C33 109.15(17) . . ? C24 N3 C33 110.60(18) . . ? C15 N3 Al1 110.87(14) . . ? C24 N3 Al1 111.50(13) . . ? C33 N3 Al1 109.53(13) . . ? C36B N4 C35A 122.2(3) . . ? C36B N4 C34A 71.3(4) . . ? C35A N4 C34A 111.6(3) . . ? C36B N4 C36A 36.7(3) . . ? C35A N4 C36A 106.1(3) . . ? C34A N4 C36A 107.9(3) . . ? C36B N4 C34B 109.6(4) . . ? C35A N4 C34B 74.4(3) . . ? C34A N4 C34B 43.4(3) . . ? C36A N4 C34B 141.7(3) . . ? C36B N4 C35B 106.5(4) . . ? C35A N4 C35B 30.2(3) . . ? C34A N4 C35B 135.0(4) . . ? C36A N4 C35B 79.5(4) . . ? C34B N4 C35B 104.1(4) . . ? C36B N4 Al1 123.2(3) . . ? C35A N4 Al1 110.8(2) . . ? C34A N4 Al1 108.18(16) . . ? C36A N4 Al1 112.28(17) . . ? C34B N4 Al1 102.5(2) . . ? C35B N4 Al1 109.3(3) . . ? N1 C1 C2 114.06(17) . . ? N1 C1 C3 125.43(18) . . ? C2 C1 C3 120.16(19) . . ? N2 C2 C9 125.95(18) . . ? N2 C2 C1 112.14(19) . . ? C9 C2 C1 121.40(17) . . ? C8 C3 C4 118.8(2) . . ? C8 C3 C1 118.94(19) . . ? C4 C3 C1 122.3(2) . . ? C5 C4 C3 119.8(2) . . ? C6 C5 C4 120.9(2) . . ? C5 C6 C7 119.3(2) . . ? C8 C7 C6 119.9(3) . . ? C3 C8 C7 121.2(2) . . ? C10 C9 C14 117.8(2) . . ? C10 C9 C2 118.33(19) . . ? C14 C9 C2 123.76(19) . . ? C11 C10 C9 121.4(2) . . ? C10 C11 C12 120.3(2) . . ? C13 C12 C11 119.0(2) . . ? C12 C13 C14 121.0(2) . . ? C13 C14 C9 120.5(2) . . ? N3 C15 C16 117.62(19) . . ? C21 C16 C17 119.7(3) . . ? C21 C16 C15 123.0(2) . . ? C17 C16 C15 116.8(2) . . ? C18 C17 C16 121.2(3) . . ? C19 C18 C17 118.2(3) . . ? C19 C18 C22 121.6(3) . . ? C17 C18 C22 120.2(3) . . ? C18 C19 C20 122.4(3) . . ? C19 C20 C21 119.4(3) . . ? C19 C20 C23 121.7(3) . . ? C21 C20 C23 118.9(2) . . ? O3 C21 C16 123.1(2) . . ? O3 C21 C20 117.9(2) . . ? C16 C21 C20 119.0(2) . . ? C25 C24 N3 115.07(17) . . ? C26 C25 C30 119.8(2) . . ? C26 C25 C24 121.7(2) . . ? C30 C25 C24 118.5(2) . . ? C27 C26 C25 121.3(2) . . ? C26 C27 C28 117.8(2) . . ? C26 C27 C31 121.0(3) . . ? C28 C27 C31 121.2(2) . . ? C29 C28 C27 123.0(2) . . ? C28 C29 C30 117.9(2) . . ? C28 C29 C32 121.7(2) . . ? C30 C29 C32 120.4(2) . . ? O4 C30 C29 120.3(2) . . ? O4 C30 C25 119.5(2) . . ? C29 C30 C25 120.2(2) . . ? C34B C33 C34A 44.4(3) . . ? C34B C33 N3 114.9(3) . . ? C34A C33 N3 112.1(2) . . ? N4 C34A C33 111.7(3) . . ? C33 C34B N4 109.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.634 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.074 # Attachment '- p7k10.cif' data_p7k10 _database_code_depnum_ccdc_archive 'CCDC 861069' #TrackingRef '- p7k10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H90 Al2 Fe N14 O16, C4 H10 O, 3.5(C4 H8 O)' _chemical_formula_sum 'C104 H128 Al2 Fe N14 O20.50' _chemical_formula_weight 2012.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 23.9420(6) _cell_length_b 27.0271(6) _cell_length_c 15.5154(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10039.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9934 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 20.39 _exptl_crystal_description Block _exptl_crystal_colour Purple/red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4264 _exptl_absorpt_coefficient_mu 0.246 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9367 _exptl_absorpt_correction_T_max 0.9782 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 7 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 110120 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 23.28 _reflns_number_total 14452 _reflns_number_gt 10567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.68A' _computing_data_reduction 'Bruker SAINT-Plus v7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ad _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(15) _refine_ls_number_reflns 14452 _refine_ls_number_parameters 1258 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.681 _refine_ls_restrained_S_all 1.686 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.31570(3) 0.14877(3) 0.82269(4) 0.02455(18) Uani 1 1 d . . . Al1 Al 0.20202(6) 0.11491(6) 0.97203(10) 0.0271(4) Uani 1 1 d . . . Al2 Al 0.42645(6) 0.20388(5) 0.69122(10) 0.0264(4) Uani 1 1 d . . . O1 O 0.27816(13) 0.11819(11) 0.99499(19) 0.0290(9) Uani 1 1 d . . . O2 O 0.43354(12) 0.15416(11) 0.77139(18) 0.0248(8) Uani 1 1 d . . . O3 O 0.20143(12) 0.11522(10) 0.85366(18) 0.0262(9) Uani 1 1 d . . . O4 O 0.35014(12) 0.20211(11) 0.6673(2) 0.0295(9) Uani 1 1 d . . . O5 O 0.18920(13) 0.18205(11) 0.97308(19) 0.0293(9) Uani 1 1 d . . . O6 O 0.20920(12) 0.04646(11) 0.9731(2) 0.0259(9) Uani 1 1 d . . . O7 O 0.19125(16) 0.32573(12) 1.2862(2) 0.0461(11) Uani 1 1 d . . . O8 O 0.18220(16) 0.37675(12) 1.1806(2) 0.0539(11) Uani 1 1 d . . . O9 O 0.11209(16) -0.15604(13) 0.8561(3) 0.0654(13) Uani 1 1 d . . . O10 O 0.04098(15) -0.10959(13) 0.8292(3) 0.0619(12) Uani 1 1 d . . . O11 O 0.43580(13) 0.15899(12) 0.60255(18) 0.0300(9) Uani 1 1 d . . . O12 O 0.42193(13) 0.24951(12) 0.77888(19) 0.0271(9) Uani 1 1 d . . . O13 O 0.65335(19) 0.05230(17) 0.4878(3) 0.0822(16) Uani 1 1 d . . . O14 O 0.59497(18) 0.02250(15) 0.3970(3) 0.0738(14) Uani 1 1 d . . . O15 O 0.37427(16) 0.46643(13) 0.8849(3) 0.0580(13) Uani 1 1 d . . . O16 O 0.35785(18) 0.47175(14) 0.7485(3) 0.0654(13) Uani 1 1 d . . . N1 N 0.32002(16) 0.12202(13) 0.9371(2) 0.0196(10) Uani 1 1 d . . . N2 N 0.39601(15) 0.14425(13) 0.8344(2) 0.0232(10) Uani 1 1 d . . . N3 N 0.23669(15) 0.14184(13) 0.8029(3) 0.0268(11) Uani 1 1 d . . . N4 N 0.31050(17) 0.17656(13) 0.7089(2) 0.0268(11) Uani 1 1 d . . . N5 N 0.19078(16) 0.11509(13) 1.1065(2) 0.0247(10) Uani 1 1 d . . . N6 N 0.11415(15) 0.10242(14) 0.9686(3) 0.0272(11) Uani 1 1 d . . . N7 N 0.18613(19) 0.33410(15) 1.2097(3) 0.0389(13) Uani 1 1 d . . . N8 N 0.0897(2) -0.1150(2) 0.8569(3) 0.0520(15) Uani 1 1 d . . . N9 N 0.51545(14) 0.21271(13) 0.6912(2) 0.0221(10) Uani 1 1 d . . . N10 N 0.43016(17) 0.26396(14) 0.6025(2) 0.0258(11) Uani 1 1 d . . . N11 N 0.6054(2) 0.0495(2) 0.4588(3) 0.0600(17) Uani 1 1 d . . . N12 N 0.37072(19) 0.44718(18) 0.8129(4) 0.0509(14) Uani 1 1 d . . . N13 N 0.32289(16) 0.08109(14) 0.7706(2) 0.0270(11) Uani 1 1 d . . . N14 N 0.30718(17) 0.21728(14) 0.8727(3) 0.0292(11) Uani 1 1 d . . . C1 C 0.36959(19) 0.10898(17) 0.9634(3) 0.0186(12) Uani 1 1 d . . . C2 C 0.41298(19) 0.11960(16) 0.9024(3) 0.0205(13) Uani 1 1 d . . . C3 C 0.38195(19) 0.08521(19) 1.0484(3) 0.0262(13) Uani 1 1 d . . . C4 C 0.4075(2) 0.03929(18) 1.0512(3) 0.0335(14) Uani 1 1 d . . . H4 H 0.4156 0.0228 0.9986 0.040 Uiso 1 1 calc R . . C5 C 0.4217(2) 0.0166(2) 1.1274(4) 0.0514(18) Uani 1 1 d . . . H5 H 0.4383 -0.0153 1.1279 0.062 Uiso 1 1 calc R . . C6 C 0.4109(2) 0.0421(2) 1.2048(4) 0.063(2) Uani 1 1 d . . . H6 H 0.4207 0.0273 1.2583 0.075 Uiso 1 1 calc R . . C7 C 0.3863(2) 0.0880(2) 1.2040(3) 0.0490(17) Uani 1 1 d . . . H7 H 0.3795 0.1049 1.2566 0.059 Uiso 1 1 calc R . . C8 C 0.37134(19) 0.1100(2) 1.1255(3) 0.0358(15) Uani 1 1 d . . . H8 H 0.3541 0.1416 1.1248 0.043 Uiso 1 1 calc R . . C9 C 0.4733(2) 0.10580(19) 0.9146(3) 0.0298(14) Uani 1 1 d . . . C10 C 0.5022(2) 0.1222(2) 0.9872(3) 0.0488(18) Uani 1 1 d . . . H10 H 0.4843 0.1430 1.0281 0.059 Uiso 1 1 calc R . . C11 C 0.5566(2) 0.1081(2) 0.9991(5) 0.065(2) Uani 1 1 d . . . H11 H 0.5767 0.1202 1.0476 0.078 Uiso 1 1 calc R . . C12 C 0.5822(3) 0.0773(3) 0.9431(5) 0.083(3) Uani 1 1 d . . . H12 H 0.6192 0.0663 0.9542 0.100 Uiso 1 1 calc R . . C13 C 0.5546(2) 0.0616(2) 0.8690(4) 0.052(2) Uani 1 1 d . . . H13 H 0.5734 0.0416 0.8278 0.062 Uiso 1 1 calc R . . C14 C 0.4987(2) 0.07566(19) 0.8560(3) 0.0420(16) Uani 1 1 d . . . H14 H 0.4788 0.0643 0.8068 0.050 Uiso 1 1 calc R . . C15 C 0.12857(19) 0.11599(19) 1.1252(3) 0.0304(14) Uani 1 1 d . . . H15 H 0.1158 0.1507 1.1152 0.036 Uiso 1 1 calc R . . C16 C 0.1122(2) 0.10287(18) 1.2163(3) 0.0384(15) Uani 1 1 d . . . H16A H 0.1288 0.0705 1.2315 0.046 Uiso 1 1 calc R . . H16B H 0.1276 0.1280 1.2561 0.046 Uiso 1 1 calc R . . C17 C 0.0498(2) 0.10015(18) 1.2283(3) 0.0383(16) Uani 1 1 d . . . H17A H 0.0411 0.0901 1.2882 0.046 Uiso 1 1 calc R . . H17B H 0.0331 0.1332 1.2182 0.046 Uiso 1 1 calc R . . C18 C 0.0254(2) 0.06355(16) 1.1666(3) 0.0408(15) Uani 1 1 d . . . H18A H -0.0154 0.0607 1.1764 0.049 Uiso 1 1 calc R . . H18B H 0.0424 0.0306 1.1762 0.049 Uiso 1 1 calc R . . C19 C 0.03639(19) 0.08037(19) 1.0744(3) 0.0400(16) Uani 1 1 d . . . H19A H 0.0191 0.1132 1.0650 0.048 Uiso 1 1 calc R . . H19B H 0.0191 0.0567 1.0337 0.048 Uiso 1 1 calc R . . C20 C 0.09905(19) 0.08358(18) 1.0567(3) 0.0293(14) Uani 1 1 d . . . H20 H 0.1146 0.0494 1.0619 0.035 Uiso 1 1 calc R . . C21 C 0.21943(18) 0.15813(16) 1.1467(3) 0.0268(13) Uani 1 1 d . . . H21A H 0.2598 0.1557 1.1336 0.032 Uiso 1 1 calc R . . H21B H 0.2152 0.1555 1.2100 0.032 Uiso 1 1 calc R . . C22 C 0.19940(19) 0.20823(18) 1.1192(3) 0.0241(13) Uani 1 1 d . . . C23 C 0.19883(18) 0.24659(18) 1.1772(3) 0.0290(13) Uani 1 1 d . . . H23 H 0.2082 0.2409 1.2359 0.035 Uiso 1 1 calc R . . C24 C 0.1844(2) 0.29382(18) 1.1494(3) 0.0255(13) Uani 1 1 d . . . C25 C 0.16659(19) 0.30223(19) 1.0648(3) 0.0379(15) Uani 1 1 d . . . H25 H 0.1556 0.3345 1.0474 0.045 Uiso 1 1 calc R . . C26 C 0.16495(19) 0.26378(19) 1.0065(3) 0.0290(14) Uani 1 1 d . . . C27 C 0.1858(2) 0.21648(17) 1.0318(3) 0.0251(12) Uani 1 1 d . . . C28 C 0.1429(2) 0.27168(17) 0.9164(3) 0.0434(16) Uani 1 1 d . . . H28A H 0.1033 0.2624 0.9142 0.065 Uiso 1 1 calc R . . H28B H 0.1641 0.2511 0.8758 0.065 Uiso 1 1 calc R . . H28C H 0.1470 0.3066 0.9005 0.065 Uiso 1 1 calc R . . C29 C 0.21775(18) 0.07046(15) 1.1458(3) 0.0310(14) Uani 1 1 d . . . H29A H 0.2558 0.0669 1.1232 0.047 Uiso 1 1 calc R . . H29B H 0.1959 0.0409 1.1314 0.047 Uiso 1 1 calc R . . H29C H 0.2192 0.0743 1.2086 0.047 Uiso 1 1 calc R . . C30 C 0.10081(19) 0.06542(17) 0.9001(3) 0.0340(15) Uani 1 1 d . . . H30A H 0.0597 0.0621 0.8968 0.041 Uiso 1 1 calc R . . H30B H 0.1137 0.0789 0.8442 0.041 Uiso 1 1 calc R . . C31 C 0.12448(19) 0.01612(19) 0.9102(3) 0.0293(14) Uani 1 1 d . . . C32 C 0.0954(2) -0.0253(2) 0.8823(3) 0.0374(15) Uani 1 1 d . . . H32 H 0.0585 -0.0218 0.8608 0.045 Uiso 1 1 calc R . . C33 C 0.1198(2) -0.0718(2) 0.8854(3) 0.0369(15) Uani 1 1 d . . . C34 C 0.1738(2) -0.07898(19) 0.9165(3) 0.0336(14) Uani 1 1 d . . . H34 H 0.1902 -0.1110 0.9162 0.040 Uiso 1 1 calc R . . C35 C 0.2030(2) -0.0391(2) 0.9477(3) 0.0298(14) Uani 1 1 d . . . C36 C 0.1800(2) 0.00934(19) 0.9440(3) 0.0283(13) Uani 1 1 d . . . C37 C 0.26025(18) -0.04493(17) 0.9881(3) 0.0399(15) Uani 1 1 d . . . H37A H 0.2573 -0.0411 1.0507 0.060 Uiso 1 1 calc R . . H37B H 0.2855 -0.0197 0.9650 0.060 Uiso 1 1 calc R . . H37C H 0.2750 -0.0779 0.9747 0.060 Uiso 1 1 calc R . . C38 C 0.08278(19) 0.14766(17) 0.9442(3) 0.0355(14) Uani 1 1 d . . . H38A H 0.0983 0.1613 0.8908 0.053 Uiso 1 1 calc R . . H38B H 0.0860 0.1723 0.9904 0.053 Uiso 1 1 calc R . . H38C H 0.0434 0.1393 0.9355 0.053 Uiso 1 1 calc R . . C39 C 0.21880(19) 0.15304(18) 0.7259(3) 0.0252(13) Uani 1 1 d . . . C40 C 0.2611(2) 0.17566(18) 0.6739(3) 0.0339(14) Uani 1 1 d . . . C41 C 0.1622(2) 0.13812(19) 0.6981(3) 0.0355(15) Uani 1 1 d D . . C42 C 0.1163(2) 0.16848(19) 0.7083(3) 0.0414(16) Uani 1 1 d D . . H42 H 0.1215 0.2019 0.7255 0.050 Uiso 1 1 calc R . . C43 C 0.0623(2) 0.1507(2) 0.6936(4) 0.0547(18) Uani 1 1 d D . . H43 H 0.0311 0.1718 0.7017 0.066 Uiso 1 1 calc R . . C44 C 0.0543(2) 0.1028(2) 0.6675(4) 0.065(2) Uani 1 1 d D . . H44 H 0.0175 0.0909 0.6582 0.077 Uiso 1 1 calc R . . C45 C 0.0994(2) 0.0718(2) 0.6547(3) 0.0566(19) Uani 1 1 d D . . H45 H 0.0938 0.0389 0.6352 0.068 Uiso 1 1 calc R . . C46 C 0.1536(2) 0.08943(19) 0.6706(3) 0.0431(15) Uani 1 1 d D . . H46 H 0.1846 0.0681 0.6627 0.052 Uiso 1 1 calc R . . C47 C 0.2497(2) 0.2024(2) 0.5920(4) 0.0433(16) Uani 1 1 d D . . C48 C 0.2715(2) 0.1864(2) 0.5152(4) 0.070(2) Uani 1 1 d D . . H48 H 0.2915 0.1560 0.5133 0.084 Uiso 1 1 calc R . . C49 C 0.2649(3) 0.2139(3) 0.4394(4) 0.111(4) Uani 1 1 d D . . H49 H 0.2795 0.2022 0.3863 0.133 Uiso 1 1 calc R . . C50 C 0.2367(3) 0.2581(3) 0.4436(5) 0.108(4) Uani 1 1 d D . . H50 H 0.2329 0.2774 0.3927 0.129 Uiso 1 1 calc R . . C51 C 0.2135(3) 0.2757(2) 0.5200(5) 0.097(3) Uani 1 1 d D . . H51 H 0.1936 0.3061 0.5220 0.117 Uiso 1 1 calc R . . C52 C 0.2207(2) 0.2467(2) 0.5937(4) 0.063(2) Uani 1 1 d D . . H52 H 0.2052 0.2577 0.6467 0.075 Uiso 1 1 calc R . . C53 C 0.5308(2) 0.24521(18) 0.6178(3) 0.0303(14) Uani 1 1 d . . . H53 H 0.5290 0.2245 0.5645 0.036 Uiso 1 1 calc R . . C54 C 0.58994(19) 0.26594(17) 0.6233(3) 0.0349(15) Uani 1 1 d . . . H54A H 0.6171 0.2383 0.6243 0.042 Uiso 1 1 calc R . . H54B H 0.5942 0.2848 0.6776 0.042 Uiso 1 1 calc R . . C55 C 0.6029(2) 0.30028(18) 0.5456(3) 0.0427(16) Uani 1 1 d . . . H55A H 0.6408 0.3145 0.5516 0.051 Uiso 1 1 calc R . . H55B H 0.6015 0.2811 0.4912 0.051 Uiso 1 1 calc R . . C56 C 0.5607(2) 0.34045(18) 0.5435(3) 0.0401(15) Uani 1 1 d . . . H56A H 0.5690 0.3630 0.4949 0.048 Uiso 1 1 calc R . . H56B H 0.5630 0.3598 0.5975 0.048 Uiso 1 1 calc R . . C57 C 0.5020(2) 0.31999(17) 0.5332(3) 0.0351(14) Uani 1 1 d . . . H57A H 0.4750 0.3477 0.5309 0.042 Uiso 1 1 calc R . . H57B H 0.4993 0.3014 0.4785 0.042 Uiso 1 1 calc R . . C58 C 0.4875(2) 0.28617(17) 0.6079(3) 0.0271(14) Uani 1 1 d . . . H58 H 0.4888 0.3066 0.6615 0.033 Uiso 1 1 calc R . . C59 C 0.54354(18) 0.16299(16) 0.6849(3) 0.0339(14) Uani 1 1 d . . . H59A H 0.5844 0.1680 0.6892 0.041 Uiso 1 1 calc R . . H59B H 0.5319 0.1428 0.7350 0.041 Uiso 1 1 calc R . . C60 C 0.5317(2) 0.13427(17) 0.6048(3) 0.0276(14) Uani 1 1 d . . . C61 C 0.5738(2) 0.10827(18) 0.5657(3) 0.0360(15) Uani 1 1 d . . . H61 H 0.6111 0.1109 0.5859 0.043 Uiso 1 1 calc R . . C62 C 0.5611(3) 0.0782(2) 0.4963(4) 0.0494(18) Uani 1 1 d . . . C63 C 0.5090(3) 0.07490(19) 0.4611(3) 0.0444(16) Uani 1 1 d . . . H63 H 0.5019 0.0536 0.4136 0.053 Uiso 1 1 calc R . . C64 C 0.4668(2) 0.1036(2) 0.4967(3) 0.0387(16) Uani 1 1 d . . . C65 C 0.4767(2) 0.13355(17) 0.5702(3) 0.0282(14) Uani 1 1 d . . . C66 C 0.4068(2) 0.10283(18) 0.4604(3) 0.0562(19) Uani 1 1 d . . . H66A H 0.4049 0.0798 0.4117 0.084 Uiso 1 1 calc R . . H66B H 0.3965 0.1361 0.4408 0.084 Uiso 1 1 calc R . . H66C H 0.3808 0.0921 0.5055 0.084 Uiso 1 1 calc R . . C67 C 0.53519(19) 0.23260(17) 0.7763(3) 0.0330(14) Uani 1 1 d . . . H67A H 0.5170 0.2144 0.8232 0.049 Uiso 1 1 calc R . . H67B H 0.5257 0.2678 0.7805 0.049 Uiso 1 1 calc R . . H67C H 0.5758 0.2286 0.7807 0.049 Uiso 1 1 calc R . . C68 C 0.3873(2) 0.30147(17) 0.6256(3) 0.0353(15) Uani 1 1 d . . . H68A H 0.3502 0.2853 0.6230 0.042 Uiso 1 1 calc R . . H68B H 0.3878 0.3276 0.5808 0.042 Uiso 1 1 calc R . . C69 C 0.3927(2) 0.3260(2) 0.7117(3) 0.0307(14) Uani 1 1 d . . . C70 C 0.3806(2) 0.37478(19) 0.7232(4) 0.0344(15) Uani 1 1 d . . . H70 H 0.3690 0.3942 0.6754 0.041 Uiso 1 1 calc R . . C71 C 0.3849(2) 0.39590(18) 0.8027(4) 0.0334(14) Uani 1 1 d . . . C72 C 0.40481(19) 0.3708(2) 0.8735(3) 0.0336(15) Uani 1 1 d . . . H72 H 0.4085 0.3874 0.9273 0.040 Uiso 1 1 calc R . . C73 C 0.4196(2) 0.3213(2) 0.8661(3) 0.0305(14) Uani 1 1 d . . . C74 C 0.4119(2) 0.2967(2) 0.7849(3) 0.0338(15) Uani 1 1 d . . . C75 C 0.44589(19) 0.29278(17) 0.9379(3) 0.0413(16) Uani 1 1 d . . . H75A H 0.4866 0.2949 0.9332 0.062 Uiso 1 1 calc R . . H75B H 0.4344 0.2580 0.9344 0.062 Uiso 1 1 calc R . . H75C H 0.4339 0.3067 0.9933 0.062 Uiso 1 1 calc R . . C76 C 0.41619(19) 0.24788(17) 0.5136(3) 0.0350(15) Uani 1 1 d . . . H76A H 0.3809 0.2295 0.5142 0.052 Uiso 1 1 calc R . . H76B H 0.4460 0.2265 0.4915 0.052 Uiso 1 1 calc R . . H76C H 0.4125 0.2770 0.4764 0.052 Uiso 1 1 calc R . . C77 C 0.29623(18) 0.04184(19) 0.8048(3) 0.0309(14) Uani 1 1 d . . . H77 H 0.2739 0.0466 0.8547 0.037 Uiso 1 1 calc R . . C78 C 0.3003(2) -0.00648(18) 0.7689(3) 0.0299(14) Uani 1 1 d . . . H78 H 0.2806 -0.0333 0.7945 0.036 Uiso 1 1 calc R . . C79 C 0.3325(2) -0.01412(19) 0.6979(3) 0.0368(15) Uani 1 1 d . . . H79 H 0.3358 -0.0461 0.6731 0.044 Uiso 1 1 calc R . . C80 C 0.3601(2) 0.02580(18) 0.6628(3) 0.0382(15) Uani 1 1 d . . . H80 H 0.3833 0.0215 0.6137 0.046 Uiso 1 1 calc R . . C81 C 0.35354(19) 0.07344(18) 0.7002(3) 0.0295(14) Uani 1 1 d . . . H81 H 0.3717 0.1008 0.6740 0.035 Uiso 1 1 calc R . . C82 C 0.3230(2) 0.22944(18) 0.9540(4) 0.0388(15) Uani 1 1 d . . . H82 H 0.3418 0.2048 0.9868 0.047 Uiso 1 1 calc R . . C83 C 0.3142(2) 0.2747(2) 0.9928(3) 0.0430(16) Uani 1 1 d . . . H83 H 0.3254 0.2805 1.0506 0.052 Uiso 1 1 calc R . . C84 C 0.2881(2) 0.3119(2) 0.9444(4) 0.0495(17) Uani 1 1 d . . . H84 H 0.2811 0.3436 0.9683 0.059 Uiso 1 1 calc R . . C85 C 0.2730(2) 0.3006(2) 0.8607(4) 0.0506(17) Uani 1 1 d . . . H85 H 0.2561 0.3253 0.8257 0.061 Uiso 1 1 calc R . . C86 C 0.2825(2) 0.25362(19) 0.8272(4) 0.0410(15) Uani 1 1 d . . . H86 H 0.2710 0.2469 0.7698 0.049 Uiso 1 1 calc R . . O3B O 0.4563(4) 0.2212(3) 0.2922(5) 0.270(4) Uani 1 1 d . . . C1B C 0.5614(4) 0.1914(3) 0.3356(6) 0.216(5) Uani 1 1 d U . . H1B1 H 0.5987 0.1834 0.3140 0.325 Uiso 1 1 calc R . . H1B2 H 0.5466 0.1631 0.3679 0.325 Uiso 1 1 calc R . . H1B3 H 0.5636 0.2203 0.3736 0.325 Uiso 1 1 calc R . . C2B C 0.5177(4) 0.2044(4) 0.2499(6) 0.184(5) Uani 1 1 d U . . H2B1 H 0.5333 0.2315 0.2145 0.221 Uiso 1 1 calc R . . H2B2 H 0.5131 0.1748 0.2129 0.221 Uiso 1 1 calc R . . C4B C 0.4332(3) 0.2305(3) 0.1977(5) 0.136(3) Uani 1 1 d U . . H4B1 H 0.4377 0.2019 0.1583 0.163 Uiso 1 1 calc R . . H4B2 H 0.4465 0.2615 0.1708 0.163 Uiso 1 1 calc R . . C5B C 0.3714(3) 0.2346(3) 0.2418(5) 0.170(4) Uani 1 1 d U . . H5B1 H 0.3435 0.2417 0.1972 0.255 Uiso 1 1 calc R . . H5B2 H 0.3714 0.2613 0.2844 0.255 Uiso 1 1 calc R . . H5B3 H 0.3622 0.2033 0.2702 0.255 Uiso 1 1 calc R . . O1C O 0.1298(2) 0.8857(2) 0.5502(4) 0.114(2) Uani 1 1 d . . . C1C C 0.1861(3) 0.8919(3) 0.5247(5) 0.107(3) Uani 1 1 d . . . H1CA H 0.1889 0.9166 0.4778 0.129 Uiso 1 1 calc R . . H1CB H 0.2017 0.8601 0.5038 0.129 Uiso 1 1 calc R . . C2C C 0.2174(3) 0.9094(3) 0.6032(5) 0.107(3) Uani 1 1 d . . . H2CA H 0.2515 0.8894 0.6126 0.129 Uiso 1 1 calc R . . H2CB H 0.2282 0.9446 0.5974 0.129 Uiso 1 1 calc R . . C3C C 0.1787(3) 0.9028(5) 0.6716(5) 0.292(9) Uani 1 1 d . . . H3CA H 0.1936 0.8782 0.7128 0.351 Uiso 1 1 calc R . . H3CB H 0.1740 0.9345 0.7028 0.351 Uiso 1 1 calc R . . C4C C 0.1277(3) 0.8871(4) 0.6415(5) 0.160(4) Uani 1 1 d . . . H4CA H 0.0980 0.9101 0.6606 0.192 Uiso 1 1 calc R . . H4CB H 0.1192 0.8537 0.6644 0.192 Uiso 1 1 calc R . . O1D O 0.0000 1.0000 0.5329(5) 0.168(5) Uani 1 2 d S . . C2D C 0.0402(5) 0.9802(5) 0.4753(5) 0.219(6) Uani 1 1 d . . . H2DA H 0.0767 0.9961 0.4868 0.263 Uiso 1 1 calc R . . H2DB H 0.0444 0.9444 0.4868 0.263 Uiso 1 1 calc R . . C3D C 0.0281(4) 0.9862(4) 0.3974(5) 0.161(5) Uani 1 1 d . . . H3DA H 0.0246 0.9539 0.3678 0.193 Uiso 1 1 calc R . . H3DB H 0.0572 1.0059 0.3678 0.193 Uiso 1 1 calc R . . O1E O 0.2181(3) 0.09631(18) 0.3690(3) 0.1085(18) Uani 1 1 d . . . C1E C 0.1769(3) 0.0701(3) 0.4250(5) 0.130(3) Uani 1 1 d . . . H1EA H 0.1654 0.0921 0.4727 0.156 Uiso 1 1 calc R . . H1EB H 0.1433 0.0618 0.3908 0.156 Uiso 1 1 calc R . . C2E C 0.2001(4) 0.0264(3) 0.4591(6) 0.128(4) Uani 1 1 d . . . H2EA H 0.1958 -0.0020 0.4193 0.153 Uiso 1 1 calc R . . H2EB H 0.1839 0.0179 0.5160 0.153 Uiso 1 1 calc R . . C3E C 0.2586(4) 0.0425(4) 0.4661(7) 0.226(7) Uani 1 1 d . . . H3EA H 0.2840 0.0137 0.4696 0.272 Uiso 1 1 calc R . . H3EB H 0.2641 0.0635 0.5177 0.272 Uiso 1 1 calc R . . C4E C 0.2690(3) 0.0721(4) 0.3833(5) 0.190(6) Uani 1 1 d . . . H4EA H 0.2997 0.0962 0.3913 0.228 Uiso 1 1 calc R . . H4EB H 0.2784 0.0499 0.3347 0.228 Uiso 1 1 calc R . . O1F O 0.1661(4) 0.3623(4) 0.7264(6) 0.288(5) Uiso 1 1 d . . . C1F C 0.2137(5) 0.3770(4) 0.6849(8) 0.236(6) Uiso 1 1 d . . . H1FA H 0.2067 0.3755 0.6221 0.283 Uiso 1 1 calc R . . H1FB H 0.2434 0.3526 0.6980 0.283 Uiso 1 1 calc R . . C2F C 0.2356(5) 0.4277(5) 0.7060(9) 0.315(8) Uiso 1 1 d . . . H2FA H 0.2756 0.4258 0.7215 0.378 Uiso 1 1 calc R . . H2FB H 0.2316 0.4497 0.6555 0.378 Uiso 1 1 calc R . . C3F C 0.2065(5) 0.4452(4) 0.7714(7) 0.258(7) Uiso 1 1 d . . . H3FA H 0.1907 0.4781 0.7576 0.309 Uiso 1 1 calc R . . H3FB H 0.2300 0.4480 0.8236 0.309 Uiso 1 1 calc R . . C4F C 0.1595(4) 0.4064(4) 0.7845(6) 0.172(4) Uiso 1 1 d . . . H4FA H 0.1598 0.3952 0.8452 0.206 Uiso 1 1 calc R . . H4FB H 0.1230 0.4222 0.7731 0.206 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0191(4) 0.0287(5) 0.0259(4) 0.0024(4) -0.0013(4) 