data_p15207 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H63 Fe K N2 O P3 Si' _chemical_formula_weight 803.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3640(4) _cell_length_b 10.9643(4) _cell_length_c 18.9571(8) _cell_angle_alpha 88.362(2) _cell_angle_beta 84.430(2) _cell_angle_gamma 83.401(2) _cell_volume 2129.46(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9168 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 74.71 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_F_000 858 _exptl_transmission_factor_min 0.5929 _exptl_transmission_factor_max 0.7538 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_absorpt_coefficient_mu 5.287 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS-2014/5 (Sheldrick, 2014)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 56751 _diffrn_reflns_av_unetI/netI 0.0552 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.342 _diffrn_reflns_theta_max 74.889 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 8671 _reflns_number_gt 6710 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+4.6723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8671 _refine_ls_number_parameters 467 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.033 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.63153(5) 0.27422(5) 0.23720(3) 0.02060(15) Uani 1 1 d . . . . . Si2 Si 0.84556(9) 0.22234(9) 0.21070(5) 0.0212(2) Uani 1 1 d . . . . . P4 P 0.62496(8) 0.16239(8) 0.14247(5) 0.0224(2) Uani 1 1 d . . . . . P5 P 0.67658(9) 0.17803(9) 0.33747(6) 0.0288(2) Uani 1 1 d . . . . . K6 K 0.10390(9) 0.44781(9) 0.27550(6) 0.0451(3) Uani 1 1 d . . . . . N1 N 0.4618(3) 0.3123(3) 0.25853(18) 0.0293(7) Uani 1 1 d . . . . . N2 N 0.3519(3) 0.3383(3) 0.2715(2) 0.0381(8) Uani 1 1 d . . . . . C3 C 0.7812(4) -0.0561(3) 0.0827(2) 0.0289(8) Uani 1 1 d . . . . . H3 H 0.7058 -0.0809 0.0650 0.035 Uiso 1 1 calc R U . . . C4 C 0.8498(4) 0.1718(3) 0.3547(2) 0.0280(8) Uani 1 1 d . . . . . C5 C 1.0695(4) 0.1662(4) 0.2988(3) 0.0366(10) Uani 1 1 d . . . . . H5 H 1.1282 0.1705 0.2574 0.044 Uiso 1 1 calc R U . . . C6 C 1.0015(4) 0.0152(3) 0.1344(2) 0.0299(8) Uani 1 1 d . . . . . H6 H 1.0777 0.0388 0.1518 0.036 Uiso 1 1 calc R U . . . C7 C 1.0544(3) 0.3491(4) 0.1311(2) 0.0284(8) Uani 1 1 d . . . . . H7 H 1.1034 0.2714 0.1224 0.034 Uiso 1 1 calc R U . . . C9 C 1.0110(4) -0.0889(4) 0.0935(2) 0.0358(10) Uani 1 1 d . . . . . H9 H 1.0932 -0.1356 0.0827 0.043 Uiso 1 1 calc R U . . . C10 C 0.9120(4) 0.5757(4) 0.1557(2) 0.0341(9) Uani 1 1 d . . . . . H10 H 0.8644 0.6538 0.1651 0.041 Uiso 1 1 calc R U . . . C12 C 1.1083(4) 0.4548(4) 0.1080(3) 0.0392(10) Uani 1 1 d . . . . . H12 H 1.1926 0.4496 0.0829 0.047 Uiso 1 1 calc R U . . . C15 C 1.1183(5) 0.1435(5) 0.3641(3) 0.0484(12) Uani 1 1 d . . . . . H15 H 1.2099 0.1321 0.3671 0.058 Uiso 1 1 calc R U . . . C16 C 0.9005(4) -0.1241(4) 0.0684(2) 0.0349(9) Uani 1 1 d . . . . . H16 H 0.9068 -0.1962 0.0411 0.042 Uiso 1 1 calc R U . . . C17 C 0.9009(5) 0.1492(4) 0.4205(2) 0.0425(11) Uani 1 1 d . . . . . H17 H 0.8436 0.1419 0.4623 0.051 Uiso 1 1 calc R U . . . C18 C 1.0340(5) 0.1374(5) 0.4245(3) 0.0500(12) Uani 1 1 d . . . . . H18 H 1.0677 0.1250 0.4693 0.060 Uiso 1 1 calc R U . . . C21 C 1.0376(4) 0.5689(4) 0.1219(3) 0.0421(11) Uani 1 1 d . . . . . H21 H 1.0753 0.6420 0.1084 0.051 Uiso 1 1 calc R U . . . C0AA C 0.7711(3) 0.0506(3) 0.12359(19) 0.0237(7) Uani 1 1 d . . . . . C1AA C 0.8825(3) 0.0854(3) 0.1504(2) 0.0244(8) Uani 1 1 d . . . . . C22 C 0.8547(4) 0.4694(3) 0.1759(2) 0.0264(8) Uani 1 1 d . . . . . C23 C 0.9296(3) 0.3541(3) 0.1670(2) 0.0241(8) Uani 1 1 d . . . . . C8 C 0.6298(4) 0.2359(4) 0.0498(2) 0.0303(8) Uani 1 1 d . . . . . H8 H 0.5596 0.3067 0.0512 0.036 Uiso 1 1 calc R U . . . C24 C 0.4856(4) 0.0697(4) 0.1354(2) 0.0312(9) Uani 1 1 d . . . . . H24 H 0.5087 0.0149 0.0937 0.037 Uiso 1 1 calc R U . . . C11 C 0.7589(4) 0.2876(4) 0.0300(2) 0.0348(9) Uani 1 1 d . . . . . H11A H 0.8290 0.2199 0.0230 0.052 Uiso 1 1 calc R U . . . H11B H 0.7771 0.3396 0.0683 0.052 Uiso 1 1 calc R U . . . H11C H 0.7536 0.3366 -0.0138 0.052 Uiso 1 1 calc R U . . . C25 C 0.6073(5) 0.1536(4) -0.0110(2) 0.0392(10) Uani 1 1 d . . . . . H25A H 0.6121 0.2005 -0.0557 0.059 Uiso 1 1 calc R U . . . H25B H 0.5210 0.1248 -0.0020 0.059 Uiso 1 1 calc R U . . . H25C H 0.6745 0.0829 -0.0139 0.059 Uiso 1 1 calc R U . . . C14 C 0.4619(4) -0.0104(4) 0.2000(3) 0.0442(11) Uani 1 1 d . . . . . H14A H 0.4451 0.0407 0.2422 0.066 Uiso 1 1 calc R U . . . H14B H 0.5390 -0.0697 0.2048 0.066 Uiso 1 1 calc R U . . . H14C H 0.3862 -0.0545 0.1951 0.066 Uiso 1 1 calc R U . . . C26 C 0.7594(5) -0.0689(4) 0.2973(3) 0.0470(12) Uani 1 1 d . . . . . H26A H 0.8487 -0.0605 0.3079 0.070 Uiso 1 1 calc R U . . . H26B H 0.7476 -0.0392 0.2488 0.070 Uiso 1 1 calc R U . . . H26C H 0.7442 -0.1555 0.3016 0.070 Uiso 1 1 calc R U . . . C27 C 0.3620(4) 0.1532(4) 0.1221(3) 0.0421(11) Uani 1 1 d . . . . . H27A H 0.2904 0.1033 0.1185 0.063 Uiso 1 1 calc R U . . . H27B H 0.3770 0.1999 0.0778 0.063 Uiso 1 1 calc R U . . . H27C H 0.3392 0.2102 0.1614 0.063 Uiso 1 1 calc R U . . . C19 C 0.6631(5) 0.0061(4) 0.3492(3) 0.0476(12) Uani 1 1 d . . . . . H19 H 0.5743 -0.0063 0.3363 0.057 Uiso 1 1 calc R U . . . O1 O 0.1322(4) 0.6337(3) 0.3580(2) 0.0581(10) Uani 1 1 d . . . . . C29 C 0.5877(5) 0.2271(5) 0.4248(2) 0.0499(12) Uani 1 1 d . . . . . H29 