data_(TPB)FeMe_(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H57 B Cl Fe P3' _chemical_formula_weight 696.85 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' 'B' 'B' 0.0013 0.0007 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9554(3) _cell_length_b 11.5075(3) _cell_length_c 15.9312(4) _cell_angle_alpha 91.4010(10) _cell_angle_beta 95.4060(10) _cell_angle_gamma 117.8130(10) _cell_volume 1763.16(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max .456 _exptl_crystal_size_mid .304 _exptl_crystal_size_min .209 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36496 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.10 _reflns_number_total 7758 _reflns_number_gt 6879 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0417P)^2^+1.1269P] 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 7758 _refine_ls_number_parameters 402 _refine_ls_number_restraints 338 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.063 _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 Fe1 Fe 0.10282(2) 0.29538(2) 0.180553(13) 0.01359(7) Uani 1 1 d U . . P3 P 0.15616(4) 0.51633(4) 0.22122(2) 0.01526(9) Uani 1 1 d U A . P4 P -0.09639(4) 0.10654(4) 0.22525(2) 0.01384(9) Uani 1 1 d U A . P5 P 0.31461(4) 0.28554(4) 0.21801(2) 0.01438(9) Uani 1 1 d U A . C1 C 0.53268(19) 0.54399(17) 0.20314(14) 0.0324(4) Uani 1 1 d U A . H1A H 0.5941 0.6250 0.2361 0.049 Uiso 1 1 calc R . . H1B H 0.4540 0.5503 0.1762 0.049 Uiso 1 1 calc R . . H1C H 0.5811 0.5280 0.1608 0.049 Uiso 1 1 calc R . . C2 C 0.2308(2) 0.59974(19) 0.06023(11) 0.0309(4) Uani 1 1 d U A . H2A H 0.2870 0.6699 0.0275 0.046 Uiso 1 1 calc R . . H2B H 0.1344 0.5671 0.0395 0.046 Uiso 1 1 calc R . . H2C H 0.2548 0.5298 0.0555 0.046 Uiso 1 1 calc R . . C3 C -0.11247(19) -0.13369(16) 0.16473(11) 0.0245(3) Uani 1 1 d U A . H3A H -0.0789 -0.1963 0.1747 0.037 Uiso 1 1 calc R . . H3B H -0.0660 -0.0794 0.1212 0.037 Uiso 1 1 calc R . . H3C H -0.2108 -0.1796 0.1472 0.037 Uiso 1 1 calc R . . C4 C 0.31905(16) 0.09186(16) 0.32613(10) 0.0196(3) Uani 1 1 d U A . H4A H 0.3763 0.0796 0.2914 0.024 Uiso 1 1 calc R . . C5 C -0.27837(19) 0.16706(18) 0.12486(13) 0.0297(4) Uani 1 1 d U A . H5A H -0.3534 0.1397 0.0800 0.045 Uiso 1 1 calc R . . H5B H -0.1961 0.2380 0.1079 0.045 Uiso 1 1 calc R . . H5C H -0.3027 0.1963 0.1746 0.045 Uiso 1 1 calc R . . C6 C -0.38828(17) -0.06934(17) 0.15770(11) 0.0255(4) Uani 1 1 d U A . H6A H -0.4470 -0.1018 0.1048 0.038 Uiso 1 1 calc R . . H6B H -0.4343 -0.0445 0.1974 0.038 Uiso 1 1 calc R . . H6C H -0.3692 -0.1371 0.1794 0.038 Uiso 1 1 calc R . . C7 C 0.4244(2) 0.27822(19) 0.06574(12) 0.0305(4) Uani 1 1 d U A . H7A H 0.4319 0.2236 0.0222 0.046 Uiso 1 1 calc R . . H7B H 0.5150 0.3492 0.0852 0.046 Uiso 1 1 calc R . . H7C H 0.3651 0.3135 0.0435 0.046 Uiso 1 1 calc R . . C8 C 0.25608(18) 0.65113(16) 0.15254(11) 0.0229(3) Uani 1 1 d U . . H8A H 0.3544 0.6790 0.1707 0.027 Uiso 1 1 calc R A . C9 C -0.17379(17) 0.28821(16) 0.46144(10) 0.0198(3) Uani 1 1 d U . . H9A H -0.1861 0.3320 0.5071 0.024 Uiso 1 1 calc R . . C10 C -0.16766(19) -0.12387(16) 0.31625(11) 0.0244(3) Uani 1 1 d U A . H10D H -0.1549 -0.2001 0.3242 0.037 Uiso 1 1 calc R . . H10E H -0.2644 -0.1512 0.3001 0.037 Uiso 1 1 calc R . . H10F H -0.1366 -0.0686 0.3681 0.037 Uiso 1 1 calc R . . C11 C 0.45492(17) 0.72611(16) 0.42347(11) 0.0237(3) Uani 1 1 d U . . H11A H 0.5249 0.8114 0.4395 0.028 Uiso 1 1 calc R . . C12 C 0.19491(17) 0.03784(16) 0.44799(10) 0.0212(3) Uani 1 1 d U . . H12A H 0.1676 -0.0114 0.4946 0.025 Uiso 1 1 calc R . . C13 C -0.26799(16) 0.11674(16) 0.34844(10) 0.0191(3) Uani 1 1 d U . . H13A H -0.3431 0.0430 0.3197 0.023 Uiso 1 1 calc R . . C14 C 0.43502(17) 0.62495(17) 0.47511(11) 0.0229(3) Uani 1 1 d U . . H14A H 0.4904 0.6427 0.5266 0.027 Uiso 1 1 calc R . . C15 C 0.01255(18) 0.63519(18) 0.30362(11) 0.0255(4) Uani 1 1 d U A . H15A H -0.0771 0.6230 0.3149 0.038 Uiso 1 1 calc R . . H15B H 0.0621 0.7187 0.2806 0.038 Uiso 1 1 calc R . . H15C H 0.0640 0.6332 0.3553 0.038 Uiso 1 1 calc R . . C16 C -0.08846(17) 0.52187(16) 0.15635(10) 0.0214(3) Uani 1 1 d U A . H16A H -0.1825 0.4975 0.1654 0.032 Uiso 1 1 calc R . . H16B H -0.0880 0.4587 0.1161 0.032 Uiso 1 1 calc R . . H16C H -0.0468 0.6076 0.1350 0.032 Uiso 1 1 calc R . . C17 C 0.36257(17) 0.19579(16) 0.13966(10) 0.0205(3) Uani 1 1 d U . . H17A H 0.4323 0.1750 0.1684 0.025 Uiso 1 1 calc R A . C18 C 0.15266(16) 0.13253(15) 0.43118(10) 0.0181(3) Uani 1 1 d U . . H18A H 0.0987 0.1465 0.4678 0.022 Uiso 1 1 calc R . . C19 C 0.24131(18) 0.77669(17) 0.15803(13) 0.0282(4) Uani 1 1 d U A . H19A H 0.3108 0.8433 0.1289 0.042 Uiso 1 1 calc R . . H19B H 0.2532 0.8074 0.2163 0.042 Uiso 1 1 calc R . . H19C H 0.1507 0.7583 0.1323 0.042 Uiso 1 1 calc R . . C20 C 0.23459(19) 0.06654(17) 0.10637(11) 0.0255(4) Uani 1 1 d U A . H20D H 0.2607 0.0177 0.0688 0.038 Uiso 1 1 calc R . . H20E H 0.1663 0.0852 0.0764 0.038 Uiso 1 1 calc R . . H20F H 0.1964 0.0155 0.1529 0.038 Uiso 1 1 calc R . . C21 C 0.27782(18) 0.01675(16) 0.39525(11) 0.0219(3) Uani 1 1 d U . . H21A H 0.3056 -0.0470 0.4060 0.026 Uiso 1 1 calc R . . C22 C -0.28735(16) 0.17974(16) 0.41790(10) 0.0196(3) Uani 1 1 d U . . H22A H -0.3753 0.1495 0.4349 0.024 Uiso 1 1 calc R . . C23 C 0.48274(16) 0.42986(16) 0.26112(11) 0.0213(3) Uani 1 1 d U . . H23A H 0.4641 0.4641 0.3126 0.026 Uiso 1 1 calc R A . C24 C -0.08317(16) -0.04674(15) 0.24650(10) 0.0178(3) Uani 1 1 d U . . H24A H 0.0144 -0.0173 0.2677 0.021 Uiso 1 1 calc R A . C25 C 0.33230(16) 0.49688(16) 0.45006(10) 0.0190(3) Uani 1 1 d U . . H25A H 0.3192 0.4305 0.4859 0.023 Uiso 1 1 calc R . . C26 C -0.04159(16) 0.33147(16) 0.43693(10) 0.0183(3) Uani 1 1 d U A . H26A H 0.0336 0.4023 0.4680 0.022 Uiso 1 1 calc R . . C27 C 0.27483(15) 0.18559(14) 0.30876(9) 0.0153(3) Uani 1 1 d U . . C29 C 0.18863(15) 0.20802(14) 0.36071(9) 0.0145(3) Uani 1 1 d U A . C30 C 0.26685(15) 0.56966(15) 0.32211(10) 0.0166(3) Uani 1 1 d U . . C31 C 0.24777(15) 0.46493(15) 0.37216(9) 0.0148(3) Uani 1 1 d U A . C32 C 0.36939(17) 0.69904(16) 0.34751(11) 0.0216(3) Uani 1 1 d U A . H32A H 0.3803 0.7669 0.3135 0.026 Uiso 1 1 calc R . . C33 C -0.01848(15) 0.27114(14) 0.36657(9) 0.0142(3) Uani 1 1 d U . . C34 C -0.13605(15) 0.16400(15) 0.32170(9) 0.0149(3) Uani 1 1 d U A . C35 C -0.00569(16) 0.52487(15) 0.24014(10) 0.0177(3) Uani 1 1 d U . . H35A H -0.0639 0.4426 0.2648 0.021 Uiso 1 1 calc R A . C38 C -0.25114(16) 0.05120(15) 0.14413(10) 0.0189(3) Uani 1 1 d U . . H38A H -0.2236 0.0281 0.0921 0.023 Uiso 1 1 calc R A . C75 C 0.59763(17) 0.39435(19) 0.28939(12) 0.0283(4) Uani 1 1 d U A . H75A H 0.6756 0.4699 0.3192 0.042 Uiso 1 1 calc R . . H75B H 0.6261 0.3672 0.2407 0.042 Uiso 1 1 calc R . . H75C H 0.5633 0.3237 0.3260 0.042 Uiso 1 1 calc R . . C100 C 0.0513(16) 0.2585(15) 0.0499(7) 0.024(2) Uani 0.698(4) 1 d PU A 1 H10A H 0.1347 0.2953 0.0229 0.035 Uiso 0.698(4) 1 calc PR A 1 H10B H -0.0055 0.2981 0.0309 0.035 Uiso 0.698(4) 1 calc PR A 1 H10C H 0.0009 0.1651 0.0358 0.035 Uiso 0.698(4) 1 calc PR A 1 Cl1 Cl 0.0430(9) 0.2526(9) 0.0358(5) 0.0246(9) Uani 0.302(4) 1 d PU A 2 B1 B 0.13479(17) 0.31482(16) 0.34008(10) 0.0138(3) Uani 1 1 d U A . 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 0.01355(11) 0.01421(11) 0.01246(11) 0.00067(8) 0.00155(8) 0.00610(8) P3 0.01706(18) 0.01595(18) 0.01527(18) 0.00324(14) 0.00328(14) 0.00951(15) P4 0.01380(17) 0.01369(18) 0.01343(18) -0.00061(13) 0.00195(13) 0.00601(14) P5 0.01533(18) 0.01533(18) 0.01426(18) 0.00132(14) 0.00368(14) 0.00836(15) C1 0.0247(9) 0.0193(8) 0.0524(12) 0.0067(8) 0.0123(8) 0.0082(7) C2 0.0355(10) 0.0297(9) 0.0233(9) 0.0073(7) 0.0073(7) 0.0109(8) C3 0.0293(9) 0.0191(8) 0.0262(9) -0.0033(6) 0.0046(7) 0.0122(7) C4 0.0205(7) 0.0220(8) 0.0206(8) 0.0008(6) 0.0022(6) 0.0136(6) C5 0.0227(8) 0.0305(9) 0.0361(10) 0.0050(8) -0.0027(7) 0.0137(7) C6 0.0166(7) 0.0251(8) 0.0264(9) -0.0022(7) -0.0002(6) 0.0036(7) C7 0.0355(10) 0.0351(10) 0.0246(9) 