0.0003(4) Al1 0.0219(10) 0.0298(10) 0.0296(10) 0.0010(9) 0.0019(8) 0.0031(8) Al2 0.0236(9) 0.0318(10) 0.0238(10) 0.0044(9) -0.0014(8) -0.0024(8) O1 0.024(2) 0.038(2) 0.026(2) -0.0019(18) -0.0011(18) -0.0062(18) O2 0.0180(19) 0.034(2) 0.0226(19) 0.0059(18) 0.0030(17) 0.0021(19) O3 0.026(2) 0.024(2) 0.029(2) 0.0045(17) 0.0030(17) -0.0040(18) O4 0.025(2) 0.039(2) 0.024(2) 0.0130(19) -0.0036(18) -0.0027(18) O5 0.035(2) 0.025(2) 0.027(2) 0.0013(18) 0.0032(19) 0.0003(19) O6 0.019(2) 0.022(2) 0.037(2) -0.0122(19) -0.0013(17) -0.0071(17) O7 0.062(3) 0.050(3) 0.027(2) 0.002(2) -0.006(2) -0.008(2) O8 0.070(3) 0.035(2) 0.057(3) 0.000(2) -0.005(3) -0.004(3) O9 0.072(3) 0.034(3) 0.090(3) -0.006(3) -0.011(3) 0.000(3) O10 0.049(3) 0.054(3) 0.082(3) -0.016(3) -0.006(3) -0.012(2) O11 0.035(2) 0.033(2) 0.022(2) -0.0016(18) -0.0035(18) -0.0089(19) O12 0.027(2) 0.022(2) 0.032(2) -0.0031(18) 0.0030(18) 0.0035(19) O13 0.080(4) 0.103(4) 0.064(3) -0.010(3) 0.017(3) 0.037(3) O14 0.094(4) 0.064(3) 0.063(3) -0.011(3) 0.033(3) 0.003(3) O15 0.077(3) 0.037(3) 0.059(3) -0.020(2) 0.021(3) -0.014(2) O16 0.086(3) 0.038(3) 0.073(3) 0.001(2) 0.007(3) 0.008(3) N1 0.015(2) 0.021(2) 0.023(2) 0.000(2) 0.001(2) -0.001(2) N2 0.026(3) 0.020(3) 0.024(3) -0.003(2) 0.001(2) 0.004(2) N3 0.022(3) 0.023(3) 0.034(3) 0.007(2) -0.002(2) 0.005(2) N4 0.020(3) 0.030(3) 0.030(3) 0.004(2) 0.001(2) -0.003(2) N5 0.023(3) 0.020(3) 0.031(3) 0.005(2) 0.005(2) 0.001(2) N6 0.025(3) 0.025(3) 0.031(3) 0.001(2) -0.003(2) 0.007(2) N7 0.041(3) 0.026(3) 0.050(4) 0.010(3) -0.002(3) 0.000(3) N8 0.037(3) 0.058(4) 0.061(4) -0.009(3) -0.004(3) 0.004(3) N9 0.025(2) 0.021(3) 0.021(2) 0.006(2) -0.001(2) -0.007(2) N10 0.030(3) 0.030(3) 0.017(3) 0.001(2) 0.001(2) 0.000(2) N11 0.080(5) 0.062(4) 0.037(4) -0.011(3) 0.015(4) 0.003(4) N12 0.050(3) 0.041(4) 0.061(4) 0.011(4) 0.008(3) -0.005(3) N13 0.018(3) 0.038(3) 0.025(3) 0.005(2) -0.001(2) -0.006(2) N14 0.026(3) 0.034(3) 0.028(3) 0.004(2) -0.005(2) 0.005(2) C1 0.013(3) 0.026(3) 0.017(3) 0.002(3) -0.003(2) -0.001(3) C2 0.024(3) 0.016(3) 0.022(3) 0.000(3) -0.008(3) 0.008(3) C3 0.019(3) 0.034(4) 0.026(4) 0.010(3) 0.001(3) -0.005(3) C4 0.040(4) 0.033(4) 0.027(4) -0.002(3) -0.007(3) 0.000(3) C5 0.062(4) 0.052(4) 0.041(4) 0.018(4) -0.015(4) -0.001(4) C6 0.055(5) 0.082(5) 0.052(5) 0.025(4) -0.007(4) 0.005(4) C7 0.051(4) 0.068(5) 0.028(4) 0.006(4) -0.004(3) 0.006(4) C8 0.029(3) 0.051(4) 0.027(4) 0.012(3) -0.003(3) -0.006(3) C9 0.027(4) 0.029(4) 0.034(4) 0.019(3) 0.010(3) -0.005(3) C10 0.034(4) 0.069(5) 0.043(4) 0.026(4) -0.016(3) -0.011(3) C11 0.027(4) 0.074(6) 0.095(6) 0.042(5) -0.023(4) -0.002(4) C12 0.022(4) 0.074(6) 0.153(9) 0.087(6) -0.011(5) 0.008(4) C13 0.022(4) 0.037(4) 0.097(6) 0.030(4) 0.023(4) 0.012(3) C14 0.028(4) 0.041(4) 0.057(4) 0.025(3) 0.002(3) 0.001(3) C15 0.026(3) 0.033(4) 0.033(4) -0.001(3) 0.004(3) -0.001(3) C16 0.043(4) 0.030(4) 0.042(4) -0.005(3) 0.008(3) 0.000(3) C17 0.037(4) 0.037(4) 0.041(4) 0.000(3) 0.019(3) -0.001(3) C18 0.035(3) 0.034(4) 0.053(4) -0.004(3) 0.022(3) 0.000(3) C19 0.023(3) 0.039(4) 0.058(4) -0.010(3) 0.000(3) 0.002(3) C20 0.030(3) 0.034(4) 0.024(3) 0.000(3) 0.012(3) -0.005(3) C21 0.024(3) 0.031(4) 0.025(3) 0.001(3) -0.002(2) -0.012(3) C22 0.021(3) 0.019(3) 0.032(3) 0.005(3) 0.007(3) 0.001(3) C23 0.022(3) 0.027(3) 0.037(3) 0.005(3) 0.010(3) -0.001(3) C24 0.031(3) 0.018(3) 0.027(3) -0.006(3) 0.003(3) -0.004(3) C25 0.023(3) 0.037(4) 0.053(4) 0.021(3) 0.003(3) -0.001(3) C26 0.023(3) 0.030(4) 0.034(4) -0.008(3) 0.009(3) -0.005(3) C27 0.023(3) 0.020(3) 0.033(4) 0.001(3) 0.003(3) -0.006(3) C28 0.040(4) 0.054(4) 0.036(4) 0.005(3) -0.006(3) 0.009(3) C29 0.022(3) 0.036(4) 0.034(3) 0.001(3) 0.003(3) 0.001(3) C30 0.020(3) 0.046(4) 0.035(4) 0.005(3) -0.006(3) -0.009(3) C31 0.019(3) 0.033(4) 0.035(4) 0.004(3) 0.000(3) 0.004(3) C32 0.030(3) 0.046(4) 0.037(4) -0.009(3) -0.005(3) -0.003(3) C33 0.039(4) 0.028(4) 0.043(4) -0.016(3) -0.004(3) -0.010(3) C34 0.035(4) 0.041(4) 0.025(3) -0.004(3) 0.004(3) 0.003(3) C35 0.025(3) 0.039(4) 0.025(3) -0.005(3) 0.005(3) -0.003(3) C36 0.028(3) 0.038(4) 0.020(3) 0.002(3) 0.014(3) 0.008(3) C37 0.036(4) 0.037(4) 0.047(4) 0.002(3) -0.001(3) 0.011(3) C38 0.031(3) 0.039(4) 0.036(3) -0.002(3) 0.000(3) -0.006(3) C39 0.023(3) 0.027(3) 0.026(3) 0.005(3) -0.006(3) -0.001(3) C40 0.027(3) 0.048(4) 0.027(3) 0.011(3) -0.010(3) -0.003(3) C41 0.024(3) 0.041(4) 0.041(4) 0.008(3) 0.001(3) 0.003(3) C42 0.025(3) 0.064(4) 0.035(4) 0.008(3) -0.006(3) -0.003(3) C43 0.030(4) 0.087(5) 0.047(4) 0.015(4) -0.007(3) 0.005(4) C44 0.038(4) 0.119(7) 0.037(4) 0.007(5) -0.004(4) -0.020(5) C45 0.050(4) 0.070(5) 0.050(4) 0.002(4) -0.016(4) -0.010(4) C46 0.038(4) 0.041(4) 0.050(4) -0.009(4) -0.006(3) -0.006(3) C47 0.029(4) 0.055(5) 0.045(4) 0.004(4) -0.012(3) -0.004(3) C48 0.038(4) 0.146(7) 0.026(4) 0.018(5) -0.001(3) 0.005(4) C49 0.058(6) 0.207(11) 0.067(6) 0.050(7) -0.020(5) 0.017(6) C50 0.088(8) 0.149(10) 0.086(7) 0.073(7) -0.068(6) -0.073(6) C51 0.119(8) 0.076(6) 0.097(6) 0.048(6) -0.079(7) -0.033(5) C52 0.061(5) 0.065(5) 0.062(5) 0.023(4) -0.029(4) -0.019(4) C53 0.030(3) 0.035(4) 0.026(3) 0.002(3) 0.001(3) -0.001(3) C54 0.026(3) 0.040(4) 0.039(4) 0.010(3) 0.010(3) 0.007(3) C55 0.035(4) 0.046(4) 0.047(4) 0.018(3) 0.010(3) 0.001(3) C56 0.039(4) 0.047(4) 0.034(3) 0.018(3) 0.004(3) -0.006(3) C57 0.036(3) 0.037(4) 0.032(3) 0.008(3) -0.004(3) 0.002(3) C58 0.035(4) 0.024(4) 0.022(3) 0.005(3) -0.001(3) -0.009(3) C59 0.024(3) 0.045(4) 0.033(3) 0.007(3) 0.006(3) -0.002(3) C60 0.033(4) 0.032(4) 0.018(3) 0.005(3) 0.002(3) -0.001(3) C61 0.039(4) 0.042(4) 0.027(4) 0.000(3) 0.007(3) 0.001(3) C62 0.053(5) 0.059(5) 0.036(4) 0.005(4) 0.021(4) 0.026(4) C63 0.058(5) 0.034(4) 0.041(4) -0.013(3) 0.017(4) -0.009(4) C64 0.041(4) 0.041(4) 0.034(4) 0.012(3) 0.000(3) -0.012(3) C65 0.049(4) 0.015(4) 0.021(3) 0.002(3) 0.001(3) -0.004(3) C66 0.088(5) 0.055(5) 0.025(4) -0.017(3) 0.009(4) -0.024(4) C67 0.023(3) 0.043(4) 0.033(3) 0.004(3) 0.002(3) -0.002(3) C68 0.031(3) 0.031(4) 0.044(4) 0.017(3) 0.001(3) 0.008(3) C69 0.024(3) 0.043(4) 0.025(4) 0.013(3) 0.001(3) -0.003(3) C70 0.034(4) 0.018(4) 0.052(4) 0.005(3) 0.010(3) 0.003(3) C71 0.042(4) 0.013(3) 0.046(4) 0.002(3) 0.008(3) 0.008(3) C72 0.027(3) 0.033(4) 0.041(4) -0.014(3) 0.012(3) -0.003(3) C73 0.026(3) 0.039(4) 0.027(4) 0.004(3) 0.006(3) -0.006(3) C74 0.027(3) 0.038(4) 0.036(4) -0.001(4) 0.013(3) -0.007(3) C75 0.043(4) 0.056(4) 0.025(3) -0.016(3) 0.007(3) -0.022(3) C76 0.035(4) 0.047(4) 0.023(3) 0.001(3) -0.007(3) -0.001(3) C77 0.012(3) 0.051(4) 0.030(3) 0.005(3) -0.006(3) 0.002(3) C78 0.037(4) 0.018(3) 0.034(3) 0.001(3) -0.003(3) -0.002(3) C79 0.045(4) 0.038(4) 0.027(4) -0.009(3) 0.004(3) 0.000(3) C80 0.047(4) 0.035(4) 0.033(4) -0.008(3) 0.008(3) -0.003(3) C81 0.020(3) 0.045(4) 0.023(3) 0.012(3) -0.001(3) -0.012(3) C82 0.035(4) 0.029(4) 0.053(4) 0.015(3) -0.003(3) -0.004(3) C83 0.043(4) 0.035(4) 0.051(4) -0.015(3) 0.009(4) 0.000(4) C84 0.050(4) 0.034(4) 0.065(5) -0.016(4) 0.014(4) -0.005(3) C85 0.054(4) 0.033(4) 0.065(5) -0.003(4) -0.012(4) 0.006(3) C86 0.046(4) 0.030(4) 0.047(4) 0.001(4) -0.001(4) 0.005(3) O3B 0.224(10) 0.410(13) 0.175(8) -0.041(8) 0.031(7) -0.025(9) C1B 0.210(6) 0.224(6) 0.216(6) 0.020(5) -0.002(5) -0.023(5) C2B 0.180(6) 0.183(6) 0.188(6) 0.002(4) -0.001(5) -0.020(5) C4B 0.147(5) 0.110(5) 0.151(5) -0.001(4) -0.012(4) 0.011(4) C5B 0.175(6) 0.163(6) 0.171(6) 0.011(4) -0.001(5) 0.014(4) O1C 0.071(4) 0.150(5) 0.121(5) -0.058(4) -0.011(4) -0.004(4) C1C 0.090(7) 0.109(7) 0.124(8) -0.011(6) -0.009(7) -0.016(6) C2C 0.094(7) 0.113(7) 0.115(7) -0.037(6) -0.058(6) -0.005(5) C3C 0.065(7) 0.75(3) 0.067(7) -0.099(12) 0.028(6) -0.130(12) C4C 0.134(9) 0.287(12) 0.060(7) -0.038(7) 0.002(6) -0.099(8) O1D 0.207(12) 0.211(11) 0.086(7) 0.000 0.000 -0.091(10) C2D 0.210(15) 0.316(16) 0.133(12) -0.065(14) 0.014(11) 0.075(12) C3D 0.108(8) 0.267(14) 0.108(7) -0.096(10) -0.026(7) 0.015(9) O1E 0.116(5) 0.123(5) 0.087(4) -0.004(3) 0.016(4) -0.008(4) C1E 0.090(7) 0.219(11) 0.082(6) 0.034(7) 0.038(6) 0.011(8) C2E 0.160(10) 0.084(6) 0.139(8) 0.048(6) -0.026(8) 0.044(7) C3E 0.098(9) 0.375(17) 0.206(13) 0.175(12) 0.021(9) 0.107(10) C4E 0.039(6) 0.424(17) 0.106(8) 0.092(10) -0.014(5) 0.044(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.920(4) . yes Fe1 N4 1.923(4) . yes Fe1 N3 1.926(4) . yes Fe1 N2 1.935(4) . yes Fe1 N13 2.007(4) . yes Fe1 N14 2.018(4) . yes Al1 O3 1.837(3) . ? Al1 O5 1.840(3) . ? Al1 O6 1.858(3) . ? Al1 O1 1.860(3) . ? Al1 N5 2.104(4) . ? Al1 N6 2.131(4) . ? Al2 O12 1.839(3) . ? Al2 O2 1.839(3) . ? Al2 O11 1.848(3) . ? Al2 O4 1.865(3) . ? Al2 N10 2.131(4) . ? Al2 N9 2.144(4) . ? O1 N1 1.349(4) . ? O2 N2 1.354(4) . ? O3 N3 1.360(4) . ? O4 N4 1.339(4) . ? O5 C27 1.304(5) . ? O6 C36 1.304(5) . ? O7 N7 1.215(5) . ? O8 N7 1.241(4) . ? O9 N8 1.231(5) . ? O10 N8 1.252(5) . ? O11 C65 1.297(5) . ? O12 C74 1.300(5) . ? O13 N11 1.236(6) . ? O14 N11 1.230(5) . ? O15 N12 1.235(5) . ? O16 N12 1.239(5) . ? N1 C1 1.303(5) . ? N2 C2 1.313(5) . ? N3 C39 1.305(5) . ? N4 C40 1.301(5) . ? N5 C21 1.487(5) . ? N5 C29 1.498(5) . ? N5 C15 1.517(5) . ? N6 C38 1.484(5) . ? N6 C30 1.493(5) . ? N6 C20 1.503(5) . ? N7 C24 1.435(5) . ? N8 C33 1.441(6) . ? N9 C53 1.484(5) . ? N9 C67 1.502(5) . ? N9 C59 1.506(5) . ? N10 C76 1.484(5) . ? N10 C68 1.486(5) . ? N10 C58 1.501(5) . ? N11 C62 1.438(7) . ? N12 C71 1.435(6) . ? N13 C81 1.332(5) . ? N13 C77 1.347(5) . ? N14 C86 1.346(5) . ? N14 C82 1.357(6) . ? C1 C2 1.434(6) . ? C1 C3 1.497(6) . ? C2 C9 1.503(6) . ? C3 C4 1.385(6) . ? C3 C8 1.394(6) . ? C4 C5 1.374(6) . ? C5 C6 1.407(7) . ? C6 C7 1.374(7) . ? C7 C8 1.401(6) . ? C9 C14 1.365(6) . ? C9 C10 1.394(6) . ? C10 C11 1.369(7) . ? C11 C12 1.351(8) . ? C12 C13 1.391(8) . ? C13 C14 1.408(6) . ? C15 C16 1.509(6) . ? C15 C20 1.548(6) . ? C16 C17 1.507(6) . ? C17 C18 1.495(6) . ? C18 C19 1.524(6) . ? C19 C20 1.528(6) . ? C21 C22 1.498(5) . ? C22 C23 1.373(6) . ? C22 C27 1.413(6) . ? C23 C24 1.391(6) . ? C24 C25 1.399(6) . ? C25 C26 1.378(6) . ? C26 C27 1.427(6) . ? C26 C28 1.511(6) . ? C30 C31 1.456(5) . ? C31 C32 1.388(6) . ? C31 C36 1.440(6) . ? C32 C33 1.386(6) . ? C33 C34 1.394(6) . ? C34 C35 1.373(6) . ? C35 C36 1.421(6) . ? C35 C37 1.515(6) . ? C39 C40 1.432(6) . ? C39 C41 1.478(6) . ? C40 C47 1.488(6) . ? C41 C42 1.380(5) . ? C41 C46 1.399(5) . ? C42 C43 1.399(6) . ? C43 C44 1.368(6) . ? C44 C45 1.381(6) . ? C45 C46 1.403(6) . ? C47 C48 1.371(6) . ? C47 C52 1.384(6) . ? C48 C49 1.400(7) . ? C49 C50 1.376(7) . ? C50 C51 1.393(8) . ? C51 C52 1.397(6) . ? C53 C58 1.525(6) . ? C53 C54 1.525(6) . ? C54 C55 1.553(6) . ? C55 C56 1.482(6) . ? C56 C57 1.519(6) . ? C57 C58 1.516(5) . ? C59 C60 1.493(6) . ? C60 C61 1.370(6) . ? C60 C65 1.422(6) . ? C61 C62 1.382(6) . ? C62 C63 1.364(7) . ? C63 C64 1.391(6) . ? C64 C65 1.417(6) . ? C64 C66 1.543(6) . ? C68 C69 1.497(6) . ? C69 C70 1.362(6) . ? C69 C74 1.460(6) . ? C70 C71 1.363(6) . ? C71 C72 1.377(6) . ? C72 C73 1.391(6) . ? C73 C74 1.435(6) . ? C73 C75 1.494(6) . ? C77 C78 1.423(6) . ? C78 C79 1.361(6) . ? C79 C80 1.377(6) . ? C80 C81 1.421(6) . ? C82 C83 1.381(6) . ? C83 C84 1.400(6) . ? C84 C85 1.382(7) . ? C85 C86 1.391(6) . ? O3B C4B 1.587(10) . ? O3B C2B 1.673(10) . ? C1B C2B 1.729(11) . ? C4B C5B 1.634(10) . ? O1C C1C 1.415(7) . ? O1C C4C 1.417(7) . ? C1C C2C 1.507(8) . ? C2C C3C 1.420(9) . ? C3C C4C 1.376(9) . ? O1D C2D 1.418(9) . ? O1D C2D 1.418(9) 2_575 ? C2D C3D 1.254(10) . ? C3D C3D 1.539(17) 2_575 ? O1E C4E 1.401(7) . ? O1E C1E 1.493(7) . ? C1E C2E 1.408(8) . ? C2E C3E 1.470(11) . ? C3E C4E 1.533(10) . ? O1F C1F 1.368(13) . ? O1F C4F 1.504(10) . ? C1F C2F 1.504(13) . ? C2F C3F 1.318(15) . ? C3F C4F 1.550(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N4 178.92(17) . . yes N1 Fe1 N3 99.41(17) . . yes N4 Fe1 N3 80.11(17) . . yes N1 Fe1 N2 80.56(17) . . yes N4 Fe1 N2 100.08(18) . . yes N3 Fe1 N2 170.04(16) . . yes N1 Fe1 N13 91.41(15) . . yes N4 Fe1 N13 89.52(15) . . yes N3 Fe1 N13 86.07(16) . . yes N2 Fe1 N13 83.97(15) . . yes N1 Fe1 N14 89.73(15) . . yes N4 Fe1 N14 89.33(16) . . yes N3 Fe1 N14 92.94(16) . . yes N2 Fe1 N14 97.02(16) . . yes N13 Fe1 N14 178.60(17) . . yes O3 Al1 O5 90.17(15) . . ? O3 Al1 O6 90.84(15) . . ? O5 Al1 O6 175.58(17) . . ? O3 Al1 O1 101.47(15) . . ? O5 Al1 O1 96.59(16) . . ? O6 Al1 O1 87.42(15) . . ? O3 Al1 N5 172.20(16) . . ? O5 Al1 N5 88.15(15) . . ? O6 Al1 N5 90.28(15) . . ? O1 Al1 N5 86.29(15) . . ? O3 Al1 N6 88.16(16) . . ? O5 Al1 N6 89.53(16) . . ? O6 Al1 N6 86.21(14) . . ? O1 Al1 N6 168.53(17) . . ? N5 Al1 N6 84.21(16) . . ? O12 Al2 O2 89.73(15) . . ? O12 Al2 O11 176.33(16) . . ? O2 Al2 O11 90.73(14) . . ? O12 Al2 O4 96.14(15) . . ? O2 Al2 O4 101.91(15) . . ? O11 Al2 O4 87.33(15) . . ? O12 Al2 N10 88.24(15) . . ? O2 Al2 N10 171.93(17) . . ? O11 Al2 N10 90.81(15) . . ? O4 Al2 N10 86.07(15) . . ? O12 Al2 N9 89.08(15) . . ? O2 Al2 N9 89.42(15) . . ? O11 Al2 N9 87.29(15) . . ? O4 Al2 N9 167.51(16) . . ? N10 Al2 N9 82.75(15) . . ? N1 O1 Al1 127.2(3) . . ? N2 O2 Al2 124.9(3) . . ? N3 O3 Al1 125.2(3) . . ? N4 O4 Al2 127.7(3) . . ? C27 O5 Al1 136.0(3) . . ? C36 O6 Al1 135.5(3) . . ? C65 O11 Al2 136.7(3) . . ? C74 O12 Al2 136.2(3) . . ? C1 N1 O1 116.6(4) . . ? C1 N1 Fe1 116.1(3) . . ? O1 N1 Fe1 127.2(3) . . ? C2 N2 O2 118.4(4) . . ? C2 N2 Fe1 114.5(3) . . ? O2 N2 Fe1 125.4(3) . . ? C39 N3 O3 116.7(4) . . ? C39 N3 Fe1 116.4(3) . . ? O3 N3 Fe1 124.7(3) . . ? C40 N4 O4 116.9(4) . . ? C40 N4 Fe1 115.7(3) . . ? O4 N4 Fe1 126.7(3) . . ? C21 N5 C29 105.1(3) . . ? C21 N5 C15 111.1(4) . . ? C29 N5 C15 111.0(4) . . ? C21 N5 Al1 111.0(3) . . ? C29 N5 Al1 110.3(3) . . ? C15 N5 Al1 108.3(3) . . ? C38 N6 C30 105.2(4) . . ? C38 N6 C20 112.9(4) . . ? C30 N6 C20 111.6(4) . . ? C38 N6 Al1 112.1(3) . . ? C30 N6 Al1 109.6(3) . . ? C20 N6 Al1 105.6(3) . . ? O7 N7 O8 122.4(5) . . ? O7 N7 C24 119.9(4) . . ? O8 N7 C24 117.8(4) . . ? O9 N8 O10 120.5(5) . . ? O9 N8 C33 121.0(5) . . ? O10 N8 C33 118.4(5) . . ? C53 N9 C67 112.6(3) . . ? C53 N9 C59 111.6(4) . . ? C67 N9 C59 103.7(3) . . ? C53 N9 Al2 108.2(3) . . ? C67 N9 Al2 110.6(3) . . ? C59 N9 Al2 110.1(3) . . ? C76 N10 C68 105.6(4) . . ? C76 N10 C58 112.0(4) . . ? C68 N10 C58 110.2(4) . . ? C76 N10 Al2 111.6(3) . . ? C68 N10 Al2 109.6(3) . . ? C58 N10 Al2 107.9(3) . . ? O14 N11 O13 120.6(6) . . ? O14 N11 C62 119.1(6) . . ? O13 N11 C62 120.3(6) . . ? O15 N12 O16 121.4(5) . . ? O15 N12 C71 119.4(5) . . ? O16 N12 C71 119.2(5) . . ? C81 N13 C77 117.5(4) . . ? C81 N13 Fe1 121.3(3) . . ? C77 N13 Fe1 121.2(3) . . ? C86 N14 C82 115.7(4) . . ? C86 N14 Fe1 120.8(4) . . ? C82 N14 Fe1 123.4(4) . . ? N1 C1 C2 113.6(4) . . ? N1 C1 C3 124.8(4) . . ? C2 C1 C3 121.6(4) . . ? N2 C2 C1 114.0(4) . . ? N2 C2 C9 121.7(4) . . ? C1 C2 C9 124.3(4) . . ? C4 C3 C8 119.0(5) . . ? C4 C3 C1 120.0(5) . . ? C8 C3 C1 120.9(5) . . ? C5 C4 C3 122.4(5) . . ? C4 C5 C6 118.1(5) . . ? C7 C6 C5 120.8(6) . . ? C6 C7 C8 120.1(6) . . ? C3 C8 C7 119.6(5) . . ? C14 C9 C10 120.4(5) . . ? C14 C9 C2 119.5(5) . . ? C10 C9 C2 120.0(5) . . ? C11 C10 C9 119.6(6) . . ? C12 C11 C10 121.1(7) . . ? C11 C12 C13 120.3(6) . . ? C12 C13 C14 119.2(6) . . ? C9 C14 C13 119.3(6) . . ? C16 C15 N5 115.5(4) . . ? C16 C15 C20 113.0(4) . . ? N5 C15 C20 107.9(4) . . ? C17 C16 C15 112.6(4) . . ? C18 C17 C16 109.9(4) . . ? C17 C18 C19 109.6(4) . . ? C18 C19 C20 110.9(4) . . ? N6 C20 C19 114.8(4) . . ? N6 C20 C15 108.8(4) . . ? C19 C20 C15 110.9(4) . . ? N5 C21 C22 116.1(4) . . ? C23 C22 C27 120.5(4) . . ? C23 C22 C21 120.0(4) . . ? C27 C22 C21 119.3(4) . . ? C22 C23 C24 119.5(5) . . ? C23 C24 C25 121.1(5) . . ? C23 C24 N7 119.1(5) . . ? C25 C24 N7 119.8(5) . . ? C26 C25 C24 120.1(5) . . ? C25 C26 C27 119.1(5) . . ? C25 C26 C28 120.7(5) . . ? C27 C26 C28 120.2(5) . . ? O5 C27 C22 122.9(4) . . ? O5 C27 C26 118.0(5) . . ? C22 C27 C26 119.0(5) . . ? C31 C30 N6 117.0(4) . . ? C32 C31 C36 118.2(5) . . ? C32 C31 C30 120.7(5) . . ? C36 C31 C30 120.9(5) . . ? C33 C32 C31 120.7(5) . . ? C32 C33 C34 121.9(5) . . ? C32 C33 N8 120.9(5) . . ? C34 C33 N8 117.2(5) . . ? C35 C34 C33 119.0(5) . . ? C34 C35 C36 120.8(5) . . ? C34 C35 C37 121.6(5) . . ? C36 C35 C37 117.6(5) . . ? O6 C36 C35 119.1(5) . . ? O6 C36 C31 121.6(5) . . ? C35 C36 C31 119.3(5) . . ? N3 C39 C40 112.5(4) . . ? N3 C39 C41 120.3(5) . . ? C40 C39 C41 126.9(5) . . ? N4 C40 C39 114.6(4) . . ? N4 C40 C47 120.9(5) . . ? C39 C40 C47 124.0(5) . . ? C42 C41 C46 118.4(5) . . ? C42 C41 C39 122.3(5) . . ? C46 C41 C39 118.8(5) . . ? C41 C42 C43 120.8(5) . . ? C44 C43 C42 120.2(5) . . ? C43 C44 C45 120.4(6) . . ? C44 C45 C46 119.4(5) . . ? C41 C46 C45 120.6(5) . . ? C48 C47 C52 118.7(5) . . ? C48 C47 C40 121.3(6) . . ? C52 C47 C40 119.7(5) . . ? C47 C48 C49 121.2(6) . . ? C50 C49 C48 118.6(7) . . ? C49 C50 C51 122.2(7) . . ? C50 C51 C52 117.1(7) . . ? C47 C52 C51 122.1(6) . . ? N9 C53 C58 109.8(4) . . ? N9 C53 C54 113.9(4) . . ? C58 C53 C54 111.7(4) . . ? C53 C54 C55 111.2(4) . . ? C56 C55 C54 108.6(4) . . ? C55 C56 C57 111.5(4) . . ? C58 C57 C56 110.6(4) . . ? N10 C58 C57 114.1(4) . . ? N10 C58 C53 109.7(4) . . ? C57 C58 C53 111.1(4) . . ? C60 C59 N9 115.7(4) . . ? C61 C60 C65 120.5(5) . . ? C61 C60 C59 119.7(5) . . ? C65 C60 C59 119.8(5) . . ? C60 C61 C62 119.0(5) . . ? C63 C62 C61 123.5(6) . . ? C63 C62 N11 118.5(6) . . ? C61 C62 N11 118.1(6) . . ? C62 C63 C64 118.0(6) . . ? C63 C64 C65 121.1(5) . . ? C63 C64 C66 121.6(5) . . ? C65 C64 C66 117.3(5) . . ? O11 C65 C64 119.2(5) . . ? O11 C65 C60 123.0(5) . . ? C64 C65 C60 117.8(5) . . ? N10 C68 C69 117.2(4) . . ? C70 C69 C74 119.4(5) . . ? C70 C69 C68 121.8(5) . . ? C74 C69 C68 118.8(5) . . ? C69 C70 C71 120.5(5) . . ? C70 C71 C72 122.9(5) . . ? C70 C71 N12 119.1(5) . . ? C72 C71 N12 117.9(5) . . ? C71 C72 C73 119.7(5) . . ? C72 C73 C74 119.1(5) . . ? C72 C73 C75 122.8(5) . . ? C74 C73 C75 118.0(5) . . ? O12 C74 C73 119.6(5) . . ? O12 C74 C69 122.3(5) . . ? C73 C74 C69 118.2(5) . . ? N13 C77 C78 122.4(4) . . ? C79 C78 C77 119.7(5) . . ? C78 C79 C80 118.2(5) . . ? C79 C80 C81 119.7(5) . . ? N13 C81 C80 122.4(4) . . ? N14 C82 C83 125.2(5) . . ? C82 C83 C84 118.1(5) . . ? C85 C84 C83 117.6(5) . . ? C84 C85 C86 120.6(6) . . ? N14 C86 C85 122.8(5) . . ? C4B O3B C2B 89.2(6) . . ? O3B C2B C1B 106.6(7) . . ? O3B C4B C5B 86.5(6) . . ? C1C O1C C4C 108.1(6) . . ? O1C C1C C2C 106.5(6) . . ? C3C C2C C1C 103.9(6) . . ? C4C C3C C2C 111.4(7) . . ? C3C C4C O1C 108.4(7) . . ? C2D O1D C2D 101.9(11) . 2_575 ? C3D C2D O1D 113.7(12) . . ? C2D C3D C3D 105.3(8) . 2_575 ? C4E O1E C1E 105.0(6) . . ? C2E C1E O1E 111.0(7) . . ? C1E C2E C3E 98.9(8) . . ? C2E C3E C4E 104.3(8) . . ? O1E C4E C3E 103.6(6) . . ? C1F O1F C4F 98.0(9) . . ? O1F C1F C2F 116.9(11) . . ? C3F C2F C1F 108.1(12) . . ? C2F C3F C4F 104.0(10) . . ? O1F C4F C3F 112.4(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.831 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.061 # Attachment '- mrr07.cif' data_mrr07 _database_code_depnum_ccdc_archive 'CCDC 862109' #TrackingRef '- mrr07.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H72 Al2 N8 O8 Pd, 0.5(C6 H14), 1.45(C4 H8 O)' _chemical_formula_sum 'C76.80 H90.60 Al2 N8 O9.45 Pd' _chemical_formula_weight 1437.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.5492(17) _cell_length_b 19.7138(17) _cell_length_c 20.515(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.794(3) _cell_angle_gamma 90.00 _cell_volume 7315.