H 0.6263 0.1743 0.4631 0.060 Uiso 1 1 calc R U . . . C31 C 0.5956(8) 0.3558(6) 0.4410(3) 0.082(2) Uani 1 1 d . . . . . H31A H 0.5478 0.3751 0.4872 0.124 Uiso 1 1 calc R U . . . H31B H 0.5571 0.4090 0.4043 0.124 Uiso 1 1 calc R U . . . H31C H 0.6872 0.3692 0.4422 0.124 Uiso 1 1 calc R U . . . C33 C 0.6743(8) -0.0513(6) 0.4202(3) 0.080(2) Uani 1 1 d . . . . . H33A H 0.6705 -0.1399 0.4174 0.121 Uiso 1 1 calc R U . . . H33B H 0.6022 -0.0155 0.4533 0.121 Uiso 1 1 calc R U . . . H33C H 0.7575 -0.0365 0.4370 0.121 Uiso 1 1 calc R U . . . C34 C 0.1354(7) 0.7626(6) 0.3419(4) 0.079(2) Uani 1 1 d . . . . . H34A H 0.2186 0.7886 0.3544 0.095 Uiso 1 1 calc R U . . . H34B H 0.0629 0.8110 0.3702 0.095 Uiso 1 1 calc R U . . . C35 C 0.4429(6) 0.2051(9) 0.4244(3) 0.100(3) Uani 1 1 d . . . . . H35A H 0.3967 0.2237 0.4712 0.150 Uiso 1 1 calc R U . . . H35B H 0.4377 0.1191 0.4135 0.150 Uiso 1 1 calc R U . . . H35C H 0.4025 0.2586 0.3885 0.150 Uiso 1 1 calc R U . . . C36 C 0.1596(9) 0.6078(7) 0.4281(4) 0.092(2) Uani 1 1 d . . . . . H36A H 0.0942 0.6554 0.4612 0.110 Uiso 1 1 calc R U . . . H36B H 0.2470 0.6308 0.4353 0.110 Uiso 1 1 calc R U . . . C37 C 0.1557(10) 0.4711(7) 0.4422(4) 0.115(4) Uani 1 1 d . . . . . H37A H 0.0718 0.4478 0.4307 0.172 Uiso 1 1 calc R U . . . H37B H 0.1661 0.4523 0.4923 0.172 Uiso 1 1 calc R U . . . H37C H 0.2267 0.4249 0.4127 0.172 Uiso 1 1 calc R U . . . C39 C 0.1233(6) 0.7847(5) 0.2668(4) 0.0713(17) Uani 1 1 d . . . . . H39A H 0.1238 0.8725 0.2559 0.107 Uiso 1 1 calc R U . . . H39B H 0.0412 0.7581 0.2547 0.107 Uiso 1 1 calc R U . . . H39C H 0.1967 0.7383 0.2392 0.107 Uiso 1 1 calc R U . . . C40 C 0.9352(4) 0.1827(3) 0.2933(2) 0.0269(8) Uani 1 1 d . . . . . C1G C 0.7679(5) 0.5552(5) 0.3323(3) 0.0596(16) Uani 1 1 d . . . . . H1GA H 0.7352 0.5940 0.3775 0.089 Uiso 1 1 calc R U . . . H1GB H 0.8511 0.5849 0.3150 0.089 Uiso 1 1 calc R U . . . H1GC H 0.7810 0.4659 0.3393 0.089 Uiso 1 1 calc R U . . . C1H C 0.5291(5) 0.6162(5) 0.3118(3) 0.0596(15) Uani 1 1 d . . . . . H1HA H 0.4937 0.5394 0.3267 0.089 Uiso 1 1 calc R U . . . H1HB H 0.4758 0.6593 0.2769 0.089 Uiso 1 1 calc R U . . . H1HC H 0.5280 0.6681 0.3531 0.089 Uiso 1 1 calc R U . . . P1 P 0.68190(9) 0.46143(8) 0.21197(6) 0.0266(2) Uani 1 1 d . . . . . C1 C 0.6366(11) 0.5713(11) 0.0741(8) 0.049(3) Uani 0.407(12) 1 d . U P A 2 H1A H 0.5818 0.6405 0.0547 0.074 Uiso 0.407(12) 1 calc R U P A 2 H1B H 0.6328 0.4978 0.0465 0.074 Uiso 0.407(12) 1 calc R U P A 2 H1C H 0.7270 0.5905 0.0717 0.074 Uiso 0.407(12) 1 calc R U P A 2 C2 C 0.6217(10) 0.6694(9) 0.1130(7) 0.076(4) Uani 0.593(12) 1 d . U P A 1 H2A H 0.5753 0.7325 0.1446 0.113 Uiso 0.593(12) 1 calc R U P A 1 H2B H 0.5927 0.6823 0.0654 0.113 Uiso 0.593(12) 1 calc R U P A 1 H2C H 0.7158 0.6747 0.1109 0.113 Uiso 0.593(12) 1 calc R U P A 1 C1B C 0.5947(5) 0.5514(6) 0.1394(4) 0.0707(19) Uani 1 1 d . U . . . C99 C 0.4506(5) 0.5335(6) 0.1445(4) 0.084(2) Uani 1 1 d . U . B 1 H99A H 0.4413 0.4457 0.1428 0.126 Uiso 1 1 calc R U . B 1 H99B H 0.4102 0.5766 0.1048 0.126 Uiso 1 1 calc R U . B 1 H99C H 0.4073 0.5667 0.1893 0.126 Uiso 1 1 calc R U . B 1 C13 C 0.6697(4) 0.5874(4) 0.2786(3) 0.0454(12) Uani 1 1 d . . . . . H13 H 0.6942 0.6630 0.2523 0.054 Uiso 1 1 calc R U . . . 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 0.0122(3) 0.0213(3) 0.0289(3) -0.0097(2) -0.0027(2) -0.0015(2) Si2 0.0128(4) 0.0218(5) 0.0294(5) -0.0063(4) -0.0032(4) -0.0009(3) P4 0.0151(4) 0.0228(4) 0.0303(5) -0.0105(4) -0.0040(3) -0.0020(3) P5 0.0233(5) 0.0299(5) 0.0329(5) -0.0037(4) 0.0001(4) -0.0039(4) K6 0.0319(5) 0.0466(6) 0.0580(6) -0.0217(5) -0.0154(4) 0.0058(4) N1 0.0227(18) 0.0298(17) 0.0357(19) -0.0104(14) -0.0011(13) -0.0034(13) N2 0.0194(18) 0.047(2) 0.047(2) -0.0121(17) 0.0003(15) -0.0015(15) C3 0.031(2) 0.0261(19) 0.030(2) -0.0065(15) -0.0009(16) -0.0040(16) C4 0.031(2) 0.0236(18) 0.030(2) -0.0052(15) -0.0083(16) -0.0017(15) C5 0.023(2) 0.039(2) 0.049(3) 0.0040(19) -0.0112(18) -0.0048(17) C6 0.0205(19) 0.0239(19) 0.044(2) -0.0035(16) 0.0029(16) 0.0004(15) C7 0.0156(17) 0.0296(19) 0.040(2) -0.0074(16) -0.0016(15) -0.0012(14) C9 0.028(2) 0.024(2) 0.051(3) -0.0085(18) 0.0099(18) 0.0031(16) C10 0.028(2) 0.0210(19) 0.053(3) -0.0024(17) 0.0013(18) -0.0034(15) C12 0.026(2) 0.035(2) 0.056(3) -0.004(2) 0.0073(19) -0.0081(17) C15 0.031(2) 0.052(3) 0.067(3) 0.007(2) -0.025(2) -0.008(2) C16 0.041(2) 0.0222(19) 0.040(2) -0.0111(17) 0.0049(18) 0.0018(17) C17 0.046(3) 0.046(3) 0.038(3) -0.002(2) -0.014(2) -0.005(2) C18 0.052(3) 0.058(3) 0.043(3) 0.006(2) -0.025(2) -0.002(2) C21 0.033(2) 0.028(2) 0.065(3) 0.001(2) 0.007(2) -0.0112(18) C0AA 0.0236(18) 0.0212(17) 0.0253(19) -0.0050(14) 0.0014(14) -0.0005(14) C1AA 0.0214(18) 0.0221(17) 0.029(2) -0.0017(14) 0.0006(14) -0.0018(14) C22 0.0218(18) 0.0234(18) 0.034(2) -0.0061(15) -0.0042(15) -0.0013(14) C23 0.0167(17) 0.0261(18) 0.031(2) -0.0036(15) -0.0071(14) -0.0031(14) C8 0.030(2) 0.0264(19) 0.035(2) -0.0088(16) -0.0058(16) 0.0013(15) C24 0.0238(19) 0.036(2) 0.036(2) -0.0150(17) -0.0055(16) -0.0060(16) C11 0.041(2) 0.032(2) 0.031(2) -0.0018(17) -0.0027(17) -0.0036(18) C25 0.047(3) 0.038(2) 0.033(2) -0.0105(18) -0.0077(19) -0.0027(19) C14 0.038(2) 0.050(3) 0.048(3) -0.009(2) -0.001(2) -0.019(2) C26 0.058(3) 0.025(2) 0.061(3) -0.002(2) -0.019(2) -0.008(2) C27 0.022(2) 0.048(3) 0.059(3) -0.022(2) -0.0092(19) -0.0031(18) C19 