0.0040(7) 0.0151(7) 0.0176(8) C8 0.0231(8) 0.0223(8) 0.0262(8) 0.0083(6) 0.0065(6) 0.0121(7) C9 0.0236(8) 0.0248(8) 0.0158(7) 0.0000(6) 0.0043(6) 0.0152(7) C10 0.0308(9) 0.0188(8) 0.0248(8) 0.0047(6) 0.0068(7) 0.0120(7) C11 0.0167(7) 0.0198(8) 0.0292(9) -0.0084(6) 0.0018(6) 0.0046(6) C12 0.0243(8) 0.0225(8) 0.0175(7) 0.0065(6) 0.0019(6) 0.0116(7) C13 0.0164(7) 0.0194(7) 0.0190(7) 0.0008(6) 0.0025(6) 0.0064(6) C14 0.0173(7) 0.0306(9) 0.0208(8) -0.0082(6) -0.0027(6) 0.0128(7) C15 0.0243(8) 0.0339(9) 0.0240(8) -0.0047(7) 0.0001(7) 0.0192(7) C16 0.0194(7) 0.0206(8) 0.0236(8) 0.0029(6) 0.0003(6) 0.0092(6) C17 0.0245(8) 0.0250(8) 0.0190(7) 0.0004(6) 0.0058(6) 0.0170(7) C18 0.0187(7) 0.0199(7) 0.0162(7) 0.0009(6) 0.0026(6) 0.0094(6) C19 0.0240(8) 0.0213(8) 0.0426(11) 0.0134(7) 0.0078(7) 0.0122(7) C20 0.0345(9) 0.0227(8) 0.0228(8) -0.0030(6) 0.0025(7) 0.0169(7) C21 0.0263(8) 0.0212(8) 0.0236(8) 0.0037(6) 0.0010(6) 0.0159(7) C22 0.0168(7) 0.0260(8) 0.0189(7) 0.0036(6) 0.0052(6) 0.0118(6) C23 0.0162(7) 0.0211(8) 0.0245(8) -0.0023(6) 0.0050(6) 0.0067(6) C24 0.0193(7) 0.0145(7) 0.0201(7) 0.0001(6) 0.0019(6) 0.0085(6) C25 0.0178(7) 0.0221(8) 0.0198(7) -0.0026(6) 0.0001(6) 0.0121(6) C26 0.0196(7) 0.0202(7) 0.0165(7) -0.0006(6) 0.0008(6) 0.0109(6) C27 0.0141(7) 0.0160(7) 0.0152(7) 0.0000(5) 0.0004(5) 0.0069(6) C29 0.0141(6) 0.0139(7) 0.0144(7) -0.0006(5) -0.0001(5) 0.0062(5) C30 0.0144(7) 0.0180(7) 0.0187(7) -0.0005(6) 0.0019(5) 0.0090(6) C31 0.0127(6) 0.0173(7) 0.0170(7) -0.0017(5) 0.0017(5) 0.0093(6) C32 0.0197(7) 0.0163(7) 0.0279(8) 0.0009(6) 0.0057(6) 0.0074(6) C33 0.0162(7) 0.0149(7) 0.0139(7) 0.0027(5) 0.0017(5) 0.0092(6) C34 0.0178(7) 0.0153(7) 0.0140(7) 0.0014(5) 0.0031(5) 0.0096(6) C35 0.0168(7) 0.0202(7) 0.0185(7) 0.0026(6) 0.0029(6) 0.0106(6) C38 0.0149(7) 0.0204(7) 0.0173(7) -0.0022(6) -0.0006(6) 0.0055(6) C75 0.0169(8) 0.0363(10) 0.0290(9) 0.0035(7) 0.0028(7) 0.0102(7) C100 0.023(3) 0.023(2) 0.022(4) 0.000(3) 0.002(3) 0.0086(19) Cl1 0.0285(15) 0.0264(16) 0.0198(17) 0.0018(12) 0.0024(12) 0.0137(12) B1 0.0161(7) 0.0161(7) 0.0110(7) 0.0004(6) 0.0011(6) 0.0090(6) _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 C100 2.083(10) . ? Fe1 Cl1 2.313(7) . ? Fe1 P3 2.3848(4) . ? Fe1 P5 2.3958(4) . ? Fe1 P4 2.4362(4) . ? Fe1 B1 2.5225(16) . ? P3 C30 1.8222(16) . ? P3 C35 1.8725(16) . ? P3 C8 1.8777(17) . ? P4 C34 1.8251(15) . ? P4 C38 1.8680(16) . ? P4 C24 1.8722(16) . ? P5 C27 1.8263(15) . ? P5 C17 1.8622(16) . ? P5 C23 1.8638(16) . ? C1 C23 1.537(2) . ? C2 C8 1.522(2) . ? C3 C24 1.536(2) . ? C4 C21 1.393(2) . ? C4 C27 1.397(2) . ? C5 C38 1.528(2) . ? C6 C38 1.536(2) . ? C7 C17 1.533(2) . ? C8 C19 1.528(2) . ? C9 C22 1.390(2) . ? C9 C26 1.393(2) . ? C10 C24 1.535(2) . ? C11 C14 1.387(3) . ? C11 C32 1.391(2) . ? C12 C21 1.389(2) . ? C12 C18 1.391(2) . ? C13 C22 1.394(2) . ? C13 C34 1.400(2) . ? C14 C25 1.392(2) . ? C15 C35 1.529(2) . ? C16 C35 1.532(2) . ? C17 C20 1.528(2) . ? C18 C29 1.408(2) . ? C23 C75 1.529(2) . ? C25 C31 1.406(2) . ? C26 C33 1.408(2) . ? C27 C29 1.417(2) . ? C29 B1 1.621(2) . ? C30 C32 1.402(2) . ? C30 C31 1.405(2) . ? C31 B1 1.618(2) . ? C33 C34 1.411(2) . ? C33 B1 1.614(2) . ? 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 C100 Fe1 Cl1 0.7(7) . . ? C100 Fe1 P3 109.8(4) . . ? Cl1 Fe1 P3 110.1(2) . . ? C100 Fe1 P5 108.5(4) . . ? Cl1 Fe1 P5 109.0(2) . . ? P3 Fe1 P5 104.979(15) . . ? C100 Fe1 P4 99.4(4) . . ? Cl1 Fe1 P4 98.7(2) . . ? P3 Fe1 P4 121.938(15) . . ? P5 Fe1 P4 111.666(15) . . ? C100 Fe1 B1 172.6(4) . . ? Cl1 Fe1 B1 171.9(2) . . ? P3 Fe1 B1 74.37(4) . . ? P5 Fe1 B1 75.54(4) . . ? P4 Fe1 B1 73.24(4) . . ? C30 P3 C35 105.78(7) . . ? C30 P3 C8 102.76(8) . . ? C35 P3 C8 108.36(7) . . ? C30 P3 Fe1 109.24(5) . . ? C35 P3 Fe1 110.41(5) . . ? C8 P3 Fe1 119.28(6) . . ? C34 P4 C38 107.75(7) . . ? C34 P4 C24 108.03(7) . . ? C38 P4 C24 104.75(7) . . ? C34 P4 Fe1 106.37(5) . . ? C38 P4 Fe1 110.40(5) . . ? C24 P4 Fe1 119.09(5) . . ? C27 P5 C17 