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9718 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 29.82 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3020 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9476 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans; 10 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 111672 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 30.52 _reflns_number_total 22234 _reflns_number_gt 13865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.68A' _computing_data_reduction 'Bruker SAINT-Plus v7.68A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22234 _refine_ls_number_parameters 875 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.788 _refine_ls_restrained_S_all 1.865 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.207788(11) 0.460582(11) 0.210464(12) 0.01720(5) Uani 1 1 d . . . Al2 Al 0.12251(4) 0.47064(4) 0.35189(5) 0.0219(2) Uani 1 1 d . . . Al3 Al 0.32605(4) 0.51107(4) 0.10303(5) 0.0183(2) Uani 1 1 d . . . O1 O 0.19527(9) 0.40402(9) 0.34460(10) 0.0213(5) Uani 1 1 d . . . O2 O 0.33254(9) 0.42509(9) 0.14469(10) 0.0196(5) Uani 1 1 d . . . O3 O 0.06172(9) 0.40368(9) 0.36650(10) 0.0256(5) Uani 1 1 d . . . O4 O 0.18116(8) 0.53926(10) 0.33551(9) 0.0213(5) Uani 1 1 d . . . O5 O 0.22069(8) 0.51775(8) 0.07686(9) 0.0189(5) Uani 1 1 d . . . O6 O 0.06903(8) 0.47249(9) 0.26308(9) 0.0194(5) Uani 1 1 d . . . O7 O 0.32688(8) 0.46816(9) 0.02536(9) 0.0195(5) Uani 1 1 d . . . O8 O 0.32680(8) 0.55201(9) 0.18202(9) 0.0190(5) Uani 1 1 d . . . N1 N 0.23280(11) 0.40718(11) 0.29619(11) 0.0176(6) Uani 1 1 d . . . N2 N 0.30269(11) 0.41792(11) 0.19767(12) 0.0191(6) Uani 1 1 d . . . N3 N 0.16634(11) 0.47662(11) 0.45593(12) 0.0255(6) Uani 1 1 d . . . N4 N 0.04386(11) 0.54569(12) 0.37515(12) 0.0232(6) Uani 1 1 d . . . N5 N 0.18043(11) 0.51086(10) 0.12316(11) 0.0165(5) Uani 1 1 d . . . N6 N 0.10504(11) 0.48946(11) 0.21595(12) 0.0186(6) Uani 1 1 d . . . N7 N 0.33540(11) 0.60541(11) 0.05554(12) 0.0182(6) Uani 1 1 d . . . N8 N 0.44705(11) 0.51559(11) 0.12562(12) 0.0208(6) Uani 1 1 d . . . C1 C 0.29222(14) 0.37054(13) 0.30077(15) 0.0177(7) Uani 1 1 d . . . C2 C 0.32945(13) 0.37507(14) 0.24423(15) 0.0181(7) Uani 1 1 d . . . C3 C 0.33432(14) 0.32460(13) 0.35025(15) 0.0185(7) Uani 1 1 d . . . C4 C 0.32768(14) 0.29991(14) 0.41098(15) 0.0249(7) Uani 1 1 d . . . H4 H 0.2867 0.3121 0.4293 0.030 Uiso 1 1 calc R . . C5 C 0.38329(15) 0.25577(14) 0.44591(16) 0.0307(8) Uani 1 1 d . . . H5 H 0.3796 0.2393 0.4886 0.037 Uiso 1 1 calc R . . C6 C 0.44227(15) 0.23593(14) 0.42017(16) 0.0292(8) Uani 1 1 d . . . H6 H 0.4789 0.2068 0.4454 0.035 Uiso 1 1 calc R . . C7 C 0.44878(14) 0.25839(14) 0.35708(16) 0.0232(7) Uani 1 1 d . . . C8 C 0.50410(15) 0.23992(14) 0.32187(17) 0.0299(8) Uani 1 1 d . . . H8 H 0.5423 0.2095 0.3420 0.036 Uiso 1 1 calc R . . C9 C 0.50310(15) 0.26509(15) 0.25981(17) 0.0310(8) Uani 1 1 d . . . H9 H 0.5406 0.2514 0.2377 0.037 Uiso 1 1 calc R . . C10 C 0.44774(14) 0.31135(14) 0.22695(16) 0.0269(8) Uani 1 1 d . . . H10 H 0.4479 0.3283 0.1836 0.032 Uiso 1 1 calc R . . C11 C 0.39416(14) 0.33061(14) 0.26007(15) 0.0200(7) Uani 1 1 d . . . C12 C 0.39518(14) 0.30314(13) 0.32384(15) 0.0189(7) Uani 1 1 d . . . C13 C 0.11451(15) 0.51498(14) 0.48797(15) 0.0281(8) Uani 1 1 d . . . H13A H 0.1423 0.5349 0.5304 0.034 Uiso 1 1 calc R . . H13B H 0.0773 0.4834 0.4987 0.034 Uiso 1 1 calc R . . C14 C 0.07527(15) 0.57101(15) 0.44336(16) 0.0289(8) Uani 1 1 d . . . H14A H 0.0351 0.5897 0.4628 0.035 Uiso 1 1 calc R . . H14B H 0.1106 0.6081 0.4411 0.035 Uiso 1 1 calc R . . C15 C 0.17759(15) 0.40734(15) 0.48622(16) 0.0337(8) Uani 1 1 d . . . H15A H 0.1996 0.4122 0.5346 0.040 Uiso 1 1 calc R . . H15B H 0.2138 0.3828 0.4660 0.040 Uiso 1 1 calc R . . C16 C 0.10911(18) 0.36467(15) 0.47819(18) 0.0338(9) Uani 1 1 d . . . C17 C 0.10035(19) 0.32261(16) 0.53061(18) 0.0457(10) Uani 1 1 d . . . H17 H 0.1371 0.3228 0.5711 0.055 Uiso 1 1 calc R . . C18 C 0.0392(2) 0.28046(17) 0.5251(2) 0.0571(13) Uani 1 1 d . . . C19 C -0.0125(2) 0.28169(17) 0.4653(2) 0.0599(14) Uani 1 1 d . . . H19 H -0.0543 0.2528 0.4610 0.072 Uiso 1 1 calc R . . C20 C -0.00762(19) 0.32252(16) 0.4107(2) 0.0418(10) Uani 1 1 d . . . C21 C 0.05595(17) 0.36491(15) 0.41794(18) 0.0324(9) Uani 1 1 d . . . C22 C 0.0318(2) 0.23405(17) 0.5822(2) 0.0879(17) Uani 1 1 d . . . H22A H -0.0181 0.2382 0.5904 0.132 Uiso 1 1 calc R . . H22B H 0.0682 0.2470 0.6227 0.132 Uiso 1 1 calc R . . H22C H 0.0405 0.1870 0.5706 0.132 Uiso 1 1 calc R . . C23 C -0.06331(17) 0.32150(17) 0.3468(2) 0.0583(12) Uani 1 1 d . . . H23A H -0.1029 0.2897 0.3501 0.087 Uiso 1 1 calc R . . H23B H -0.0398 0.3071 0.3107 0.087 Uiso 1 1 calc R . . H23C H -0.0841 0.3671 0.3371 0.087 Uiso 1 1 calc R . . C24 C 0.24110(15) 0.50898(15) 0.46976(16) 0.0339(9) Uani 1 1 d . . . H24A H 0.2749 0.4796 0.4512 0.041 Uiso 1 1 calc R . . H24B H 0.2601 0.5109 0.5188 0.041 Uiso 1 1 calc R . . C25 C 0.24377(15) 0.57904(17) 0.44201(18) 0.0317(8) Uani 1 1 d . . . C26 C 0.27674(16) 0.63210(19) 0.48240(19) 0.0471(10) Uani 1 1 d . . . H26 H 0.2951 0.6248 0.5289 0.056 Uiso 1 1 calc R . . C27 C 0.2831(2) 0.6960(2) 0.4552(2) 0.0584(13) Uani 1 1 d . . . C28 C 0.25739(18) 0.70549(17) 0.3877(2) 0.0482(11) Uani 1 1 d . . . H28 H 0.2626 0.7489 0.3692 0.058 Uiso 1 1 calc R . . C29 C 0.22381(16) 0.65351(16) 0.34551(18) 0.0322(9) Uani 1 1 d . . . C30 C 0.21549(14) 0.58958(15) 0.37407(17) 0.0246(8) Uani 1 1 d . . . C31 C 0.3203(2) 0.7538(2) 0.4995(2) 0.1021(19) Uani 1 1 d . . . H31A H 0.3738 0.7521 0.5028 0.153 Uiso 1 1 calc R . . H31B H 0.3102 0.7492 0.5442 0.153 Uiso 1 1 calc R . . H31C H 0.3008 0.7973 0.4800 0.153 Uiso 1 1 calc R . . C32 C 0.19755(15) 0.66332(15) 0.27145(17) 0.0374(9) Uani 1 1 d . . . H32A H 0.1437 0.6688 0.2604 0.056 Uiso 1 1 calc R . . H32B H 0.2111 0.6236 0.2480 0.056 Uiso 1 1 calc R . . H32C H 0.2207 0.7039 0.2576 0.056 Uiso 1 1 calc R . . C33 C 0.03152(14) 0.60444(14) 0.32866(16) 0.0311(8) Uani 1 1 d . . . H33A H -0.0044 0.6354 0.3413 0.047 Uiso 1 1 calc R . . H33B H 0.0125 0.5883 0.2829 0.047 Uiso 1 1 calc R . . H33C H 0.0784 0.6284 0.3311 0.047 Uiso 1 1 calc R . . C34 C -0.03035(13) 0.51492(14) 0.37243(15) 0.0314(8) Uani 1 1 d . . . H34A H -0.0259 0.4790 0.4061 0.047 Uiso 1 1 calc R . . H34B H -0.0495 0.4957 0.3279 0.047 Uiso 1 1 calc R . . H34C H -0.0643 0.5499 0.3815 0.047 Uiso 1 1 calc R . . C35 C 0.11210(13) 0.53199(13) 0.11017(14) 0.0163(6) Uani 1 1 d . . . C36 C 0.07061(13) 0.51815(13) 0.16190(15) 0.0170(7) Uani 1 1 d . . . C37 C -0.00643(12) 0.53842(14) 0.13507(14) 0.0198(6) Uani 1 1 d . . . C38 C -0.07168(12) 0.53157(14) 0.15618(14) 0.0231(7) Uani 1 1 d . . . H38 H -0.0722 0.5136 0.1990 0.028 Uiso 1 1 calc R . . C39 C -0.13711(14) 0.55200(14) 0.11222(16) 0.0283(8) Uani 1 1 d . . . H39 H -0.1823 0.5475 0.1264 0.034 Uiso 1 1 calc R . . C40 C -0.13948(14) 0.57832(14) 0.04958(16) 0.0257(8) Uani 1 1 d . . . H40 H -0.1854 0.5913 0.0218 0.031 Uiso 1 1 calc R . . C41 C -0.07252(14) 0.58600(13) 0.02654(15) 0.0200(7) Uani 1 1 d . . . C42 C -0.06513(14) 0.60880(13) -0.03690(15) 0.0229(7) Uani 1 1 d . . . H42 H -0.1073 0.6247 -0.0683 0.028 Uiso 1 1 calc R . . C43 C 0.00294(14) 0.60800(13) -0.05336(15) 0.0247(7) Uani 1 1 d . . . H43 H 0.0067 0.6241 -0.0961 0.030 Uiso 1 1 calc R . . C44 C 0.06744(14) 0.58413(13) -0.00892(15) 0.0223(7) Uani 1 1 d . . . H44 H 0.1134 0.5827 -0.0222 0.027 Uiso 1 1 calc R . . C45 C 0.06246(13) 0.56315(13) 0.05328(15) 0.0180(7) Uani 1 1 d . . . C46 C -0.00813(13) 0.56522(13) 0.07086(15) 0.0183(7) Uani 1 1 d . . . C47 C 0.41409(13) 0.61583(14) 0.05211(15) 0.0242(8) Uani 1 1 d . . . H47A H 0.4237 0.6650 0.0488 0.029 Uiso 1 1 calc R . . H47B H 0.4232 0.5936 0.0114 0.029 Uiso 1 1 calc R . . C48 C 0.46667(13) 0.58703(14) 0.11294(15) 0.0244(7) Uani 1 1 d . . . H48A H 0.5178 0.5886 0.1060 0.029 Uiso 1 1 calc R . . H48B H 0.4648 0.6152 0.1525 0.029 Uiso 1 1 calc R . . C49 C 0.28819(14) 0.60683(14) -0.01297(15) 0.0227(7) Uani 1 1 d . . . H49A H 0.2930 0.6520 -0.0326 0.027 Uiso 1 1 calc R . . H49B H 0.2360 0.6016 -0.0097 0.027 Uiso 1 1 calc R . . C50 C 0.30484(13) 0.55403(14) -0.05982(15) 0.0209(7) Uani 1 1 d . . . C51 C 0.29845(14) 0.56975(15) -0.12707(16) 0.0281(8) Uani 1 1 d . . . H51 H 0.2872 0.6151 -0.1414 0.034 Uiso 1 1 calc R . . C52 C 0.30790(15) 0.52148(16) -0.17436(16) 0.0301(8) Uani 1 1 d . . . C53 C 0.32569(13) 0.45615(16) -0.15097(15) 0.0289(8) Uani 1 1 d . . . H53 H 0.3328 0.4224 -0.1820 0.035 Uiso 1 1 calc R . . C54 C 0.33363(13) 0.43775(14) -0.08395(16) 0.0232(7) Uani 1 1 d . . . C55 C 0.32184(13) 0.48678(14) -0.03739(15) 0.0198(7) Uani 1 1 d . . . C56 C 0.29808(16) 0.54002(18) -0.24764(15) 0.0478(9) Uani 1 1 d . . . H56A H 0.3017 0.4990 -0.2737 0.072 Uiso 1 1 calc R . . H56B H 0.3367 0.5721 -0.2529 0.072 Uiso 1 1 calc R . . H56C H 0.2494 0.5609 -0.2637 0.072 Uiso 1 1 calc R . . C57 C 0.35240(15) 0.36683(14) -0.06021(16) 0.0325(8) Uani 1 1 d . . . H57A H 0.3577 0.3384 -0.0981 0.049 Uiso 1 1 calc R . . H57B H 0.3128 0.3487 -0.0405 0.049 Uiso 1 1 calc R . . H57C H 0.3990 0.3669 -0.0265 0.049 Uiso 1 1 calc R . . C58 C 0.30877(14) 0.66235(14) 0.09248(15) 0.0238(7) Uani 1 1 d . . . H58A H 0.3154 0.7053 0.0695 0.029 Uiso 1 1 calc R . . H58B H 0.2550 0.6563 0.0889 0.029 Uiso 1 1 calc R . . C59 C 0.34510(14) 0.66985(14) 0.16485(15) 0.0211(7) Uani 1 1 d . . . C60 C 0.37026(14) 0.73266(15) 0.19192(17) 0.0274(8) Uani 1 1 d . . . H60 H 0.3689 0.7705 0.1630 0.033 Uiso 1 1 calc R . . C61 C 0.39714(16) 0.74114(15) 0.25982(18) 0.0301(8) Uani 1 1 d . . . C62 C 0.39865(14) 0.68484(15) 0.30098(16) 0.0304(8) Uani 1 1 d . . . H62 H 0.4168 0.6901 0.3478 0.036 Uiso 1 1 calc R . . C63 C 0.37457(14) 0.62106(15) 0.27611(16) 0.0241(7) Uani 1 1 d . . . C64 C 0.34864(13) 0.61351(15) 0.20714(16) 0.0204(7) Uani 1 1 d . . . C65 C 0.42431(17) 0.80866(15) 0.28889(17) 0.0462(10) Uani 1 1 d . . . H65A H 0.4265 0.8405 0.2527 0.069 Uiso 1 1 calc R . . H65B H 0.4738 0.8034 0.3177 0.069 Uiso 1 1 calc R . . H65C H 0.3904 0.8262 0.3153 0.069 Uiso 1 1 calc R . . C66 C 0.37335(14) 0.56110(14) 0.32177(15) 0.0297(8) Uani 1 1 d . . . H66A H 0.3236 0.5415 0.3127 0.045 Uiso 1 1 calc R . . H66B H 0.3870 0.5761 0.3684 0.045 Uiso 1 1 calc R . . H66C H 0.4087 0.5268 0.3138 0.045 Uiso 1 1 calc R . . C67 C 0.47895(12) 0.46785(14) 0.08337(14) 0.0260(7) Uani 1 1 d . . . H67A H 0.5330 0.4703 0.0958 0.039 Uiso 1 1 calc R . . H67B H 0.4619 0.4803 0.0362 0.039 Uiso 1 1 calc R . . H67C H 0.4630 0.4215 0.0903 0.039 Uiso 1 1 calc R . . C68 C 0.48070(13) 0.49904(14) 0.19593(15) 0.0270(8) Uani 1 1 d . . . H68A H 0.4672 0.4526 0.2056 0.040 Uiso 1 1 calc R . . H68B H 0.4626 0.5308 0.2254 0.040 Uiso 1 1 calc R . . H68C H 0.5346 0.5027 0.2034 0.040 Uiso 1 1 calc R . . C1C C 0.55489(19) 0.4362(2) 0.3764(2) 0.0923(16) Uani 1 1 d . . . H1C1 H 0.5372 0.4738 0.3458 0.138 Uiso 1 1 calc R . . H1C2 H 0.5477 0.3933 0.3517 0.138 Uiso 1 1 calc R . . H1C3 H 0.6076 0.4425 0.3962 0.138 Uiso 1 1 calc R . . C2C C 0.5104(2) 0.4348(2) 0.4333(2) 0.0854(15) Uani 1 1 d . . . H2C1 H 0.4568 0.4308 0.4133 0.103 Uiso 1 1 calc R . . H2C2 H 0.5255 0.3949 0.4624 0.103 Uiso 1 1 calc R . . C3C C 0.52541(18) 0.5000(2) 0.4748(2) 0.0707(13) Uani 1 1 d . . . H3C1 H 0.5149 0.5402 0.4453 0.085 Uiso 1 1 calc R . . H3C2 H 0.5779 0.5017 0.4989 0.085 Uiso 1 1 calc R . . O1D O 0.1545(3) 0.3032(4) 0.6972(3) 0.134(2) Uiso 0.524(2) 1 d PD A 1 C1D C 0.1778(5) 0.3442(4) 0.7571(5) 0.134(2) Uiso 0.524(2) 1 d PD A 1 H1D1 H 0.2139 0.3789 0.7503 0.160 Uiso 0.524(2) 1 calc PR A 1 H1D2 H 0.1347 0.3673 0.7682 0.160 Uiso 0.524(2) 1 calc PR A 1 C2D C 0.2111(5) 0.2987(5) 0.8101(4) 0.134(2) Uiso 0.524(2) 1 d PD A 1 H2D1 H 0.2558 0.3195 0.8384 0.160 Uiso 0.524(2) 1 calc PR A 1 H2D2 H 0.1759 0.2882 0.8386 0.160 Uiso 0.524(2) 1 calc PR A 1 C3D C 0.2293(5) 0.2409(4) 0.7805(5) 0.134(2) Uiso 0.524(2) 1 d PD A 1 H3D1 H 0.2012 0.2019 0.7926 0.160 Uiso 0.524(2) 1 calc PR A 1 H3D2 H 0.2827 0.2313 0.7966 0.160 Uiso 0.524(2) 1 calc PR A 1 C4D C 0.2125(5) 0.2493(4) 0.7096(5) 0.134(2) Uiso 0.524(2) 1 d PD A 1 H4D1 H 0.1935 0.2065 0.6868 0.160 Uiso 0.524(2) 1 calc PR A 1 H4D2 H 0.2569 0.2637 0.6938 0.160 Uiso 0.524(2) 1 calc PR A 1 O1E O 0.3996(4) 0.2865(4) 0.6427(4) 0.052(2) Uiso 0.309(4) 1 d PD B 2 C1E C 0.4152(5) 0.3220(6) 0.7078(5) 0.052(2) Uiso 0.309(4) 1 d PD B 2 H1E1 H 0.4205 0.2887 0.7446 0.063 Uiso 0.309(4) 1 calc PR B 2 H1E2 H 0.4620 0.3477 0.7135 0.063 Uiso 0.309(4) 1 calc PR B 2 C2E C 0.3554(5) 0.3676(5) 0.7098(5) 0.052(2) Uiso 0.309(4) 1 d PD B 2 H2E1 H 0.3232 0.3482 0.7377 0.063 Uiso 0.309(4) 1 calc PR B 2 H2E2 H 0.3749 0.4115 0.7296 0.063 Uiso 0.309(4) 1 calc PR B 2 C3E C 0.3140(5) 0.3775(5) 0.6428(5) 0.052(2) Uiso 0.309(4) 1 d PD B 2 H3E1 H 0.3289 0.4204 0.6244 0.063 Uiso 0.309(4) 1 calc PR B 2 H3E2 H 0.2604 0.3797 0.6418 0.063 Uiso 0.309(4) 1 calc PR B 2 C4E C 0.3304(5) 0.3184(6) 0.6028(5) 0.052(2) Uiso 0.309(4) 1 d PD B 2 H4E1 H 0.3379 0.3336 0.5588 0.063 Uiso 0.309(4) 1 calc PR B 2 H4E2 H 0.2890 0.2855 0.5954 0.063 Uiso 0.309(4) 1 calc PR B 2 O1F O 0.3830(4) 0.3611(4) 0.6025(4) 0.206(3) Uiso 0.617(5) 1 d PD C 3 C1F C 0.3283(6) 0.3036(6) 0.5905(5) 0.206(3) Uiso 0.617(5) 1 d PD C 3 H1F1 H 0.2773 0.3213 0.5838 0.247 Uiso 0.617(5) 1 calc PR C 3 H1F2 H 0.3326 0.2780 0.5500 0.247 Uiso 0.617(5) 1 calc PR C 3 C2F C 0.3449(6) 0.2593(5) 0.6491(6) 0.206(3) Uiso 0.617(5) 1 d PD C 3 H2F1 H 0.3944 0.2381 0.6568 0.247 Uiso 0.617(5) 1 calc PR C 3 H2F2 H 0.3063 0.2249 0.6500 0.247 Uiso 0.617(5) 1 calc PR C 3 C3F C 0.3412(6) 0.3200(6) 0.6937(5) 0.206(3) Uiso 0.617(5) 1 d PD C 3 H3F1 H 0.2926 0.3430 0.6815 0.247 Uiso 0.617(5) 1 calc PR C 3 H3F2 H 0.3515 0.3071 0.7415 0.247 Uiso 0.617(5) 1 calc PR C 3 C4F C 0.4022(6) 0.3634(5) 0.6779(5) 0.206(3) Uiso 0.617(5) 1 d PD C 3 H4F1 H 0.4004 0.4103 0.6948 0.247 Uiso 0.617(5) 1 calc PR C 3 H4F2 H 0.4516 0.3437 0.6963 0.247 Uiso 0.617(5) 1 calc PR C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01619(10) 0.01876(11) 0.01883(13) 0.00284(12) 0.00855(9) 0.00235(10) Al2 0.0241(4) 0.0211(5) 0.0244(6) 0.0016(4) 0.0139(4) 0.0009(4) Al3 0.0174(4) 0.0203(5) 0.0189(6) 0.0019(4) 0.0073(4) 0.0012(4) O1 0.0242(10) 0.0223(12) 0.0223(14) 0.0058(10) 0.0154(10) 0.0026(8) O2 0.0213(10) 0.0218(11) 0.0196(13) 0.0037(10) 0.0129(10) 0.0038(8) O3 0.0301(11) 0.0203(12) 0.0322(15) 0.0031(10) 0.0192(11) -0.0030(9) O4 0.0233(9) 0.0213(11) 0.0225(13) 0.0005(11) 0.0116(9) -0.0032(9) O5 0.0167(9) 0.0239(12) 0.0196(13) 0.0018(9) 0.0113(9) 0.0013(8) O6 0.0195(9) 0.0214(12) 0.0217(13) 0.0016(9) 0.0138(9) -0.0009(8) O7 0.0201(9) 0.0243(12) 0.0170(13) 0.0020(10) 0.0101(9) 0.0019(9) O8 0.0224(9) 0.0185(12) 0.0181(13) -0.0009(9) 0.0083(9) -0.0004(8) N1 0.0220(12) 0.0183(14) 0.0147(15) 0.0021(11) 0.0091(12) 0.0015(10) N2 0.0205(12) 0.0190(14) 0.0220(17) 0.0000(12) 0.0135(12) 0.0007(10) N3 0.0277(13) 0.0245(16) 0.0289(17) 0.0033(12) 0.0161(13) 0.0028(11) N4 0.0272(12) 0.0230(14) 0.0228(17) 0.0020(13) 0.0132(12) 0.0016(11) N5 0.0179(11) 0.0183(13) 0.0143(15) 0.0005(11) 0.0060(11) 0.0008(9) N6 0.0183(12) 0.0190(13) 0.0220(17) -0.0002(12) 0.0124(12) 0.0005(10) N7 0.0181(12) 0.0219(14) 0.0165(16) 0.0006(12) 0.0076(11) -0.0003(10) N8 0.0194(12) 0.0260(15) 0.0186(16) 0.0026(12) 0.0074(12) 0.0011(10) C1 0.0217(14) 0.0154(15) 0.018(2) 0.0011(14) 0.0081(14) -0.0014(12) C2 0.0205(14) 0.0188(16) 0.0176(19) 0.0024(14) 0.0096(14) 0.0030(12) C3 0.0231(15) 0.0156(16) 0.0186(19) 0.0007(14) 0.0081(14) 0.0006(12) C4 0.0310(17) 0.0220(18) 0.024(2) 0.0026(15) 0.0109(16) 0.0036(13) C5 0.0378(18) 0.0277(19) 0.028(2) 0.0080(16) 0.0104(17) 0.0065(14) C6 0.0351(18) 0.0246(18) 0.027(2) 0.0037(16) 0.0041(17) 0.0039(14) C7 0.0274(16) 0.0210(17) 0.022(2) 0.0017(15) 0.0069(15) 0.0036(13) C8 0.0306(17) 0.0248(18) 0.034(2) 0.0058(16) 0.0074(17) 0.0099(14) C9 0.0330(18) 0.0290(19) 0.035(2) 0.0017(17) 0.0166(18) 0.0109(14) C10 0.0327(17) 0.0256(18) 0.025(2) 0.0037(15) 0.0130(16) 0.0056(14) C11 0.0220(15) 0.0172(16) 0.022(2) -0.0023(14) 0.0069(15) 0.0011(12) C12 0.0216(15) 0.0156(16) 0.020(2) -0.0008(14) 0.0056(14) 0.0008(12) C13 0.0402(18) 0.0258(19) 0.023(2) -0.0013(16) 0.0180(16) 0.0001(14) C14 0.0314(17) 0.0254(19) 0.035(2) -0.0041(17) 0.0187(17) -0.0009(14) C15 0.050(2) 0.032(2) 0.023(2) 0.0099(16) 0.0178(18) 0.0133(16) C16 0.058(2) 0.0187(18) 0.036(3) 0.0020(17) 0.034(2) 0.0074(16) C17 0.089(3) 0.024(2) 0.035(3) 0.0047(18) 0.038(2) 0.0132(19) C18 0.119(4) 0.017(2) 0.057(3) -0.001(2) 0.068(3) 0.000(2) C19 0.099(3) 0.023(2) 0.084(4) -0.014(2) 0.074(3) -0.019(2) C20 0.060(2) 0.025(2) 0.056(3) -0.0106(19) 0.046(2) -0.0111(17) C21 0.049(2) 0.0199(18) 0.040(3) -0.0042(17) 0.035(2) 0.0010(15) C22 0.196(5) 0.026(2) 0.073(4) -0.003(2) 0.096(4) -0.016(3) C23 0.058(2) 0.048(3) 0.081(4) -0.017(2) 0.041(3) -0.0296(19) C24 0.0301(17) 0.046(2) 0.026(2) -0.0012(18) 0.0071(16) -0.0024(15) C25 0.0279(17) 0.038(2) 0.032(2) -0.0070(19) 0.0136(17) -0.0078(15) C26 0.043(2) 0.064(3) 0.038(3) -0.016(2) 0.016(2) -0.0231(19) C27 0.072(3) 0.054(3) 0.059(3) -0.032(3) 0.036(3) -0.037(2) C28 0.062(2) 0.030(2) 0.064(3) -0.013(2) 0.039(3) -0.0189(18) C29 0.0320(18) 0.028(2) 0.043(3) -0.0007(18) 0.0229(18) -0.0002(14) C30 0.0209(16) 0.0262(19) 0.031(2) -0.0003(17) 0.0150(16) -0.0004(13) C31 0.147(4) 0.083(4) 0.097(5) -0.057(3) 0.070(4) -0.074(3) C32 0.0328(18) 0.029(2) 0.057(3) 0.0159(19) 0.0227(19) 0.0049(15) C33 0.0320(17) 0.0280(19) 0.038(2) 0.0040(17) 0.0176(17) 0.0051(14) C34 0.0251(16) 0.034(2) 0.040(2) -0.0027(17) 0.0190(16) -0.0012(13) C35 0.0171(13) 0.0166(16) 0.0162(17) -0.0008(14) 0.0060(13) -0.0015(12) C36 0.0162(14) 0.0184(16) 0.0180(19) -0.0010(13) 0.0072(13) 0.0007(11) C37 0.0171(13) 0.0190(15) 0.0232(19) -0.0032(15) 0.0042(13) 0.0010(13) C38 0.0206(14) 0.0267(18) 0.0231(19) -0.0018(15) 0.0075(14) 0.0017(13) C39 0.0176(14) 0.032(2) 0.038(2) -0.0064(17) 0.0100(15) 0.0011(13) C40 0.0181(15) 0.0239(18) 0.033(2) -0.0038(16) 0.0009(15) 0.0039(12) C41 0.0209(15) 0.0148(15) 0.024(2) -0.0037(14) 0.0034(14) 0.0018(12) C42 0.0222(15) 0.0179(17) 0.025(2) -0.0049(15) -0.0016(15) 0.0035(12) C43 0.0311(16) 0.0176(17) 0.024(2) 0.0023(14) 0.0023(15) 0.0017(13) C44 0.0251(15) 0.0190(16) 0.022(2) -0.0022(15) 0.0044(15) -0.0017(12) C45 0.0194(14) 0.0139(15) 0.021(2) -0.0032(13) 0.0058(14) 0.0009(11) C46 0.0166(14) 0.0165(15) 0.022(2) -0.0044(14) 0.0042(14) -0.0002(11) C47 0.0223(15) 0.0260(18) 0.028(2) 0.0042(15) 0.0125(15) -0.0047(13) C48 0.0188(15) 0.0289(19) 0.028(2) -0.0014(16) 0.0109(15) -0.0039(13) C49 0.0268(16) 0.0227(17) 0.019(2) 0.0052(15) 0.0054(15) -0.0009(13) C50 0.0166(14) 0.031(2) 0.0164(19) 0.0019(15) 0.0065(13) -0.0005(12) C51 0.0269(16) 0.0304(19) 0.027(2) 0.0045(17) 0.0070(16) 0.0024(13) C52 0.0290(16) 0.044(2) 0.019(2) 0.0002(17) 0.0098(15) 0.0010(15) C53 0.0248(15) 0.038(2) 0.026(2) -0.0086(18) 0.0111(15) 0.0012(15) C54 0.0185(14) 0.0292(19) 0.024(2) -0.0026(15) 0.0093(15) 0.0003(12) C55 0.0111(13) 0.0284(18) 0.022(2) 0.0028(15) 0.0079(14) -0.0009(12) C56 0.059(2) 0.061(3) 0.026(2) 0.006(2) 0.0162(19) 0.010(2) C57 0.0394(18) 0.030(2) 0.033(2) -0.0051(17) 0.0187(17) 0.0035(15) C58 0.0284(16) 0.0192(17) 0.026(2) 0.0024(15) 0.0114(16) 0.0029(13) C59 0.0227(15) 0.0219(17) 0.021(2) -0.0017(15) 0.0085(15) 0.0026(13) C60 0.0323(17) 0.0219(18) 0.030(2) 0.0017(16) 0.0106(17) -0.0001(13) C61 0.0376(19) 0.0227(19) 0.030(2) -0.0066(17) 0.0081(18) -0.0018(15) C62 0.0343(18) 0.036(2) 0.020(2) -0.0081(17) 0.0048(16) 0.0017(15) C63 0.0232(16) 0.0273(19) 0.024(2) 0.0002(16) 0.0098(15) 0.0036(13) C64 0.0158(14) 0.0248(18) 0.023(2) -0.0030(15) 0.0086(14) 0.0021(12) C65 0.063(2) 0.033(2) 0.039(3) -0.0091(19) 0.001(2) -0.0008(18) C66 0.0313(16) 0.034(2) 0.024(2) 0.0002(16) 0.0082(16) 0.0052(14) C67 0.0194(14) 0.0352(19) 0.027(2) 0.0008(16) 0.0130(14) 0.0049(14) C68 0.0210(15) 0.036(2) 0.025(2) 0.0036(16) 0.0072(15) -0.0001(13) C1C 0.075(3) 0.117(5) 0.079(4) -0.012(3) 0.004(3) 0.004(3) C2C 0.086(3) 0.077(4) 0.082(4) -0.007(3) -0.006(3) 0.003(3) C3C 0.063(3) 0.072(3) 0.061(4) -0.007(3) -0.018(2) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N5 2.011(2) . yes Pd1 N1 2.014(2) . yes Pd1 N6 2.0160(19) . yes Pd1 N2 2.0198(19) . yes Al2 O3 1.8038(18) . ? Al2 O4 1.8133(19) . ? Al2 O6 1.872(2) . ? Al2 O1 1.9126(18) . ? Al2 N3 2.112(3) . ? Al2 N4 2.203(2) . ? Al3 O7 1.807(2) . ? Al3 O8 1.808(2) . ? Al3 O2 1.8900(19) . ? Al3 O5 1.9133(17) . ? Al3 N7 2.124(2) . ? Al3 N8 2.191(2) . ? O1 N1 1.335(2) . ? O2 N2 1.332(2) . ? O3 C21 1.326(3) . ? O4 C30 1.339(3) . ? O5 N5 1.339(2) . ? O6 N6 1.334(2) . ? O7 C55 1.322(3) . ? O8 C64 1.344(3) . ? N1 C1 1.304(3) . ? N2 C2 1.289(3) . ? N3 C13 1.486(3) . ? N3 C24 1.495(3) . ? N3 C15 1.496(3) . ? N4 C14 1.478(4) . ? N4 C33 1.486(3) . ? N4 C34 1.494(3) . ? N5 C35 1.304(3) . ? N6 C36 1.282(3) . ? N7 C49 1.483(3) . ? N7 C47 1.491(3) . ? N7 C58 1.498(3) . ? N8 C68 1.476(3) . ? N8 C67 1.488(3) . ? N8 C48 1.492(3) . ? C1 C3 1.452(4) . ? C1 C2 1.478(3) . ? C2 C11 1.464(3) . ? C3 C4 1.368(4) . ? C3 C12 1.420(3) . ? C4 C5 1.417(4) . ? C5 C6 1.373(3) . ? C6 C7 1.398(4) . ? C7 C12 1.390(4) . ? C7 C8 1.427(3) . ? C8 C9 1.363(4) . ? C9 C10 