0.044(3) 0.041(3) 0.060(3) 0.011(2) -0.009(2) -0.017(2) O1 0.065(2) 0.050(2) 0.061(2) -0.0238(18) -0.0172(18) 0.0039(17) C29 0.046(3) 0.067(3) 0.031(2) 0.001(2) 0.008(2) 0.009(2) C31 0.130(6) 0.064(4) 0.042(3) -0.013(3) 0.010(4) 0.023(4) C33 0.131(7) 0.055(4) 0.053(4) 0.007(3) 0.012(4) -0.020(4) C34 0.094(5) 0.059(4) 0.088(5) -0.028(3) -0.025(4) 0.002(3) C35 0.042(3) 0.200(9) 0.049(4) 0.017(5) 0.011(3) 0.006(4) C36 0.137(7) 0.084(5) 0.057(4) -0.027(4) -0.033(4) 0.004(5) C37 0.205(11) 0.086(5) 0.045(4) -0.016(4) -0.029(5) 0.041(6) C39 0.069(4) 0.049(3) 0.095(5) -0.010(3) -0.014(3) 0.002(3) C40 0.0232(19) 0.0232(18) 0.036(2) -0.0045(15) -0.0086(15) -0.0032(14) C1G 0.045(3) 0.067(4) 0.070(4) -0.041(3) 0.005(3) -0.019(3) C1H 0.049(3) 0.044(3) 0.080(4) -0.021(3) 0.015(3) 0.006(2) P1 0.0161(4) 0.0214(4) 0.0428(6) -0.0094(4) -0.0039(4) -0.0006(3) C1 0.033(6) 0.033(7) 0.083(7) 0.009(5) -0.024(5) 0.005(5) C2 0.053(6) 0.055(6) 0.129(10) 0.041(6) -0.053(6) -0.025(5) C1B 0.034(3) 0.079(4) 0.106(5) 0.049(3) -0.033(3) -0.025(3) C99 0.037(3) 0.076(4) 0.146(7) 0.051(4) -0.046(3) -0.021(3) C13 0.038(3) 0.032(2) 0.065(3) -0.022(2) 0.008(2) -0.0071(19) _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 1.771(3) . ? Fe1 P1 2.2037(11) . ? Fe1 P5 2.2110(12) . ? Fe1 P4 2.2141(10) . ? Fe1 Si2 2.2375(10) . ? Si2 C1AA 1.895(4) . ? Si2 C23 1.901(4) . ? Si2 C40 1.911(4) . ? P4 C0AA 1.849(4) . ? P4 C24 1.876(4) . ? P4 C8 1.910(4) . ? P5 C4 1.849(4) . ? P5 C29 1.876(5) . ? P5 C19 1.911(5) . ? K6 O1 2.663(3) . ? K6 N2 2.704(4) . ? K6 C7 3.081(4) 1_455 ? K6 C23 3.134(4) 1_455 ? K6 C5 3.163(4) 1_455 ? K6 C12 3.170(5) 1_455 ? K6 C21 3.266(5) 1_455 ? K6 C22 3.327(4) 1_455 ? K6 C10 3.337(5) 1_455 ? N1 N2 1.147(5) . ? C3 C16 1.375(6) . ? C3 C0AA 1.410(5) . ? C4 C40 1.403(6) . ? C4 C17 1.407(6) . ? C5 C15 1.386(6) . ? C5 C40 1.396(5) . ? C5 K6 3.163(4) 1_655 ? C6 C9 1.387(5) . ? C6 C1AA 1.389(5) . ? C7 C12 1.386(6) . ? C7 C23 1.398(5) . ? C7 K6 3.081(4) 1_655 ? C9 C16 1.380(6) . ? C10 C21 1.388(6) . ? C10 C22 1.396(5) . ? C10 K6 3.337(5) 1_655 ? C12 C21 1.393(6) . ? C12 K6 3.170(5) 1_655 ? C15 C18 1.377(7) . ? C17 C18 1.379(7) . ? C21 K6 3.266(5) 1_655 ? C0AA C1AA 1.400(5) . ? C22 C23 1.410(5) . ? C22 P1 1.865(4) . ? C22 K6 3.327(4) 1_655 ? C23 K6 3.134(4) 1_655 ? C8 C11 1.522(6) . ? C8 C25 1.535(5) . ? C24 C14 1.503(6) . ? C24 C27 1.524(6) . ? C26 C19 1.519(7) . ? C19 C33 1.480(8) . ? O1 C36 1.401(7) . ? O1 C34 1.440(7) . ? C29 C31 1.465(8) . ? C29 C35 1.548(8) . ? C34 C39 1.452(9) . ? C36 C37 1.520(10) . ? C1G C13 1.516(8) . ? C1H C13 1.532(6) . ? P1 C13 1.883(4) . ? P1 C1B 1.908(6) . ? C1 C1B 1.292(15) . ? C2 C1B 1.421(10) . ? C1B C99 1.523(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 N1 Fe1 P1 97.71(11) . . ? N1 Fe1 P5 98.13(12) . . ? P1 Fe1 P5 122.02(4) . . ? N1 Fe1 P4 98.89(11) . . ? P1 Fe1 P4 113.68(4) . . ? P5 Fe1 P4 118.24(4) . . ? N1 Fe1 Si2 178.92(12) . . ? P1 Fe1 Si2 83.37(4) . . ? P5 Fe1 Si2 81.25(4) . . ? P4 Fe1 Si2 80.66(4) . . ? C1AA Si2 C23 108.00(16) . . ? C1AA Si2 C40 107.02(16) . . ? C23 Si2 C40 103.92(16) . . ? C1AA Si2 Fe1 112.83(12) . . ? C23 Si2 Fe1 112.23(12) . . ? C40 Si2 Fe1 112.30(13) . . ? C0AA P4 C24 103.71(17) . . ? C0AA P4 C8 95.81(17) . . ? C24 P4 C8 98.07(18) . . ? C0AA P4 Fe1 113.80(12) . . ? C24 P4 Fe1 120.46(13) . . ? C8 P4 Fe1 120.90(12) . . ? C4 P5 C29 102.8(2) . . ? C4 P5 C19 96.8(2) . . ? C29 P5 C19 97.3(2) . . ? C4 P5 Fe1 113.68(13) . . ? C29 P5 Fe1 121.61(17) . . ? C19 P5 Fe1 120.36(17) . . ? O1 K6 N2 97.33(11) . . ? O1 K6 C7 150.68(12) . 1_455 ? N2 K6 C7 94.44(11) . 1_455 ? O1 K6 C23 144.52(11) . 1_455 ? N2 K6 C23 116.16(10) . 1_455 ? C7 K6 C23 25.97(9) 1_455 1_455 ? O1 K6 C5 135.90(13) . 1_455 ? N2 K6 C5 76.48(11) . 1_455 ? C7 K6 C5 73.04(11) 1_455 1_455 ? C23 K6 C5 67.75(10) 1_455 1_455 ? O1 K6 C12 126.70(12) . 1_455 ? N2 K6 C12 92.70(12) . 1_455 ? C7 K6 C12 25.56(10) 1_455 1_455 ? C23 K6 C12 45.30(10) 1_455 1_455 ? C5 K6 C12 97.36(12) 1_455 1_455 ? O1 K6 C21 106.42(12) . 1_455 ? N2 K6 C21 111.79(12) . 1_455 ? C7 K6 C21 44.29(11) 1_455 1_455 ? C23 K6 C21 51.82(10) 1_455 1_455 ? C5 K6 C21 116.49(11) 1_455 1_455 ? C12 K6 C21 24.95(11) 1_455 1_455 ? O1 K6 C22 119.55(11) . 1_455 ? N2 K6 C22 138.52(11) . 1_455 ? C7 K6 C22 44.08(9) 1_455 1_455 ? C23 K6 C22 24.98(9) 1_455 1_455 ? C5 K6 C22 87.89(10) 1_455 1_455 ? C12 K6 C22 51.00(10) 1_455 1_455 ? C21 K6 C22 43.08(10) 1_455 1_455 ? O1 K6 C10 103.87(11) . 1_455 ? N2 K6 C10 135.29(12) . 1_455 ? C7 K6 C10 50.90(10) 1_455 1_455 ? C23 K6 C10 43.80(9) 1_455 1_455 ? C5 K6 C10 110.91(10) 1_455 1_455 ? C12 K6 C10 43.36(11) 1_455 1_455 ? C21 K6 C10 24.24(10) 1_455 1_455 ? C22 K6 C10 24.18(9) 1_455 1_455 ? N2 N1 Fe1 179.0(4) . . ? N1 N2 K6 164.4(3) . . ? C16 C3 C0AA 119.9(4) . . ? C40 C4 C17 119.5(4) . . ? C40 C4 P5 113.8(3) . . ? C17 C4 P5 126.5(3) . . ? C15 C5 C40 120.9(4) . . ? C15 C5 K6 100.9(3) . 1_655 ? C40 C5 K6 94.3(2) . 1_655 ? C9 C6 C1AA 121.1(4) . . ? C12 C7 C23 121.5(4) . . ? C12 C7 K6 80.8(3) . 1_655 ? C23 C7 K6 79.1(2) . 1_655 ? C16 C9 C6 119.7(4) . . ? C21 C10 C22 120.8(4) . . ? C21 C10 K6 75.0(3) . 1_655 ? C22 C10 K6 77.5(2) . 1_655 ? C7 C12 C21 119.4(4) . . ? C7 C12 K6 73.7(3) . 1_655 ? C21 C12 K6 81.4(3) . 1_655 ? C18 C15 C5 120.0(4) . . ? C3 C16 C9 120.7(4) . . ? C18 C17 C4 120.2(5) . . ? C15 C18 C17 120.5(4) . . ? C10 C21 C12 120.0(4) . . ? C10 C21 K6 80.8(3) . 