105.26(7) . . ? C27 P5 C23 101.11(7) . . ? C17 P5 C23 104.58(7) . . ? C27 P5 Fe1 102.31(5) . . ? C17 P5 Fe1 116.52(5) . . ? C23 P5 Fe1 124.34(5) . . ? C21 C4 C27 120.33(15) . . ? C2 C8 C19 109.14(15) . . ? C2 C8 P3 111.64(12) . . ? C19 C8 P3 118.22(12) . . ? C22 C9 C26 120.20(14) . . ? C14 C11 C32 119.49(15) . . ? C21 C12 C18 120.03(15) . . ? C22 C13 C34 120.31(14) . . ? C11 C14 C25 120.13(15) . . ? C20 C17 C7 109.91(14) . . ? C20 C17 P5 109.57(11) . . ? C7 C17 P5 112.17(12) . . ? C12 C18 C29 122.38(14) . . ? C12 C21 C4 119.48(15) . . ? C9 C22 C13 119.33(14) . . ? C75 C23 C1 111.70(14) . . ? C75 C23 P5 113.89(12) . . ? C1 C23 P5 113.50(12) . . ? C10 C24 C3 112.67(13) . . ? C10 C24 P4 114.15(11) . . ? C3 C24 P4 111.66(11) . . ? C14 C25 C31 121.93(15) . . ? C9 C26 C33 121.96(14) . . ? C4 C27 C29 121.48(14) . . ? C4 C27 P5 124.94(12) . . ? C29 C27 P5 113.55(11) . . ? C18 C29 C27 116.27(13) . . ? C18 C29 B1 121.97(13) . . ? C27 C29 B1 121.76(13) . . ? C32 C30 C31 121.28(14) . . ? C32 C30 P3 125.43(12) . . ? C31 C30 P3 113.13(11) . . ? C30 C31 C25 116.90(14) . . ? C30 C31 B1 120.96(13) . . ? C25 C31 B1 122.14(13) . . ? C11 C32 C30 120.19(15) . . ? C26 C33 C34 116.76(13) . . ? C26 C33 B1 122.70(13) . . ? C34 C33 B1 120.46(13) . . ? C13 C34 C33 121.32(14) . . ? C13 C34 P4 125.91(12) . . ? C33 C34 P4 112.64(11) . . ? C15 C35 C16 112.10(13) . . ? C15 C35 P3 116.29(11) . . ? C16 C35 P3 110.87(11) . . ? C5 C38 C6 109.43(14) . . ? C5 C38 P4 109.89(11) . . ? C6 C38 P4 119.63(12) . . ? C33 B1 C31 114.11(12) . . ? C33 B1 C29 112.78(12) . . ? C31 B1 C29 113.74(12) . . ? C33 B1 Fe1 104.89(9) . . ? C31 B1 Fe1 108.33(9) . . ? C29 B1 Fe1 101.70(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.890 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.061 data_(TPB)FeBArF_(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H66 B2 F24 Fe N0 P3 Si0' _chemical_formula_weight 1509.59 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 26.4056(9) _cell_length_b 19.7833(7) _cell_length_c 26.4402(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13812.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9087 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 31.31 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6168 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8844 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details 'SADABS v2008/1 (Bruker-AXS, 2008)' _exptl_special_details ; 'Bruker KAPPA APEX II' ; _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 and \f scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 379408 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 33.73 _reflns_number_total 27590 _reflns_number_gt 20411 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7-0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT-Plus v7.66A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0584P)^2^+10.8070P] 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 27590 _refine_ls_number_parameters 951 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.002 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 0.841048(8) 0.775044(11) 0.491603(8) 0.01953(5) Uani 1 1 d . . . P2 P 0.801796(15) 0.88246(2) 0.493295(15) 0.02082(7) Uani 1 1 d . . . P3 P 0.838976(14) 0.67752(2) 0.437751(15) 0.01924(7) Uani 1 1 d . . . P1 P 0.881014(15) 0.75461(2) 0.571183(16) 0.02170(8) Uani 1 1 d . . . F12 F 1.11813(5) 0.88887(7) 0.13410(5) 0.0442(3) Uani 1 1 d . . . F9 F 0.89315(4) 0.85712(6) 0.24933(5) 0.0364(2) Uani 1 1 d . . . C14 C 0.77010(5) 0.67958(7) 0.43597(5) 0.0194(2) Uani 1 1 d . . . C63 C 1.06116(6) 0.74924(9) 0.40175(6) 0.0258(3) Uani 1 1 d . . . C36 C 0.83599(7) 0.55714(8) 0.49392(7) 0.0278(3) Uani 1 1 d . . . H36A H 0.7989 0.5597 0.4928 0.042 Uiso 1 1 calc R . . H36B H 0.8484 0.5823 0.5233 0.042 Uiso 1 1 calc R . . H36C H 0.8465 0.5098 0.4967 0.042 Uiso 1 1 calc R . . C8 C 0.75171(6) 0.86779(7) 0.53896(5) 0.0185(2) Uani 1 1 d . . . C55 C 1.19931(6) 0.61208(9) 