1.426(4) . ? C10 C11 1.376(3) . ? C11 C12 1.412(4) . ? C13 C14 1.514(4) . ? C15 C16 1.502(4) . ? C16 C17 1.396(4) . ? C16 C21 1.400(4) . ? C17 C18 1.390(4) . ? C18 C19 1.379(5) . ? C18 C22 1.518(5) . ? C19 C20 1.399(5) . ? C20 C21 1.426(4) . ? C20 C23 1.479(5) . ? C24 C25 1.499(4) . ? C25 C26 1.389(4) . ? C25 C30 1.392(4) . ? C26 C27 1.393(5) . ? C27 C28 1.373(5) . ? C27 C31 1.524(5) . ? C28 C29 1.396(4) . ? C29 C30 1.413(4) . ? C29 C32 1.502(4) . ? C35 C45 1.453(4) . ? C35 C36 1.468(3) . ? C36 C37 1.469(3) . ? C37 C38 1.379(3) . ? C37 C46 1.413(4) . ? C38 C39 1.401(4) . ? C39 C40 1.377(4) . ? C40 C41 1.431(3) . ? C41 C46 1.393(4) . ? C41 C42 1.412(4) . ? C42 C43 1.377(3) . ? C43 C44 1.415(4) . ? C44 C45 1.364(4) . ? C45 C46 1.434(3) . ? C47 C48 1.514(4) . ? C49 C50 1.495(4) . ? C50 C51 1.393(4) . ? C50 C55 1.416(4) . ? C51 C52 1.398(4) . ? C52 C53 1.388(4) . ? C52 C56 1.518(4) . ? C53 C54 1.398(4) . ? C54 C55 1.410(4) . ? C54 C57 1.496(4) . ? C58 C59 1.496(4) . ? C59 C60 1.394(4) . ? C59 C64 1.402(4) . ? C60 C61 1.382(4) . ? C61 C62 1.391(4) . ? C61 C65 1.499(4) . ? C62 C63 1.393(4) . ? C63 C64 1.398(4) . ? C63 C66 1.512(4) . ? C1C C2C 1.572(5) . ? C2C C3C 1.534(5) . ? C3C C3C 1.545(6) 3_666 ? O1D C1D 1.453(7) . ? O1D C4D 1.494(7) . ? C1D C2D 1.438(7) . ? C2D C3D 1.369(7) . ? C3D C4D 1.427(7) . ? O1E C1E 1.478(7) . ? O1E C4E 1.499(8) . ? C1E C2E 1.436(7) . ? C2E C3E 1.432(7) . ? C3E C4E 1.496(7) . ? O1F C1F 1.507(8) . ? O1F C4F 1.508(7) . ? C1F C2F 1.463(8) . ? C2F C3F 1.516(7) . ? C3F C4F 1.510(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Pd1 N1 177.77(9) . . yes N5 Pd1 N6 81.68(9) . . yes N1 Pd1 N6 97.86(9) . . yes N5 Pd1 N2 98.33(9) . . yes N1 Pd1 N2 81.77(9) . . yes N6 Pd1 N2 170.67(9) . . yes O3 Al2 O4 178.20(10) . . ? O3 Al2 O6 87.70(9) . . ? O4 Al2 O6 90.89(9) . . ? O3 Al2 O1 89.34(8) . . ? O4 Al2 O1 92.01(8) . . ? O6 Al2 O1 99.69(8) . . ? O3 Al2 N3 89.30(9) . . ? O4 Al2 N3 91.90(9) . . ? O6 Al2 N3 169.99(8) . . ? O1 Al2 N3 89.82(9) . . ? O3 Al2 N4 89.26(8) . . ? O4 Al2 N4 89.56(8) . . ? O6 Al2 N4 87.94(9) . . ? O1 Al2 N4 172.17(10) . . ? N3 Al2 N4 82.46(9) . . ? O7 Al3 O8 178.34(10) . . ? O7 Al3 O2 88.10(9) . . ? O8 Al3 O2 90.46(9) . . ? O7 Al3 O5 89.57(8) . . ? O8 Al3 O5 91.46(8) . . ? O2 Al3 O5 98.48(8) . . ? O7 Al3 N7 89.31(9) . . ? O8 Al3 N7 92.00(9) . . ? O2 Al3 N7 171.49(8) . . ? O5 Al3 N7 89.60(8) . . ? O7 Al3 N8 89.84(8) . . ? O8 Al3 N8 89.32(9) . . ? O2 Al3 N8 88.92(8) . . ? O5 Al3 N8 172.55(9) . . ? N7 Al3 N8 82.97(8) . . ? N1 O1 Al2 121.30(15) . . ? N2 O2 Al3 117.90(14) . . ? C21 O3 Al2 135.8(2) . . ? C30 O4 Al2 132.05(18) . . ? N5 O5 Al3 119.31(15) . . ? N6 O6 Al2 117.89(14) . . ? C55 O7 Al3 135.74(19) . . ? C64 O8 Al3 133.49(18) . . ? C1 N1 O1 119.5(2) . . ? C1 N1 Pd1 112.35(18) . . ? O1 N1 Pd1 128.11(15) . . ? C2 N2 O2 120.8(2) . . ? C2 N2 Pd1 112.34(17) . . ? O2 N2 Pd1 126.40(17) . . ? C13 N3 C24 111.2(2) . . ? C13 N3 C15 109.0(2) . . ? C24 N3 C15 105.8(2) . . ? C13 N3 Al2 109.48(17) . . ? C24 N3 Al2 110.41(17) . . ? C15 N3 Al2 110.85(18) . . ? C14 N4 C33 108.5(2) . . ? C14 N4 C34 109.8(2) . . ? C33 N4 C34 106.4(2) . . ? C14 N4 Al2 106.90(16) . . ? C33 N4 Al2 113.56(15) . . ? C34 N4 Al2 111.60(16) . . ? C35 N5 O5 119.5(2) . . ? C35 N5 Pd1 112.42(17) . . ? O5 N5 Pd1 127.69(15) . . ? C36 N6 O6 120.3(2) . . ? C36 N6 Pd1 111.87(17) . . ? O6 N6 Pd1 126.94(17) . . ? C49 N7 C47 109.4(2) . . ? C49 N7 C58 105.9(2) . . ? C47 N7 C58 110.9(2) . . ? C49 N7 Al3 111.11(16) . . ? C47 N7 Al3 108.80(16) . . ? C58 N7 Al3 110.76(16) . . ? C68 N8 C67 107.0(2) . . ? C68 N8 C48 108.2(2) . . ? C67 N8 C48 110.6(2) . . ? C68 N8 Al3 112.92(15) . . ? C67 N8 Al3 111.84(16) . . ? C48 N8 Al3 106.24(15) . . ? N1 C1 C3 135.3(3) . . ? N1 C1 C2 116.4(2) . . ? C3 C1 C2 108.3(2) . . ? N2 C2 C11 136.0(2) . . ? N2 C2 C1 116.8(2) . . ? C11 C2 C1 107.0(2) . . ? C4 C3 C12 118.7(3) . . ? C4 C3 C1 135.7(2) . . ? C12 C3 C1 105.6(2) . . ? C3 C4 C5 118.5(3) . . ? C6 C5 C4 122.2(3) . . ? C5 C6 C7 120.4(3) . . ? C12 C7 C6 117.1(3) . . ? C12 C7 C8 115.5(3) . . ? C6 C7 C8 127.4(3) . . ? C9 C8 C7 121.2(3) . . ? C8 C9 C10 122.3(3) . . ? C11 C10 C9 117.8(3) . . ? C10 C11 C12 119.3(3) . . ? C10 C11 C2 134.6(3) . . ? C12 C11 C2 106.1(2) . . ? C7 C12 C11 124.0(2) . . ? C7 C12 C3 123.0(3) . . ? C11 C12 C3 113.0(2) . . ? N3 C13 C14 112.1(2) . . ? N4 C14 C13 111.2(2) . . ? N3 C15 C16 115.4(2) . . ? C17 C16 C21 120.2(3) . . ? C17 C16 C15 119.2(3) . . ? C21 C16 C15 120.5(3) . . ? C18 C17 C16 121.6(4) . . ? C19 C18 C17 117.2(3) . . ? C19 C18 C22 122.2(4) . . ? C17 C18 C22 120.6(4) . . ? C18 C19 C20 124.5(4) . . ? C19 C20 C21 116.9(4) . . ? C19 C20 C23 123.1(3) . . ? C21 C20 C23 120.0(3) . . ? O3 C21 C16 122.6(3) . . ? O3 C21 C20 117.7(3) . . ? C16 C21 C20 119.7(3) . . ? N3 C24 C25 115.4(3) . . ? C26 C25 C30 120.2(3) . . ? C26 C25 C24 121.0(3) . . ? C30 C25 C24 118.8(3) . . ? C25 C26 C27 120.4(4) . . ? C28 C27 C26 119.1(3) . . ? C28 C27 C31 120.6(4) . . ? C26 C27 C31 120.3(4) . . ? C27 C28 C29 122.2(4) . . ? C28 C29 C30 118.2(4) . . ? C28 C29 C32 122.2(3) . . ? C30 C29 C32 119.6(3) . . ? O4 C30 C25 120.4(3) . . ? O4 C30 C29 119.8(3) . . ? C25 C30 C29 119.8(3) . . ? N5 C35 C45 135.5(2) . . ? N5 C35 C36 115.7(2) . . ? C45 C35 C36 108.6(2) . . ? N6 C36 C35 117.8(2) . . ? N6 C36 C37 134.5(2) . . ? C35 C36 C37 107.5(2) . . ? C38 C37 C46 119.3(2) . . ? C38 C37 C36 134.8(3) . . ? C46 C37 C36 105.7(2) . . ? C37 C38 C39 117.7(3) . . ? C40 C39 C38 123.6(2) . . ? C39 C40 C41 119.8(3) . . ? C46 C41 C42 116.8(2) . . ? C46 C41 C40 115.8(3) . . ? C42 C41 C40 127.3(3) . . ? C43 C42 C41 120.3(3) . . ? C42 C43 C44 122.4(3) . . ? C45 C44 C43 118.7(2) . . ? C44 C45 C46 118.8(3) . . ? C44 C45 C35 135.8(2) . . ? C46 C45 C35 105.2(2) . . ? C41 C46 C37 123.9(2) . . ? C41 C46 C45 122.9(3) . . ? C37 C46 C45 113.0(2) . . ? N7 C47 C48 111.6(2) . . ? N8 C48 C47 111.1(2) . . ? N7 C49 C50 115.7(2) . . ? C51 C50 C55 119.6(3) . . ? C51 C50 C49 119.8(3) . . ? C55 C50 C49 120.4(3) . . ? C50 C51 C52 122.7(3) . . ? C53 C52 C51 116.6(3) . . ? C53 C52 C56 122.2(3) . . ? C51 C52 C56 121.2(3) . . ? C52 C53 C54 123.1(3) . . ? C53 C54 C55 119.4(3) . . ? C53 C54 C57 121.9(3) . . ? C55 C54 C57 118.7(3) . . ? O7 C55 C54 118.8(3) . . ? O7 C55 C50 122.6(3) . . ? C54 C55 C50 118.6(3) . . ? C59 C58 N7 116.7(2) . . ? C60 C59 C64 119.4(3) . . ? C60 C59 C58 121.4(3) . . ? C64 C59 C58 119.0(3) . . ? C61 C60 C59 121.5(3) . . ? C60 C61 C62 118.0(3) . . ? C60 C61 C65 121.5(3) . . ? C62 C61 C65 120.5(3) . . ? C61 C62 C63 122.4(3) . . ? C62 C63 C64 118.5(3) . . ? C62 C63 C66 121.8(3) . . ? C64 C63 C66 119.7(3) . . ? O8 C64 C63 119.4(3) . . ? O8 C64 C59 120.6(3) . . ? C63 C64 C59 120.0(3) . . ? C3C C2C C1C 109.7(3) . . ? C2C C3C C3C 108.0(4) . 3_666 ? C1D O1D C4D 100.6(6) . . ? C2D C1D O1D 106.9(7) . . ? C3D C2D C1D 106.9(7) . . ? C2D C3D C4D 109.6(7) . . ? C3D C4D O1D 104.0(6) . . ? C1E O1E C4E 105.5(6) . . ? C2E C1E O1E 109.0(7) . . ? C3E C2E C1E 108.1(7) . . ? C2E C3E C4E 106.9(7) . . ? C3E C4E O1E 106.3(6) . . ? C1F O1F C4F 100.8(6) . . ? C2F C1F O1F 107.6(8) . . ? C1F C2F C3F 89.8(7) . . ? C4F C3F C2F 100.5(8) . . ? O1F C4F C3F 100.7(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.745 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.085 # Attachment '- mrr26_sad.cif' data_mrr26_sad _database_code_depnum_ccdc_archive 'CCDC 867795' #TrackingRef '- mrr26_sad.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H70 Al2 N8 O8' _chemical_formula_sum 'C68 H70 Al2 N8 O8' _chemical_formula_weight 1181.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0569(6) _cell_length_b 18.5625(10) _cell_length_c 18.9548(11) _cell_angle_alpha 78.418(3) _cell_angle_beta 76.313(3) _cell_angle_gamma 76.094(3) _cell_volume 3954.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9451 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 36.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8200 _exptl_absorpt_correction_T_max 0.8626 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 143111 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 30.00 _reflns_number_total 22895 _reflns_number_gt 17531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+0.1146P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22895 _refine_ls_number_parameters 818 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.14821(3) 1.058454(19) 0.169602(19) 0.01929(8) Uani 1 1 d . . . Al2 Al 0.31387(3) 0.69175(2) 0.38533(2) 0.02404(9) Uani 1 1 d . . . C4 C 0.17517(11) 1.12750(8) 0.01281(7) 0.0286(3) Uani 1 1 d . . . C5 C 0.31330(11) 1.15088(7) 0.07826(7) 0.0274(2) Uani 1 1 d . . . H5A H 0.3650 1.1263 0.1135 0.033 Uiso 1 1 calc R A 1 H5B H 0.3635 1.1656 0.0306 0.033 Uiso 1 1 calc R A 1 C6 C 0.23765(12) 1.22076(7) 0.10512(7) 0.0289(3) Uani 1 1 d . F . C7 C 0.26771(16) 1.29031(9) 0.07512(9) 0.0445(4) Uani 1 1 d . . . H7 H 0.3321 1.2929 0.0352 0.053 Uiso 1 1 calc R F . C8 C 0.20575(19) 1.35580(9) 0.10228(10) 0.0526(5) Uani 1 1 d . F . C9 C 0.10994(16) 1.35012(8) 0.15919(9) 0.0419(4) Uani 1 1 d . . . H9 H 0.0661 1.3945 0.1779 0.050 Uiso 1 1 calc R F . C10 C 0.07546(12) 1.28263(7) 0.18991(7) 0.0289(3) Uani 1 1 d . F . C11 C 0.14125(11) 1.21625(7) 0.16367(7) 0.0241(2) Uani 1 1 d . . . C12 C 0.2439(3) 1.42983(12) 0.07211(14) 0.0845(9) Uani 1 1 d . . . H12A H 0.1759 1.4692 0.0634 0.127 Uiso 1 1 calc R F . H12B H 0.3003 1.4253 0.0258 0.127 Uiso 1 1 calc R . . H12C H 0.2802 1.4430 0.1076 0.127 Uiso 1 1 calc R . . C13 C -0.03069(13) 1.27908(8) 0.25024(8) 0.0345(3) Uani 1 1 d . . . H13A H -0.0407 1.3182 0.2804 0.052 Uiso 1 1 calc R F . H13B H -0.0208 1.2297 0.2810 0.052 Uiso 1 1 calc R . . H13C H -0.0997 1.2870 0.2286 0.052 Uiso 1 1 calc R . . C14 C 0.34348(10) 1.03025(7) 0.04273(7) 0.0250(2) Uani 1 1 d . . . H14A H 0.3961 1.0138 0.0784 0.030 Uiso 1 1 calc R B 1 H14B H 0.3899 1.0493 -0.0049 0.030 Uiso 1 1 calc R B 1 C15 C 0.30388(10) 0.96270(7) 0.03312(7) 0.0242(2) Uani 1 1 d . F . C16 C 0.35640(11) 0.92705(8) -0.02845(7) 0.0279(3) Uani 1 1 d . . . H16 H 0.4084 0.9502 -0.0672 0.034 Uiso 1 1 calc R F . C17 C 0.33423(11) 0.85852(8) -0.03407(8) 0.0311(3) Uani 1 1 d . F . C18 C 0.25650(11) 0.82696(8) 0.02297(8) 0.0301(3) Uani 1 1 d . . . H18 H 0.2405 0.7802 0.0198 0.036 Uiso 1 1 calc R F . C19 C 0.20070(11) 0.86082(7) 0.08485(7) 0.0264(2) Uani 1 1 d . F . C20 C 0.22431(10) 0.93026(7) 0.08981(7) 0.0225(2) Uani 1 1 d . . . C21 C 0.39359(14) 0.81940(10) -0.09971(9) 0.0416(4) Uani 1 1 d . . . H21A H 0.4766 0.8012 -0.0986 0.062 Uiso 1 1 calc R F . H21B H 0.3849 0.8548 -0.1450 0.062 Uiso 1 1 calc R . . H21C H 0.3578 0.7768 -0.0982 0.062 Uiso 1 1 calc R . . C22 C 0.12143(13) 0.82369(8) 0.14759(8) 0.0330(3) Uani 1 1 d . . . H22A H 0.1150 0.7758 0.1361 0.050 Uiso 1 1 calc R F . H22B H 0.0441 0.8565 0.1553 0.050 Uiso 1 1 calc R . . H22C H 0.1535 0.8145 0.1923 0.050 Uiso 1 1 calc R . . C23 C 0.01831(9) 0.93696(6) 0.35285(6) 0.0190(2) Uani 1 1 d . . . C24 C 0.04879(9) 0.85878(6) 0.39021(6) 0.0202(2) Uani 1 1 d . F . C25 C -0.06095(9) 0.98199(6) 0.40617(6) 0.0190(2) Uani 1 1 d . . . C26 C -0.07969(9) 0.93134(6) 0.47243(6) 0.0201(2) Uani 1 1 d . . . C27 C -0.01979(10) 0.85646(7) 0.46553(7) 0.0219(2) Uani 1 1 d . F . C28 C -0.03005(11) 0.80213(7) 0.52640(7) 0.0283(3) Uani 1 1 d . . . H28 H 0.0085 0.7514 0.5238 0.034 Uiso 1 1 calc R F . C29 C -0.09985(13) 0.82390(8) 0.59331(8) 0.0337(3) Uani 1 1 d . . . H29 H -0.1097 0.7862 0.6350 0.040 Uiso 1 1 calc R . . C30 C -0.15369(12) 0.89678(8) 0.60056(7) 0.0313(3) Uani 1 1 d . . . H30 H -0.1972 0.9089 0.6469 0.038 Uiso 1 1 calc R F . C31 C -0.14433(10) 0.95426(7) 0.53860(7) 0.0239(2) Uani 1 1 d . . . C32 C -0.19051(10) 1.03222(8) 0.53584(7) 0.0265(2) Uani 1 1 d . . . H32 H -0.2334 1.0510 0.5796 0.032 Uiso 1 1 calc R F . C33 C -0.17462(10) 1.08142(7) 0.47125(7) 0.0253(2) Uani 1 1 d . . . H33 H -0.2086 1.1332 0.4715 0.030 Uiso 1 1 calc R . . C34 C -0.10925(10) 1.05746(7) 0.40443(7) 0.0219(2) Uani 1 1 d . . . H34 H -0.0991 1.0920 0.3602 0.026 Uiso 1 1 calc R F . C38 C 0.36508(12) 0.53003(7) 0.37702(10) 0.0389(4) Uani 1 1 d . . . H38A H 0.3561 0.4912 0.3510 0.047 Uiso 1 1 calc R C 1 H38B H 0.3651 0.5076 0.4290 0.047 Uiso 1 1 calc R C 1 C39 C 0.22040(12) 0.60655(8) 0.30364(8) 0.0324(3) Uani 1 1 d . . . H39A H 0.1479 0.6455 0.3076 0.039 Uiso 1 1 calc R D 1 H39B H 0.1993 0.5593 0.2998 0.039 Uiso 1 1 calc R D 1 C40 C 0.30141(13) 0.62926(8) 0.23349(9) 0.0345(3) Uani 1 1 d . . . C41 C 0.31771(19) 0.59520(10) 0.17154(11) 0.0571(5) Uani 1 1 d . . . H41 H 0.2851 0.5524 0.1758 0.068 Uiso 1 1 calc R G . C42 C 0.3800(2) 0.62194(11) 0.10388(12) 0.0663(6) Uani 1 1 d . . . C43 C 0.42796(16) 0.68387(9) 0.09956(10) 0.0467(4) Uani 1 1 d . . . H43 H 0.4710 0.7029 0.0536 0.056 Uiso 1 1 calc R G . C44 C 0.41549(11) 0.71925(7) 0.15985(8) 0.0315(3) Uani 1 1 d . . . C45 C 0.35238(10) 0.69104(7) 0.22783(8) 0.0269(3) Uani 1 1 d . . . C46 C 0.3995(4) 0.58433(19) 0.03707(16) 0.1273(17) Uani 1 1 d . . . H46A H 0.4537 0.6075 -0.0032 0.191 Uiso 1 1 calc R G . H46B H 0.3251 0.5903 0.0220 0.191 Uiso 1 1 calc R . . H46C H 0.4326 0.5308 0.0490 0.191 Uiso 1 1 calc R . . C47 C 0.46282(13) 0.78880(8) 0.15289(9) 0.0351(3) Uani 1 1 d . . . H47A H 0.5025 0.8018 0.1020 0.053 Uiso 1 1 calc R G . H47B H 0.5183 0.7796 0.1856 0.053 Uiso 1 1 calc R . . H47C H 0.3986 0.8304 0.1665 0.053 Uiso 1 1 calc R . . C48 C 0.16393(11) 0.57868(7) 0.43366(8) 0.0306(3) Uani 1 1 d . . . H48A H 0.0964 0.6207 0.4287 0.037 Uiso 1 1 calc R E 1 H48B H 0.1423 0.5329 0.4265 0.037 Uiso 1 1 calc R E 1 C49 C 0.18448(11) 0.56763(7) 0.51058(8) 0.0300(3) Uani 1 1 d . . . C50 C 0.13231(12) 0.51526(8) 0.56405(9) 0.0355(3) Uani 1 1 d . . . H50 H 0.0925 0.4841 0.5495 0.043 Uiso 1 1 calc R G . C51 C 0.13721(12) 0.50759(8) 0.63783(9) 0.0368(3) Uani 1 1 d . . . C52 C 0.19795(12) 0.55333(8) 0.65715(9) 0.0345(3) Uani 1 1 d . . . H52 H 0.2020 0.5490 0.7073 0.041 Uiso 1 1 calc R G . C53 C 0.25269(11) 0.60500(7) 0.60585(8) 0.0313(3) Uani 1 1 d . . . C54 C 0.24581(10) 0.61291(7) 0.53106(8) 0.0281(3) Uani 1 1 d . . . C55 C 0.07609(15) 0.45356(10) 0.69592(11) 0.0495(4) Uani 1 1 d . . . H55A H 0.1283 0.4262 0.7293 0.074 Uiso 1 1 calc R G . H55B H 0.0549 0.4178 0.6723 0.074 Uiso 1 1 calc R . . H55C H 0.0055 0.4816 0.7238 0.074 Uiso 1 1 calc R . . C56 C 0.31719(14) 0.65394(9) 0.62763(9) 0.0393(3) Uani 1 1 d . . . H56A H 0.3160 0.6413 0.6805 0.059 Uiso 1 1 calc R G . H56B H 0.2797 0.7067 0.6161 0.059 Uiso 1 1 calc R . . H56C H 0.3981 0.6458 0.6006 0.059 Uiso 1 1 calc R . . C57 C 0.38559(10) 0.95934(6) 0.28952(6) 0.0199(2) Uani 1 1 d . . . C58 C 0.41511(9) 0.88836(6) 0.33952(6) 0.0198(2) Uani 1 1 d . F . C59 C 0.49057(10) 0.89904(7) 0.38453(6) 0.0211(2) Uani 1 1 d . . . C60 C 0.50792(10) 0.97351(7) 0.36057(6) 0.0210(2) Uani 1 1 d . F . C61 C 0.44665(10) 1.01256(6) 0.30449(6) 0.0211(2) Uani 1 1 d . F . C62 C 0.45203(12) 1.08666(7) 0.27876(7) 0.0272(3) Uani 1 1 d . . . H62 H 0.4103 1.1149 0.2421 0.033 Uiso 1 1 calc R F . C63 C 0.52173(13) 1.11965(8) 0.30859(8) 0.0329(3) Uani 1 1 d . . . H63 H 0.5267 1.1706 0.2906 0.039 Uiso 1 1 calc R . . C64 C 0.58223(13) 1.08130(8) 0.36219(8) 0.0319(3) Uani 1 1 d . . . H64 H 0.6288 1.1056 0.3799 0.038 Uiso 1 1 calc R F . C65 C 0.57547(11) 1.00550(7) 0.39134(7) 0.0259(2) Uani 1 1 d . F . C66 C 0.62821(12) 0.95863(8) 0.44812(8) 0.0317(3) Uani 1 1 d . . . H66 H 0.6758 0.9775 0.4704 0.038 Uiso 1 1 calc R F . C67 C 0.61170(12) 0.88621(8) 0.47156(8) 0.0315(3) Uani 1 1 d . F . H67 H 0.6483 0.8563 0.5099 0.038 Uiso 1 1 calc R . . C68 C 0.54176(11) 0.85472(7) 0.44031(7) 0.0262(2) Uani 1 1 d . F . H68 H 0.5307 0.8047 0.4574 0.031 Uiso 1 1 calc R . . C1A C -0.0264(3) 1.0375(2) 0.0813(2) 0.0315(8) Uani 0.450(3) 1 d P F 1 H1A1 H -0.0911 1.0606 0.0558 0.047 Uiso 0.450(3) 1 calc PR F 1 H1A2 H -0.0517 1.0006 0.1232 0.047 Uiso 0.450(3) 1 calc PR F 1 H1A3 H 0.0393 1.0123 0.0473 0.047 Uiso 0.450(3) 1 calc PR F 1 C2A C -0.1040(3) 1.13484(19) 0.15532(19) 0.0301(7) Uani 0.450(3) 1 d P F 1 H2A1 H -0.1613 1.1605 0.1247 0.045 Uiso 0.450(3) 1 calc PR F 1 H2A2 H -0.0828 1.1718 0.1774 0.045 Uiso 0.450(3) 1 calc PR F 1 H2A3 H -0.1376 1.0983 0.1943 0.045 Uiso 0.450(3) 1 calc PR F 1 C3A C 0.0470(2) 1.15190(16) 0.04768(15) 0.0254(7) Uani 0.450(3) 1 d P F 1 H3A1 H 0.0361 1.1986 0.0683 0.030 Uiso 0.450(3) 1 calc PR F 1 H3A2 H -0.0011 1.1624 0.0096 0.030 Uiso 0.450(3) 1 calc PR F 1 C1B C -0.0643(3) 1.03406(17) 0.1185(2) 0.0333(6) Uani 0.550(3) 1 d P F 2 H1B1 H -0.1199 1.0493 0.0854 0.050 Uiso 0.550(3) 1 calc PR F 2 H1B2 H -0.1070 1.0287 0.1696 0.050 Uiso 0.550(3) 1 calc PR F 2 H1B3 H -0.0134 0.9859 0.1086 0.050 Uiso 0.550(3) 1 calc PR F 2 C2B C -0.0666(2) 1.16346(15) 0.11533(16) 0.0305(6) Uani 0.550(3) 1 d P F 2 H2B1 H -0.1254 1.1731 0.0848 0.046 Uiso 0.550(3) 1 calc PR F 2 H2B2 H -0.0210 1.2031 0.1005 0.046 Uiso 0.550(3) 1 calc PR F 2 H2B3 H -0.1055 1.1630 0.1670 0.046 Uiso 0.550(3) 1 calc PR F 2 C3B C 0.07353(19) 1.09387(13) 0.02543(12) 0.0248(5) Uani 0.550(3) 1 d P F 2 H3B1 H 0.0983 1.0419 0.0141 0.030 Uiso 0.550(3) 1 calc PR F 2 H3B2 H 0.0205 1.1230 -0.0076 0.030 Uiso 0.550(3) 1 calc PR F 2 C35 C 0.57886(13) 0.65739(9) 0.31966(10) 0.0444(4) Uani 1 1 d . G 1 H35A H 0.6548 0.6228 0.3150 0.067 Uiso 1 1 calc R G 1 H35B H 0.5839 0.7021 0.3379 0.067 Uiso 1 1 calc R G 1 H35C H 0.5565 0.6722 0.2715 0.067 Uiso 1 1 calc R G 1 C36 C 0.53345(14) 0.59585(10) 0.44137(10) 0.0457(4) Uani 1 1 d . G 1 H36A H 0.4821 0.5664 0.4773 0.069 Uiso 1 1 calc R G 1 H36B H 0.5355 0.6404 0.4609 0.069 Uiso 1 1 calc R G 1 H36C H 0.6123 0.5652 0.4317 0.069 Uiso 1 1 calc R G 1 C37 C 0.47982(13) 0.55399(8) 0.34283(11) 0.0426(4) Uani 1 1 d . G 1 H37A H 0.5449 0.5117 0.3527 0.051 Uiso 1 1 calc R G 1 H37B H 0.4864 0.5669 0.2889 0.051 Uiso 1 1 calc R G 1 N10 N 0.00841(9) 1.09296(6) 0.10630(6) 0.0265(2) Uani 1 1 d . F 1 N11 N 0.24979(9) 1.09422(6) 0.06840(6) 0.0224(2) Uani 1 1 d . F 1 N12 N 0.30752(8) 0.96639(5) 0.25045(6) 0.02109(19) Uani 1 1 d . F 1 N13 N 0.37072(9) 0.83087(5) 0.34326(6) 0.0237(2) Uani 1 1 d . F 1 N14 N 0.26470(9) 0.59499(6) 0.37325(7) 0.0283(2) Uani 1 1 d . G 1 N15 N 0.48909(9) 0.61918(6) 0.37255(7) 0.0299(2) Uani 1 1 d . G 1 N16 N 0.06239(8) 0.95939(5) 0.28538(5) 0.02042(19) Uani 1 1 d . F 1 N17 N 0.13463(9) 0.81214(5) 0.35787(6) 0.0228(2) Uani 1 1 d . F 1 O1 O 0.11040(7) 1.15147(5) 0.19350(5) 0.02331(17) Uani 1 1 d . F 1 O2 O 0.17047(7) 0.96350(5) 0.14845(5) 0.02199(17) Uani 1 1 d . F 1 O3 O 0.28117(7) 1.03579(5) 0.21265(5) 0.02302(17) Uani 1 1 d . F 1 O4 O 0.38395(8) 0.77043(5) 0.39488(5) 0.02757(19) Uani 1 1 d . F 1 O5 O 0.29889(8) 0.66258(5) 0.48292(5) 0.0286(2) Uani 1 1 d . G 1 O6 O 0.34089(7) 0.72330(5) 0.28670(5) 0.02525(18) Uani 1 1 d . G 1 O7 O 0.04003(7) 1.03150(5) 0.25502(5) 0.02314(17) Uani 1 1 d . F 1 O8 O 0.15818(7) 0.74431(5) 0.40003(5) 0.02610(19) Uani 1 1 d . F 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.01855(16) 0.01921(16) 0.01989(17) -0.00311(12) -0.00611(12) -0.00107(12) Al2 0.01768(16) 0.01623(16) 0.0369(2) 0.00054(14) -0.00796(14) -0.00223(12) C4 0.0268(6) 0.0338(6) 0.0223(6) -0.0019(5) -0.0082(5) 0.0005(5) C5 0.0260(6) 0.0282(6) 0.0290(6) -0.0059(5) -0.0018(5) -0.0098(5) C6 0.0340(6) 0.0256(6) 0.0292(6) -0.0060(5) -0.0051(5) -0.0095(5) C7 0.0552(10) 0.0345(7) 0.0441(9) -0.0106(6) 0.0081(7) -0.0235(7) C8 0.0790(13) 0.0295(7) 0.0498(10) -0.0093(7) 0.0041(9) -0.0257(8) C9 0.0603(10) 0.0243(6) 0.0417(8) -0.0116(6) -0.0062(7) -0.0084(6) C10 0.0366(7) 0.0234(6) 0.0279(6) -0.0068(5) -0.0103(5) -0.0021(5) C11 0.0292(6) 0.0213(5) 0.0244(6) -0.0039(4) -0.0105(5) -0.0046(4) C12 0.130(2) 0.0378(10) 0.0803(16) -0.0186(10) 0.0258(15) -0.0435(13) C13 0.0384(7) 0.0276(6) 0.0351(7) -0.0106(5) -0.0066(6) 0.0021(5) C14 0.0190(5) 0.0276(6) 0.0278(6) -0.0073(5) -0.0034(4) -0.0022(4) C15 0.0194(5) 0.0258(6) 0.0275(6) -0.0077(5) -0.0071(4) 0.0010(4) C16 0.0200(5) 0.0331(6) 0.0303(6) -0.0113(5) -0.0052(5) 0.0008(5) C17 0.0233(6) 0.0347(7) 0.0369(7) -0.0174(6) -0.0086(5) 0.0038(5) C18 0.0279(6) 0.0269(6) 0.0383(7) -0.0130(5) -0.0109(5) -0.0002(5) C19 0.0239(6) 0.0245(6) 0.0319(6) -0.0067(5) -0.0098(5) -0.0006(4) C20 0.0185(5) 0.0238(5) 0.0257(6) -0.0062(4) -0.0081(4) 0.0005(4) C21 0.0330(7) 0.0491(9) 0.0464(9) -0.0288(7) -0.0020(6) -0.0033(6) C22 0.0370(7) 0.0253(6) 