1_655 ? C12 C21 K6 73.7(3) . 1_655 ? C1AA C0AA C3 119.6(3) . . ? C1AA C0AA P4 113.1(3) . . ? C3 C0AA P4 127.1(3) . . ? C6 C1AA C0AA 119.0(3) . . ? C6 C1AA Si2 127.9(3) . . ? C0AA C1AA Si2 113.0(3) . . ? C10 C22 C23 119.3(3) . . ? C10 C22 P1 126.3(3) . . ? C23 C22 P1 114.4(3) . . ? C10 C22 K6 78.3(2) . 1_655 ? C23 C22 K6 69.8(2) . 1_655 ? P1 C22 K6 123.84(17) . 1_655 ? C7 C23 C22 118.7(3) . . ? C7 C23 Si2 127.9(3) . . ? C22 C23 Si2 113.3(3) . . ? C7 C23 K6 74.9(2) . 1_655 ? C22 C23 K6 85.2(2) . 1_655 ? Si2 C23 K6 108.02(15) . 1_655 ? C11 C8 C25 107.3(3) . . ? C11 C8 P4 111.0(3) . . ? C25 C8 P4 116.5(3) . . ? C14 C24 C27 110.5(4) . . ? C14 C24 P4 112.0(3) . . ? C27 C24 P4 110.6(3) . . ? C33 C19 C26 107.3(5) . . ? C33 C19 P5 118.8(4) . . ? C26 C19 P5 111.7(3) . . ? C36 O1 C34 110.3(5) . . ? C36 O1 K6 118.6(4) . . ? C34 O1 K6 130.9(3) . . ? C31 C29 C35 109.5(6) . . ? C31 C29 P5 113.7(4) . . ? C35 C29 P5 108.5(4) . . ? O1 C34 C39 109.3(5) . . ? O1 C36 C37 108.2(5) . . ? C5 C40 C4 118.9(4) . . ? C5 C40 Si2 128.4(3) . . ? C4 C40 Si2 112.7(3) . . ? C22 P1 C13 97.91(18) . . ? C22 P1 C1B 99.7(2) . . ? C13 P1 C1B 98.5(3) . . ? C22 P1 Fe1 114.57(12) . . ? C13 P1 Fe1 124.38(17) . . ? C1B P1 Fe1 117.40(18) . . ? C2 C1B C99 113.6(6) . . ? C1 C1B P1 129.2(6) . . ? C2 C1B P1 124.8(5) . . ? C99 C1B P1 111.7(4) . . ? C1G C13 C1H 113.7(5) . . ? C1G C13 P1 110.0(3) . . ? C1H C13 P1 110.9(3) . . ? _refine_diff_density_max 0.887 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.082 _shelxl_version_number 2013-3 _shelx_res_file ; TITL p15207 in P-1 CELL 1.54178 10.364 10.9643 18.9571 88.362 84.43 83.401 ZERR 2 0.0004 0.0004 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H N O Si P K Fe UNIT 80 126 4 2 2 6 2 2 L.S. 5 PLAN 20 TEMP -173 FREE K6 C37 FMAP 2 GRID BOND RIGU C99 C1B C2 C1 ACTA MERG 2 OMIT 1 2 2 WGHT 0.059000 4.672300 FVAR 0.16940 0.40666 FE1 8 0.631533 0.274223 0.237198 11.00000 0.01219 0.02127 = 0.02895 -0.00972 -0.00275 -0.00155 SI2 5 0.845562 0.222338 0.210704 11.00000 0.01283 0.02178 = 0.02942 -0.00626 -0.00320 -0.00092 P4 6 0.624960 0.162388 0.142466 11.00000 0.01510 0.02284 = 0.03031 -0.01053 -0.00401 -0.00198 P5 6 0.676582 0.178027 0.337474 11.00000 0.02332 0.02992 = 0.03288 -0.00368 0.00006 -0.00394 K6 7 0.103896 0.447813 0.275500 11.00000 0.03189 0.04658 = 0.05795 -0.02167 -0.01542 0.00580 N1 3 0.461817 0.312345 0.258529 11.00000 0.02274 0.02982 = 0.03574 -0.01038 -0.00113 -0.00337 N2 3 0.351892 0.338319 0.271529 11.00000 0.01944 0.04699 = 0.04725 -0.01215 0.00027 -0.00148 C3 1 0.781235 -0.056070 0.082685 11.00000 0.03094 0.02608 = 0.02976 -0.00654 -0.00089 -0.00396 AFIX 43 H3 2 0.705808 -0.080894 0.065005 11.00000 -1.20000 AFIX 0 C4 1 0.849840 0.171830 0.354702 11.00000 0.03130 0.02363 = 0.03004 -0.00517 -0.00833 -0.00167 C5 1 1.069482 0.166171 0.298836 11.00000 0.02333 0.03872 = 0.04937 0.00401 -0.01124 -0.00475 AFIX 43 H5 2 1.128185 0.170532 0.257353 11.00000 -1.20000 AFIX 0 C6 1 1.001501 0.015173 0.134409 11.00000 0.02053 0.02388 = 0.04375 -0.00350 0.00290 0.00041 AFIX 43 H6 2 1.077704 0.038797 0.151835 11.00000 -1.20000 AFIX 0 C7 1 1.054390 0.349074 0.131128 11.00000 0.01557 0.02959 = 0.03996 -0.00736 -0.00164 -0.00122 AFIX 43 H7 2 1.103411 0.271427 0.122420 11.00000 -1.20000 AFIX 0 C9 1 1.010980 -0.088852 0.093464 11.00000 0.02850 0.02446 = 0.05081 -0.00852 0.00989 0.00310 AFIX 43 H9 2 1.093196 -0.135625 0.082697 11.00000 -1.20000 AFIX 0 C10 1 0.911986 0.575742 0.155664 11.00000 0.02759 0.02103 = 0.05305 -0.00238 0.00127 -0.00338 AFIX 43 H10 2 0.864401 0.653809 0.165104 11.00000 -1.20000 AFIX 0 C12 1 1.108257 0.454812 0.108024 11.00000 0.02599 0.03510 = 0.05558 -0.00401 0.00727 -0.00810 AFIX 43 H12 2 1.192570 0.449580 0.082929 11.00000 -1.20000 AFIX 0 C15 1 1.118275 0.143475 0.364063 11.00000 0.03108 0.05175 = 0.06672 0.00741 -0.02476 -0.00833 AFIX 43 H15 2 1.209857 0.132116 0.367055 11.00000 -1.20000 AFIX 0 C16 1 0.900464 -0.124146 0.068422 11.00000 0.04052 0.02222 = 0.03958 -0.01112 0.00489 0.00183 AFIX 43 H16 2 0.906810 -0.196198 0.041052 11.00000 -1.20000 AFIX 0 C17 1 0.900919 0.149157 0.420539 11.00000 0.04596 0.04577 = 0.03797 -0.00216 -0.01388 -0.00538 AFIX 43 H17 2 0.843636 0.141931 0.462338 11.00000 -1.20000 AFIX 0 C18 1 1.033954 0.137399 0.424527 11.00000 0.05156 0.05775 = 0.04337 0.00592 -0.02514 -0.00223 AFIX 43 H18 2 1.067690 0.125010 0.469338 11.00000 -1.20000 AFIX 0 C21 1 1.037578 0.568893 0.121949 11.00000 0.03344 0.02769 = 0.06461 0.00112 0.00716 -0.01119 AFIX 43 H21 2 1.075339 0.641990 0.108369 11.00000 -1.20000 AFIX 0 C0AA 1 0.771107 0.050632 0.123591 11.00000 0.02359 0.02121 = 0.02530 -0.00495 0.00140 -0.00048 C1AA 1 0.882492 0.085379 0.150361 11.00000 0.02135 0.02212 = 0.02913 -0.00173 0.00062 -0.00185 C22 1 0.854740 0.469360 0.175871 11.00000 0.02177 0.02342 = 0.03437 -0.00611 -0.00420 -0.00135 C23 1 0.929564 0.354083 0.166954 11.00000 0.01667 0.02614 = 0.03077 -0.00358 -0.00715 -0.00306 C8 1 0.629771 0.235926 0.049808 11.00000 0.02955 0.02636 = 0.03488 -0.00879 -0.00577 0.00133 AFIX 13 H8 2 0.559574 0.306714 0.051243 11.00000 -1.20000 AFIX 0 C24 1 0.485608 0.069664 0.135415 11.00000 0.02381 0.03569 = 0.03597 -0.01499 -0.00548 -0.00595 AFIX 13 H24 2 0.508689 0.014929 0.093705 11.00000 -1.20000 AFIX 0 C11 1 0.758865 0.287592 0.030049 11.00000 0.04121 0.03176 = 0.03138 -0.00176 -0.00273 -0.00364 AFIX 137 H11A 2 0.829008 0.219868 0.023015 11.00000 -1.50000 H11B 2 0.777082 0.339604 0.068257 11.00000 -1.50000 H11C 2 0.753635 0.336573 -0.013849 11.00000 -1.50000 AFIX 0 C25 1 0.607341 0.153601 -0.010952 11.00000 0.04712 0.03791 = 0.03326 -0.01055 -0.00766 -0.00267 AFIX 137 H25A 2 0.612128 0.200532 -0.055726 11.00000 -1.50000 H25B 2 0.521042 0.124839 -0.002038 11.00000 -1.50000 H25C 2 0.674530 0.082860 -0.013893 11.00000 -1.50000 AFIX 0 C14 1 0.461927 -0.010434 0.199990 11.00000 0.03759 0.04970 = 0.04818 -0.00852 -0.00055 -0.01877 AFIX 137 H14A 2 0.445093 0.040697 0.242177 11.00000 -1.50000 H14B 2 0.539003 -0.069744 0.204754 11.00000 -1.50000 H14C 2 0.386247 -0.054471 0.195135 11.00000 -1.50000 AFIX 0 C26 1 0.759438 -0.068937 0.297268 11.00000 0.05840 0.02486 = 0.06116 -0.00172 -0.01917 -0.00783 AFIX 137 H26A 2 0.848653 -0.060549 0.307864 11.00000 -1.50000 H26B 2 0.747566 -0.039156 0.248832 11.00000 -1.50000 H26C 2 0.744204 -0.155520 0.301625 11.00000 -1.50000 AFIX 0 C27 1 0.362001 0.153224 0.122109 11.00000 0.02221 0.04758 = 0.05850 -0.02163 -0.00920 -0.00308 AFIX 137 H27A 2 0.290367 0.103318 0.118540 11.00000 -1.50000 H27B 2 0.376976 0.199899 0.077784 11.00000 -1.50000 H27C 2 0.339198 0.210172 0.161449 11.00000 -1.50000 AFIX 0 C19 1 0.663144 0.006124 0.349178 11.00000 0.04409 0.04113 = 0.06044 0.01134 -0.00854 -0.01713 AFIX 13 H19 2 0.574346 -0.006320 0.336265 11.00000 -1.20000 AFIX 0 O1 4 0.132214 0.633731 0.357958 11.00000 0.06474 0.04994 = 0.06070 -0.02380 -0.01716 0.00389 C29 1 0.587732 0.227148 0.424820 11.00000 0.04579 0.06684 = 0.03092 0.00139 0.00822 0.00924 AFIX 13 H29 2 0.626287 0.174333 0.463075 11.00000 -1.20000 AFIX 0 C31 1 0.595602 0.355761 0.440984 11.00000 0.12960 0.06431 = 0.04244 -0.01301 0.01020 0.02301 AFIX 137 H31A 2 0.547789 0.375120 0.487201 11.00000 -1.50000 H31B 2 0.557075 0.409020 0.404327 11.00000 -1.50000 H31C 2 0.687209 0.369200 0.442240 11.00000 -1.50000 AFIX 0 C33 1 0.674284 -0.051324 0.420229 11.00000 0.13053 0.05506 = 0.05307 0.00725 0.01160 -0.01951 AFIX 137 H33A 2 0.670493 -0.139932 0.417415 11.00000 -1.50000 H33B 2 0.602220 -0.015544 0.453291 11.00000 -1.50000 H33C 2 0.757518 -0.036546 0.437040 11.00000 -1.50000 AFIX 0 C34 1 0.135436 0.762598 0.341932 11.00000 0.09371 0.05864 = 0.08768 -0.02842 -0.02548 0.00151 AFIX 23 H34A 2 0.218614 0.788611 0.354386 11.00000 -1.20000 H34B 2 0.062872 0.811031 0.370151 11.00000 -1.20000 AFIX 0 C35 1 0.442893 0.205094 0.424443 11.00000 0.04207 0.19978 = 0.04880 0.01678 0.01115 0.00638 AFIX 137 H35A 2 0.396741 0.223651 0.471166 11.00000 -1.50000 H35B 2 0.437742 0.119086 0.413463 11.00000 -1.50000 H35C 2 0.402524 0.258586 0.388463 11.00000 -1.50000 AFIX 0 C36 1 0.159627 0.607805 0.428103 11.00000 0.13729 0.08377 = 0.05693 -0.02656 -0.03314 0.00385 AFIX 23 H36A 2 0.094168 0.655419 0.461152 11.00000 -1.20000 H36B 2 0.246964 0.630783 0.435338 11.00000 -1.20000 AFIX 0 C37 1 0.155699 0.471056 0.442213 11.00000 0.20477 0.08553 = 0.04547 -0.01615 -0.02887 0.04067 AFIX 137 H37A 2 0.071801 0.447762 0.430666 11.00000 -1.50000 H37B 2 0.166097 0.452347 0.492342 11.00000 -1.50000 H37C 2 0.226667 0.424890 0.412729 11.00000 -1.50000 AFIX 0 C39 1 0.123302 0.784672 0.266831 11.00000 0.06927 0.04921 = 0.09522 -0.01022 -0.01419 0.00167 AFIX 137 H39A 2 0.123832 0.872530 0.255914 11.00000 -1.50000 H39B 2 0.041211 0.758070 0.254720 11.00000 -1.50000 H39C 2 0.196676 0.738311 0.239182 11.00000 -1.50000 AFIX 0 C40 1 0.935220 0.182709 0.293280 11.00000 0.02316 0.02324 = 0.03592 -0.00455 -0.00858 -0.00315 C1G 1 0.767911 0.555172 0.332343 11.00000 0.04466 0.06742 = 0.07002 -0.04124 0.00458 -0.01911 AFIX 137 H1GA 2 0.735150 0.593970 0.377504 11.00000 -1.50000 H1GB 2 0.851070 0.584860 0.314977 11.00000 -1.50000 H1GC 2 0.780995 0.465856 0.339311 11.00000 -1.50000 AFIX 0 C1H 1 0.529124 0.616153 0.311809 11.00000 0.04949 0.04395 = 0.07977 -0.02115 0.01465 0.00599 AFIX 137 H1HA 2 0.493660 0.539387 0.326678 11.00000 -1.50000 H1HB 2 0.475794 0.659330 0.276904 11.00000 -1.50000 H1HC 2 0.527992 0.668136 0.353117 11.00000 -1.50000 AFIX 0 P1 6 0.681896 0.461434 0.211966 11.00000 0.01606 0.02135 = 0.04283 -0.00941 -0.00386 -0.00055 PART 2 C1 1 0.636600 0.571253 0.074115 21.00000 0.03309 0.03339 = 0.08281 0.00910 -0.02431 0.00462 AFIX 137 H1A 2 0.581811 0.640528 0.054692 21.00000 -1.50000 H1B 2 0.632786 0.497773 0.046487 21.00000 -1.50000 H1C 2 0.726961 0.590542 0.071652 21.00000 -1.50000 AFIX 0 PART 1 C2 1 0.621701 0.669356 0.113049 -21.00000 0.05340 0.05534 = 0.12913 0.04101 -0.05349 -0.02549 AFIX 137 H2A 2 0.575263 0.732468 0.144644 -21.00000 -1.50000 H2B 2 0.592678 0.682283 0.065449 -21.00000 -1.50000 H2C 2 0.715752 0.674676 0.110899 -21.00000 -1.50000 AFIX 0 PART 0 C1B 1 0.594742 0.551370 0.139379 11.00000 0.03387 0.07861 = 0.10643 0.04853 -0.03322 -0.02542 PART 1 C99 1 0.450575 0.533476 0.144528 11.00000 0.03737 0.07588 = 0.14602 0.05135 -0.04588 -0.02094 AFIX 137 H99A 2 0.441344 0.445684 0.142786 11.00000 -1.50000 H99B 2 0.410250 0.576553 0.104798 11.00000 -1.50000 H99C 2 0.407343 0.566673 0.189314 11.00000 -1.50000 AFIX 0 PART 0 C13 1 0.669696 0.587399 0.278558 11.00000 0.03826 0.03183 = 0.06549 -0.02232 0.00756 -0.00707 AFIX 13 H13 2 0.694177 0.663013 0.252283 11.00000 -1.20000 AFIX 0 HKLF 4 REM p15207 in P-1 REM R1 = 0.0607 for 6710 Fo > 4sig(Fo) and 0.0841 