0.24653(6) 0.0246(3) Uani 1 1 d . . . F11 F 1.07606(5) 0.82420(7) 0.08483(5) 0.0438(3) Uani 1 1 d . . . F15 F 1.25844(5) 0.54018(7) 0.20670(5) 0.0450(3) Uani 1 1 d . . . F21 F 1.07888(5) 0.81063(7) 0.47637(5) 0.0442(3) Uani 1 1 d . . . C58 C 1.15482(6) 0.73746(9) 0.25281(6) 0.0245(3) Uani 1 1 d . . . H58 H 1.1402 0.7813 0.2551 0.029 Uiso 1 1 calc R . . C24 C 0.83177(7) 0.83563(9) 0.64389(6) 0.0293(3) Uani 1 1 d . . . H24A H 0.8137 0.7960 0.6569 0.044 Uiso 1 1 calc R . . H24B H 0.8127 0.8551 0.6156 0.044 Uiso 1 1 calc R . . H24C H 0.8352 0.8693 0.6709 0.044 Uiso 1 1 calc R . . C66 C 1.05164(6) 0.62949(8) 0.34970(6) 0.0214(3) Uani 1 1 d . . . H66 H 1.0486 0.5875 0.3325 0.026 Uiso 1 1 calc R . . C49 C 1.04303(6) 0.84367(8) 0.16661(6) 0.0238(3) Uani 1 1 d . . . F24 F 0.99633(5) 0.55005(6) 0.43767(6) 0.0451(3) Uani 1 1 d . . . F14 F 1.24970(5) 0.52972(7) 0.28684(5) 0.0484(3) Uani 1 1 d . . . F13 F 1.19193(5) 0.49327(6) 0.23716(6) 0.0441(3) Uani 1 1 d . . . C13 C 0.74516(5) 0.70959(7) 0.47765(5) 0.0178(2) Uani 1 1 d . . . B2 B 1.06124(6) 0.68870(8) 0.25952(6) 0.0199(3) Uani 1 1 d . . . C1 C 0.79247(6) 0.68266(7) 0.56864(5) 0.0186(2) Uani 1 1 d . . . C37 C 1.02952(5) 0.62812(7) 0.23212(6) 0.0194(2) Uani 1 1 d . . . F10 F 1.04904(5) 0.92397(7) 0.10073(5) 0.0461(3) Uani 1 1 d . . . F23 F 1.06564(6) 0.51206(6) 0.40635(5) 0.0448(3) Uani 1 1 d . . . C61 C 1.05538(5) 0.68916(8) 0.32125(6) 0.0206(3) Uani 1 1 d . . . C9 C 0.72461(6) 0.92092(8) 0.56135(6) 0.0230(3) Uani 1 1 d . . . H9 H 0.7300 0.9661 0.5504 0.028 Uiso 1 1 calc R . . C42 C 1.04324(6) 0.60544(7) 0.18371(6) 0.0208(3) Uani 1 1 d . . . H42 H 1.0726 0.6237 0.1682 0.025 Uiso 1 1 calc R . . C56 C 1.23027(6) 0.66885(10) 0.24795(6) 0.0279(3) Uani 1 1 d . . . H56 H 1.2661 0.6647 0.2468 0.034 Uiso 1 1 calc R . . F8 F 0.92923(6) 0.95171(6) 0.23542(7) 0.0578(4) Uani 1 1 d . . . C53 C 1.12265(5) 0.68099(8) 0.25128(5) 0.0207(3) Uani 1 1 d . . . C7 C 0.74413(5) 0.80053(7) 0.55425(5) 0.0172(2) Uani 1 1 d . . . C50 C 1.06094(6) 0.78476(8) 0.18927(6) 0.0223(3) Uani 1 1 d . . . H50 H 1.0883 0.7613 0.1739 0.027 Uiso 1 1 calc R . . F22 F 1.06618(6) 0.56649(7) 0.47660(5) 0.0483(3) Uani 1 1 d . . . C12 C 0.70944(6) 0.78921(7) 0.59375(6) 0.0202(2) Uani 1 1 d . . . H12 H 0.7041 0.7444 0.6054 0.024 Uiso 1 1 calc R . . C19 C 0.94649(6) 0.72142(9) 0.56725(7) 0.0304(3) Uani 1 1 d . . . H19 H 0.9560 0.7037 0.6014 0.036 Uiso 1 1 calc R . . C5 C 0.77450(7) 0.58433(8) 0.62156(6) 0.0267(3) Uani 1 1 d . . . H5 H 0.7514 0.5505 0.6324 0.032 Uiso 1 1 calc R . . C45 C 1.03999(6) 0.75903(8) 0.23392(6) 0.0211(3) Uani 1 1 d . . . C18 C 0.69187(6) 0.71489(9) 0.47443(6) 0.0246(3) Uani 1 1 d . . . H18 H 0.6739 0.7357 0.5014 0.030 Uiso 1 1 calc R . . C57 C 1.20738(6) 0.73152(10) 0.25111(6) 0.0275(3) Uani 1 1 d . . . C64 C 1.05695(6) 0.68974(9) 0.42917(6) 0.0254(3) Uani 1 1 d . . . H64 H 1.0573 0.6900 0.4651 0.030 Uiso 1 1 calc R . . C34 C 0.85798(6) 0.58773(8) 0.44567(7) 0.0256(3) Uani 1 1 d . . . H34 H 0.8957 0.5864 0.4487 0.031 Uiso 1 1 calc R . . C65 C 1.05223(6) 0.62988(8) 0.40241(6) 0.0227(3) Uani 1 1 d . . . C6 C 0.75996(6) 0.63081(7) 0.58467(6) 0.0230(3) Uani 1 1 d . . . H6 H 0.7272 0.6273 0.5700 0.028 Uiso 1 1 calc R . . B1 B 0.77158(6) 0.73674(8) 0.52893(6) 0.0169(3) Uani 1 1 d . . . C30 C 0.83020(9) 1.01951(10) 0.51657(11) 0.0481(6) Uani 1 1 d . . . H30A H 0.8530 1.0477 0.5369 0.072 Uiso 1 1 calc R . . H30B H 0.7954 1.0251 0.5286 0.072 Uiso 1 1 calc R . . H30C H 0.8323 1.0332 0.4810 0.072 Uiso 1 1 calc R . . C52 C 1.07096(7) 0.87031(9) 0.12170(7) 0.0299(3) Uani 1 1 d . . . C35 C 0.84311(8) 0.54385(9) 0.40019(7) 0.0351(4) Uani 1 1 d . . . H35A H 0.8549 0.4974 0.4057 0.053 Uiso 1 1 calc R . . H35B H 0.8588 0.5621 0.3695 0.053 Uiso 1 1 calc R . . H35C H 0.8062 0.5440 0.3964 0.053 Uiso 1 1 calc R . . F18 F 1.23680(6) 0.82722(7) 0.20760(5) 0.0530(4) Uani 1 1 d . . . C62 C 1.06040(6) 0.74873(8) 0.34910(6) 0.0236(3) Uani 1 1 d . . . H62 H 1.0634 0.7904 