0.0385(8) -0.0076(5) -0.0076(6) -0.0072(5) C23 0.0165(5) 0.0193(5) 0.0223(5) -0.0040(4) -0.0064(4) -0.0026(4) C24 0.0175(5) 0.0190(5) 0.0253(6) -0.0020(4) -0.0082(4) -0.0033(4) C25 0.0161(5) 0.0202(5) 0.0223(5) -0.0048(4) -0.0057(4) -0.0038(4) C26 0.0171(5) 0.0239(5) 0.0222(5) -0.0033(4) -0.0076(4) -0.0064(4) C27 0.0195(5) 0.0224(5) 0.0259(6) -0.0020(4) -0.0084(4) -0.0058(4) C28 0.0286(6) 0.0261(6) 0.0315(7) 0.0021(5) -0.0106(5) -0.0088(5) C29 0.0364(7) 0.0385(7) 0.0261(6) 0.0051(5) -0.0091(5) -0.0131(6) C30 0.0294(6) 0.0429(7) 0.0235(6) -0.0032(5) -0.0055(5) -0.0124(6) C31 0.0196(5) 0.0330(6) 0.0230(6) -0.0068(5) -0.0070(4) -0.0078(4) C32 0.0207(5) 0.0352(7) 0.0279(6) -0.0146(5) -0.0051(4) -0.0052(5) C33 0.0197(5) 0.0251(6) 0.0350(7) -0.0127(5) -0.0082(5) -0.0023(4) C34 0.0192(5) 0.0211(5) 0.0271(6) -0.0049(4) -0.0079(4) -0.0032(4) C38 0.0248(6) 0.0171(6) 0.0667(10) -0.0021(6) -0.0009(6) -0.0005(5) C39 0.0292(6) 0.0275(6) 0.0433(8) -0.0103(5) -0.0016(6) -0.0122(5) C40 0.0336(7) 0.0259(6) 0.0439(8) -0.0123(6) 0.0016(6) -0.0094(5) C41 0.0765(13) 0.0408(9) 0.0566(11) -0.0256(8) 0.0158(9) -0.0306(9) C42 0.0930(16) 0.0486(10) 0.0565(12) -0.0323(9) 0.0263(11) -0.0335(11) C43 0.0521(9) 0.0337(8) 0.0469(9) -0.0130(7) 0.0139(7) -0.0124(7) C44 0.0244(6) 0.0244(6) 0.0426(8) -0.0047(5) -0.0031(5) -0.0033(5) C45 0.0199(5) 0.0196(5) 0.0390(7) -0.0066(5) -0.0042(5) 0.0005(4) C46 0.215(4) 0.103(2) 0.0741(17) -0.0644(17) 0.067(2) -0.104(3) C47 0.0339(7) 0.0315(7) 0.0400(8) 0.0045(6) -0.0096(6) -0.0129(6) C48 0.0204(5) 0.0249(6) 0.0449(8) -0.0013(5) -0.0042(5) -0.0073(5) C49 0.0206(5) 0.0213(6) 0.0435(8) 0.0012(5) -0.0047(5) -0.0021(4) C50 0.0227(6) 0.0280(6) 0.0513(9) 0.0018(6) -0.0039(6) -0.0065(5) C51 0.0238(6) 0.0304(7) 0.0478(9) 0.0043(6) -0.0009(6) -0.0041(5) C52 0.0238(6) 0.0292(6) 0.0400(8) 0.0012(5) 0.0006(5) 0.0026(5) C53 0.0224(6) 0.0244(6) 0.0415(8) -0.0024(5) -0.0036(5) 0.0011(5) C54 0.0185(5) 0.0190(5) 0.0412(7) 0.0009(5) -0.0047(5) 0.0008(4) C55 0.0394(8) 0.0444(9) 0.0557(10) 0.0094(8) 0.0002(7) -0.0149(7) C56 0.0406(8) 0.0349(7) 0.0405(8) -0.0029(6) -0.0066(6) -0.0079(6) C57 0.0203(5) 0.0184(5) 0.0223(5) -0.0002(4) -0.0074(4) -0.0056(4) C58 0.0170(5) 0.0190(5) 0.0234(5) -0.0018(4) -0.0060(4) -0.0028(4) C59 0.0166(5) 0.0235(5) 0.0236(6) -0.0019(4) -0.0060(4) -0.0044(4) C60 0.0172(5) 0.0248(5) 0.0220(5) -0.0030(4) -0.0051(4) -0.0055(4) C61 0.0205(5) 0.0219(5) 0.0224(5) -0.0023(4) -0.0056(4) -0.0069(4) C62 0.0338(6) 0.0241(6) 0.0271(6) 0.0011(5) -0.0100(5) -0.0125(5) C63 0.0421(7) 0.0278(6) 0.0344(7) -0.0016(5) -0.0096(6) -0.0182(6) C64 0.0346(7) 0.0348(7) 0.0341(7) -0.0071(5) -0.0105(5) -0.0167(6) C65 0.0232(5) 0.0306(6) 0.0275(6) -0.0062(5) -0.0071(5) -0.0088(5) C66 0.0270(6) 0.0393(7) 0.0353(7) -0.0085(6) -0.0154(5) -0.0075(5) C67 0.0294(6) 0.0370(7) 0.0308(7) -0.0029(5) -0.0172(5) -0.0028(5) C68 0.0225(5) 0.0277(6) 0.0281(6) -0.0005(5) -0.0106(5) -0.0025(4) C1A 0.0263(17) 0.0339(16) 0.039(2) -0.0085(16) -0.0180(15) -0.0014(13) C2A 0.0196(13) 0.0345(16) 0.0331(17) -0.0082(13) -0.0063(12) 0.0041(11) C3A 0.0257(13) 0.0276(13) 0.0218(13) -0.0043(10) -0.0106(10) 0.0026(10) C1B 0.0229(13) 0.0360(14) 0.0431(18) 0.0015(13) -0.0129(12) -0.0097(11) C2B 0.0231(11) 0.0335(13) 0.0318(14) -0.0057(11) -0.0100(10) 0.0052(10) C3B 0.0253(10) 0.0269(11) 0.0223(11) -0.0032(8) -0.0097(8) -0.0014(8) C35 0.0232(6) 0.0390(8) 0.0618(11) 0.0090(7) -0.0065(6) -0.0043(6) C36 0.0293(7) 0.0433(9) 0.0607(10) -0.0009(7) -0.0207(7) 0.0060(6) C37 0.0289(7) 0.0272(7) 0.0658(11) -0.0072(7) -0.0064(7) 0.0026(5) N10 0.0204(5) 0.0295(5) 0.0294(5) -0.0003(4) -0.0093(4) -0.0038(4) N11 0.0200(4) 0.0240(5) 0.0238(5) -0.0054(4) -0.0064(4) -0.0020(4) N12 0.0207(4) 0.0183(4) 0.0250(5) -0.0014(4) -0.0089(4) -0.0025(3) N13 0.0218(5) 0.0177(4) 0.0326(6) 0.0017(4) -0.0118(4) -0.0041(4) N14 0.0193(5) 0.0180(5) 0.0444(7) -0.0023(4) -0.0030(4) -0.0030(4) N15 0.0191(5) 0.0237(5) 0.0421(7) 0.0037(4) -0.0067(4) -0.0016(4) N16 0.0196(4) 0.0175(4) 0.0232(5) -0.0023(3) -0.0052(4) -0.0016(3) N17 0.0189(4) 0.0177(4) 0.0319(5) -0.0022(4) -0.0080(4) -0.0021(3) O1 0.0267(4) 0.0191(4) 0.0226(4) -0.0020(3) -0.0048(3) -0.0027(3) O2 0.0204(4) 0.0230(4) 0.0235(4) -0.0061(3) -0.0056(3) -0.0028(3) O3 0.0262(4) 0.0179(4) 0.0266(4) 0.0007(3) -0.0124(3) -0.0040(3) O4 0.0283(4) 0.0186(4) 0.0367(5) 0.0064(3) -0.0156(4) -0.0060(3) O5 0.0237(4) 0.0216(4) 0.0392(5) 0.0030(4) -0.0092(4) -0.0056(3) O6 0.0221(4) 0.0185(4) 0.0360(5) -0.0030(3) -0.0093(3) -0.0034(3) O7 0.0239(4) 0.0175(4) 0.0246(4) -0.0005(3) -0.0043(3) -0.0004(3) O8 0.0208(4) 0.0169(4) 0.0380(5) 0.0013(3) -0.0080(4) -0.0012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.7978(9) . ? Al1 O2 1.8289(9) . ? Al1 O7 1.8873(9) . ? Al1 O3 1.8894(9) . ? Al1 N11 2.0947(11) . ? Al1 N10 2.1956(11) . ? Al2 O5 1.7983(10) . ? Al2 O6 1.8188(10) . ? Al2 O8 1.8800(9) . ? Al2 O4 1.9107(10) . ? Al2 N14 2.0908(11) . ? Al2 N15 2.2040(11) . ? C4 C3B 1.455(3) . ? C4 N11 1.4904(15) . ? C4 C3A 1.527(3) . ? C5 C6 1.5000(18) . ? C5 N11 1.5038(16) . ? C6 C7 1.3979(19) . ? C6 C11 1.4102(19) . ? C7 C8 1.391(2) . ? C8 C9 1.390(3) . ? C8 C12 1.514(2) . ? C9 C10 1.387(2) . ? C10 C11 1.4087(17) . ? C10 C13 1.506(2) . ? C11 O1 1.3215(14) . ? C14 N11 1.5000(15) . ? C14 C15 1.5014(18) . ? C15 C16 1.3999(17) . ? C15 C20 1.4028(18) . ? C16 C17 1.3900(19) . ? C17 C18 1.386(2) . ? C17 C21 1.5097(19) . ? C18 C19 1.3937(18) . ? C19 C20 1.4104(17) . ? C19 C22 1.501(2) . ? C20 O2 1.3338(14) . ? C23 N16 1.2892(15) . ? C23 C25 1.4600(16) . ? C23 C24 1.4821(15) . ? C24 N17 1.2956(15) . ? C24 C27 1.4688(17) . ? C25 C34 1.3789(16) . ? C25 C26 1.4163(16) . ? C26 C31 1.3979(17) . ? C26 C27 1.4200(16) . ? C27 C28 1.3744(17) . ? C28 C29 1.420(2) . ? C29 C30 1.371(2) . ? C30 C31 1.4222(18) . ? C31 C32 1.4153(18) . ? C32 C33 1.3763(19) . ? C33 C34 1.4171(17) . ? C38 N14 1.4929(16) . ? C38 C37 1.512(2) . ? C39 N14 1.4956(19) . ? C39 C40 1.503(2) . ? C40 C41 1.395(2) . ? C40 C45 1.4008(18) . ? C41 C42 1.387(3) . ? C42 C43 1.386(2) . ? C42 C46 1.510(3) . ? C43 C44 1.390(2) . ? C44 C45 1.4036(19) . ? C44 C47 1.5033(19) . ? C45 O6 1.3335(16) . ? C48 C49 1.502(2) . ? C48 N14 1.5029(17) . ? C49 C50 1.4016(19) . ? C49 C54 1.4036(19) . ? C50 C51 1.391(2) . ? C51 C52 1.394(2) . ? C51 C55 1.513(2) . ? C52 C53 1.388(2) . ? C53 C54 1.416(2) . ? C53 C56 1.497(2) . ? C54 O5 1.3273(15) . ? C57 N12 1.2974(14) . ? C57 C61 1.4696(16) . ? C57 C58 1.4811(15) . ? C58 N13 1.2871(15) . ? C58 C59 1.4550(16) . ? C59 C68 1.3751(16) . ? C59 C60 1.4151(16) . ? C60 C65 1.3973(16) . ? C60 C61 1.4164(15) . ? C61 C62 1.3756(16) . ? C62 C63 1.4185(18) . ? C63 C64 1.372(2) . ? C64 C65 1.4189(19) . ? C65 C66 1.4148(18) . ? C66 C67 1.375(2) . ? C67 C68 1.4197(18) . ? C1A N10 1.400(4) . ? C2A N10 1.579(3) . ? C3A N10 1.470(3) . ? C1B N10 1.510(3) . ? C2B N10 1.417(3) . ? C3B N10 1.547(3) . ? C35 N15 1.4998(18) . ? C36 N15 1.472(2) . ? C37 N15 1.471(2) . ? N12 O3 1.3470(12) . ? N13 O4 1.3374(12) . ? N16 O7 1.3366(12) . ? N17 O8 1.3549(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O2 174.00(4) . . ? O1 Al1 O7 86.97(4) . . ? O2 Al1 O7 88.39(4) . . ? O1 Al1 O3 90.81(4) . . ? O2 Al1 O3 93.60(4) . . ? O7 Al1 O3 97.68(4) . . ? O1 Al1 N11 91.70(4) . . ? O2 Al1 N11 92.41(4) . . ? O7 Al1 N11 172.65(4) . . ? O3 Al1 N11 89.56(4) . . ? O1 Al1 N10 87.79(4) . . ? O2 Al1 N10 88.40(4) . . ? O7 Al1 N10 90.13(4) . . ? O3 Al1 N10 171.98(4) . . ? N11 Al1 N10 82.59(4) . . ? O5 Al2 O6 175.05(4) . . ? O5 Al2 O8 89.56(4) . . ? O6 Al2 O8 93.86(4) . . ? O5 Al2 O4 88.29(4) . . ? O6 Al2 O4 87.71(4) . . ? O8 Al2 O4 97.67(4) . . ? O5 Al2 N14 91.23(5) . . ? O6 Al2 N14 92.24(5) . . ? O8 Al2 N14 91.67(4) . . ? O4 Al2 N14 170.64(4) . . ? O5 Al2 N15 87.91(4) . . ? O6 Al2 N15 89.02(4) . . ? O8 Al2 N15 173.93(4) . . ? O4 Al2 N15 87.77(4) . . ? N14 Al2 N15 82.87(4) . . ? C3B C4 N11 112.62(13) . . ? C3B C4 C3A 46.56(15) . . ? N11 C4 C3A 112.68(13) . . ? C6 C5 N11 115.67(10) . . ? C7 C6 C11 119.80(13) . . ? C7 C6 C5 119.57(13) . . ? C11 C6 C5 120.50(11) . . ? C8 C7 C6 121.63(15) . . ? C9 C8 C7 117.50(14) . . ? C9 C8 C12 121.62(16) . . ? C7 C8 C12 120.86(18) . . ? C10 C9 C8 122.98(14) . . ? C9 C10 C11 119.02(13) . . ? C9 C10 C13 121.39(12) . . ? C11 C10 C13 119.59(12) . . ? O1 C11 C10 119.49(12) . . ? O1 C11 C6 121.48(11) . . ? C10 C11 C6 119.02(12) . . ? N11 C14 C15 116.53(10) . . ? C16 C15 C20 119.87(12) . . ? C16 C15 C14 119.90(12) . . ? C20 C15 C14 119.81(11) . . ? C17 C16 C15 121.47(13) . . ? C18 C17 C16 117.73(12) . . ? C18 C17 C21 121.08(13) . . ? C16 C17 C21 121.20(14) . . ? C17 C18 C19 122.93(13) . . ? C18 C19 C20 118.67(12) . . ? C18 C19 C22 121.89(12) . . ? C20 C19 C22 119.37(11) . . ? O2 C20 C15 121.54(11) . . ? O2 C20 C19 119.14(11) . . ? C15 C20 C19 119.32(11) . . ? N16 C23 C25 127.85(10) . . ? N16 C23 C24 123.47(10) . . ? C25 C23 C24 108.57(10) . . ? N17 C24 C27 133.32(10) . . ? N17 C24 C23 119.33(11) . . ? C27 C24 C23 106.49(9) . . ? C34 C25 C26 120.23(11) . . ? C34 C25 C23 134.16(11) . . ? C26 C25 C23 105.48(10) . . ? C31 C26 C25 122.92(11) . . ? C31 C26 C27 123.89(11) . . ? C25 C26 C27 113.05(10) . . ? C28 C27 C26 118.56(12) . . ? C28 C27 C24 135.03(11) . . ? C26 C27 C24 106.23(10) . . ? C27 C28 C29 118.19(12) . . ? C30 C29 C28 123.11(13) . . ? C29 C30 C31 119.95(13) . . ? C26 C31 C32 115.79(11) . . ? C26 C31 C30 116.17(12) . . ? C32 C31 C30 128.03(12) . . ? C33 C32 C31 121.47(12) . . ? C32 C33 C34 122.20(11) . . ? C25 C34 C33 117.35(11) . . ? N14 C38 C37 111.33(11) . . ? N14 C39 C40 116.81(11) . . ? C41 C40 C45 119.08(14) . . ? C41 C40 C39 121.47(13) . . ? C45 C40 C39 119.12(12) . . ? C42 C41 C40 122.04(16) . . ? C43 C42 C41 117.66(16) . . ? C43 C42 C46 120.20(18) . . ? C41 C42 C46 122.11(18) . . ? C42 C43 C44 122.53(15) . . ? C43 C44 C45 118.81(13) . . ? C43 C44 C47 121.52(14) . . ? C45 C44 C47 119.61(13) . . ? O6 C45 C40 120.28(12) . . ? O6 C45 C44 119.87(12) . . ? C40 C45 C44 119.85(13) . . ? C49 C48 N14 115.87(11) . . ? C50 C49 C54 119.67(14) . . ? C50 C49 C48 118.69(13) . . ? C54 C49 C48 121.41(12) . . ? C51 C50 C49 121.92(14) . . ? C50 C51 C52 117.55(13) . . ? C50 C51 C55 121.79(15) . . ? C52 C51 C55 120.63(16) . . ? C53 C52 C51 122.48(15) . . ? C52 C53 C54 119.40(14) . . ? C52 C53 C56 121.76(14) . . ? C54 C53 C56 118.83(12) . . ? O5 C54 C49 122.61(13) . . ? O5 C54 C53 118.41(12) . . ? C49 C54 C53 118.97(12) . . ? N12 C57 C61 133.22(11) . . ? N12 C57 C58 119.73(10) . . ? C61 C57 C58 106.47(9) . . ? N13 C58 C59 128.65(10) . . ? N13 C58 C57 122.52(10) . . ? C59 C58 C57 108.62(10) . . ? C68 C59 C60 119.91(11) . . ? C68 C59 C58 134.54(11) . . ? C60 C59 C58 105.55(10) . . ? C65 C60 C59 122.96(11) . . ? C65 C60 C61 123.88(11) . . ? C59 C60 C61 113.12(10) . . ? C62 C61 C60 118.82(11) . . ? C62 C61 C57 134.94(11) . . ? C60 C61 C57 106.20(10) . . ? C61 C62 C63 118.01(12) . . ? C64 C63 C62 122.96(12) . . ? C63 C64 C65 120.25(12) . . ? C60 C65 C66 116.14(12) . . ? C60 C65 C64 116.04(11) . . ? C66 C65 C64 127.82(12) . . ? C67 C66 C65 121.11(12) . . ? C66 C67 C68 122.11(12) . . ? C59 C68 C67 117.76(12) . . ? N10 C3A C4 110.61(18) . . ? C4 C3B N10 110.28(15) . . ? N15 C37 C38 111.14(13) . . ? C1A N10 C2B 121.39(19) . . ? C1A N10 C3A 114.0(2) . . ? C2B N10 C3A 69.43(17) . . ? C1A N10 C1B 29.37(17) . . ? C2B N10 C1B 109.01(18) . . ? C3A N10 C1B 138.55(19) . . ? C1A N10 C3B 74.9(2) . . ? C2B N10 C3B 109.99(16) . . ? C3A N10 C3B 45.99(14) . . ? C1B N10 C3B 104.23(18) . . ? C1A N10 C2A 106.4(2) . . ? C2B N10 C2A 35.36(15) . . ? C3A N10 C2A 104.78(19) . . ? C1B N10 C2A 82.49(19) . . ? C3B N10 C2A 141.31(16) . . ? C1A N10 Al1 118.44(15) . . ? C2B N10 Al1 116.41(12) . . ? C3A N10 Al1 104.05(12) . . ? C1B N10 Al1 112.28(12) . . ? C3B N10 Al1 104.11(9) . . ? C2A N10 Al1 108.33(12) . . ? C4 N11 C14 110.97(9) . . ? C4 N11 C5 110.36(10) . . ? C14 N11 C5 105.25(9) . . ? C4 N11 Al1 110.48(8) . . ? C14 N11 Al1 110.45(8) . . ? C5 N11 Al1 109.20(7) . . ? C57 N12 O3 113.67(9) . . ? C58 N13 O4 123.02(10) . . ? C38 N14 C39 112.29(12) . . ? C38 N14 C48 109.09(10) . . ? C39 N14 C48 105.13(10) . . ? C38 N14 Al2 109.38(8) . . ? C39 N14 Al2 110.86(8) . . ? C48 N14 Al2 110.02(8) . . ? C37 N15 C36 111.35(12) . . ? C37 N15 C35 108.57(13) . . ? C36 N15 C35 105.17(12) . . ? C37 N15 Al2 105.91(8) . . ? C36 N15 Al2 113.50(9) . . ? C35 N15 Al2 112.35(8) . . ? C23 N16 O7 121.94(9) . . ? C24 N17 O8 113.23(10) . . ? C11 O1 Al1 135.25(8) . . ? C20 O2 Al1 134.29(8) . . ? N12 O3 Al1 117.34(7) . . ? N13 O4 Al2 114.26(7) . . ? C54 O5 Al2 134.24(9) . . ? C45 O6 Al2 134.49(8) . . ? N16 O7 Al1 115.10(7) . . ? N17 O8 Al2 116.94(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.066 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.056 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.063 0.500 0.937 1274 311 ' ' _platon_squeeze_details ; ; # Attachment '- p7k05_sad.cif' data_p7k05_sad _database_code_depnum_ccdc_archive 'CCDC 867796' #TrackingRef '- p7k05_sad.cif' _audit_creation_method SHELXL-97 # start Validation Reply Form: Alert A issues _vrf_PLAT222_p7k05_sad ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 10.0 Ratio RESPONSE: The elongated thermal parameters are due to unresolved disorder, namely in the tert-butyl groups, along with less than ideal crystal quality ; # end Validation Reply Form _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H114 Al2 Fe N10 O8' _chemical_formula_sum 'C94 H114 Al2 Fe N10 O8' _chemical_formula_weight 1621.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7358(11) _cell_length_b 20.2952(15) _cell_length_c 33.354(3) _cell_angle_alpha 77.202(2) _cell_angle_beta 88.031(2) _cell_angle_gamma 74.307(2) _cell_volume 9361.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 23.84 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6949 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 162520 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 31783 _reflns_number_gt 18086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31783 _refine_ls_number_parameters 2140 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1279 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2A C 0.8942 0.6325 0.3921 0.054 Uani 1 1 d . . . Al1A Al 0.96866(8) 0.85032(6) 0.29213(4) 0.0287(3) Uani 1 1 d . . . Al2A Al 0.61521(7) 0.68918(5) 0.41172(3) 0.0202(3) Uani 1 1 d . . . Al1B Al 0.20310(9) 0.19453(6) 0.12763(4) 0.0332(3) Uani 1 1 d . A . Al2B Al -0.16005(8) 0.40554(6) 0.24274(3) 0.0227(3) Uani 1 1 d . A . C1A C 0.9620(2) 0.66932(17) 0.37120(10) 0.0188(8) Uani 1 1 d . . . C3A C 1.12435(15) 0.62018(12) 0.34823(5) 0.0259(9) Uani 1 1 d G . . H3A H 1.0982 0.6249 0.3218 0.031 Uiso 1 1 calc R . . C4A C 1.22108(14) 0.59376(12) 0.35560(7) 0.0307(10) Uani 1 1 d G . . H4A H 1.2611 0.5804 0.3342 0.037 Uiso 1 1 calc R . . C5A C 1.25928(11) 0.58691(12) 0.39432(8) 0.0307(10) Uani 1 1 d G . . H5A H 1.3254 0.5689 0.3994 0.037 Uiso 1 1 calc R . . C6A C 1.20075(16) 0.60648(13) 0.42567(6) 0.0332(10) Uani 1 1 d G . . H6A H 1.2269 0.6018 0.4521 0.040 Uiso 1 1 calc R . . C7A C 1.10401(15) 0.63290(12) 0.41830(6) 0.0266(9) Uani 1 1 d G . . H7A H 1.0640 0.6463 0.4397 0.032 Uiso 1 1 calc R . . C8A C 1.06581(11) 0.63975(11) 0.37959(7) 0.0203(8) Uani 1 1 d G . . C9A C 0.9184(2) 0.56220(17) 0.41612(11) 0.0192(8) Uani 1 1 d . . . C10A C 0.9701(2) 0.50728(18) 0.39981(11) 0.0252(9) Uani 1 1 d . . . H10A H 0.9893 0.5160 0.3721 0.030 Uiso 1 1 calc R . . C11A C 0.9942(3) 0.43947(19) 0.42358(12) 0.0294(10) Uani 1 1 d . . . H11A H 1.0300 0.4018 0.4122 0.035 Uiso 1 1 calc R . . C12A C 0.9660(3) 0.4269(2) 0.46382(13) 0.0345(10) Uani 1 1 d . . . H12A H 0.9818 0.3804 0.4800 0.041 Uiso 1 1 calc R . . C13A C 0.9153(3) 0.4813(2) 0.48057(12) 0.0329(10) Uani 1 1 d . . . H13A H 0.8965 0.4725 0.5083 0.039 Uiso 1 1 calc R . . C14A C 0.8918(3) 0.54864(19) 0.45686(11) 0.0271(9) Uani 1 1 d . . . H14A H 0.8570 0.5863 0.4685 0.033 Uiso 1 1 calc R . . C15A C 0.6904(2) 0.89162(19) 0.29971(11) 0.0232(9) Uani 1 1 d . . . C16A C 0.6663(3) 0.9541(3) 0.26400(14) 0.0466(13) Uani 1 1 d . . . C17A C 0.6800(3) 1.0178(2) 0.26774(17) 0.0668(17) Uani 1 1 d . . . H17A H 0.6993 1.0230 0.2935 0.080 Uiso 1 1 calc R . . C18A C 0.6651(4) 1.0741(3) 0.2334(3) 0.104(3) Uani 1 1 d . . . H18A H 0.6735 1.1180 0.2355 0.125 Uiso 1 1 calc R . . C19A C 0.6382(4) 1.0641(6) 0.1971(3) 0.132(5) Uani 1 1 d . . . H19A H 0.6288 1.1020 0.1737 0.159 Uiso 1 1 calc R . . C20A C 0.6238(4) 1.0017(5) 0.1925(2) 0.123(4) Uani 1 1 d . . . H20A H 0.6045 0.9969 0.1666 0.147 Uiso 1 1 calc R . . C21A C 0.6384(3) 0.9452(3) 0.22703(15) 0.082(2) Uani 1 1 d . . . H21A H 0.6290 0.9015 0.2249 0.099 Uiso 1 1 calc R . . C22A C 0.6201(2) 0.86497(18) 0.32499(10) 0.0196(8) Uani 1 1 d . . . C23A C 0.5211(2) 0.90552(18) 0.32548(10) 0.0215(9) Uani 1 1 d . . . C24A C 0.4997(3) 0.97284(19) 0.33269(11) 0.0283(9) Uani 1 1 d . . . H24A H 0.5493 0.9931 0.3359 0.034 Uiso 1 1 calc R . . C25A C 0.4065(3) 1.0111(2) 0.33525(12) 0.0374(11) Uani 1 1 d . . . H25A H 0.3928 1.0574 0.3397 0.045 Uiso 1 1 calc R . . C26A C 0.3352(3) 0.9820(2) 0.33135(13) 0.0441(12) Uani 1 1 d . . . H26A H 0.2716 1.0077 0.3336 0.053 Uiso 1 1 calc R . . C27A C 0.3551(3) 0.9155(2) 0.32415(14) 0.0478(13) Uani 1 1 d . . . H27A H 0.3050 0.8955 0.3212 0.057 Uiso 1 1 calc R . . C28A C 0.4476(3) 0.8773(2) 0.32116(12) 0.0326(10) Uani 1 1 d . . . H28A H 0.4604 0.8315 0.3161 0.039 Uiso 1 1 calc R . . C29A C 1.1798(3) 0.78149(18) 0.28784(12) 0.0316(10) Uani 1 1 d . . . H29A H 1.2453 0.7813 0.2920 0.047 Uiso 1 1 calc R . . H29B H 1.1679 0.7840 0.2587 0.047 Uiso 1 1 calc R . . H29C H 1.1684 0.7384 0.3045 0.047 Uiso 1 1 calc R . . C30A C 1.1321(3) 0.90914(19) 0.27498(13) 0.0365(11) Uani 1 1 d . . . H30A H 1.2002 0.9020 0.2697 0.044 Uiso 1 1 calc R . . H30B H 1.1121 0.9471 0.2902 0.044 Uiso 1 1 calc R . . C31A C 1.0775(3) 0.9302(2) 0.23474(13) 0.0429(12) Uani 1 1 d . . . H31A H 1.0859 0.9754 0.2188 0.052 Uiso 1 1 calc R . . H31B H 1.1009 0.8942 0.2183 0.052 Uiso 1 1 calc R . . C32A C 0.9321(3) 1.0065(2) 0.25376(15) 0.0630(16) Uani 1 1 d . . . H32A H 0.9407 1.0442 0.2312 0.094 Uiso 1 1 calc R . . H32B H 0.9622 1.0089 0.2789 0.094 Uiso 1 1 calc R . . H32C H 0.8646 1.0119 0.2581 0.094 Uiso 1 1 calc R . . C33A C 1.1376(2) 0.83605(18) 0.34483(12) 0.0278(9) Uani 1 1 d . . . H33A H 1.2065 0.8280 0.3484 0.033 Uiso 1 1 calc R . . H33B H 1.1209 0.7940 0.3610 0.033 Uiso 1 1 calc R . . C34A C 1.0881(3) 0.89773(18) 0.36232(13) 0.0310(10) Uani 1 1 d . . . C35A C 0.9922(3) 0.92890(19) 0.35386(13) 0.0319(10) Uani 1 1 d . . . C36A C 0.9464(3) 0.98536(19) 0.37226(14) 0.0368(11) Uani 1 1 d . . . C37A C 0.9986(3) 1.0087(2) 0.39714(14) 0.0438(12) Uani 1 1 d . . . H37A H 0.9675 1.0468 0.4092 0.053 Uiso 1 1 calc R . . C38A C 1.0951(3) 0.9786(2) 0.40528(13) 0.0384(11) Uani 1 1 d . . . C39A C 1.1375(3) 0.92317(19) 0.38757(12) 0.0330(10) Uani 1 1 d . . . H39A H 1.2030 0.9014 0.3927 0.040 Uiso 1 1 calc R . . C40A C 0.8423(3) 1.0178(2) 0.36369(15) 0.0519(14) Uani 1 1 d . . . H40A H 0.8182 1.0510 0.3814 0.078 Uiso 1 1 calc R . . H40B H 0.8093 0.9810 0.3693 0.078 Uiso 1 1 calc R . . H40C H 0.8316 1.0428 0.3348 0.078 Uiso 1 1 calc R . . C41A C 1.1487(3) 1.0084(2) 0.43280(14) 0.0440(12) Uani 1 1 d . . . C42A C 1.2514(3) 0.9656(2) 0.44083(14) 0.0495(13) Uani 1 1 d . . . H42A H 1.2539 0.9172 0.4547 0.074 Uiso 1 1 calc R . . H42B H 1.2826 0.9863 0.4584 0.074 Uiso 1 1 calc R . . H42C H 1.2836 0.9659 0.4146 0.074 Uiso 1 1 calc R . . C43A C 1.1462(3) 1.0844(2) 0.41213(15) 0.0555(14) Uani 1 1 d . . . H43A H 1.1783 1.1038 0.4301 0.083 Uiso 1 1 calc R . . H43B H 1.0806 1.1126 0.4072 0.083 Uiso 1 1 calc R . . H43C H 1.1783 1.0854 0.3859 0.083 Uiso 1 1 calc R . . C44A C 1.1004(4) 1.0068(3) 0.47457(15) 0.0671(16) Uani 1 1 d . . . H44A H 1.0938 0.9595 0.4860 0.101 Uiso 1 1 calc R . . H44B H 1.0378 1.0404 0.4708 0.101 Uiso 1 1 calc R . . H44C H 1.1387 1.0193 0.4936 0.101 Uiso 1 1 calc R . . C45A C 0.9252(3) 0.9360(3) 0.20538(16) 0.0749(19) Uani 1 1 d . . . H45A H 0.8589 0.9373 0.2121 0.090 Uiso 1 1 calc R . . H45B H 0.9248 0.9789 0.1842 0.090 Uiso 1 1 calc R . . C46A C 0.9674(3) 0.8733(3) 0.18766(14) 0.0610(15) Uani 1 1 d . . . C47A C 1.0031(3) 0.8064(3) 0.21300(14) 0.0530(14) Uani 1 1 d . . . C48A C 1.0442(4) 0.7480(4) 0.19546(15) 