for all 8671 data REM 467 parameters refined using 12 restraints END WGHT 0.0586 4.7040 REM Highest difference peak 0.887, deepest hole -0.618, 1-sigma level 0.082 Q1 1 0.6363 0.2488 0.2773 11.00000 0.05 0.89 Q2 1 0.5073 -0.0008 0.3805 11.00000 0.05 0.88 Q3 1 0.6231 0.1836 0.5056 11.00000 0.05 0.56 Q4 1 0.6798 0.3997 0.2420 11.00000 0.05 0.53 Q5 1 0.6277 0.3600 0.1848 11.00000 0.05 0.52 Q6 1 0.4774 0.3255 0.4328 11.00000 0.05 0.48 Q7 1 0.1849 0.4535 0.2524 11.00000 0.05 0.47 Q8 1 0.5944 0.6784 0.1690 11.00000 0.05 0.46 Q9 1 0.1023 0.3819 0.3057 11.00000 0.05 0.46 Q10 1 0.7591 0.1732 0.3499 11.00000 0.05 0.43 Q11 1 0.5595 0.2803 0.2297 11.00000 0.05 0.42 Q12 1 0.8088 0.4807 0.3491 11.00000 0.05 0.42 Q13 1 0.6479 0.2394 0.1967 11.00000 0.05 0.41 Q14 1 0.6364 0.4928 0.0744 11.00000 0.05 0.41 Q15 1 0.6583 0.1980 0.2268 11.00000 0.05 0.41 Q16 1 0.7357 0.2871 0.2330 11.00000 0.05 0.40 Q17 1 0.1187 0.4057 0.2338 11.00000 0.05 0.38 Q18 1 0.6159 0.2203 0.0865 11.00000 0.05 0.37 Q19 1 0.7571 0.2234 0.2124 11.00000 0.05 0.36 Q20 1 0.6465 0.2222 0.3860 11.00000 0.05 0.35 ; _shelx_res_checksum 48282 _shelx_hkl_file ; -1 0 0 2.48 0.38 -1 0 0 2.14 0.35 -1 0 0 2.42 0.33 -1 0 0 1.87 0.23 1 0 0 1.89 0.25 1 0 0 1.64 0.35 1 0 0 2.12 0.24 1 0 0 1.87 0.28 1 0 0 1.91 0.34 1 0 0 2.03 0.37 -2 0 0 21.91 1.41 -2 0 0 24.10 1.58 -2 0 0 23.14 1.41 -2 0 0 25.43 1.65 2 0 0 23.48 1.78 2 0 0 22.94 1.44 2 0 0 23.04 1.64 2 0 0 24.27 1.66 2 0 0 24.02 1.61 2 0 0 24.36 1.60 2 0 0 25.34 1.43 -3 0 0 29.21 1.71 -3 0 0 33.01 2.04 -3 0 0 29.83 1.72 3 0 0 31.90 1.80 3 0 0 33.70 2.22 3 0 0 31.54 2.15 3 0 0 27.91 2.13 3 0 0 27.57 2.26 3 0 0 29.76 1.81 3 0 0 33.55 2.26 -4 0 0 773.96 40.42 4 0 0 680.66 40.14 4 0 0 747.05 40.50 4 0 0 819.04 40.40 4 0 0 768.54 40.66 4 0 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0 41.61 3.16 -8 -1 0 44.61 3.62 8 1 0 45.63 2.63 -9 -1 0 6.76 1.91 -9 -1 0 8.64 2.03 -9 -1 0 9.73 1.73 -9 -1 0 7.72 1.40 9 1 0 7.16 0.96 -10 -1 0 11.20 2.03 -10 -1 0 11.52 2.18 -10 -1 0 10.13 1.74 -10 -1 0 10.90 2.02 10 1 0 9.56 1.17 -11 -1 0 2.05 1.22 -11 -1 0 4.13 1.90 -11 -1 0 0.02 1.69 -11 -1 0 1.36 0.95 -12 -1 0 8.29 1.39 -12 -1 0 7.55 1.63 -12 -1 0 11.56 2.20 -12 -1 0 9.68 1.48 -12 2 0 5.03 1.36 -11 2 0 12.64 2.39 -11 2 0 9.43 2.11 -11 2 0 13.41 2.15 -11 2 0 15.14 1.92 -10 2 0 34.40 3.66 -10 2 0 38.68 2.93 -10 2 0 37.67 3.16 -10 2 0 36.06 3.71 -9 2 0 40.59 3.97 -9 2 0 44.94 5.20 -9 2 0 42.54 3.55 -9 2 0 36.32 3.19 -9 2 0 41.69 3.91 -8 2 0 9.95 2.71 -8 2 0 6.53 2.92 -8 2 0 6.56 1.99 -8 2 0 8.43 2.10 -7 2 0 20.53 3.86 -7 2 0 19.71 3.24 -7 2 0 20.65 2.74 -7 2 0 23.72 3.38 -7 2 0 21.95 2.89 -7 2 0 24.98 4.02 6 -2 0 -0.16 2.74 6 -2 0 -2.12 3.22 5 -2 0 12.74 2.50 5 -2 0 8.49 1.99 5 -2 0 11.34 2.15 4 -2 0 153.33 8.46 4 -2 0 143.49 8.35 4 -2 0 143.12 8.59 4 -2 0 150.96 8.43 4 -2 0 159.88 9.49 4 -2 0 143.64 8.85 3 -2 0 148.39 8.18 3 -2 0 146.10 8.39 3 -2 0 148.32 8.22 3 -2 0 142.57 8.32 3 -2 0 151.43 8.17 -3 2 0 156.36 8.25 2 -2 0 6.51 0.93 2 -2 0 7.74 0.84 2 -2 0 7.03 1.05 2 -2 0 8.00 0.85 2 -2 0 7.45 0.98 2 -2 0 8.32 1.25 -2 2 0 7.75 1.17 -2 2 0 7.49 0.73 1 -2 0 4.37 0.60 1 -2 0 4.01 0.75 1 -2 0 4.55 0.81 1 -2 0 2.74 0.59 1 -2 0 4.35 0.69 1 -2 0 4.59 0.55 -1 2 0 5.14 0.78 -1 2 0 3.81 0.76 -1 2 0 4.69 0.75 -1 2 0 4.42 0.73 0 -2 0 3.01 0.62 0 -2 0 2.16 0.57 0 -2 0 3.01 0.60 0 -2 0 2.52 0.51 0 2 0 2.46 0.46 0 2 0 2.51 0.56 0 2 0 3.25 0.57 0 2 0 2.95 0.68 -1 -2 0 181.06 10.16 -1 -2 0 184.62 10.07 -1 -2 0 181.09 10.15 -1 -2 0 173.69 9.92 1 2 0 200.43 10.05 1 2 0 183.45 10.11 1 2 0 189.13 9.90 1 2 0 198.91 9.96 1 2 0 203.98 10.10 1 2 0 190.97 10.11 -2 -2 0 8.24 1.24 -2 -2 0 7.72 1.56 -2 -2 0 8.73 1.21 -2 -2 0 6.81 0.75 2 2 0 7.38 0.60 2 2 0 8.87 1.14 2 2 0 9.16 1.22 2 2 0 8.05 1.24 2 2 0 7.67 0.97 2 2 0 7.47 1.11 -3 -2 0 4.81 1.07 -3 -2 0 5.82 1.49 -3 -2 0 2.76 0.88 -3 -2 0 3.36 0.95 -3 -2 0 4.48 0.69 3 2 0 3.85 0.85 3 2 0 2.58 0.92 3 2 0 4.44 0.85 3 2 0 2.99 0.45 3 2 0 2.90 1.04 3 2 0 3.78 0.91 -4 -2 0 216.98 11.58 -4 -2 0 218.73 11.42 -4 -2 0 198.35 11.65 -4 -2 0 213.65 11.70 4 2 0 219.47 11.51 4 2 0 219.38 11.94 4 2 0 210.01 11.69 4 2 0 227.36 11.53 4 2 0 204.11 11.79 4 2 0 202.05 11.12 4 2 0 210.15 11.15 -5 -2 0 142.59 9.20 -5 -2 0 163.38 8.77 -5 -2 0 160.53 8.93 5 2 0 164.11 9.52 5 2 0 162.28 8.85 5 2 0 157.58 8.34 5 2 0 156.80 9.27 -6 -2 0 7.00 1.87 6 2 0 6.99 1.97 6 2 0 7.42 1.99 6 2 0 9.66 2.93 -7 -2 0 4.31 1.75 -7 -2 0 3.94 1.75 -7 -2 0 1.49 1.83 -7 -2 0 2.44 1.36 -7 -2 0 3.12 1.10 7 2 0 2.51 0.55 -8 -2 0 29.80 2.93 -8 -2 0 30.44 3.33 -8 -2 0 26.78 2.56 -8 -2 0 24.72 3.60 -8 -2 0 29.72 3.30 -8 -2 0 31.10 3.31 8 2 0 26.43 1.83 -9 -2 0 61.89 3.99 -9 -2 0 59.37 4.51 -9 -2 0 59.53 4.83 -9 -2 0 62.84 4.35 -9 -2 0 63.01 4.65 -9 -2 0 57.49 4.61 9 2 0 60.48 3.51 -10 -2 0 30.91 2.98 -10 -2 0 29.85 2.58 -10 -2 0 27.61 3.22 -10 -2 0 37.61 3.58 10 2 0 31.40 2.16 10 2 0 23.50 2.90 -11 -2 0 5.59 1.78 -11 -2 0 3.17 1.00 -11 -2 0 6.69 1.93 -11 -2 0 4.87 1.43 11 2 0 3.64 1.08 -12 -2 0 5.07 0.98 -12 -2 0 5.24 1.66 -12 -2 0 6.32 1.26 -12 -2 0 5.56 1.51 -11 3 0 1.37 1.54 -11 3 0 2.05 1.13 -10 3 0 28.00 2.57 -10 3 0 29.12 3.78 -10 3 0 35.37 4.89 -10 3 0 24.26 2.95 -9 3 0 9.39 1.79 -9 3 0 7.19 2.34 -9 3 0 8.91 2.37 -9 3 0 7.00 2.48 -9 3 0 8.70 1.46 -9 3 0 9.00 2.60 -8 3 0 0.27 2.24 -8 3 0 2.23 1.61 -8 3 0 2.42 1.26 -8 3 0 4.01 1.72 -8 3 0 2.05 2.11 -8 3 0 0.32 2.06 -8 3 0 