0.3315 0.028 Uiso 1 1 calc R . . C4 C 0.82267(7) 0.58737(8) 0.64246(6) 0.0277(3) Uani 1 1 d . . . H4 H 0.8329 0.5550 0.6669 0.033 Uiso 1 1 calc R . . C3 C 0.85580(7) 0.63782(8) 0.62746(6) 0.0243(3) Uani 1 1 d . . . H3 H 0.8889 0.6398 0.6415 0.029 Uiso 1 1 calc R . . C31 C 0.86129(6) 0.69874(9) 0.37350(6) 0.0268(3) Uani 1 1 d . . . H31 H 0.8444 0.6681 0.3486 0.032 Uiso 1 1 calc R . . C10 C 0.68986(6) 0.90772(8) 0.59957(6) 0.0254(3) Uani 1 1 d . . . H10 H 0.6710 0.9436 0.6142 0.031 Uiso 1 1 calc R . . C47 C 0.98060(6) 0.85407(8) 0.23103(7) 0.0246(3) Uani 1 1 d . . . F7 F 0.94292(5) 0.89831(8) 0.30467(5) 0.0526(4) Uani 1 1 d . . . C54 C 1.14674(6) 0.61779(8) 0.24824(6) 0.0218(3) Uani 1 1 d . . . H54 H 1.1267 0.5779 0.2473 0.026 Uiso 1 1 calc R . . C11 C 0.68279(6) 0.84205(8) 0.61621(6) 0.0232(3) Uani 1 1 d . . . H11 H 0.6597 0.8330 0.6430 0.028 Uiso 1 1 calc R . . C15 C 0.74295(6) 0.65724(9) 0.39357(6) 0.0277(3) Uani 1 1 d . . . H15 H 0.7606 0.6384 0.3656 0.033 Uiso 1 1 calc R . . C38 C 0.98541(6) 0.59970(8) 0.25219(6) 0.0221(3) Uani 1 1 d . . . H38 H 0.9743 0.6139 0.2847 0.027 Uiso 1 1 calc R . . C68 C 1.04554(7) 0.56480(9) 0.43056(7) 0.0296(3) Uani 1 1 d . . . C22 C 0.88450(7) 0.81441(8) 0.62558(7) 0.0271(3) Uani 1 1 d . . . H22 H 0.9022 0.8561 0.6135 0.033 Uiso 1 1 calc R . . C33 C 0.84741(9) 0.77152(11) 0.36100(8) 0.0422(5) Uani 1 1 d . . . H33A H 0.8643 0.8020 0.3848 0.063 Uiso 1 1 calc R . . H33B H 0.8106 0.7773 0.3637 0.063 Uiso 1 1 calc R . . H33C H 0.8583 0.7821 0.3265 0.063 Uiso 1 1 calc R . . C48 C 1.00279(6) 0.87914(8) 0.18725(7) 0.0262(3) Uani 1 1 d . . . H48 H 0.9907 0.9195 0.1719 0.031 Uiso 1 1 calc R . . F20 F 1.02111(9) 0.84803(9) 0.42924(8) 0.0926(8) Uani 1 1 d . . . C17 C 0.66487(6) 0.69045(10) 0.43293(7) 0.0308(4) Uani 1 1 d . . . H17 H 0.6289 0.6930 0.4325 0.037 Uiso 1 1 calc R . . F17 F 1.28742(5) 0.78361(9) 0.26030(7) 0.0689(5) Uani 1 1 d . . . C21 C 0.95119(7) 0.66378(11) 0.52948(8) 0.0371(4) Uani 1 1 d . . . H21A H 0.9442 0.6807 0.4953 0.056 Uiso 1 1 calc R . . H21B H 0.9268 0.6282 0.5380 0.056 Uiso 1 1 calc R . . H21C H 0.9856 0.6452 0.5308 0.056 Uiso 1 1 calc R . . C40 C 0.97163(6) 0.52931(8) 0.17886(7) 0.0266(3) Uani 1 1 d . . . H40 H 0.9525 0.4962 0.1612 0.032 Uiso 1 1 calc R . . F19 F 1.09890(12) 0.85600(10) 0.40672(7) 0.1191(11) Uani 1 1 d . . . C25 C 0.76976(7) 0.92359(9) 0.43936(6) 0.0302(3) Uani 1 1 d . . . H25 H 0.7530 0.9654 0.4525 0.036 Uiso 1 1 calc R . . C16 C 0.69059(7) 0.66241(11) 0.39222(7) 0.0355(4) Uani 1 1 d . . . H16 H 0.6724 0.6468 0.3635 0.043 Uiso 1 1 calc R . . C27 C 0.72844(8) 0.87752(11) 0.41902(7) 0.0365(4) Uani 1 1 d . . . H27A H 0.7117 0.8994 0.3902 0.055 Uiso 1 1 calc R . . H27B H 0.7035 0.8688 0.4457 0.055 Uiso 1 1 calc R . . H27C H 0.7434 0.8347 0.4080 0.055 Uiso 1 1 calc R . . C2 C 0.84064(6) 0.68581(7) 0.59171(5) 0.0197(2) Uani 1 1 d . . . C23 C 0.91484(9) 0.78638(10) 0.67052(8) 0.0405(5) Uani 1 1 d . . . H23A H 0.9147 0.8194 0.6981 0.061 Uiso 1 1 calc R . . H23B H 0.9498 0.7777 0.6599 0.061 Uiso 1 1 calc R . . H23C H 0.8993 0.7442 0.6822 0.061 Uiso 1 1 calc R . . F16 F 1.22280(7) 0.83906(10) 0.28597(7) 0.0762(6) Uani 1 1 d . . . C60 C 1.23859(7) 0.79480(11) 0.25159(7) 0.0367(4) Uani 1 1 d . . . C51 C 0.93678(7) 0.89018(9) 0.25473(7) 0.0305(3) Uani 1 1 d . . . C29 C 0.89912(8) 0.93441(11) 0.50087(11) 0.0464(6) Uani 1 1 d . . . H29A H 0.8992 0.9422 0.4643 0.070 Uiso 1 1 calc R . . H29B H 0.9099 0.8879 0.5078 0.070 Uiso 1 1 calc R . . H29C H 0.9225 0.9660 0.5172 0.070 Uiso 1 1 calc R . . C67 C 1.06551(10) 0.81567(10) 0.42820(8) 0.0412(5) Uani 1 1 d . . . C59 C 1.22427(7) 0.54429(10) 0.24426(6) 0.0302(3) Uani 1 1 d . . . C46 C 0.99879(6) 0.79520(8) 0.25350(6) 0.0228(3) Uani 1 1 d . . . H46 H 0.9827 0.7790 0.2832 0.027 Uiso 1 1 calc R . . C28 C 0.84576(7) 0.94540(9) 0.52158(8) 0.0320(4) Uani 1 1 d . . . H28 H 0.8473 0.9354 0.5586 0.038 Uiso 1 1 calc R . . C26 C 0.80654(10) 0.94528(11) 0.39726(8) 0.0445(5) Uani 