0.0648(16) Uani 1 1 d . . . C49A C 1.0451(5) 0.7593(4) 0.15238(19) 0.100(3) Uani 1 1 d . . . H49A H 1.0715 0.7205 0.1402 0.120 Uiso 1 1 calc R . . C50A C 1.0089(5) 0.8253(5) 0.12663(18) 0.104(3) Uani 1 1 d . . . C51A C 0.9717(4) 0.8815(4) 0.14491(17) 0.096(2) Uani 1 1 d . . . H51A H 0.9483 0.9270 0.1279 0.115 Uiso 1 1 calc R . . C52A C 1.0880(3) 0.6770(3) 0.22384(16) 0.0671(16) Uani 1 1 d . . . H52A H 1.1134 0.6421 0.2073 0.101 Uiso 1 1 calc R . . H52B H 1.0398 0.6625 0.2419 0.101 Uiso 1 1 calc R . . H52C H 1.1390 0.6808 0.2406 0.101 Uiso 1 1 calc R . . C53A C 1.0163(8) 0.8350(7) 0.0798(2) 0.176(5) Uani 1 1 d . . . C54A C 0.9182(8) 0.8823(6) 0.0603(2) 0.218(7) Uani 1 1 d . . . H54A H 0.9194 0.8881 0.0304 0.327 Uiso 1 1 calc R . . H54B H 0.9054 0.9284 0.0672 0.327 Uiso 1 1 calc R . . H54C H 0.8686 0.8600 0.0712 0.327 Uiso 1 1 calc R . . C55A C 1.0806(6) 0.8807(5) 0.06355(19) 0.196(5) Uani 1 1 d . . . H55A H 1.1448 0.8569 0.0745 0.294 Uiso 1 1 calc R . . H55B H 1.0585 0.9254 0.0722 0.294 Uiso 1 1 calc R . . H55C H 1.0804 0.8896 0.0334 0.294 Uiso 1 1 calc R . . C56A C 1.0328(9) 0.7704(5) 0.0652(2) 0.217(6) Uani 1 1 d U . . H56A H 1.0983 0.7427 0.0715 0.326 Uiso 1 1 calc R . . H56B H 1.0209 0.7817 0.0354 0.326 Uiso 1 1 calc R . . H56C H 0.9902 0.7433 0.0789 0.326 Uiso 1 1 calc R . . C57A C 0.6583(3) 0.57741(19) 0.49488(11) 0.0290(9) Uani 1 1 d . . . H57A H 0.6370 0.6169 0.5085 0.043 Uiso 1 1 calc R . . H57B H 0.7255 0.5701 0.4891 0.043 Uiso 1 1 calc R . . H57C H 0.6483 0.5349 0.5129 0.043 Uiso 1 1 calc R . . C58A C 0.5023(2) 0.60383(18) 0.46526(11) 0.0258(9) Uani 1 1 d . . . H58A H 0.4955 0.5699 0.4908 0.031 Uiso 1 1 calc R . . H58B H 0.4681 0.5956 0.4426 0.031 Uiso 1 1 calc R . . C59A C 0.4603(3) 0.67793(18) 0.47087(11) 0.0278(9) Uani 1 1 d . . . H59A H 0.3922 0.6855 0.4762 0.033 Uiso 1 1 calc R . . H59B H 0.4913 0.6851 0.4948 0.033 Uiso 1 1 calc R . . C60A C 0.3983(2) 0.7392(2) 0.40262(12) 0.0301(10) Uani 1 1 d . . . H60A H 0.3374 0.7606 0.4134 0.045 Uiso 1 1 calc R . . H60B H 0.3978 0.6936 0.3974 0.045 Uiso 1 1 calc R . . H60C H 0.4095 0.7699 0.3769 0.045 Uiso 1 1 calc R . . C61A C 0.4644(2) 0.79905(18) 0.44338(11) 0.0261(9) Uani 1 1 d . . . H61A H 0.4767 0.8320 0.4184 0.031 Uiso 1 1 calc R . . H61B H 0.3984 0.8177 0.4510 0.031 Uiso 1 1 calc R . . C62A C 0.5288(3) 0.79725(18) 0.47758(11) 0.0250(9) Uani 1 1 d . . . C63A C 0.6226(3) 0.75556(18) 0.48078(11) 0.0238(9) Uani 1 1 d . . . C64A C 0.6810(3) 0.75587(19) 0.51361(11) 0.0257(9) Uani 1 1 d . . . C65A C 0.6429(3) 0.79692(19) 0.54139(11) 0.0321(10) Uani 1 1 d . . . H65A H 0.6825 0.7967 0.5633 0.039 Uiso 1 1 calc R . . C66A C 0.5496(3) 0.8388(2) 0.53909(12) 0.0316(10) Uani 1 1 d . . . C67A C 0.4942(3) 0.83696(18) 0.50690(12) 0.0291(10) Uani 1 1 d . . . H67A H 0.4301 0.8638 0.5046 0.035 Uiso 1 1 calc R . . C68A C 0.7816(3) 0.7126(2) 0.51698(12) 0.0341(10) Uani 1 1 d . . . H68A H 0.8152 0.7242 0.5382 0.051 Uiso 1 1 calc R . . H68B H 0.8117 0.7226 0.4905 0.051 Uiso 1 1 calc R . . H68C H 0.7838 0.6627 0.5245 0.051 Uiso 1 1 calc R . . C69A C 0.5124(3) 0.8840(2) 0.57055(13) 0.0413(11) Uani 1 1 d . . . C70A C 0.5564(3) 0.9447(2) 0.56294(13) 0.0508(13) Uani 1 1 d . . . H70A H 0.5328 0.9741 0.5828 0.076 Uiso 1 1 calc R . . H70B H 0.5399 0.9728 0.5349 0.076 Uiso 1 1 calc R . . H70C H 0.6251 0.9266 0.5662 0.076 Uiso 1 1 calc R . . C71A C 0.5368(5) 0.8417(2) 0.61357(14) 0.096(2) Uani 1 1 d . . . H71A H 0.6055 0.8236 0.6171 0.143 Uiso 1 1 calc R . . H71B H 0.5083 0.8023 0.6186 0.143 Uiso 1 1 calc R . . H71C H 0.5126 0.8715 0.6331 0.143 Uiso 1 1 calc R . . C72A C 0.4055(4) 0.9166(3) 0.56555(19) 0.103(2) Uani 1 1 d . . . H72A H 0.3858 0.9505 0.5831 0.154 Uiso 1 1 calc R . . H72B H 0.3731 0.8795 0.5736 0.154 Uiso 1 1 calc R . . H72C H 0.3894 0.9405 0.5368 0.154 Uiso 1 1 calc R . . C73A C 0.6397(2) 0.53146(17) 0.43638(11) 0.0241(9) Uani 1 1 d . . . H73A H 0.6426 0.4880 0.4574 0.029 Uiso 1 1 calc R . . H73B H 0.7047 0.5300 0.4272 0.029 Uiso 1 1 calc R . . C74A C 0.5802(2) 0.53288(18) 0.40033(11) 0.0227(9) Uani 1 1 d . . . C75A C 0.5454(2) 0.59639(18) 0.37043(11) 0.0201(8) Uani 1 1 d . . . C76A C 0.4892(2) 0.59573(18) 0.33766(11) 0.0219(9) Uani 1 1 d . . . C77A C 0.4695(2) 0.53330(19) 0.33493(11) 0.0245(9) Uani 1 1 d . . . H77A H 0.4333 0.5332 0.3119 0.029 Uiso 1 1 calc R . . C78A C 0.5002(3) 0.47151(19) 0.36428(12) 0.0260(9) Uani 1 1 d . . . C79A C 0.5560(2) 0.47319(19) 0.39673(12) 0.0248(9) Uani 1 1 d . . . H79A H 0.5784 0.4315 0.4173 0.030 Uiso 1 1 calc R . . C80A C 0.4470(3) 0.66264(18) 0.30687(11) 0.0290(9) Uani 1 1 d . . . H80A H 0.3841 0.6850 0.3155 0.043 Uiso 1 1 calc R . . H80B H 0.4420 0.6522 0.2799 0.043 Uiso 1 1 calc R . . H80C H 0.4874 0.6944 0.3051 0.043 Uiso 1 1 calc R . . C81A C 0.4733(3) 0.40343(19) 0.36354(12) 0.0303(10) Uani 1 1 d . . . C82A C 0.5622(3) 0.34447(19) 0.36216(13) 0.0424(11) Uani 1 1 d . . . H82A H 0.6021 0.3366 0.3866 0.064 Uiso 1 1 calc R . . H82B H 0.5969 0.3575 0.3374 0.064 Uiso 1 1 calc R . . H82C H 0.5448 0.3014 0.3616 0.064 Uiso 1 1 calc R . . C83A C 0.4107(3) 0.4134(2) 0.32544(13) 0.0438(12) Uani 1 1 d . . . H83A H 0.4462 0.4232 0.3005 0.066 Uiso 1 1 calc R . . H83B H 0.3546 0.4527 0.3251 0.066 Uiso 1 1 calc R . . H83C H 0.3914 0.3705 0.3265 0.066 Uiso 1 1 calc R . . C84A C 0.4177(3) 0.3835(2) 0.40177(12) 0.0384(11) Uani 1 1 d . . . H84A H 0.3981 0.3416 0.4005 0.058 Uiso 1 1 calc R . . H84B H 0.3619 0.4224 0.4029 0.058 Uiso 1 1 calc R . . H84C H 0.4577 0.3739 0.4264 0.058 Uiso 1 1 calc R . . C85A C 0.8878(3) 0.81723(18) 0.40773(12) 0.0283(9) Uani 1 1 d . . . H85A H 0.9431 0.7960 0.3948 0.034 Uiso 1 1 calc R . . C86A C 0.8969(3) 0.8499(2) 0.43883(13) 0.0417(11) Uani 1 1 d . . . H86A H 0.9575 0.8513 0.4467 0.050 Uiso 1 1 calc R . . C87A C 0.8186(3) 0.8803(2) 0.45845(13) 0.0479(12) Uani 1 1 d . . . H87A H 0.8245 0.9018 0.4805 0.057 Uiso 1 1 calc R . . C88A C 0.7324(3) 0.87919(19) 0.44576(12) 0.0348(10) Uani 1 1 d . . . H88A H 0.6768 0.9013 0.4581 0.042 Uiso 1 1 calc R . . C89A C 0.7273(3) 0.84532(18) 0.41455(11) 0.0258(9) Uani 1 1 d . . . H89A H 0.6669 0.8437 0.4065 0.031 Uiso 1 1 calc R . . C90A C 0.6959(2) 0.70334(17) 0.29629(11) 0.0227(9) Uani 1 1 d . . . H90A H 0.6564 0.6975 0.3192 0.027 Uiso 1 1 calc R . . C91A C 0.6720(2) 0.68915(18) 0.26024(11) 0.0242(9) Uani 1 1 d . . . H91A H 0.6162 0.6749 0.2584 0.029 Uiso 1 1 calc R . . C92A C 0.7293(3) 0.69554(18) 0.22649(11) 0.0282(9) Uani 1 1 d . . . H92A H 0.7132 0.6868 0.2012 0.034 Uiso 1 1 calc R . . C93A C 0.8105(3) 0.71511(19) 0.23093(11) 0.0300(10) Uani 1 1 d . . . H93A H 0.8523 0.7191 0.2087 0.036 Uiso 1 1 calc R . . C94A C 0.8303(3) 0.72871(19) 0.26771(11) 0.0299(10) Uani 1 1 d . . . H94A H 0.8871 0.7412 0.2704 0.036 Uiso 1 1 calc R . . C1B C -0.0740(3) 0.23455(19) 0.14298(11) 0.0286(9) Uani 1 1 d . . . C2B C -0.1465(3) 0.28036(18) 0.16265(11) 0.0253(9) Uani 1 1 d . A . C3B C -0.0899(3) 0.1949(2) 0.11319(13) 0.047(6) Uani 0.388(7) 1 d PG A 1 C4B C -0.1266(4) 0.2268(2) 0.07365(13) 0.043(4) Uani 0.388(7) 1 d PG A 1 H4BA H -0.1422 0.2765 0.0647 0.051 Uiso 0.388(7) 1 calc PR A 1 C5B C -0.1405(4) 0.1861(3) 0.04718(10) 0.070(6) Uani 0.388(7) 1 d PG A 1 H5BA H -0.1656 0.2079 0.0202 0.084 Uiso 0.388(7) 1 calc PR A 1 C6B C -0.1178(4) 0.1135(3) 0.06025(15) 0.117(10) Uani 0.388(7) 1 d PG A 1 H6BA H -0.1273 0.0857 0.0422 0.140 Uiso 0.388(7) 1 calc PR A 1 C7B C -0.0811(4) 0.0816(2) 0.09979(19) 0.103(7) Uani 0.388(7) 1 d PG A 1 H7BA H -0.0655 0.0320 0.1087 0.124 Uiso 0.388(7) 1 calc PR A 1 C8B C -0.0671(3) 0.1223(2) 0.12626(15) 0.089(7) Uani 0.388(7) 1 d PG A 1 H8BA H -0.0420 0.1005 0.1533 0.106 Uiso 0.388(7) 1 calc PR A 1 C3C C -0.1050(3) 0.1873(2) 0.12029(12) 0.028(3) Uani 0.612(7) 1 d PG A 2 C4C C -0.0878(3) 0.1977(3) 0.07843(13) 0.041(2) Uani 0.612(7) 1 d PG A 2 H4CA H -0.0587 0.2333 0.0657 0.050 Uiso 0.612(7) 1 calc PR A 2 C5C C -0.1132(4) 0.1562(3) 0.05517(12) 0.059(3) Uani 0.612(7) 1 d PG A 2 H5CA H -0.1014 0.1633 0.0266 0.071 Uiso 0.612(7) 1 calc PR A 2 C6C C -0.1557(4) 0.1042(3) 0.07377(15) 0.071(3) Uani 0.612(7) 1 d PG A 2 H6CA H -0.1730 0.0758 0.0579 0.085 Uiso 0.612(7) 1 calc PR A 2 C7C C -0.1729(4) 0.0938(2) 0.11564(15) 0.051(2) Uani 0.612(7) 1 d PG A 2 H7CA H -0.2020 0.0582 0.1284 0.061 Uiso 0.612(7) 1 calc PR A 2 C8C C -0.1475(4) 0.1353(2) 0.13889(10) 0.0309(19) Uani 0.612(7) 1 d PG A 2 H8CA H -0.1592 0.1282 0.1675 0.037 Uiso 0.612(7) 1 calc PR A 2 C9B C -0.2481(3) 0.2927(2) 0.15495(12) 0.0278(9) Uani 1 1 d . . . C10B C -0.3142(12) 0.2732(8) 0.1882(5) 0.036(4) Uani 0.466(12) 1 d P A 1 H10B H -0.2900 0.2504 0.2152 0.043 Uiso 0.466(12) 1 calc PR A 1 C11B C -0.4090(16) 0.2878(10) 0.1798(7) 0.052(5) Uani 0.466(12) 1 d P A 1 H11B H -0.4508 0.2761 0.2008 0.062 Uiso 0.466(12) 1 calc PR A 1 C12B C -0.4410(3) 0.3188(3) 0.14168(19) 0.0678(16) Uani 0.466(12) 1 d P A 1 H12B H -0.5067 0.3286 0.1363 0.081 Uiso 0.466(12) 1 calc PR A 1 C13B C -0.3834(11) 0.3387(9) 0.1079(5) 0.057(3) Uani 0.466(12) 1 d P A 1 H13B H -0.4102 0.3625 0.0814 0.068 Uiso 0.466(12) 1 calc PR A 1 C14B C -0.2856(13) 0.3212(10) 0.1159(5) 0.054(5) Uani 0.466(12) 1 d P A 1 H14B H -0.2448 0.3292 0.0938 0.065 Uiso 0.466(12) 1 calc PR A 1 C10C C -0.2920(11) 0.2493(9) 0.1744(5) 0.075(5) Uani 0.534(12) 1 d P A 2 H10C H -0.2576 0.2083 0.1932 0.090 Uiso 0.534(12) 1 calc PR A 2 C11C C -0.3885(13) 0.2603(11) 0.1689(6) 0.090(6) Uani 0.534(12) 1 d P A 2 H11C H -0.4187 0.2272 0.1840 0.109 Uiso 0.534(12) 1 calc PR A 2 C12C C -0.4410(3) 0.3188(3) 0.14168(19) 0.0678(16) Uani 0.534(12) 1 d P A 2 H12C H -0.5063 0.3257 0.1367 0.081 Uiso 0.534(12) 1 calc PR A 2 C13C C -0.3957(10) 0.3649(9) 0.1228(4) 0.057(3) Uani 0.534(12) 1 d P A 2 H13C H -0.4304 0.4082 0.1061 0.068 Uiso 0.534(12) 1 calc PR A 2 C14C C -0.2980(10) 0.3507(7) 0.1271(4) 0.044(4) Uani 0.534(12) 1 d P A 2 H14C H -0.2658 0.3814 0.1107 0.053 Uiso 0.534(12) 1 calc PR A 2 C15B C 0.1937(3) 0.28737(18) 0.22435(11) 0.0226(9) Uani 1 1 d . . . C16B C 0.1208(3) 0.32646(18) 0.24733(11) 0.0230(9) Uani 1 1 d . . . C17B C 0.2946(3) 0.2658(2) 0.23679(11) 0.0268(9) Uani 1 1 d . . . C18B C 0.3410(3) 0.3117(2) 0.24537(15) 0.0526(13) Uani 1 1 d . . . H18B H 0.3097 0.3603 0.2411 0.063 Uiso 1 1 calc R . . C19B C 0.4342(3) 0.2866(3) 0.26044(18) 0.0760(18) Uani 1 1 d . . . H19B H 0.4662 0.3185 0.2662 0.091 Uiso 1 1 calc R . . C20B C 0.4796(3) 0.2168(3) 0.26697(16) 0.0657(15) Uani 1 1 d . . . H20B H 0.5426 0.2003 0.2778 0.079 Uiso 1 1 calc R . . C21B C 0.4356(3) 0.1708(2) 0.25817(13) 0.0461(12) Uani 1 1 d . . . H21B H 0.4675 0.1223 0.2624 0.055 Uiso 1 1 calc R . . C22B C 0.3443(3) 0.1954(2) 0.24312(12) 0.0352(10) Uani 1 1 d . . . H22B H 0.3139 0.1630 0.2368 0.042 Uiso 1 1 calc R . . C23B C 0.1414(3) 0.3495(2) 0.28446(12) 0.0306(10) Uani 1 1 d . . . C24B C 0.1267(3) 0.4212(3) 0.28249(15) 0.0475(12) Uani 1 1 d . . . H24B H 0.1046 0.4537 0.2574 0.057 Uiso 1 1 calc R . . C25B C 0.1434(3) 0.4454(4) 0.3157(2) 0.0748(19) Uani 1 1 d . . . H25B H 0.1320 0.4943 0.3138 0.090 Uiso 1 1 calc R . . C26B C 0.1757(4) 0.4001(5) 0.3507(2) 0.091(3) Uani 1 1 d . . . H26B H 0.1882 0.4177 0.3734 0.109 Uiso 1 1 calc R . . C27B C 0.1919(4) 0.3290(4) 0.35546(16) 0.088(2) Uani 1 1 d . . . H27B H 0.2149 0.2977 0.3809 0.105 Uiso 1 1 calc R . . C28B C 0.1728(3) 0.3033(3) 0.32060(14) 0.0613(15) Uani 1 1 d . . . H28B H 0.1822 0.2544 0.3228 0.074 Uiso 1 1 calc R . . C29B C 0.1513(3) 0.1716(2) 0.04429(12) 0.0484(12) Uani 1 1 d . . . H29D H 0.1706 0.2140 0.0320 0.073 Uiso 1 1 calc R . . H29E H 0.0853 0.1847 0.0522 0.073 Uiso 1 1 calc R . . H29F H 0.1581 0.1419 0.0243 0.073 Uiso 1 1 calc R . . C30B C 0.3115(3) 0.1141(2) 0.06955(14) 0.0509(13) Uani 1 1 d . . . H30C H 0.3157 0.1013 0.0425 0.061 Uiso 1 1 calc R . . H30D H 0.3481 0.0730 0.0900 0.061 Uiso 1 1 calc R . . C31B C 0.3530(3) 0.1755(2) 0.06719(12) 0.0478(12) Uani 1 1 d . . . H31C H 0.4206 0.1618 0.0605 0.057 Uiso 1 1 calc R . . H31D H 0.3201 0.2154 0.0452 0.057 Uiso 1 1 calc R . . C32B C 0.4204(3) 0.1508(2) 0.13620(12) 0.0447(12) Uani 1 1 d . . . H32D H 0.4205 0.1017 0.1391 0.067 Uiso 1 1 calc R . . H32E H 0.4110 0.1631 0.1631 0.067 Uiso 1 1 calc R . . H32F H 0.4809 0.1573 0.1255 0.067 Uiso 1 1 calc R . . C33B C -0.3723(3) 0.41811(19) 0.23943(12) 0.0332(10) Uani 1 1 d . . . H33C H -0.3688 0.3976 0.2690 0.050 Uiso 1 1 calc R . . H33D H -0.3548 0.3805 0.2243 0.050 Uiso 1 1 calc R . . H33E H -0.4367 0.4466 0.2314 0.050 Uiso 1 1 calc R . . C34B C -0.3290(3) 0.51670(18) 0.25569(11) 0.0286(9) Uani 1 1 d . . . H34A H -0.3978 0.5307 0.2597 0.034 Uiso 1 1 calc R . . H34B H -0.3099 0.5590 0.2415 0.034 Uiso 1 1 calc R . . C35B C -0.2782(2) 0.48731(19) 0.29707(11) 0.0255(9) Uani 1 1 d . . . H35A H -0.2907 0.5241 0.3133 0.031 Uiso 1 1 calc R . . H35B H -0.3017 0.4479 0.3125 0.031 Uiso 1 1 calc R . . C36B C -0.1338(3) 0.52320(18) 0.28229(12) 0.0283(9) Uani 1 1 d . . . H36A H -0.1440 0.5463 0.3056 0.042 Uiso 1 1 calc R . . H36B H -0.1644 0.5566 0.2575 0.042 Uiso 1 1 calc R . . H36C H -0.0660 0.5068 0.2780 0.042 Uiso 1 1 calc R . . C37B C 0.1790(3) 0.0676(2) 0.09865(13) 0.0458(12) Uani 1 1 d . . . H37B H 0.1144 0.0821 0.1089 0.055 Uiso 1 1 calc R . . H37C H 0.1761 0.0433 0.0762 0.055 Uiso 1 1 calc R . . C38B C 0.2417(3) 0.0173(2) 0.13286(13) 0.0446(12) Uani 1 1 d . . . C39B C 0.2760(3) 0.0418(2) 0.16366(12) 0.0357(10) Uani 1 1 d . A . C40B C 0.3369(3) -0.0061(2) 0.19453(12) 0.0344(10) Uani 1 1 d . . . C41B C 0.3603(3) -0.0776(2) 0.19435(14) 0.0438(12) Uani 1 1 d . . . H41B H 0.4011 -0.1100 0.2155 0.053 Uiso 1 1 calc R . . C42B C 0.3257(3) -0.1030(2) 0.16410(14) 0.0471(12) Uani 1 1 d . . . C43B C 0.2676(3) -0.0543(2) 0.13330(14) 0.0484(12) Uani 1 1 d . . . H43D H 0.2447 -0.0700 0.1119 0.058 Uiso 1 1 calc R . . C44B C 0.3780(3) 0.0195(2) 0.22649(12) 0.0371(11) Uani 1 1 d . . . H44D H 0.4136 0.0524 0.2131 0.056 Uiso 1 1 calc R . . H44E H 0.4203 -0.0204 0.2451 0.056 Uiso 1 1 calc R . . H44F H 0.3271 0.0434 0.2422 0.056 Uiso 1 1 calc R . . C45B C 0.3554(5) -0.1823(3) 0.1642(2) 0.1089(19) Uani 1 1 d . . . C46B C 0.4434(7) -0.2207(3) 0.1872(3) 0.205(6) Uani 1 1 d U . . H46A H 0.4303 -0.2339 0.2165 0.308 Uiso 1 1 calc R . . H46B H 0.4868 -0.1909 0.1836 0.308 Uiso 1 1 calc R . . H46C H 0.4723 -0.2631 0.1770 0.308 Uiso 1 1 calc R . . C47B C 0.3704(5) -0.1923(3) 0.1208(2) 0.107(2) Uani 1 1 d . . . H47A H 0.4256 -0.1769 0.1099 0.161 Uiso 1 1 calc R . . H47B H 0.3146 -0.1645 0.1037 0.161 Uiso 1 1 calc R . . H47C H 0.3807 -0.2420 0.1207 0.161 Uiso 1 1 calc R . . C48B C 0.2723(4) -0.2096(3) 0.1768(2) 0.1089(19) Uani 1 1 d . . . H48A H 0.2777 -0.2520 0.1663 0.163 Uiso 1 1 calc R . . H48B H 0.2146 -0.1739 0.1654 0.163 Uiso 1 1 calc R . . H48C H 0.2699 -0.2210 0.2068 0.163 Uiso 1 1 calc R . . C49B C 0.3541(3) 0.2690(2) 0.10211(12) 0.0382(11) Uani 1 1 d . . . H49B H 0.4200 0.2680 0.0946 0.046 Uiso 1 1 calc R . . H49C H 0.3434 0.2830 0.1289 0.046 Uiso 1 1 calc R . . C50B C 0.2887(3) 0.3240(2) 0.07006(12) 0.0364(10) Uani 1 1 d . . . C51B C 0.1962(3) 0.3220(2) 0.06448(12) 0.0330(10) Uani 1 1 d . A . C52B C 0.1388(3) 0.3740(2) 0.03374(12) 0.0333(10) Uani 1 1 d . . . C53B C 0.1749(3) 0.4273(2) 0.01099(12) 0.0410(11) Uani 1 1 d . . . H53B H 0.1356 0.4623 -0.0097 0.049 Uiso 1 1 calc R . . C54B C 0.2663(3) 0.4314(2) 0.01733(13) 0.0417(11) Uani 1 1 d . . . C55B C 0.3220(3) 0.3780(2) 0.04651(13) 0.0425(11) Uani 1 1 d . . . H55D H 0.3854 0.3781 0.0507 0.051 Uiso 1 1 calc R . . C56B C 0.0395(3) 0.3720(2) 0.02695(12) 0.0395(11) Uani 1 1 d . . . H56D H 0.0046 0.4164 0.0093 0.059 Uiso 1 1 calc R . . H56E H 0.0087 0.3648 0.0535 0.059 Uiso 1 1 calc R . . H56F H 0.0403 0.3333 0.0137 0.059 Uiso 1 1 calc R . . C57B C 0.3029(3) 0.4917(2) -0.00772(14) 0.0510(12) Uani 1 1 d . . . C58B C 0.2255(4) 0.5598(2) -0.01859(16) 0.0705(16) Uani 1 1 d . . . H58C H 0.1807 0.5557 -0.0384 0.106 Uiso 1 1 calc R . . H58D H 0.2531 0.5983 -0.0308 0.106 Uiso 1 1 calc R . . H58E H 0.1925 0.5695 0.0064 0.106 Uiso 1 1 calc R . . C59B C 0.3453(4) 0.4714(3) -0.04688(17) 0.095(2) Uani 1 1 d . . . H59C H 0.3952 0.4273 -0.0398 0.143 Uiso 1 1 calc R . . H59D H 0.3718 0.5084 -0.0624 0.143 Uiso 1 1 calc R . . H59E H 0.2961 0.4653 -0.0636 0.143 Uiso 1 1 calc R . . C60B C 0.3782(5) 0.5046(3) 0.0162(2) 0.117(3) Uani 1 1 d . . . H60D H 0.3513 0.5199 0.0409 0.176 Uiso 1 1 calc R . . H60E H 0.4035 0.5410 -0.0009 0.176 Uiso 1 1 calc R . . H60F H 0.4289 0.4611 0.0241 0.176 Uiso 1 1 calc R . . C61B C -0.1264(3) 0.41613(18) 0.32972(11) 0.0252(9) Uani 1 1 d . . . H61C H -0.1336 0.4443 0.3509 0.030 Uiso 1 1 calc R . . H61D H -0.0582 0.4004 0.3245 0.030 Uiso 1 1 calc R . . C62B C -0.1609(2) 0.35207(17) 0.34693(11) 0.0219(9) Uani 1 1 d . . . C63B C -0.1915(2) 0.31614(18) 0.32128(11) 0.0214(8) Uani 1 1 d . A . C64B C -0.2214(2) 0.25611(18) 0.33942(11) 0.0227(9) Uani 1 1 d . . . C65B C -0.2156(2) 0.23279(19) 0.38180(12) 0.0279(9) Uani 1 1 d . . . H65B H -0.2331 0.1911 0.3936 0.034 Uiso 1 1 calc R . . C66B C -0.1849(3) 0.26813(19) 0.40807(12) 0.0301(10) Uani 1 1 d . . . C67B C -0.1583(2) 0.32806(18) 0.38928(11) 0.0267(9) Uani 1 1 d . . . H67B H -0.1377 0.3536 0.4061 0.032 Uiso 1 1 calc R . . C68B C -0.2613(3) 0.22009(18) 0.31251(11) 0.0279(9) Uani 1 1 d . . . H68D H -0.2802 0.1804 0.3296 0.042 Uiso 1 1 calc R . . H68E H -0.2134 0.2031 0.2934 0.042 Uiso 1 1 calc R . . H68F H -0.3164 0.2533 0.2969 0.042 Uiso 1 1 calc R . . C69B C -0.1795(3) 0.2427(2) 0.45512(12) 0.0369(11) Uani 1 1 d . . . C70B C -0.2102(4) 0.3044(2) 0.47612(13) 0.0601(15) Uani 1 1 d . . . H70D H -0.2095 0.2868 0.5060 0.090 Uiso 1 1 calc R . . H70E H -0.2742 0.3320 0.4665 0.090 Uiso 1 1 calc R . . H70F H -0.1668 0.3340 0.4694 0.090 Uiso 1 1 calc R . . C71B C -0.2453(5) 0.1968(3) 0.47000(15) 0.106(3) Uani 1 1 d . . . H71D H -0.2233 0.1528 0.4606 0.160 Uiso 1 1 calc R . . H71E H -0.3092 0.2214 0.4589 0.160 Uiso 1 1 calc R . . H71F H -0.2460 0.1865 0.5001 0.160 Uiso 1 1 calc R . . C72B C -0.0785(4) 0.2035(3) 0.46821(16) 0.116(3) Uani 1 1 d . . . H72D H -0.0738 0.1882 0.4982 0.173 Uiso 1 1 calc R . . H72E H -0.0376 0.2346 0.4590 0.173 Uiso 1 1 calc R . . H72F H -0.0586 0.1625 0.4559 0.173 Uiso 1 1 calc R . . C73B C -0.3237(3) 0.4983(2) 0.18510(11) 0.0305(10) Uani 1 1 d . . . H73C H -0.3915 0.5231 0.1807 0.037 Uiso 1 1 calc R . . H73D H -0.3094 0.4616 0.1688 0.037 Uiso 1 1 calc R . . C74B C -0.2674(3) 0.54982(18) 0.16877(11) 0.0251(9) Uani 1 1 d . . . C75B C -0.1739(3) 0.53649(19) 0.18117(10) 0.0240(9) Uani 1 1 d . A . C76B C -0.1228(3) 0.58555(19) 0.16463(11) 0.0276(9) Uani 1 1 d . . . C77B C -0.1662(3) 0.64456(19) 0.13532(12) 0.0322(10) Uani 1 1 d . . . H77B H -0.1314 0.6773 0.1243 0.039 Uiso 1 1 calc R . . C78B C -0.2585(3) 0.65813(19) 0.12128(11) 0.0328(10) Uani 1 1 d . . . C79B C -0.3083(3) 0.61020(19) 0.13892(11) 0.0298(10) Uani 1 1 d . . . H79B H -0.3721 0.6187 0.1304 0.036 Uiso 1 1 calc R . . C80B C -0.0221(3) 0.5713(2) 0.17867(12) 0.0348(10) Uani 1 1 d . . . H80D H 0.0063 0.6061 0.1618 0.052 Uiso 1 1 calc R . . H80E H 0.0132 0.5242 0.1758 0.052 Uiso 1 1 calc R . . H80F H -0.0202 0.5742 0.2076 0.052 Uiso 1 1 calc R . . C81B C -0.3025(3) 0.7250(2) 0.08820(12) 0.0432(12) Uani 1 1 d . . . C82B C -0.3073(4) 0.7899(2) 0.10594(15) 0.0744(18) Uani 1 1 d . . . H82D H -0.3328 0.8326 0.0848 0.112 Uiso 1 1 calc R . . H82E H -0.2438 0.7887 0.1145 0.112 Uiso 1 1 calc R . . H82F H -0.3483 0.7895 0.1297 0.112 Uiso 1 1 calc R . . C83B C -0.3997(3) 0.7280(2) 0.07361(15) 0.0663(16) Uani 1 1 d . . . H83D H -0.3961 0.6876 0.0615 0.100 Uiso 1 1 calc R . . H83E H -0.4242 0.7715 0.0529 0.100 Uiso 1 1 calc R . . H83F H -0.4418 0.7268 0.0970 0.100 Uiso 1 1 calc R . . C84B C -0.2389(4) 0.7266(3) 0.05034(13) 0.0680(16) Uani 1 1 d . . . H84D H -0.2370 0.6862 0.0385 0.102 Uiso 1 1 calc R . . H84E H -0.1750 0.7246 0.0588 0.102 Uiso 1 1 calc R . . H84F H -0.2645 0.7700 0.0298 0.102 Uiso 1 1 calc R . . C85B C -0.0201(2) 0.20594(19) 0.26807(12) 0.0259(9) Uani 1 1 d . . . H85B H -0.0710 0.2462 0.2684 0.031 Uiso 1 1 calc R . . C86B C -0.0048(3) 0.15122(19) 0.30168(12) 0.0340(10) Uani 1 1 d . . . H86B H -0.0441 0.1540 0.3248 0.041 Uiso 1 1 calc R . . C87B C 0.0685(3) 0.0916(2) 0.30172(14) 0.0421(12) Uani 1 1 d . . . H87B H 0.0816 0.0533 0.3249 0.050 Uiso 1 1 calc R . . C88B C 0.1215(3) 0.0898(2) 0.26710(13) 0.0359(11) Uani 1 1 d . . . H88B H 0.1712 0.0493 0.2658 0.043 Uiso 1 1 calc R . . C89B C 0.1027(3) 0.14639(19) 0.23432(12) 0.0279(9) Uani 1 1 d . . . H89B H 0.1399 0.1437 0.2106 0.033 Uiso 1 1 calc R . . C90B C -0.0633(3) 0.4267(2) 0.12959(11) 0.0321(10) Uani 1 1 d . . . H90B H -0.1207 0.4159 0.1381 0.039 Uiso 1 1 calc R . . C91B C -0.0680(3) 0.4887(2) 0.10125(12) 0.0360(11) Uani 1 1 d . . . H91B H -0.1273 0.5192 0.0907 0.043 Uiso 1 1 calc R . . C92B C 0.0140(3) 0.5059(2) 0.08843(12) 0.0382(11) Uani 1 1 d . . . H92B H 0.0125 0.5481 0.0690 0.046 Uiso 1 1 calc R . . C93B C 0.0983(3) 0.4600(2) 0.10461(12) 0.0361(10) Uani 1 1 d . . . H93B H 0.1563 0.4704 0.0967 0.043 Uiso 1 1 calc R . . C94B C 0.0974(3) 0.3986(2) 0.13265(12) 0.0320(10) Uani 1 1 d . . . H94B H 0.1562 0.3672 0.1432 0.038 Uiso 1 1 calc R . . Fe1A Fe 0.79042(3) 0.76623(3) 0.348099(15) 0.01859(13) Uani 1 1 d . . . Fe1B Fe 0.02328(4) 0.29179(3) 0.189655(16) 0.02333(14) Uani 1 1 d . . . N1A N 0.92560(19) 0.73147(15) 0.34767(8) 0.0197(7) Uani 1 1 d . . . N2A N 0.80565(19) 0.67523(14) 0.38472(8) 0.0190(7) Uani 1 1 d . . . N3A N 0.65530(19) 0.80263(14) 0.34877(8) 0.0190(7) Uani 1 1 d . . . N4A N 0.7766(2) 0.85292(15) 0.30761(9) 0.0222(7) Uani 1 1 d . . . N5A N 1.1157(2) 0.84303(14) 0.30038(10) 0.0272(8) Uani 1 1 d . . . N6A N 0.9758(2) 0.93728(18) 0.24326(11) 0.0466(10) Uani 1 1 d . . . N7A N 0.60356(19) 0.59315(14) 0.45555(9) 0.0216(7) Uani 1 1 d . . . N8A N 0.4742(2) 0.72900(14) 0.43307(9) 0.0234(7) Uani 1 1 d . . . N9A N 0.8033(2) 0.81427(14) 0.39482(8) 0.0209(7) Uani 1 1 d . . . N10A N 0.7729(2) 0.72516(14) 0.30040(9) 0.0225(7) Uani 1 1 d . . . N1B N 0.0123(2) 0.23557(15) 0.15085(9) 0.0287(8) Uani 1 1 d . A . N2B N -0.1126(2) 0.31149(15) 0.18687(9) 0.0259(7) Uani 1 1 d . A . N3B N 0.0348(2) 0.33723(14) 0.23376(8) 0.0202(7) Uani 1 1 d . A . N4B N 0.1592(2) 0.26991(14) 0.19351(9) 0.0239(7) Uani 1 1 d . A . N5B N 0.2120(2) 0.13213(18) 0.08149(10) 0.0402(9) Uani 1 1 d . . . N6B N 0.3427(2) 0.19682(17) 0.10726(10) 0.0385(9) Uani 1 1 d . . . N7B N -0.3061(2) 0.46318(15) 0.22968(9) 0.0245(7) Uani 1 1 d . . . N8B N -0.1750(2) 0.46235(14) 0.29110(9) 0.0219(7) Uani 1 1 d . . . N9B N 0.0338(2) 0.20562(15) 0.23434(9) 0.0237(7) Uani 1 1 d . A . N10B N 0.0183(2) 0.38056(15) 0.14586(9) 0.0265(8) Uani 1 1 d . A . O1A O 0.98924(15) 0.76691(11) 0.33180(7) 0.0224(6) Uani 1 1 d . . . O2A O 0.73651(15) 0.64432(11) 0.39899(7) 0.0205(6) Uani 1 1 d . . . O3A O 0.59383(15) 0.77595(11) 0.37445(7) 0.0207(6) Uani 1 1 d . . . O4A O 0.84135(17) 0.87018(13) 0.28070(8) 0.0334(7) Uani 1 1 d . . . O5A O 0.94258(17) 0.90731(12) 0.32904(8) 0.0319(7) Uani 1 1 d . . . O6A O 1.00244(18) 0.79615(14) 0.25378(8) 0.0371(7) Uani 1 1 d . . . O7A O 0.65951(16) 0.71639(12) 0.45378(7) 0.0235(6) Uani 1 1 d . . . O8A O 0.56303(16) 0.65600(11) 0.37394(7) 0.0215(6) Uani 1 1 d . . . O1B O 0.08137(18) 0.18771(13) 0.13701(7) 0.0329(7) Uani 1 1 d . . . O2B O -0.17757(16) 0.35979(12) 0.20206(7) 0.0255(6) Uani 1 1 d . . . O3B O -0.03411(16) 0.36545(12) 0.25747(7) 0.0232(6) Uani 1 1 d . . . O4B O 0.22303(17) 0.23903(12) 0.16862(7) 0.0280(6) Uani 1 1 d . . . O5B O 0.25421(18) 0.11040(13) 0.16354(8) 0.0356(7) Uani 1 1 d . . . O6B O 0.15998(18) 0.27378(13) 0.08780(7) 0.0326(7) Uani 1 1 d . . . O7B O -0.19842(17) 0.33832(12) 0.28037(7) 0.0256(6) Uani 1 1 d . . . O8B O -0.12846(16) 0.47796(12) 0.20796(7) 0.0244(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2A 0.050 0.050 0.050 0.000 0.000 0.000 Al1A 0.0194(6) 0.0307(7) 0.0302(7) 0.0030(6) 0.0065(5) -0.0058(5) Al2A 0.0191(6) 0.0218(6) 0.0208(6) -0.0061(5) 0.0055(5) -0.0071(5) Al1B 0.0350(8) 0.0370(7) 0.0245(7) -0.0136(6) -0.0030(5) 0.0013(6) Al2B 0.0222(6) 0.0236(6) 0.0231(6) -0.0051(5) 0.0006(5) -0.0075(5) C1A 0.019(2) 0.016(2) 0.021(2) -0.0053(17) 0.0009(16) -0.0026(16) C3A 0.024(2) 0.026(2) 0.029(2) -0.0091(18) 0.0028(17) -0.0055(18) C4A 0.027(2) 0.027(2) 0.039(3) -0.011(2) 0.0113(19) -0.0076(19) C5A 0.015(2) 0.025(2) 0.049(3) -0.003(2) -0.0013(19) -0.0041(17) C6A 0.032(3) 0.036(2) 0.030(2) -0.001(2) -0.0063(19) -0.010(2) C7A 0.022(2) 0.032(2) 0.026(2) -0.0058(18) 0.0030(17) -0.0071(18) C8A 0.022(2) 0.0084(18) 0.032(2) -0.0037(17) 0.0069(17) -0.0071(16) C9A 0.019(2) 0.0149(19) 0.024(2) -0.0016(17) -0.0007(16) -0.0070(16) C10A 0.022(2) 0.028(2) 0.028(2) -0.0066(19) 0.0038(17) -0.0102(18) C11A 0.031(2) 0.019(2) 0.038(3) -0.0057(19) -0.0024(19) -0.0060(18) C12A 0.036(3) 0.023(2) 0.040(3) 0.006(2) -0.005(2) -0.012(2) C13A 0.035(3) 0.035(3) 0.028(2) -0.002(2) 0.0057(19) -0.013(2) C14A 0.030(2) 0.023(2) 0.029(2) -0.0057(19) 0.0038(18) -0.0084(18) C15A 0.016(2) 0.029(2) 0.022(2) -0.0005(18) 0.0032(16) -0.0052(18) C16A 0.013(2) 0.064(3) 0.040(3) 0.019(3) 0.008(2) 0.003(2) C17A 0.040(3) 0.034(3) 0.095(4) 0.033(3) 0.026(3) 0.001(2) C18A 0.040(4) 0.059(4) 0.159(7) 0.057(5) 0.033(4) 0.009(3) C19A 0.022(4) 0.208(10) 0.089(6) 0.088(8) 0.005(4) 0.000(5) C20A 0.039(4) 0.202(9) 0.075(5) 0.058(7) -0.005(3) -0.015(5) C21A 0.042(3) 0.142(6) 0.033(3) 0.030(4) -0.004(2) -0.013(3) C22A 0.020(2) 0.021(2) 0.018(2) -0.0029(17) 0.0019(16) -0.0081(17) C23A 0.019(2) 0.024(2) 0.020(2) -0.0015(17) 0.0019(16) -0.0055(17) C24A 0.027(2) 0.032(2) 0.024(2) -0.0047(19) -0.0005(17) -0.0079(19) C25A 0.037(3) 0.037(3) 0.028(2) -0.007(2) 0.002(2) 0.006(2) C26A 0.027(3) 0.045(3) 0.043(3) 0.004(2) 0.008(2) 0.006(2) C27A 0.022(3) 0.055(3) 0.058(3) 0.017(3) -0.006(2) -0.018(2) C28A 0.027(2) 0.031(2) 0.040(3) 0.001(2) -0.0074(19) -0.013(2) C29A 0.022(2) 0.028(2) 0.045(3) -0.012(2) 0.0073(19) -0.0061(18) C30A 0.027(2) 0.028(2) 0.052(3) -0.001(2) 0.018(2) -0.0115(19) C31A 0.034(3) 0.039(3) 0.046(3) 0.009(2) 0.020(2) -0.011(2) C32A 0.042(3) 0.035(3) 0.083(4) 0.029(3) 0.024(3) 0.003(2) C33A 0.018(2) 0.025(2) 0.041(3) -0.0060(19) 0.0040(18) -0.0080(17) C34A 0.025(2) 0.019(2) 0.048(3) -0.005(2) 0.0151(19) -0.0073(18) C35A 0.028(3) 0.020(2) 0.046(3) -0.002(2) 0.015(2) -0.0102(19) C36A 0.029(3) 0.022(2) 0.058(3) -0.007(2) 0.018(2) -0.008(2) C37A 0.046(3) 0.026(2) 0.067(3) -0.020(2) 0.030(2) -0.017(2) C38A 0.039(3) 0.028(2) 0.054(3) -0.011(2) 0.024(2) -0.021(2) C39A 0.029(2) 0.023(2) 0.049(3) -0.009(2) 0.017(2) -0.0118(19) C40A 0.038(3) 0.029(2) 0.084(4) -0.011(2) 0.030(3) -0.004(2) C41A 0.048(3) 0.039(3) 0.061(3) -0.025(2) 0.030(2) -0.031(2) C42A 0.069(4) 0.044(3) 0.048(3) -0.013(2) 0.020(2) -0.036(3) C43A 0.058(3) 0.043(3) 0.081(4) -0.027(3) 0.017(3) -0.031(2) C44A 0.085(4) 0.067(3) 0.071(4) -0.037(3) 0.046(3) -0.046(3) C45A 0.032(3) 0.106(5) 0.054(4) 0.035(3) 0.008(3) -0.008(3) C46A 0.040(3) 0.121(5) 0.026(3) 0.000(3) 0.006(2) -0.043(3) C47A 0.038(3) 0.107(4) 0.027(3) -0.014(3) 0.010(2) -0.043(3) C48A 0.060(4) 0.132(5) 0.037(3) -0.044(4) 0.026(3) -0.069(4) C49A 0.118(6) 0.189(8) 0.054(4) -0.063(5) 0.047(4) -0.118(6) C50A 0.114(6) 0.216(9) 0.023(3) -0.017(5) 0.017(3) -0.124(6) C51A 0.069(4) 0.198(8) 0.035(4) 0.002(4) 0.009(3) -0.086(5) C52A 0.060(4) 0.099(4) 0.074(4) -0.061(4) 0.033(3) -0.044(3) C53A 0.210(10) 0.389(15) 0.029(4) -0.050(7) 0.032(5) -0.248(11) C54A 0.321(15) 0.366(17) 0.045(5) 0.009(7) -0.029(7) -0.266(14) C55A 0.262(11) 0.397(14) 0.049(4) -0.080(6) 0.081(6) -0.274(11) C56A 0.457(19) 0.210(11) 0.037(5) -0.064(6) 0.064(7) -0.155(12) C57A 0.034(2) 0.032(2) 0.020(2) -0.0024(18) 0.0025(18) -0.0111(19) C58A 0.025(2) 0.029(2) 0.027(2) -0.0065(18) 0.0099(17) -0.0138(18) C59A 0.025(2) 0.030(2) 0.033(2) -0.0091(19) 0.0116(18) -0.0137(18) C60A 0.014(2) 0.039(2) 0.038(3) -0.016(2) 0.0057(18) -0.0053(18) C61A 0.021(2) 0.027(2) 0.032(2) -0.0097(18) 0.0100(17) -0.0078(18) C62A 0.032(2) 0.023(2) 0.024(2) -0.0061(18) 0.0092(18) -0.0147(19) C63A 0.031(2) 0.024(2) 0.020(2) -0.0046(18) 0.0102(17) -0.0148(19) C64A 0.030(2) 0.029(2) 0.022(2) -0.0057(18) 0.0012(17) -0.0135(19) C65A 0.050(3) 0.034(2) 0.019(2) -0.0077(19) 0.0020(19) -0.022(2) C66A 0.045(3) 0.030(2) 0.029(2) -0.0141(19) 0.015(2) -0.020(2) C67A 0.033(2) 0.024(2) 0.033(2) -0.0098(19) 0.0160(19) -0.0127(19) C68A 0.042(3) 0.039(2) 0.025(2) -0.013(2) -0.0040(19) -0.013(2) C69A 0.050(3) 0.045(3) 0.042(3) -0.025(2) 0.020(2) -0.024(2) C70A 0.090(4) 0.035(3) 0.031(3) -0.012(2) 0.008(2) -0.021(3) C71A 0.217(8) 0.044(3) 0.041(3) -0.024(3) 0.060(4) -0.056(4) C72A 0.058(4) 0.162(6) 0.135(6) -0.130(5) 0.037(4) -0.032(4) C73A 0.026(2) 0.019(2) 0.027(2) -0.0047(17) 0.0063(17) -0.0076(17) C74A 0.017(2) 0.027(2) 0.026(2) -0.0086(18) 0.0042(16) -0.0071(17) C75A 0.015(2) 0.025(2) 0.025(2) -0.0123(18) 0.0087(16) -0.0079(17) C76A 0.017(2) 0.027(2) 0.024(2) -0.0112(18) 0.0094(16) -0.0076(17) C77A 0.018(2) 0.032(2) 0.026(2) -0.0116(19) 0.0056(17) -0.0087(18) C78A 0.023(2) 0.026(2) 0.032(2) -0.013(2) 0.0100(18) -0.0075(18) C79A 0.018(2) 0.024(2) 0.032(2) -0.0095(18) 0.0083(17) -0.0046(17) C80A 0.026(2) 0.034(2) 0.028(2) -0.0094(19) -0.0037(17) -0.0066(19) C81A 0.027(2) 0.032(2) 0.040(3) -0.016(2) 0.0058(19) -0.0157(19) C82A 0.046(3) 0.027(2) 0.056(3) -0.015(2) 0.011(2) -0.009(2) C83A 0.058(3) 0.036(3) 0.052(3) -0.021(2) 0.004(2) -0.027(2) C84A 0.044(3) 0.037(2) 0.043(3) -0.013(2) 0.009(2) -0.023(2) C85A 0.026(2) 0.029(2) 0.034(2) -0.0091(19) 0.0019(18) -0.0123(19) C86A 0.038(3) 0.057(3) 0.043(3) -0.021(2) 0.001(2) -0.026(2) C87A 0.060(3) 0.058(3) 0.045(3) -0.034(2) 0.014(2) -0.032(3) C88A 0.052(3) 0.029(2) 0.030(2) -0.015(2) 0.016(2) -0.017(2) C89A 0.032(2) 0.023(2) 0.025(2) -0.0067(18) 0.0031(18) -0.0101(18) C90A 0.018(2) 0.026(2) 0.025(2) -0.0089(18) 0.0055(16) -0.0054(17) C91A 0.020(2) 0.026(2) 0.028(2) -0.0113(18) 0.0011(17) -0.0056(17) C92A 0.033(2) 0.030(2) 0.020(2) -0.0089(18) -0.0016(18) -0.0025(19) C93A 0.034(2) 0.036(2) 0.024(2) -0.0111(19) 0.0102(18) -0.013(2) C94A 0.026(2) 0.041(2) 0.025(2) -0.013(2) 0.0050(18) -0.0082(19) C1B 0.037(3) 0.024(2) 0.025(2) -0.0074(18) -0.0069(18) -0.0068(19) C2B 0.028(2) 0.024(2) 0.025(2) -0.0060(18) -0.0079(17) -0.0068(18) C3B 0.051(11) 0.063(12) 0.049(12) -0.018(10) 0.024(9) -0.048(10) C4B 0.039(8) 0.059(9) 0.031(8) -0.026(7) -0.009(6) 0.001(7) C5B 0.063(11) 0.089(12) 0.062(12) -0.039(9) -0.007(9) -0.011(10) C6B 0.21(3) 0.16(2) 0.059(12) -0.064(13) 0.067(14) -0.16(2) C7B 0.22(2) 0.078(11) 0.065(11) -0.037(9) 0.035(13) -0.109(14) C8B 0.20(2) 0.067(11) 0.027(8) -0.008(7) 0.009(10) -0.087(12) C3C 0.035(5) 0.029(6) 0.022(5) -0.009(4) -0.010(4) -0.010(4) C4C 0.053(6) 0.053(6) 0.030(5) -0.016(4) 0.008(4) -0.031(5) C5C 0.077(7) 0.102(9) 0.029(5) -0.036(6) 0.006(5) -0.058(7) C6C 0.103(9) 0.103(8) 0.042(7) -0.036(6) 0.004(6) -0.070(7) C7C 0.066(6) 0.057(5) 0.050(5) -0.021(4) 0.012(4) -0.043(5) C8C 0.031(4) 0.035(4) 0.036(4) -0.016(3) 0.017(3) -0.020(3) C9B 0.030(2) 0.030(2) 0.028(2) -0.009(2) -0.0007(19) -0.015(2) C10B 0.045(9) 0.033(7) 0.030(7) -0.011(5) 0.028(6) -0.013(6) C11B 0.040(9) 0.066(10) 0.072(11) -0.043(9) 0.027(7) -0.033(8) C12B 0.037(3) 0.100(5) 0.078(4) -0.014(4) -0.010(3) -0.040(3) C13B 0.039(5) 0.088(9) 0.042(8) -0.013(4) -0.011(5) -0.015(6) C14B 0.037(8) 0.093(14) 0.032(8) -0.018(8) -0.009(6) -0.011(9) C10C 0.044(9) 0.094(13) 0.073(12) 0.041(9) -0.025(8) -0.042(9) C11C 0.060(13) 0.121(17) 0.092(14) 0.036(12) -0.022(10) -0.071(12) C12C 0.037(3) 0.100(5) 0.078(4) -0.014(4) -0.010(3) -0.040(3) C13C 0.039(5) 0.088(9) 0.042(8) -0.013(4) -0.011(5) -0.015(6) C14C 0.029(6) 0.058(9) 0.040(8) 0.014(6) 0.001(6) -0.022(7) C15B 0.027(2) 0.021(2) 0.020(2) -0.0040(17) -0.0005(17) -0.0077(17) C16B 0.028(2) 0.025(2) 0.019(2) -0.0051(17) 0.0002(17) -0.0099(18) C17B 0.026(2) 0.034(2) 0.023(2) -0.0115(19) 0.0034(17) -0.010(2) C18B 0.029(3) 0.053(3) 0.092(4) -0.051(3) 0.009(2) -0.011(2) C19B 0.035(3) 0.086(4) 0.134(5) -0.081(4) -0.001(3) -0.015(3) C20B 0.027(3) 0.091(4) 0.087(4) -0.053(3) -0.010(3) -0.002(3) C21B 0.032(3) 0.054(3) 0.044(3) -0.009(2) -0.008(2) 0.001(2) C22B 0.032(3) 0.039(3) 0.034(3) -0.006(2) -0.0025(19) -0.010(2) C23B 0.017(2) 0.048(3) 0.025(2) -0.013(2) 0.0027(17) -0.0016(19) C24B 0.028(3) 0.072(3) 0.063(3) -0.049(3) 0.010(2) -0.021(2) C25B 0.028(3) 0.119(5) 0.109(5) -0.086(5) 0.011(3) -0.024(3) C26B 0.023(3) 0.185(8) 0.084(5) -0.096(6) 0.002(3) -0.005(4) C27B 0.041(4) 0.162(7) 0.036(3) -0.033(4) -0.014(2) 0.022(4) C28B 0.042(3) 0.099(4) 0.031(3) -0.019(3) -0.008(2) 0.007(3) C29B 0.054(3) 0.062(3) 0.027(3) -0.023(2) -0.007(2) 0.000(2) C30B 0.051(3) 0.062(3) 0.039(3) -0.033(3) 0.001(2) 0.003(3) C31B 0.038(3) 0.066(3) 0.029(3) -0.018(2) 0.007(2) 0.008(2) C32B 0.034(3) 0.053(3) 0.037(3) -0.012(2) -0.009(2) 0.009(2) C33B 0.025(2) 0.034(2) 0.043(3) -0.007(2) -0.0005(19) -0.0129(19) C34B 0.028(2) 0.023(2) 0.035(2) -0.0060(19) 0.0056(18) -0.0062(18) C35B 0.022(2) 0.027(2) 0.027(2) -0.0048(18) 0.0038(17) -0.0071(18) C36B 0.033(2) 0.023(2) 0.031(2) -0.0049(18) 0.0010(18) -0.0122(18) C37B 0.060(3) 0.039(3) 0.041(3) -0.021(2) -0.007(2) -0.007(2) C38B 0.052(3) 0.041(3) 0.041(3) -0.019(2) -0.004(2) -0.004(2) C39B 0.037(3) 0.033(3) 0.033(3) -0.017(2) -0.005(2) 0.004(2) C40B 0.036(3) 0.033(2) 0.034(3) -0.015(2) -0.002(2) -0.002(2) C41B 0.046(3) 0.033(3) 0.045(3) -0.013(2) -0.001(2) 0.005(2) C42B 0.051(3) 0.042(3) 0.048(3) -0.021(2) 0.007(2) -0.002(2) C43B 0.052(3) 0.050(3) 0.049(3) -0.029(3) -0.004(2) -0.007(2) C44B 0.038(3) 0.035(2) 0.035(3) -0.010(2) -0.006(2) -0.002(2) C45B 0.134(5) 0.045(2) 0.161(5) -0.051(3) 0.096(4) -0.035(3) C46B 0.303(12) 0.035(4) 0.229(10) -0.058(5) -0.206(9) 0.085(5) C47B 0.130(6) 0.054(4) 0.126(6) -0.053(4) 0.015(5) 0.022(4) C48B 0.134(5) 0.045(2) 0.161(5) -0.051(3) 0.096(4) -0.035(3) C49B 0.027(2) 0.059(3) 0.025(2) -0.012(2) 0.0011(18) -0.002(2) C50B 0.035(3) 0.047(3) 0.025(2) -0.013(2) 0.007(2) -0.004(2) C51B 0.032(3) 0.043(3) 0.021(2) -0.012(2) 0.0006(19) 0.000(2) C52B 0.032(3) 0.042(3) 0.022(2) -0.010(2) 0.0033(19) -0.002(2) C53B 0.044(3) 0.042(3) 0.029(3) -0.007(2) 0.002(2) 0.002(2) C54B 0.037(3) 0.049(3) 0.038(3) -0.008(2) 0.007(2) -0.011(2) C55B 0.030(3) 0.061(3) 0.033(3) -0.015(2) 0.002(2) -0.003(2) C56B 0.039(3) 0.047(3) 0.027(2) -0.010(2) 0.0012(19) 0.000(2) C57B 0.043(3) 0.058(3) 0.047(3) -0.007(3) -0.002(2) -0.009(3) C58B 0.066(4) 0.055(3) 0.082(4) -0.003(3) 0.023(3) -0.015(3) C59B 0.115(5) 0.077(4) 0.090(5) -0.014(4) 0.069(4) -0.032(4) C60B 0.116(6) 0.103(5) 0.133(6) 0.028(5) -0.050(5) -0.068(5) C61B 0.029(2) 0.023(2) 0.022(2) -0.0033(18) 0.0011(17) -0.0074(18) C62B 0.024(2) 0.019(2) 0.022(2) 0.0007(17) 0.0002(16) -0.0082(17) C63B 0.023(2) 0.022(2) 0.019(2) -0.0023(17) -0.0020(16) -0.0079(17) C64B 0.019(2) 0.022(2) 0.027(2) -0.0057(18) -0.0007(16) -0.0051(17) C65B 0.025(2) 0.025(2) 0.033(3) -0.0030(19) 0.0033(18) -0.0092(18) C66B 0.034(2) 0.027(2) 0.029(2) -0.0038(19) -0.0001(18) -0.0101(19) C67B 0.026(2) 0.027(2) 0.030(2) -0.0075(19) -0.0026(17) -0.0115(18) C68B 0.025(2) 0.026(2) 0.037(2) -0.0116(19) 0.0012(18) -0.0106(18) C69B 0.054(3) 0.031(2) 0.026(2) 0.002(2) -0.006(2) -0.016(2) C70B 0.089(4) 0.059(3) 0.038(3) -0.012(2) 0.030(3) -0.031(3) C71B 0.214(8) 0.115(5) 0.030(3) 0.004(3) 0.008(4) -0.128(5) C72B 0.089(5) 0.157(6) 0.033(3) 0.003(4) -0.015(3) 0.063(4) C73B 0.024(2) 0.037(2) 0.027(2) -0.0068(19) -0.0033(17) -0.0023(19) C74B 0.024(2) 0.023(2) 0.027(2) -0.0070(18) 0.0011(17) -0.0032(18) C75B 0.031(2) 0.028(2) 0.013(2) -0.0093(18) 0.0025(17) -0.0042(19) C76B 0.037(3) 0.026(2) 0.022(2) -0.0103(19) 0.0087(18) -0.0096(19) C77B 0.044(3) 0.025(2) 0.027(2) -0.0070(19) 0.013(2) -0.009(2) C78B 0.048(3) 0.022(2) 0.022(2) -0.0044(18) 0.005(2) 0.000(2) C79B 0.035(2) 0.030(2) 0.022(2) -0.0098(19) 0.0000(18) -0.001(2) C80B 0.045(3) 0.034(2) 0.028(2) -0.0035(19) 0.007(2) -0.018(2) C81B 0.061(3) 0.033(3) 0.024(2) -0.002(2) 0.004(2) 0.003(2) C82B 0.130(5) 0.028(3) 0.050(3) -0.004(2) 0.006(3) 0.000(3) C83B 0.070(4) 0.052(3) 0.049(3) 0.014(3) -0.004(3) 0.011(3) C84B 0.081(4) 0.070(4) 0.028(3) 0.010(3) 0.012(3) 0.003(3) C85B 0.020(2) 0.021(2) 0.037(2) -0.0088(19) 0.0028(18) -0.0044(17) C86B 0.032(3) 0.030(2) 0.038(3) 0.003(2) 0.0081(19) -0.014(2) C87B 0.029(3) 0.028(2) 0.059(3) 0.008(2) 0.009(2) -0.006(2) C88B 0.022(2) 0.020(2) 0.061(3) 0.001(2) 0.001(2) -0.0058(18) C89B 0.024(2) 0.025(2) 0.038(3) -0.010(2) -0.0034(18) -0.0099(19) C90B 0.036(3) 0.032(2) 0.026(2) -0.009(2) -0.0001(19) -0.003(2) C91B 0.048(3) 0.030(2) 0.022(2) -0.006(2) -0.001(2) 0.004(2) C92B 0.060(3) 0.027(2) 0.023(2) -0.0008(19) 0.008(2) -0.009(2) C93B 0.047(3) 0.033(2) 0.027(2) -0.006(2) 0.008(2) -0.011(2) C94B 0.034(3) 0.033(2) 0.027(2) -0.010(2) 0.0025(19) -0.003(2) Fe1A 0.0174(3) 0.0208(3) 0.0182(3) -0.0052(2) 0.0030(2) -0.0057(2) Fe1B 0.0259(3) 0.0233(3) 0.0216(3) -0.0075(2) -0.0027(2) -0.0054(2) N1A 0.0212(17) 0.0230(17) 0.0186(17) -0.0073(14) 0.0071(13) -0.0110(14) N2A 0.0240(18) 0.0217(17) 0.0174(17) -0.0092(13) 0.0040(13) -0.0128(14) N3A 0.0207(17) 0.0226(17) 0.0156(16) -0.0053(14) 0.0065(13) -0.0089(14) N4A 0.0166(18) 0.0275(18) 0.0225(18) -0.0029(14) 0.0067(13) -0.0087(15) N5A 0.0222(18) 0.0172(17) 0.039(2) -0.0025(15) 0.0079(15) -0.0041(14) N6A 0.028(2) 0.049(2) 0.045(2) 0.0177(19) 0.0110(18) -0.0044(18) N7A 0.0193(17) 0.0226(17) 0.0243(18) -0.0071(14) 0.0040(13) -0.0067(14) N8A 0.0219(18) 0.0217(17) 0.0297(19) -0.0089(15) 0.0075(14) -0.0093(14) N9A 0.0243(18) 0.0206(17) 0.0191(17) -0.0043(14) 0.0054(14) -0.0086(14) N10A 0.0195(18) 0.0269(18) 0.0206(17) -0.0059(14) 0.0035(13) -0.0054(14) N1B 0.032(2) 0.0272(19) 0.0248(19) -0.0049(15) -0.0051(15) -0.0047(16) N2B 0.031(2) 0.0229(17) 0.0230(18) -0.0046(15) -0.0064(15) -0.0059(15) N3B 0.0211(18) 0.0218(17) 0.0165(17) -0.0036(14) 0.0017(14) -0.0045(14) N4B 0.0280(19) 0.0231(17) 0.0196(18) -0.0066(15) -0.0001(14) -0.0037(15) N5B 0.038(2) 0.047(2) 0.030(2) -0.0170(18) -0.0051(17) 0.0054(18) N6B 0.037(2) 0.042(2) 0.032(2) -0.0158(18) 0.0015(16) 0.0031(17) N7B 0.0205(18) 0.0281(18) 0.0246(18) -0.0066(15) -0.0001(14) -0.0052(14) N8B 0.0270(18) 0.0176(16) 0.0215(18) -0.0009(14) 0.0023(14) -0.0097(14) N9B 0.0217(18) 0.0224(18) 0.0298(19) -0.0095(15) -0.0037(14) -0.0068(15) N10B 0.028(2) 0.0325(19) 0.0210(18) -0.0113(15) 0.0022(15) -0.0074(16) O1A 0.0190(14) 0.0194(13) 0.0302(15) -0.0044(11) 0.0083(11) -0.0093(11) O2A 0.0196(14) 0.0211(13) 0.0249(14) -0.0082(11) 0.0076(11) -0.0110(11) O3A 0.0170(14) 0.0218(13) 0.0246(14) -0.0058(11) 0.0065(11) -0.0077(11) O4A 0.0207(15) 0.0392(16) 0.0315(16) 0.0077(13) 0.0088(12) -0.0072(12) O5A 0.0218(15) 0.0219(14) 0.0489(18) -0.0042(13) 0.0093(13) -0.0046(12) O6A 0.0308(17) 0.0561(19) 0.0265(17) -0.0116(14) 0.0096(12) -0.0141(14) O7A 0.0270(15) 0.0257(14) 0.0226(14) -0.0112(12) 0.0075(11) -0.0113(12) O8A 0.0241(14) 0.0229(14) 0.0211(14) -0.0069(11) 0.0031(11) -0.0107(11) O1B 0.0383(17) 0.0302(15) 0.0298(16) -0.0161(13) -0.0028(13) -0.0003(13) O2B 0.0216(15) 0.0280(14) 0.0278(15) -0.0106(12) 0.0012(11) -0.0048(12) O3B 0.0250(15) 0.0269(14) 0.0187(14) -0.0077(11) 0.0023(11) -0.0067(12) O4B 0.0278(15) 0.0335(15) 0.0220(15) -0.0129(12) 0.0029(12) -0.0022(12) O5B 0.0445(18) 0.0317(16) 0.0284(16) -0.0153(13) -0.0086(13) 0.0016(14) O6B 0.0336(16) 0.0393(16) 0.0194(15) -0.0058(13) 0.0027(12) -0.0012(13) O7B 0.0321(16) 0.0226(14) 0.0247(16) -0.0073(12) 0.0013(12) -0.0103(12) O8B 0.0243(15) 0.0229(14) 0.0255(15) -0.0028(12) -0.0003(11) -0.0071(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2A N2A 1.353(3) . ? C2A C9A 1.429(3) . ? C2A C1A 1.473(3) . ? Al1A O5A 1.833(3) . ? Al1A O6A 1.837(3) . ? Al1A O4A 1.844(3) . ? Al1A O1A 1.862(2) . ? Al1A N6A 2.144(3) . ? Al1A N5A 2.155(3) . ? Al2A O7A 1.817(3) . ? Al2A O8A 1.832(3) . ? Al2A O2A 1.856(2) . ? Al2A O3A 1.872(2) . ? Al2A N8A 2.173(3) . ? Al2A N7A 2.206(3) . ? Al1B O6B 1.821(3) . ? Al1B O5B 1.838(3) . ? Al1B O1B 1.847(3) . ? Al1B O4B 1.868(3) . ? Al1B N6B 2.153(4) . ? Al1B N5B 2.179(3) . ? Al2B O8B 1.817(2) . ? Al2B O7B 1.835(3) . ? Al2B O3B 1.848(3) . ? Al2B O2B 1.866(3) . ? Al2B N8B 2.155(3) . ? Al2B N7B 2.160(3) . ? C1A N1A 1.311(4) . ? C1A C8A 1.495(4) . ? C3A C4A 1.3900 . ? C3A C8A 1.3900 . ? C4A C5A 1.3900 . ? C5A C6A 1.3900 . ? C6A C7A 1.3900 . ? C7A C8A 1.3900 . ? C9A C10A 1.378(5) . ? C9A C14A 1.390(5) . ? C10A C11A 1.386(5) . ? C11A C12A 1.381(5) . ? C12A C13A 1.373(5) . ? C13A C14A 1.377(5) . ? C15A N4A 1.300(4) . ? C15A C22A 1.456(5) . ? C15A C16A 1.507(5) . ? C16A C21A 1.378(7) . ? C16A C17A 1.392(7) . ? C17A C18A 1.401(7) . ? C18A C19A 1.362(11) . ? C19A C20A 1.381(12) . ? C20A C21A 