2.22 2.38 -7 3 0 66.90 4.38 -7 3 0 60.81 4.93 -7 3 0 56.55 5.00 -7 3 0 59.84 4.56 -7 3 0 50.92 5.01 -7 3 0 49.41 7.08 -7 3 0 60.97 5.16 -6 3 0 5.43 2.41 -6 3 0 5.49 2.28 5 -3 0 2.35 1.90 5 -3 0 -2.79 2.26 5 -3 0 1.94 2.42 4 -3 0 182.21 9.21 4 -3 0 144.88 9.60 4 -3 0 163.11 9.37 -4 3 0 172.50 9.48 3 -3 0 38.68 2.75 3 -3 0 29.28 2.51 3 -3 0 35.16 2.61 3 -3 0 39.13 2.45 3 -3 0 35.15 2.29 3 -3 0 37.92 2.30 3 -3 0 34.92 3.46 3 -3 0 33.26 2.34 -3 3 0 41.17 2.83 2 -3 0 19.10 1.96 2 -3 0 19.96 1.50 2 -3 0 18.92 2.18 2 -3 0 21.01 1.66 2 -3 0 23.98 1.56 2 -3 0 17.54 1.37 -2 3 0 18.97 1.50 -2 3 0 21.24 1.96 -2 3 0 17.21 1.71 1 -3 0 80.96 4.57 1 -3 0 79.94 4.48 1 -3 0 73.64 4.52 1 -3 0 75.91 4.28 -1 3 0 85.05 4.63 -1 3 0 74.37 4.51 -1 3 0 77.34 4.41 -1 3 0 74.53 4.36 0 -3 0 213.21 11.10 0 -3 0 196.82 11.14 0 -3 0 205.08 11.11 0 -3 0 203.46 11.01 0 3 0 192.54 11.11 0 3 0 212.76 11.06 0 3 0 210.41 10.95 0 3 0 212.19 10.96 -1 -3 0 778.43 40.92 -1 -3 0 790.65 40.86 -1 -3 0 719.37 40.60 -1 -3 0 849.84 40.94 1 3 0 805.56 40.85 1 3 0 763.97 40.83 1 3 0 758.49 40.61 1 3 0 761.27 40.91 -2 -3 0 3.35 1.01 -2 -3 0 5.26 1.27 -2 -3 0 1.17 1.18 -2 -3 0 2.96 0.95 -2 -3 0 2.72 0.52 2 3 0 3.37 1.24 2 3 0 4.64 0.92 2 3 0 3.02 0.76 2 3 0 4.03 1.01 2 3 0 4.22 0.55 2 3 0 3.82 0.95 -3 -3 0 63.74 4.33 -3 -3 0 61.80 4.01 -3 -3 0 58.32 4.12 -3 -3 0 67.84 4.76 3 3 0 60.45 3.88 3 3 0 66.17 3.41 3 3 0 64.00 4.28 3 3 0 61.44 4.14 3 3 0 62.69 3.91 3 3 0 62.10 3.80 -4 -3 0 168.87 8.83 -4 -3 0 167.75 9.19 -4 -3 0 158.38 9.36 4 3 0 151.91 9.26 4 3 0 163.89 8.99 4 3 0 153.18 9.52 4 3 0 162.94 9.47 4 3 0 167.73 9.06 4 3 0 162.28 8.54 -5 -3 0 111.89 6.38 -5 -3 0 112.27 6.93 -5 -3 0 99.30 7.61 5 3 0 118.36 6.65 5 3 0 116.30 7.38 5 3 0 109.98 5.94 6 3 0 15.35 3.40 6 3 0 14.39 2.89 6 3 0 18.60 2.67 6 3 0 17.57 1.21 -7 -3 0 10.92 2.25 -7 -3 0 14.13 2.51 -7 -3 0 14.98 2.19 -7 -3 0 11.32 1.91 -7 -3 0 11.92 1.80 -7 -3 0 12.02 1.92 -7 -3 0 13.26 1.57 7 3 0 8.92 3.57 7 3 0 8.84 1.51 7 3 0 10.91 1.06 -8 -3 0 20.08 2.93 -8 -3 0 14.94 2.17 -8 -3 0 18.07 2.64 -8 -3 0 17.31 2.91 -8 -3 0 18.51 2.66 -8 -3 0 19.10 3.25 8 3 0 18.11 1.44 8 3 0 17.46 1.85 -9 -3 0 20.41 3.24 -9 -3 0 13.22 2.20 -9 -3 0 14.43 2.49 -9 -3 0 18.46 2.31 -9 -3 0 18.47 2.28 -9 -3 0 17.48 2.99 9 3 0 14.63 2.01 9 3 0 17.59 1.54 -10 -3 0 1.65 1.97 -10 -3 0 5.75 1.93 -10 -3 0 2.61 1.10 -10 -3 0 2.47 1.39 -10 -3 0 0.26 1.66 10 3 0 3.68 0.89 10 3 0 4.82 1.17 -11 -3 0 4.18 1.05 -11 -3 0 5.70 1.46 -11 -3 0 8.91 2.06 -11 -3 0 3.16 1.58 11 3 0 2.34 1.01 11 3 0 5.29 1.17 -12 -3 0 4.82 0.93 -12 -3 0 4.88 1.59 -12 -3 0 3.72 1.46 -12 -3 0 5.12 1.16 -10 4 0 0.91 1.17 -10 4 0 0.56 2.10 -10 4 0 -3.97 3.44 -9 4 0 0.94 2.13 -9 4 0 1.12 1.93 -9 4 0 3.50 1.56 -9 4 0 1.10 1.86 -8 4 0 20.94 2.94 -8 4 0 21.85 3.55 -8 4 0 21.88 2.92 -8 4 0 20.26 3.47 -8 4 0 18.88 3.61 -7 4 0 110.76 6.73 -7 4 0 98.69 6.32 -7 4 0 98.66 6.75 -7 4 0 92.55 6.78 -7 4 0 107.26 6.35 -6 4 0 6.94 2.07 -6 4 0 9.32 2.21 -6 4 0 4.54 1.65 5 -4 0 -4.87 3.66 4 -4 0 4.21 1.65 -4 4 0 4.00 2.07 3 -4 0 11.25 2.20 3 -4 0 8.82 1.51 3 -4 0 9.71 0.95 3 -4 0 10.53 1.78 3 -4 0 8.75 1.61 -3 4 0 9.34 1.74 -3 4 0 9.04 1.36 -3 4 0 10.39 1.56 2 -4 0 147.94 8.01 2 -4 0 158.18 8.46 2 -4 0 150.55 8.11 2 -4 0 148.77 8.48 -2 4 0 162.16 8.72 -2 4 0 153.21 8.35 -2 4 0 142.86 8.26 1 -4 0 3.92 1.38 1 -4 0 4.33 1.12 1 -4 0 3.36 0.49 1 -4 0 5.76 1.49 1 -4 0 4.85 0.91 1 -4 0 5.27 0.95 1 -4 0 4.60 1.29 -1 4 0 4.38 1.19 -1 4 0 3.85 0.94 -1 4 0 5.52 0.98 -1 4 0 5.13 1.45 0 -4 0 2.13 1.13 0 -4 0 2.58 1.00 0 -4 0 1.74 0.55 0 -4 0 2.18 0.38 0 -4 0 0.74 1.36 0 -4 0 2.58 1.09 0 4 0 0.74 0.85 0 4 0 2.24 1.39 0 4 0 1.04 0.80 0 4 0 3.93 0.78 -1 -4 0 136.75 7.78 -1 -4 0 153.25 8.31 -1 -4 0 143.59 8.27 -1 -4 0 142.21 8.31 -1 -4 0 146.10 8.50 1 4 0 134.24 8.40 1 4 0 145.69 8.09 1 4 0 159.13 8.04 1 4 0 151.84 8.18 -2 -4 0 10.61 1.78 -2 -4 0 7.53 0.95 -2 -4 0 12.40 2.23 -2 -4 0 11.45 1.56 -2 -4 0 7.02 2.02 -2 -4 0 10.37 1.86 2 4 0 8.39 1.63 2 4 0 9.64 1.68 2 4 0 9.18 1.19 2 4 0 7.53 1.94 2 4 0 7.53 0.84 -3 -4 0 11.25 2.10 -3 -4 0 7.56 2.67 -3 -4 0 6.37 1.60 3 4 0 1.35 2.22 3 4 0 3.59 1.42 3 4 0 4.65 1.27 3 4 0 5.54 1.30 -4 -4 0 0.04 1.66 -4 -4 0 1.03 1.03 4 4 0 1.77 1.78 4 4 0 0.97 1.84 4 4 0 1.34 3.14 4 4 0 0.63 1.32 4 4 0 2.24 1.20 -5 -4 0 49.93 4.96 -5 -4 0 47.83 4.38 5 4 0 53.46 2.90 5 4 0 50.33 3.03 5 4 0 52.84 4.04 5 4 0 50.95 4.23 5 4 0 52.52 5.10 -6 -4 0 28.75 2.71 -6 -4 0 30.38 3.49 -6 -4 0 44.22 4.45 6 4 0 31.96 6.33 6 4 0 34.36 2.21 6 4 0 35.54 2.05 -7 -4 0 67.04 4.74 -7 -4 0 65.71 5.20 -7 -4 0 59.53 4.24 -7 -4 0 58.86 4.31 -7 -4 0 57.24 3.92 -7 -4 0 64.96 4.70 -7 -4 0 56.85 4.63 7 4 0 65.45 3.49 7 4 0 55.02 4.11 7 4 0 62.32 3.59 -8 -4 0 2.79 1.07 -8 -4 0 5.22 2.01 -8 -4 0 2.51 2.72 -8 -4 0 4.77 1.65 -8 -4 0 4.26 1.54 -8 -4 0 3.79 1.71 8 4 0 4.46 0.80 8 4 0 5.35 0.97 -9 -4 0 -0.34 1.75 -9 -4 0 -0.16 1.28 -9 -4 0 -0.74 1.57 -9 -4 0 2.91 1.72 -9 -4 0 1.31 0.95 -9 -4 0 0.80 1.76 9 4 0 1.26 0.74 9 4 0 -0.51 0.90 -10 -4 0 7.20 1.51 -10 -4 0 6.60 1.93 -10 -4 0 4.88 1.75 -10 -4 0 6.98 2.06 -10 -4 0 10.40 1.82 10 4 0 7.88 1.19 10 4 0 8.36 1.41 -11 -4 0 5.49 1.40 -11 -4 0 3.99 1.79 -11 -4 0 7.20 1.70 11 4 0 4.54 1.07 11 4 0 6.64 1.08 -12 -4 0 25.26 2.15 -12 -4 0 22.94 2.42 -12 -4 0 20.26 2.25 -12 -4 0 24.99 2.06 12 4 0 20.02 2.14 -10 5 0 0.91 1.86 -10 5 0 3.84 1.81 -9 5 0 11.65 3.25 -9 5 0 15.18 1.88 -9 5 0 17.84 