1 1 d . . . H26A H 0.8245 0.9055 0.3844 0.067 Uiso 1 1 calc R . . H26B H 0.8311 0.9777 0.4109 0.067 Uiso 1 1 calc R . . H26C H 0.7875 0.9665 0.3697 0.067 Uiso 1 1 calc R . . C20 C 0.98246(8) 0.77947(12) 0.55427(12) 0.0518(6) Uani 1 1 d . . . H20A H 1.0170 0.7620 0.5511 0.078 Uiso 1 1 calc R . . H20B H 0.9813 0.8135 0.5812 0.078 Uiso 1 1 calc R . . H20C H 0.9721 0.8001 0.5222 0.078 Uiso 1 1 calc R . . C32 C 0.91875(7) 0.68885(10) 0.36993(8) 0.0359(4) Uani 1 1 d . . . H32A H 0.9301 0.6994 0.3355 0.054 Uiso 1 1 calc R . . H32B H 0.9272 0.6418 0.3779 0.054 Uiso 1 1 calc R . . H32C H 0.9357 0.7190 0.3940 0.054 Uiso 1 1 calc R . . C39 C 0.95712(6) 0.55127(9) 0.22632(7) 0.0270(3) Uani 1 1 d D A . C43 C 0.91006(7) 0.52443(11) 0.25090(8) 0.0388(4) Uani 1 1 d D . . F1A F 0.8983(5) 0.4619(4) 0.2323(2) 0.076(3) Uani 0.55(2) 1 d PD A 1 F2A F 0.8726(3) 0.5638(6) 0.2518(5) 0.081(3) Uani 0.55(2) 1 d PD A 1 F3A F 0.9197(2) 0.5058(3) 0.29959(15) 0.0365(10) Uani 0.55(2) 1 d PD A 1 F1B F 0.8793(3) 0.4927(8) 0.2177(5) 0.083(4) Uani 0.45(2) 1 d PD A 2 F2B F 0.8783(2) 0.5781(4) 0.2627(3) 0.0370(12) Uani 0.45(2) 1 d PD A 2 F3B F 0.9158(4) 0.4937(7) 0.2917(5) 0.087(3) Uani 0.45(2) 1 d PD A 2 C41 C 1.01523(6) 0.55720(8) 0.15778(6) 0.0230(3) Uani 1 1 d D B . C44 C 1.03279(8) 0.53326(9) 0.10716(7) 0.0312(3) Uani 1 1 d D . . F4A F 1.0442(2) 0.46904(13) 0.10581(11) 0.0722(18) Uani 0.607(8) 1 d PD B 1 F5A F 1.06856(17) 0.5674(2) 0.08649(13) 0.0719(19) Uani 0.607(8) 1 d PD B 1 F6A F 0.99435(13) 0.5367(3) 0.07277(10) 0.0791(17) Uani 0.607(8) 1 d PD B 1 F4B F 1.0104(3) 0.4840(3) 0.0897(2) 0.079(3) Uani 0.393(8) 1 d PD B 2 F5B F 1.08244(16) 0.5140(4) 0.11216(17) 0.081(3) Uani 0.393(8) 1 d PD B 2 F6B F 1.0355(4) 0.5795(3) 0.07416(19) 0.092(4) Uani 0.393(8) 1 d PD B 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 0.02148(10) 0.01892(9) 0.01818(9) -0.00113(7) 0.00173(7) 0.00161(7) P2 0.02211(17) 0.02003(16) 0.02032(16) 0.00340(13) 0.00268(13) 0.00253(13) P3 0.01759(15) 0.02037(16) 0.01976(16) -0.00326(12) 0.00334(12) 0.00114(12) P1 0.02090(17) 0.02012(16) 0.02407(18) 0.00300(13) -0.00331(14) -0.00106(13) F12 0.0312(6) 0.0507(7) 0.0508(7) 0.0177(6) -0.0005(5) -0.0171(5) F9 0.0236(5) 0.0420(6) 0.0436(6) -0.0083(5) 0.0055(4) -0.0037(4) C14 0.0188(6) 0.0221(6) 0.0172(6) -0.0034(5) 0.0017(5) 0.0014(5) C63 0.0261(7) 0.0274(7) 0.0239(7) -0.0045(6) -0.0032(6) -0.0021(6) C36 0.0325(8) 0.0194(6) 0.0315(8) -0.0005(6) 0.0063(6) 0.0022(6) C8 0.0206(6) 0.0180(5) 0.0169(6) -0.0002(4) 0.0001(5) 0.0016(5) C55 0.0197(6) 0.0379(8) 0.0163(6) 0.0048(6) -0.0008(5) 0.0019(6) F11 0.0575(8) 0.0399(6) 0.0341(6) 0.0026(5) 0.0130(6) -0.0084(6) F15 0.0387(6) 0.0571(8) 0.0392(6) 0.0141(6) 0.0187(5) 0.0174(6) F21 0.0502(7) 0.0505(7) 0.0318(6) -0.0164(5) -0.0113(5) -0.0011(6) C58 0.0225(7) 0.0308(7) 0.0203(6) 0.0026(5) -0.0025(5) -0.0065(6) C24 0.0373(9) 0.0288(8) 0.0218(7) -0.0044(6) -0.0054(6) -0.0030(7) C66 0.0194(6) 0.0237(6) 0.0212(6) -0.0006(5) 0.0001(5) -0.0006(5) C49 0.0219(7) 0.0226(6) 0.0268(7) 0.0041(5) -0.0028(5) -0.0049(5) F24 0.0376(6) 0.0377(6) 0.0599(8) 0.0139(6) 0.0104(6) -0.0057(5) F14 0.0557(8) 0.0571(8) 0.0324(6) 0.0135(6) -0.0116(6) 0.0178(6) F13 0.0317(6) 0.0383(6) 0.0621(8) -0.0007(6) 0.0043(6) 0.0062(5) C13 0.0183(6) 0.0183(5) 0.0168(5) -0.0024(4) 0.0016(5) 0.0010(5) B2 0.0181(7) 0.0220(7) 0.0197(7) 0.0010(5) -0.0013(5) -0.0019(5) C1 0.0222(6) 0.0171(5) 0.0167(6) -0.0025(4) 0.0018(5) -0.0003(5) C37 0.0180(6) 0.0196(6) 0.0206(6) 0.0012(5) -0.0012(5) 0.0002(5) F10 0.0490(7) 0.0420(7) 0.0472(7) 0.0245(6) 0.0058(6) 0.0080(6) F23 0.0662(8) 0.0293(5) 0.0391(6) 0.0077(5) 0.0146(6) 0.0142(5) C61 0.0166(6) 0.0236(6) 0.0217(6) -0.0001(5) -0.0009(5) -0.0014(5) C9 0.0251(7) 0.0194(6) 0.0247(7) -0.0013(5) 0.0012(5) 0.0046(5) C42 0.0194(6) 0.0215(6) 0.0213(6) 0.0003(5) -0.0010(5) -0.0003(5) C56 0.0184(6) 0.0465(10) 0.0189(6) 0.0066(6) -0.0014(5) -0.0039(6) F8 0.0507(8) 0.0291(6) 0.0936(12) 0.0151(7) 0.0266(8) 