1.411(8) . ? C22A N3A 1.314(4) . ? C22A C23A 1.470(5) . ? C23A C28A 1.380(5) . ? C23A C24A 1.390(5) . ? C24A C25A 1.393(5) . ? C25A C26A 1.359(6) . ? C26A C27A 1.375(6) . ? C27A C28A 1.386(5) . ? C29A N5A 1.481(4) . ? C30A N5A 1.494(4) . ? C30A C31A 1.505(6) . ? C31A N6A 1.488(5) . ? C32A N6A 1.492(5) . ? C33A N5A 1.496(5) . ? C33A C34A 1.497(5) . ? C34A C35A 1.393(5) . ? C34A C39A 1.394(5) . ? C35A O5A 1.337(5) . ? C35A C36A 1.418(5) . ? C36A C37A 1.386(6) . ? C36A C40A 1.506(5) . ? C37A C38A 1.396(6) . ? C38A C39A 1.376(5) . ? C38A C41A 1.546(6) . ? C41A C42A 1.527(6) . ? C41A C43A 1.535(5) . ? C41A C44A 1.540(6) . ? C45A C46A 1.494(7) . ? C45A N6A 1.498(6) . ? C46A C51A 1.400(7) . ? C46A C47A 1.404(7) . ? C47A O6A 1.330(5) . ? C47A C48A 1.417(7) . ? C48A C49A 1.404(7) . ? C48A C52A 1.524(7) . ? C49A C50A 1.396(10) . ? C50A C51A 1.386(10) . ? C50A C53A 1.536(8) . ? C53A C56A 1.455(13) . ? C53A C55A 1.505(8) . ? C53A C54A 1.572(14) . ? C57A N7A 1.490(4) . ? C58A N7A 1.484(4) . ? C58A C59A 1.514(5) . ? C59A N8A 1.491(4) . ? C60A N8A 1.478(4) . ? C61A C62A 1.498(5) . ? C61A N8A 1.504(4) . ? C62A C67A 1.399(5) . ? C62A C63A 1.405(5) . ? C63A O7A 1.337(4) . ? C63A C64A 1.418(5) . ? C64A C65A 1.386(5) . ? C64A C68A 1.499(5) . ? C65A C66A 1.402(5) . ? C66A C67A 1.383(5) . ? C66A C69A 1.536(5) . ? C69A C71A 1.499(6) . ? C69A C70A 1.512(5) . ? C69A C72A 1.533(6) . ? C73A N7A 1.494(4) . ? C73A C74A 1.503(5) . ? C74A C79A 1.382(5) . ? C74A C75A 1.424(5) . ? C75A O8A 1.334(4) . ? C75A C76A 1.399(5) . ? C76A C77A 1.397(5) . ? C76A C80A 1.501(5) . ? C77A C78A 1.384(5) . ? C78A C79A 1.393(5) . ? C78A C81A 1.542(5) . ? C81A C82A 1.524(5) . ? C81A C84A 1.529(5) . ? C81A C83A 1.540(5) . ? C85A N9A 1.353(4) . ? C85A C86A 1.376(5) . ? C86A C87A 1.372(6) . ? C87A C88A 1.360(6) . ? C88A C89A 1.383(5) . ? C89A N9A 1.355(4) . ? C90A N10A 1.346(4) . ? C90A C91A 1.374(5) . ? C91A C92A 1.388(5) . ? C92A C93A 1.381(5) . ? C93A C94A 1.373(5) . ? C94A N10A 1.358(4) . ? C1B N1B 1.314(5) . ? C1B C2B 1.456(5) . ? C1B C3B 1.470(5) . ? C1B C3C 1.511(4) . ? C2B N2B 1.314(4) . ? C2B C9B 1.472(5) . ? C3B C4B 1.3900 . ? C3B C8B 1.3900 . ? C4B C5B 1.3900 . ? C5B C6B 1.3900 . ? C6B C7B 1.3900 . ? C7B C8B 1.3900 . ? C3C C4C 1.3900 . ? C3C C8C 1.3900 . ? C4C C5C 1.3900 . ? C5C C6C 1.3900 . ? C6C C7C 1.3900 . ? C7C C8C 1.3900 . ? C9B C10C 1.283(14) . ? C9B C14B 1.371(17) . ? C9B C14C 1.372(15) . ? C9B C10B 1.508(14) . ? C10B C11B 1.37(3) . ? C11B C12B 1.33(2) . ? C12B C13B 1.439(17) . ? C13B C14B 1.41(2) . ? C10C C11C 1.39(2) . ? C13C C14C 1.397(19) . ? C15B N4B 1.318(4) . ? C15B C16B 1.457(5) . ? C15B C17B 1.478(5) . ? C16B N3B 1.306(4) . ? C16B C23B 1.484(5) . ? C17B C18B 1.375(5) . ? C17B C22B 1.392(5) . ? C18B C19B 1.398(6) . ? C19B C20B 1.366(7) . ? C20B C21B 1.356(6) . ? C21B C22B 1.373(5) . ? C23B C28B 1.360(6) . ? C23B C24B 1.398(5) . ? C24B C25B 1.362(6) . ? C25B C26B 1.326(8) . ? C26B C27B 1.371(8) . ? C27B C28B 1.440(7) . ? C29B N5B 1.493(5) . ? C30B N5B 1.475(5) . ? C30B C31B 1.516(6) . ? C31B N6B 1.485(5) . ? C32B N6B 1.488(5) . ? C33B N7B 1.491(4) . ? C34B N7B 1.498(4) . ? C34B C35B 1.512(5) . ? C35B N8B 1.489(4) . ? C36B N8B 1.487(4) . ? C37B C38B 1.498(6) . ? C37B N5B 1.508(5) . ? C38B C43B 1.396(6) . ? C38B C39B 1.398(5) . ? C39B O5B 1.341(4) . ? C39B C40B 1.400(5) . ? C40B C41B 1.398(5) . ? C40B C44B 1.495(5) . ? C41B C42B 1.398(6) . ? C42B C43B 1.385(6) . ? C42B C45B 1.548(6) . ? C45B C46B 1.461(9) . ? C45B C48B 1.487(8) . ? C45B C47B 1.506(8) . ? C49B N6B 1.492(5) . ? C49B C50B 1.508(5) . ? C50B C51B 1.394(5) . ? C50B C55B 1.395(6) . ? C51B O6B 1.329(4) . ? C51B C52B 1.406(5) . ? C52B C53B 1.396(5) . ? C52B C56B 1.503(5) . ? C53B C54B 1.398(6) . ? C54B C55B 1.379(6) . ? C54B C57B 1.537(6) . ? C57B C60B 1.497(7) . ? C57B C58B 1.516(6) . ? C57B C59B 1.520(7) . ? C61B N8B 1.489(4) . ? C61B C62B 1.511(5) . ? C62B C67B 1.387(5) . ? C62B C63B 1.396(5) . ? C63B O7B 1.337(4) . ? C63B C64B 1.411(5) . ? C64B C65B 1.385(5) . ? C64B C68B 1.498(5) . ? C65B C66B 1.403(5) . ? C66B C67B 1.389(5) . ? C66B C69B 1.537(5) . ? C69B C72B 1.512(6) . ? C69B C71B 1.519(6) . ? C69B C70B 1.525(6) . ? C73B N7B 1.498(4) . ? C73B C74B 1.504(5) . ? C74B C75B 1.389(5) . ? C74B C79B 1.399(5) . ? C75B O8B 1.341(4) . ? C75B C76B 1.414(5) . ? C76B C77B 1.382(5) . ? C76B C80B 1.503(5) . ? C77B C78B 1.389(5) . ? C78B C79B 1.391(5) . ? C78B C81B 1.546(5) . ? C81B C83B 1.510(6) . ? C81B C82B 1.542(6) . ? C81B C84B 1.546(6) . ? C85B N9B 1.355(4) . ? C85B C86B 1.368(5) . ? C86B C87B 1.387(5) . ? C87B C88B 1.373(6) . ? C88B C89B 1.372(5) . ? C89B N9B 1.348(4) . ? C90B N10B 1.351(4) . ? C90B C91B 1.383(5) . ? C91B C92B 1.374(5) . ? C92B C93B 1.378(5) . ? C93B C94B 1.387(5) . ? C94B N10B 1.346(5) . ? Fe1A N1A 1.926(3) . ? Fe1A N3A 1.928(3) . ? Fe1A N4A 1.932(3) . ? Fe1A N2A 1.936(3) . ? Fe1A N10A 2.006(3) . ? Fe1A N9A 2.051(3) . ? Fe1B N4B 1.934(3) . ? Fe1B N2B 1.934(3) . ? Fe1B N3B 1.935(3) . ? Fe1B N1B 1.942(3) . ? Fe1B N9B 2.005(3) . ? Fe1B N10B 2.038(3) . ? N1A O1A 1.356(3) . ? N2A O2A 1.356(3) . ? N3A O3A 1.362(3) . ? N4A O4A 1.350(3) . ? N1B O1B 1.350(4) . ? N2B O2B 1.347(4) . ? N3B O3B 1.347(3) . ? N4B O4B 1.350(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2A C2A C9A 125.37(17) . . ? N2A C2A C1A 109.53(17) . . ? C9A C2A C1A 125.10(19) . . ? O5A Al1A O6A 175.54(13) . . ? O5A Al1A O4A 89.55(12) . . ? O6A Al1A O4A 93.76(13) . . ? O5A Al1A O1A 95.09(12) . . ? O6A Al1A O1A 87.18(12) . . ? O4A Al1A O1A 101.63(11) . . ? O5A Al1A N6A 90.97(14) . . ? O6A Al1A N6A 86.09(14) . . ? O4A Al1A N6A 89.14(12) . . ? O1A Al1A N6A 167.66(13) . . ? O5A Al1A N5A 87.88(12) . . ? O6A Al1A N5A 88.41(12) . . ? O4A Al1A N5A 171.35(12) . . ? O1A Al1A N5A 86.83(11) . . ? N6A Al1A N5A 82.65(13) . . ? O7A Al2A O8A 173.18(11) . . ? O7A Al2A O2A 91.43(11) . . ? O8A Al2A O2A 91.87(11) . . ? O7A Al2A O3A 96.10(11) . . ? O8A Al2A O3A 89.08(11) . . ? O2A Al2A O3A 101.56(10) . . ? O7A Al2A N8A 87.45(11) . . ? O8A Al2A N8A 88.48(11) . . ? O2A Al2A N8A 172.25(11) . . ? O3A Al2A N8A 86.19(10) . . ? O7A Al2A N7A 88.71(11) . . ? O8A Al2A N7A 85.27(11) . . ? O2A Al2A N7A 91.02(10) . . ? O3A Al2A N7A 166.39(11) . . ? N8A Al2A N7A 81.29(11) . . ? O6B Al1B O5B 173.83(13) . . ? O6B Al1B O1B 90.48(12) . . ? O5B Al1B O1B 92.71(13) . . ? O6B Al1B O4B 96.74(12) . . ? O5B Al1B O4B 87.74(12) . . ? O1B Al1B O4B 102.28(12) . . ? O6B Al1B N6B 86.74(13) . . ? O5B Al1B N6B 89.25(13) . . ? O1B Al1B N6B 170.31(13) . . ? O4B Al1B N6B 87.27(12) . . ? O6B Al1B N5B 89.27(13) . . ? O5B Al1B N5B 85.56(12) . . ? O1B Al1B N5B 88.23(13) . . ? O4B Al1B N5B 167.80(13) . . ? N6B Al1B N5B 82.46(13) . . ? O8B Al2B O7B 174.75(12) . . ? O8B Al2B O3B 89.38(11) . . ? O7B Al2B O3B 93.16(11) . . ? O8B Al2B O2B 95.85(11) . . ? O7B Al2B O2B 88.09(11) . . ? O3B Al2B O2B 102.51(11) . . ? O8B Al2B N8B 89.37(11) . . ? O7B Al2B N8B 86.04(11) . . ? O3B Al2B N8B 89.89(11) . . ? O2B Al2B N8B 166.56(12) . . ? O8B Al2B N7B 87.79(11) . . ? O7B Al2B N7B 89.11(11) . . ? O3B Al2B N7B 172.35(12) . . ? O2B Al2B N7B 84.86(11) . . ? N8B Al2B N7B 82.97(11) . . ? N1A C1A C2A 116.0(3) . . ? N1A C1A C8A 122.5(3) . . ? C2A C1A C8A 121.3(2) . . ? C4A C3A C8A 120.0 . . ? C3A C4A C5A 120.0 . . ? C6A C5A C4A 120.0 . . ? C7A C6A C5A 120.0 . . ? C6A C7A C8A 120.0 . . ? C7A C8A C3A 120.0 . . ? C7A C8A C1A 120.33(19) . . ? C3A C8A C1A 119.66(19) . . ? C10A C9A C14A 119.0(3) . . ? C10A C9A C2A 120.9(3) . . ? C14A C9A C2A 120.0(3) . . ? C9A C10A C11A 120.4(3) . . ? C12A C11A C10A 119.7(4) . . ? C13A C12A C11A 120.5(4) . . ? C12A C13A C14A 119.6(4) . . ? C13A C14A C9A 120.8(4) . . ? N4A C15A C22A 114.5(3) . . ? N4A C15A C16A 121.5(3) . . ? C22A C15A C16A 123.6(3) . . ? C21A C16A C17A 121.2(5) . . ? C21A C16A C15A 118.6(5) . . ? C17A C16A C15A 120.0(4) . . ? C16A C17A C18A 119.8(6) . . ? C19A C18A C17A 118.3(8) . . ? C18A C19A C20A 123.2(8) . . ? C19A C20A C21A 118.5(9) . . ? C16A C21A C20A 119.0(7) . . ? N3A C22A C15A 113.1(3) . . ? N3A C22A C23A 123.6(3) . . ? C15A C22A C23A 123.2(3) . . ? C28A C23A C24A 118.3(3) . . ? C28A C23A C22A 121.8(3) . . ? C24A C23A C22A 119.8(3) . . ? C23A C24A C25A 120.9(4) . . ? C26A C25A C24A 119.9(4) . . ? C25A C26A C27A 120.0(4) . . ? C26A C27A C28A 120.6(4) . . ? C23A C28A C27A 120.4(4) . . ? N5A C30A C31A 110.4(3) . . ? N6A C31A C30A 108.9(3) . . ? N5A C33A C34A 115.1(3) . . ? C35A C34A C39A 120.1(4) . . ? C35A C34A C33A 119.8(4) . . ? C39A C34A C33A 120.0(3) . . ? O5A C35A C34A 122.1(3) . . ? O5A C35A C36A 119.3(4) . . ? C34A C35A C36A 118.6(4) . . ? C37A C36A C35A 119.1(4) . . ? C37A C36A C40A 122.6(4) . . ? C35A C36A C40A 118.3(4) . . ? C36A C37A C38A 122.8(4) . . ? C39A C38A C37A 116.9(4) . . ? C39A C38A C41A 123.4(4) . . ? C37A C38A C41A 119.6(4) . . ? C38A C39A C34A 122.5(4) . . ? C42A C41A C43A 108.7(3) . . ? C42A C41A C44A 108.0(4) . . ? C43A C41A C44A 109.4(4) . . ? C42A C41A C38A 112.2(3) . . ? C43A C41A C38A 109.7(4) . . ? C44A C41A C38A 108.8(3) . . ? C46A C45A N6A 114.2(4) . . ? C51A C46A C47A 119.3(6) . . ? C51A C46A C45A 119.4(6) . . ? C47A C46A C45A 121.4(4) . . ? O6A C47A C46A 121.6(5) . . ? O6A C47A C48A 118.1(5) . . ? C46A C47A C48A 120.3(5) . . ? C49A C48A C47A 117.7(6) . . ? C49A C48A C52A 123.2(6) . . ? C47A C48A C52A 119.0(4) . . ? C50A C49A C48A 122.8(7) . . ? C51A C50A C49A 117.8(6) . . ? C51A C50A C53A 121.8(9) . . ? C49A C50A C53A 120.4(9) . . ? C50A C51A C46A 122.1(7) . . ? C56A C53A C55A 116.1(9) . . ? C56A C53A C50A 114.3(9) . . ? C55A C53A C50A 110.6(6) . . ? C56A C53A C54A 105.6(7) . . ? C55A C53A C54A 101.9(9) . . ? C50A C53A C54A 107.1(9) . . ? N7A C58A C59A 109.9(3) . . ? N8A C59A C58A 109.6(3) . . ? C62A C61A N8A 114.4(3) . . ? C67A C62A C63A 120.0(4) . . ? C67A C62A C61A 119.2(3) . . ? C63A C62A C61A 120.8(3) . . ? O7A C63A C62A 122.7(3) . . ? O7A C63A C64A 118.6(3) . . ? C62A C63A C64A 118.7(3) . . ? C65A C64A C63A 118.6(4) . . ? C65A C64A C68A 122.2(3) . . ? C63A C64A C68A 119.2(3) . . ? C64A C65A C66A 124.0(4) . . ? C67A C66A C65A 116.0(3) . . ? C67A C66A C69A 122.6(4) . . ? C65A C66A C69A 121.3(4) . . ? C66A C67A C62A 122.7(4) . . ? C71A C69A C70A 109.3(4) . . ? C71A C69A C72A 109.9(4) . . ? C70A C69A C72A 106.2(4) . . ? C71A C69A C66A 110.7(4) . . ? C70A C69A C66A 108.8(3) . . ? C72A C69A C66A 111.7(4) . . ? N7A C73A C74A 113.5(3) . . ? C79A C74A C75A 119.4(3) . . ? C79A C74A C73A 120.3(3) . . ? C75A C74A C73A 120.3(3) . . ? O8A C75A C76A 120.2(3) . . ? O8A C75A C74A 121.3(3) . . ? C76A C75A C74A 118.5(3) . . ? C77A C76A C75A 119.5(3) . . ? C77A C76A C80A 120.6(3) . . ? C75A C76A C80A 119.8(3) . . ? C78A C77A C76A 122.9(4) . . ? C77A C78A C79A 116.7(3) . . ? C77A C78A C81A 123.8(3) . . ? C79A C78A C81A 119.5(3) . . ? C74A C79A C78A 122.9(4) . . ? C82A C81A C84A 110.1(3) . . ? C82A C81A C83A 108.5(3) . . ? C84A C81A C83A 107.9(3) . . ? C82A C81A C78A 109.7(3) . . ? C84A C81A C78A 109.7(3) . . ? C83A C81A C78A 110.9(3) . . ? N9A C85A C86A 122.5(4) . . ? C87A C86A C85A 120.2(4) . . ? C88A C87A C86A 118.6(4) . . ? C87A C88A C89A 118.8(4) . . ? N9A C89A C88A 123.9(4) . . ? N10A C90A C91A 122.6(3) . . ? C90A C91A C92A 120.2(3) . . ? C93A C92A C91A 117.7(4) . . ? C94A C93A C92A 119.4(3) . . ? N10A C94A C93A 123.3(4) . . ? N1B C1B C2B 114.0(3) . . ? N1B C1B C3B 119.5(4) . . ? C2B C1B C3B 126.3(4) . . ? N1B C1B C3C 128.2(4) . . ? C2B C1B C3C 117.5(3) . . ? C3B C1B C3C 13.7 . . ? N2B C2B C1B 113.6(3) . . ? N2B C2B C9B 123.1(3) . . ? C1B C2B C9B 123.2(3) . . ? C4B C3B C8B 120.0 . . ? C4B C3B C1B 123.1(3) . . ? C8B C3B C1B 116.9(3) . . ? C3B C4B C5B 120.0 . . ? C4B C5B C6B 120.0 . . ? C7B C6B C5B 120.0 . . ? C6B C7B C8B 120.0 . . ? C7B C8B C3B 120.0 . . ? C4C C3C C8C 120.0 . . ? C4C C3C C1B 116.1(3) . . ? C8C C3C C1B 123.9(3) . . ? C5C C4C C3C 120.0 . . ? C6C C5C C4C 120.0 . . ? C5C C6C C7C 120.0 . . ? C8C C7C C6C 120.0 . . ? C7C C8C C3C 120.0 . . ? C10C C9B C14B 110.3(10) . . ? C10C C9B C14C 118.6(9) . . ? C14B C9B C14C 31.9(6) . . ? C10C C9B C2B 120.3(7) . . ? C14B C9B C2B 119.8(8) . . ? C14C C9B C2B 121.1(6) . . ? C10C C9B C10B 29.6(10) . . ? C14B C9B C10B 117.2(11) . . ? C14C C9B C10B 108.0(9) . . ? C2B C9B C10B 122.9(8) . . ? C11B C10B C9B 120.8(15) . . ? C12B C11B C10B 118.5(16) . . ? C11B C12B C13B 124.8(12) . . ? C14B C13B C12B 116.9(14) . . ? C9B C14B C13B 121.4(14) . . ? C9B C10C C11C 121.9(14) . . ? C9B C14C C13C 120.4(11) . . ? N4B C15B C16B 112.9(3) . . ? N4B C15B C17B 124.5(3) . . ? C16B C15B C17B 122.5(3) . . ? N3B C16B C15B 114.7(3) . . ? N3B C16B C23B 122.1(3) . . ? C15B C16B C23B 123.1(3) . . ? C18B C17B C22B 117.6(4) . . ? C18B C17B C15B 122.9(4) . . ? C22B C17B C15B 119.3(3) . . ? C17B C18B C19B 119.9(4) . . ? C20B C19B C18B 120.5(5) . . ? C21B C20B C19B 120.5(5) . . ? C20B C21B C22B 119.1(4) . . ? C21B C22B C17B 122.4(4) . . ? C28B C23B C24B 118.8(4) . . ? C28B C23B C16B 122.2(4) . . ? C24B C23B C16B 119.0(4) . . ? C25B C24B C23B 121.6(5) . . ? C26B C25B C24B 119.5(6) . . ? C25B C26B C27B 122.9(6) . . ? C26B C27B C28B 117.8(5) . . ? C23B C28B C27B 119.5(5) . . ? N5B C30B C31B 110.7(3) . . ? N6B C31B C30B 109.5(3) . . ? N7B C34B C35B 110.6(3) . . ? N8B C35B C34B 109.6(3) . . ? C38B C37B N5B 113.1(4) . . ? C43B C38B C39B 120.0(4) . . ? C43B C38B C37B 119.5(4) . . ? C39B C38B C37B 120.5(4) . . ? O5B C39B C38B 121.4(4) . . ? O5B C39B C40B 119.2(4) . . ? C38B C39B C40B 119.3(4) . . ? C41B C40B C39B 119.2(4) . . ? C41B C40B C44B 120.9(4) . . ? C39B C40B C44B 119.9(3) . . ? C42B C41B C40B 122.3(4) . . ? C43B C42B C41B 117.3(4) . . ? C43B C42B C45B 121.8(5) . . ? C41B C42B C45B 120.8(5) . . ? C42B C43B C38B 121.9(4) . . ? C46B C45B C48B 116.0(7) . . ? C46B C45B C47B 106.5(6) . . ? C48B C45B C47B 103.1(6) . . ? C46B C45B C42B 113.6(6) . . ? C48B C45B C42B 107.2(5) . . ? C47B C45B C42B 109.8(5) . . ? N6B C49B C50B 114.5(3) . . ? C51B C50B C55B 120.3(4) . . ? C51B C50B C49B 121.1(4) . . ? C55B C50B C49B 118.6(4) . . ? O6B C51B C50B 122.3(4) . . ? O6B C51B C52B 119.0(4) . . ? C50B C51B C52B 118.7(4) . . ? C53B C52B C51B 119.1(4) . . ? C53B C52B C56B 121.6(4) . . ? C51B C52B C56B 119.3(4) . . ? C52B C53B C54B 122.8(4) . . ? C55B C54B C53B 116.6(4) . . ? C55B C54B C57B 122.0(4) . . ? C53B C54B C57B 121.3(4) . . ? C54B C55B C50B 122.4(4) . . ? C60B C57B C58B 107.5(5) . . ? C60B C57B C59B 108.4(5) . . ? C58B C57B C59B 109.6(4) . . ? C60B C57B C54B 110.5(4) . . ? C58B C57B C54B 112.0(4) . . ? C59B C57B C54B 108.7(4) . . ? N8B C61B C62B 115.7(3) . . ? C67B C62B C63B 120.3(3) . . ? C67B C62B C61B 118.1(3) . . ? C63B C62B C61B 121.6(3) . . ? O7B C63B C62B 122.7(3) . . ? O7B C63B C64B 118.6(3) . . ? C62B C63B C64B 118.6(3) . . ? C65B C64B C63B 119.3(3) . . ? C65B C64B C68B 121.4(3) . . ? C63B C64B C68B 119.3(3) . . ? C64B C65B C66B 122.9(3) . . ? C67B C66B C65B 116.3(3) . . ? C67B C66B C69B 120.9(3) . . ? C65B C66B C69B 122.8(3) . . ? C62B C67B C66B 122.6(3) . . ? C72B C69B C71B 111.0(5) . . ? C72B C69B C70B 108.6(4) . . ? C71B C69B C70B 105.8(4) . . ? C72B C69B C66B 108.7(4) . . ? C71B C69B C66B 111.8(4) . . ? C70B C69B C66B 111.0(3) . . ? N7B C73B C74B 115.2(3) . . ? C75B C74B C79B 119.5(3) . . ? C75B C74B C73B 121.0(3) . . ? C79B C74B C73B 119.4(3) . . ? O8B C75B C74B 122.9(3) . . ? O8B C75B C76B 117.6(3) . . ? C74B C75B C76B 119.5(3) . . ? C77B C76B C75B 119.0(4) . . ? C77B C76B C80B 121.9(3) . . ? C75B C76B C80B 119.1(3) . . ? C76B C77B C78B 122.9(4) . . ? C77B C78B C79B 117.1(3) . . ? C77B C78B C81B 120.2(4) . . ? C79B C78B C81B 122.7(4) . . ? C78B C79B C74B 122.1(4) . . ? C83B C81B C82B 109.6(4) . . ? C83B C81B C84B 107.4(4) . . ? C82B C81B C84B 109.1(4) . . ? C83B C81B C78B 113.1(4) . . ? C82B C81B C78B 108.8(4) . . ? C84B C81B C78B 108.8(3) . . ? N9B C85B C86B 123.3(3) . . ? C85B C86B C87B 119.4(4) . . ? C88B C87B C86B 117.8(4) . . ? C89B C88B C87B 120.2(4) . . ? N9B C89B C88B 122.8(4) . . ? N10B C90B C91B 123.9(4) . . ? C92B C91B C90B 119.4(4) . . ? C91B C92B C93B 118.2(4) . . ? C92B C93B C94B 119.1(4) . . ? N10B C94B C93B 124.0(4) . . ? N1A Fe1A N3A 178.93(12) . . ? N1A Fe1A N4A 98.15(12) . . ? N3A Fe1A N4A 81.25(12) . . ? N1A Fe1A N2A 80.85(12) . . ? N3A Fe1A N2A 99.83(12) . . ? N4A Fe1A N2A 174.99(12) . . ? N1A Fe1A N10A 92.39(11) . . ? N3A Fe1A N10A 88.45(11) . . ? N4A Fe1A N10A 85.40(12) . . ? N2A Fe1A N10A 89.73(11) . . ? N1A Fe1A N9A 89.76(11) . . ? N3A Fe1A N9A 89.36(11) . . ? N4A Fe1A N9A 91.38(11) . . ? N2A Fe1A N9A 93.52(11) . . ? N10A Fe1A N9A 176.36(11) . . ? N4B Fe1B N2B 178.51(13) . . ? N4B Fe1B N3B 81.07(12) . . ? N2B Fe1B N3B 98.89(12) . . ? N4B Fe1B N1B 98.84(13) . . ? N2B Fe1B N1B 81.01(13) . . ? N3B Fe1B N1B 172.68(12) . . ? N4B Fe1B N9B 86.75(12) . . ? N2B Fe1B N9B 91.76(12) . . ? N3B Fe1B N9B 85.33(11) . . ? N1B Fe1B N9B 87.36(12) . . ? N4B Fe1B N10B 90.83(12) . . ? N2B Fe1B N10B 90.66(12) . . ? N3B Fe1B N10B 92.32(11) . . ? N1B Fe1B N10B 95.00(12) . . ? N9B Fe1B N10B 176.86(12) . . ? C1A N1A O1A 114.8(3) . . ? C1A N1A Fe1A 115.8(2) . . ? O1A N1A Fe1A 128.4(2) . . ? C2A N2A O2A 114.6(2) . . ? C2A N2A Fe1A 117.56(16) . . ? O2A N2A Fe1A 127.0(2) . . ? C22A N3A O3A 116.0(3) . . ? C22A N3A Fe1A 115.6(2) . . ? O3A N3A Fe1A 127.9(2) . . ? C15A N4A O4A 115.8(3) . . ? C15A N4A Fe1A 115.3(2) . . ? O4A N4A Fe1A 127.2(2) . . ? C29A N5A C30A 109.9(3) . . ? C29A N5A C33A 106.7(3) . . ? C30A N5A C33A 110.7(3) . . ? C29A N5A Al1A 113.3(2) . . ? C30A N5A Al1A 106.5(2) . . ? C33A N5A Al1A 109.8(2) . . ? C31A N6A C32A 109.7(3) . . ? C31A N6A C45A 109.7(3) . . ? C32A N6A C45A 107.0(4) . . ? C31A N6A Al1A 107.0(2) . . ? C32A N6A Al1A 112.8(3) . . ? C45A N6A Al1A 110.6(3) . . ? C58A N7A C57A 108.2(3) . . ? C58A N7A C73A 111.7(3) . . ? C57A N7A C73A 106.7(3) . . ? C58A N7A Al2A 106.6(2) . . ? C57A N7A Al2A 114.3(2) . . ? C73A N7A Al2A 109.4(2) . . ? C60A N8A C59A 108.9(3) . . ? C60A N8A C61A 106.8(3) . . ? C59A N8A C61A 109.2(3) . . ? C60A N8A Al2A 113.9(2) . . ? C59A N8A Al2A 107.8(2) . . ? C61A N8A Al2A 110.1(2) . . ? C85A N9A C89A 115.8(3) . . ? C85A N9A Fe1A 122.2(2) . . ? C89A N9A Fe1A 121.9(2) . . ? C90A N10A C94A 116.7(3) . . ? C90A N10A Fe1A 121.5(2) . . ? C94A N10A Fe1A 120.9(2) . . ? C1B N1B O1B 115.2(3) . . ? C1B N1B Fe1B 115.3(3) . . ? O1B N1B Fe1B 128.2(2) . . ? C2B N2B O2B 115.0(3) . . ? C2B N2B Fe1B 115.9(2) . . ? O2B N2B Fe1B 128.5(2) . . ? C16B N3B O3B 115.6(3) . . ? C16B N3B Fe1B 115.1(2) . . ? O3B N3B Fe1B 127.7(2) . . ? C15B N4B O4B 116.1(3) . . ? C15B N4B Fe1B 115.7(2) . . ? O4B N4B Fe1B 128.2(2) . . ? C30B N5B C29B 109.2(3) . . ? C30B N5B C37B 111.9(3) . . ? C29B N5B C37B 106.7(3) . . ? C30B N5B Al1B 106.5(2) . . ? C29B N5B Al1B 112.2(2) . . ? C37B N5B Al1B 110.5(2) . . ? C31B N6B C32B 109.8(3) . . ? C31B N6B C49B 110.2(3) . . ? C32B N6B C49B 105.2(3) . . ? C31B N6B Al1B 106.7(3) . . ? C32B N6B Al1B 114.8(3) . . ? C49B N6B Al1B 110.2(2) . . ? C33B N7B C73B 105.8(3) . . ? C33B N7B C34B 108.7(3) . . ? C73B N7B C34B 110.4(3) . . ? C33B N7B Al2B 113.3(2) . . ? C73B N7B Al2B 111.8(2) . . ? C34B N7B Al2B 106.9(2) . . ? C36B N8B C61B 105.3(3) . . ? C36B N8B C35B 109.5(3) . . ? C61B N8B C35B 110.7(3) . . ? C36B N8B Al2B 114.6(2) . . ? C61B N8B Al2B 110.9(2) . . ? C35B N8B Al2B 105.9(2) . . ? C89B N9B C85B 116.5(3) . . ? C89B N9B Fe1B 120.8(3) . . ? C85B N9B Fe1B 122.3(2) . . ? C94B N10B C90B 115.4(3) . . ? C94B N10B Fe1B 121.3(3) . . ? C90B N10B Fe1B 123.2(3) . . ? N1A O1A Al1A 128.1(2) . . ? N2A O2A Al2A 126.53(18) . . ? N3A O3A Al2A 129.06(19) . . ? N4A O4A Al1A 125.5(2) . . ? C35A O5A Al1A 136.6(2) . . ? C47A O6A Al1A 137.1(3) . . ? C63A O7A Al2A 136.4(2) . . ? C75A O8A Al2A 138.5(2) . . ? N1B O1B Al1B 124.6(2) . . ? N2B O2B Al2B 127.7(2) . . ? N3B O3B Al2B 127.0(2) . . ? N4B O4B Al1B 128.3(2) . . ? C39B O5B Al1B 138.1(2) . . ? C51B O6B Al1B 136.7(3) . . ? C63B O7B Al2B 135.2(2) . . ? C75B O8B Al2B 136.6(2) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.799 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.064 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.045 0.242 0.381 19 2 ' ' 2 0.036 0.037 0.029 10 1 ' ' 3 0.500 1.000 0.000 1149 218 ' ' 4 0.111 0.781 0.435 7 1 ' ' 5 0.201 0.458 0.437 8 1 ' ' 6 0.799 0.542 0.562 8 1 ' ' 7 0.889 0.219 0.565 7 1 ' ' 8 0.955 0.758 0.619 19 2 ' ' 9 0.972 0.960 0.970 9 1 ' ' _platon_squeeze_details ; ;