3.22 -9 5 0 15.66 1.84 -8 5 0 20.30 3.63 -8 5 0 24.08 3.32 -8 5 0 24.43 3.02 -8 5 0 24.42 2.67 -7 5 0 9.89 1.63 -7 5 0 9.96 2.11 -7 5 0 12.04 2.36 -7 5 0 12.16 1.91 -6 5 0 -2.25 1.88 -6 5 0 2.11 1.76 -6 5 0 1.61 1.28 5 -5 0 1.54 0.70 -5 5 0 -1.41 1.94 -5 5 0 2.63 2.05 -5 5 0 1.10 1.31 -5 5 0 0.81 1.95 4 -5 0 8.21 0.99 4 -5 0 6.82 2.02 -4 5 0 11.13 3.04 3 -5 0 1.13 1.65 3 -5 0 0.18 0.48 -3 5 0 0.20 2.14 2 -5 0 40.37 3.35 2 -5 0 38.39 4.25 2 -5 0 37.14 2.14 -2 5 0 30.24 3.97 -2 5 0 36.21 3.69 1 -5 0 9.96 0.88 1 -5 0 12.00 2.18 1 -5 0 10.22 1.52 1 -5 0 9.46 1.49 1 -5 0 9.92 2.41 -1 5 0 9.61 1.51 -1 5 0 10.06 1.90 -1 5 0 9.37 1.54 0 -5 0 25.70 3.93 0 -5 0 27.51 2.81 0 -5 0 30.65 2.99 0 -5 0 24.51 1.77 0 -5 0 25.90 3.01 0 5 0 22.35 2.41 0 5 0 19.69 2.63 0 5 0 29.39 2.13 -1 -5 0 5.14 0.97 -1 -5 0 6.07 1.71 -1 -5 0 5.62 2.11 1 5 0 6.69 1.54 1 5 0 4.73 1.31 1 5 0 4.09 1.21 -2 -5 0 23.99 1.61 -2 -5 0 21.72 2.94 -2 -5 0 20.51 1.68 -2 -5 0 22.30 4.40 2 5 0 25.79 2.86 2 5 0 22.12 1.97 2 5 0 24.40 2.66 2 5 0 26.65 2.63 2 5 0 23.99 1.52 -3 -5 0 4.20 0.81 -3 -5 0 3.76 1.99 3 5 0 2.92 0.65 3 5 0 2.15 0.48 3 5 0 2.95 1.58 3 5 0 3.91 1.87 3 5 0 2.31 2.72 -4 -5 0 9.05 1.77 -4 -5 0 9.64 2.69 4 5 0 9.16 1.10 4 5 0 8.95 2.12 4 5 0 8.15 0.90 4 5 0 7.22 2.26 -5 -5 0 19.39 3.92 5 5 0 16.14 2.99 5 5 0 22.37 1.62 5 5 0 18.85 3.80 5 5 0 21.53 1.46 -6 -5 0 26.60 4.72 -6 -5 0 23.05 3.20 -6 -5 0 20.20 2.79 -6 -5 0 24.52 3.41 -6 -5 0 16.61 2.17 -6 -5 0 16.87 2.13 6 5 0 15.80 2.12 6 5 0 21.30 1.66 6 5 0 22.79 1.52 -7 -5 0 53.76 4.47 -7 -5 0 57.72 4.02 -7 -5 0 54.63 5.08 -7 -5 0 55.31 4.20 -7 -5 0 56.05 4.53 -7 -5 0 57.25 3.73 -7 -5 0 62.22 4.64 7 5 0 59.56 3.32 7 5 0 58.59 3.43 7 5 0 53.61 3.66 -8 -5 0 1.10 0.94 -8 -5 0 1.17 1.71 -8 -5 0 2.14 1.46 -8 -5 0 1.55 1.46 -8 -5 0 1.77 1.91 -8 -5 0 4.58 1.73 -8 -5 0 4.54 1.87 8 5 0 1.70 1.08 8 5 0 2.00 0.89 8 5 0 1.74 0.74 -9 -5 0 12.49 2.06 -9 -5 0 10.77 1.82 -9 -5 0 19.62 3.48 -9 -5 0 11.13 2.24 -9 -5 0 12.27 2.37 -9 -5 0 16.84 2.33 -9 -5 0 13.36 2.45 9 5 0 15.98 2.86 9 5 0 13.84 2.16 9 5 0 15.28 1.58 -10 -5 0 -0.37 1.57 -10 -5 0 1.40 1.87 -10 -5 0 2.65 1.72 -10 -5 0 2.34 1.01 -10 -5 0 1.59 1.29 10 5 0 1.58 0.85 10 5 0 0.66 1.34 10 5 0 1.83 0.95 -11 -5 0 17.33 2.13 -11 -5 0 10.87 2.10 -11 -5 0 12.10 1.86 -11 -5 0 13.40 2.13 11 5 0 10.09 1.67 11 5 0 11.94 1.63 -12 -5 0 8.14 1.49 -12 -5 0 5.30 1.75 12 5 0 6.06 1.11 -10 6 0 3.71 1.92 -10 6 0 2.60 1.65 -9 6 0 1.23 1.57 -9 6 0 -0.89 1.40 -9 6 0 0.70 1.68 -8 6 0 9.98 2.21 -8 6 0 16.14 2.26 -8 6 0 11.62 1.81 -8 6 0 13.86 2.20 -7 6 0 4.32 2.04 -7 6 0 1.50 1.82 -7 6 0 2.51 1.66 -7 6 0 4.17 1.42 6 -6 0 24.69 2.27 -6 6 0 27.15 3.77 -6 6 0 26.18 2.82 -6 6 0 30.80 3.42 5 -6 0 0.31 0.70 -5 6 0 3.66 1.71 -5 6 0 1.19 1.25 -5 6 0 2.63 1.76 -5 6 0 -2.99 1.87 4 -6 0 2.54 0.64 -4 6 0 -0.01 1.91 -4 6 0 2.71 3.09 -4 6 0 0.35 1.91 -4 6 0 2.70 1.38 -4 6 0 4.98 2.01 3 -6 0 3.90 2.77 3 -6 0 -0.35 1.03 3 -6 0 0.57 0.51 -3 6 0 3.09 2.67 -3 6 0 -4.21 3.39 -3 6 0 0.94 1.77 -3 6 0 -1.33 1.97 -3 6 0 0.85 1.33 2 -6 0 117.70 7.51 2 -6 0 117.15 6.08 2 -6 0 108.55 6.23 -2 6 0 107.61 7.92 1 -6 0 22.21 1.86 1 -6 0 28.92 3.69 1 -6 0 22.35 1.55 -1 6 0 27.43 4.26 -1 6 0 22.35 3.46 0 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0 4.59 1.96 -8 -6 0 5.99 1.59 -8 -6 0 5.16 1.55 -8 -6 0 5.90 1.96 -8 -6 0 6.81 1.97 -8 -6 0 2.16 2.29 -8 -6 0 5.19 1.18 8 6 0 6.52 2.06 8 6 0 4.80 1.06 8 6 0 8.64 1.40 -9 -6 0 1.04 1.85 -9 -6 0 1.21 1.44 -9 -6 0 2.96 1.71 -9 -6 0 0.24 1.39 -9 -6 0 2.00 1.07 -9 -6 0 2.95 1.98 -9 -6 0 4.73 2.20 9 6 0 2.71 2.25 9 6 0 3.47 0.95 9 6 0 2.87 1.02 9 6 0 1.87 0.86 -10 -6 0 1.45 1.46 -10 -6 0 -0.68 1.37 -10 -6 0 0.32 1.96 -10 -6 0 2.86 1.12 -10 -6 0 -0.34 1.60 10 6 0 2.87 1.57 10 6 0 1.13 1.01 10 6 0 0.74 0.85 -11 -6 0 4.67 1.48 -11 -6 0 3.78 1.33 -11 -6 0 1.02 1.13 -11 -6 0 1.97 0.76 -11 -6 0 -0.50 1.73 11 6 0 1.09 0.97 11 6 0 2.19 1.69 -12 -6 0 0.97 1.13 -12 -6 0 -1.93 1.18 -10 7 0 1.99 1.41 -10 7 0 0.17 1.26 -9 7 0 10.20 1.47 -9 7 0 11.01 2.02 -9 7 0 12.20 2.41 -8 7 0 8.09 1.86 -8 7 0 9.13 1.55 -8 7 0 11.31 2.16 -7 7 0 68.94 4.99 -7 7 0 69.93 4.58 -7 7 0 66.42 5.29 -7 7 0 79.78 4.88 -6 7 0 5.47 1.81 -6 7 0 5.28 1.87 -6 7 0 -0.25 1.90 -6 7 0 1.19 1.31 5 -7 0 -0.11 1.28 5 -7 0 0.90 1.37 -5 7 0 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5.65 -2 8 0 63.59 5.04 -2 8 0 65.91 4.90 -2 8 0 60.77 4.28 -2 8 0 61.70 5.50 1 -8 0 2.00 1.28 1 -8 0 3.49 0.88 1 -8 0 3.28 0.89 -1 8 0 2.85 1.87 -1 8 0 2.18 1.37 -1 8 0 8.28 2.50 -1 8 0 2.92 2.20 -1 8 0 3.85 2.79 0 -8 0 32.12 2.32 0 -8 0 29.66 2.69 0 -8 0 34.01 2.31 0 8 0 38.85 6.49 0 8 0 35.05 3.86 0 8 0 29.87 3.17 0 8 0 25.62 4.01 -1 -8 0 -2.94 2.36 -1 -8 0 1.33 0.85 -1 -8 0 3.61 1.09 -1 -8 0 1.66 0.88 1 8 0 4.67 1.14 1 8 0 1.93 1.57 1 8 0 1.55 2.07 1 8 0 2.22 1.93 -2 -8 0 22.52 4.16 -2 -8 0 20.20 1.94 -2 -8 0 17.12 2.16 -2 -8 0 22.92 3.18 2 8 0 26.29 3.47 2 8 0 21.57 2.50 2 8 0 19.47 2.87 2 8 0 16.34 1.94 -3 -8 0 5.38 1.80 -3 -8 0 -2.36 1.36 -3 -8 0 4.48 2.83 -3 -8 0 1.11 1.05 -3 -8 0 2.82 1.13 3 8 0 0.99 1.40 3 8 0 1.00 1.81 3 8 0 -0.84 2.45 3 8 0 2.65 0.92 -4 -8 0 3.37 2.38 -4 -8 0 0.59 1.14 -4 -8 0 3.34 1.67 4 8 0 0.28 0.95 4 8 0 1.08 1.72 4 8 0 -0.49 0.80 4 8 0 0.26 0.86 4 8 0 4.91 2.75 -5 -8 0 2.36 2.16 -5 -8 0 2.38 1.89 -5 -8 0 4.82 1.64 5 8 0 5.58 1.06 5 8 0 6.05 1.75 5 8 0 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