0.0143(5) C53 0.0186(6) 0.0269(7) 0.0168(6) 0.0018(5) -0.0020(5) -0.0037(5) C7 0.0173(6) 0.0183(6) 0.0161(5) -0.0025(4) 0.0000(4) 0.0006(4) C50 0.0207(6) 0.0217(6) 0.0245(7) 0.0016(5) -0.0015(5) -0.0028(5) F22 0.0689(9) 0.0472(7) 0.0287(6) 0.0125(5) -0.0112(6) -0.0005(6) C12 0.0211(6) 0.0197(6) 0.0197(6) -0.0021(5) 0.0037(5) -0.0013(5) C19 0.0206(7) 0.0323(8) 0.0381(9) 0.0055(7) -0.0034(6) 0.0004(6) C5 0.0377(9) 0.0183(6) 0.0242(7) 0.0009(5) 0.0058(6) -0.0039(6) C45 0.0194(6) 0.0214(6) 0.0223(6) -0.0004(5) -0.0032(5) -0.0040(5) C18 0.0190(6) 0.0317(8) 0.0233(7) -0.0077(6) 0.0009(5) 0.0012(6) C57 0.0223(7) 0.0411(9) 0.0190(6) 0.0057(6) -0.0044(5) -0.0106(6) C64 0.0232(7) 0.0330(8) 0.0200(6) -0.0021(6) -0.0001(5) 0.0009(6) C34 0.0248(7) 0.0209(6) 0.0310(8) -0.0031(6) 0.0066(6) 0.0039(5) C65 0.0200(6) 0.0267(7) 0.0215(6) 0.0023(5) 0.0006(5) 0.0011(5) C6 0.0275(7) 0.0185(6) 0.0229(7) -0.0021(5) 0.0031(5) -0.0021(5) B1 0.0171(6) 0.0171(6) 0.0165(6) -0.0016(5) 0.0027(5) -0.0008(5) C30 0.0436(11) 0.0244(8) 0.0762(17) -0.0068(9) 0.0081(11) -0.0063(8) C52 0.0288(8) 0.0279(8) 0.0331(8) 0.0090(6) -0.0012(6) -0.0037(6) C35 0.0476(11) 0.0243(7) 0.0335(9) -0.0094(6) 0.0113(8) 0.0009(7) F18 0.0575(8) 0.0526(8) 0.0488(8) 0.0212(6) -0.0113(6) -0.0244(7) C62 0.0236(7) 0.0246(7) 0.0225(7) -0.0012(5) -0.0030(5) -0.0029(5) C4 0.0421(9) 0.0193(6) 0.0217(7) 0.0029(5) 0.0000(6) 0.0009(6) C3 0.0310(7) 0.0206(6) 0.0213(6) 0.0013(5) -0.0034(6) 0.0022(5) C31 0.0254(7) 0.0327(8) 0.0223(7) -0.0003(6) 0.0069(6) 0.0027(6) C10 0.0267(7) 0.0231(7) 0.0265(7) -0.0057(5) 0.0045(6) 0.0051(6) C47 0.0204(6) 0.0212(6) 0.0321(8) -0.0026(6) -0.0036(6) -0.0026(5) F7 0.0473(7) 0.0663(9) 0.0441(7) -0.0280(7) -0.0076(6) 0.0161(7) C54 0.0184(6) 0.0304(7) 0.0167(6) 0.0036(5) -0.0008(5) -0.0008(5) C11 0.0221(7) 0.0256(7) 0.0218(6) -0.0040(5) 0.0049(5) 0.0018(5) C15 0.0237(7) 0.0373(8) 0.0221(7) -0.0119(6) 0.0019(5) 0.0009(6) C38 0.0185(6) 0.0244(6) 0.0234(6) -0.0011(5) 0.0007(5) -0.0014(5) C68 0.0324(8) 0.0307(8) 0.0256(7) 0.0041(6) 0.0029(6) 0.0035(6) C22 0.0306(8) 0.0221(7) 0.0287(8) 0.0014(6) -0.0105(6) -0.0042(6) C33 0.0483(12) 0.0415(11) 0.0369(10) 0.0148(8) 0.0153(9) 0.0114(9) C48 0.0242(7) 0.0208(6) 0.0336(8) 0.0028(6) -0.0045(6) -0.0031(5) F20 0.1267(17) 0.0565(10) 0.0946(13) -0.0456(10) -0.0682(13) 0.0545(11) C17 0.0190(7) 0.0456(10) 0.0279(8) -0.0114(7) -0.0026(6) 0.0031(6) F17 0.0309(6) 0.0735(10) 0.1024(13) 0.0371(10) -0.0260(8) -0.0275(7) C21 0.0263(8) 0.0491(11) 0.0360(9) -0.0009(8) -0.0014(7) 0.0087(8) C40 0.0252(7) 0.0252(7) 0.0293(8) -0.0034(6) -0.0038(6) -0.0047(6) F19 0.226(3) 0.0763(12) 0.0548(10) -0.0341(9) 0.0475(14) -0.1021(17) C25 0.0369(9) 0.0304(8) 0.0233(7) 0.0088(6) 0.0037(6) 0.0121(7) C16 0.0256(8) 0.0548(12) 0.0261(8) -0.0157(8) -0.0030(6) 0.0003(8) C27 0.0386(10) 0.0478(11) 0.0231(8) 0.0014(7) -0.0060(7) 0.0140(8) C2 0.0239(6) 0.0171(5) 0.0181(6) 0.0003(5) -0.0009(5) 0.0010(5) C23 0.0517(12) 0.0327(9) 0.0371(10) -0.0050(7) -0.0259(9) 0.0032(8) F16 0.0769(11) 0.0802(12) 0.0714(11) -0.0374(9) 0.0225(9) -0.0532(10) C60 0.0293(8) 0.0503(11) 0.0306(8) 0.0055(8) -0.0051(7) -0.0161(8) C51 0.0281(8) 0.0246(7) 0.0387(9) -0.0036(6) -0.0009(7) -0.0001(6) C29 0.0276(9) 0.0352(10) 0.0764(16) 0.0204(10) 0.0070(10) -0.0044(7) C67 0.0627(14) 0.0317(9) 0.0293(9) -0.0070(7) -0.0078(9) -0.0049(9) C59 0.0238(7) 0.0449(10) 0.0219(7) 0.0082(7) 0.0016(6) 0.0070(7) C46 0.0202(6) 0.0224(6) 0.0259(7) -0.0012(5) -0.0022(5) -0.0039(5) C28 0.0295(8) 0.0279(8) 0.0385(9) 0.0035(7) 0.0020(7) -0.0066(6) C26 0.0605(13) 0.0411(10) 0.0318(9) 0.0184(8) 0.0151(9) 0.0146(10) C20 0.0227(8) 0.0453(12) 0.0873(19) 0.0149(12) 0.0035(10) -0.0027(8) C32 0.0287(8) 0.0398(10) 0.0392(10) 0.0029(8) 0.0140(7) 0.0025(7) C39 0.0220(7) 0.0293(7) 0.0296(8) -0.0011(6) 0.0001(6) -0.0067(6) C43 0.0294(9) 0.0453(11) 0.0418(10) -0.0046(9) 0.0049(8) -0.0167(8) F1A 0.085(5) 0.081(4) 0.062(2) -0.024(2) 0.028(3) -0.067(4) F2A 0.0165(14) 0.110(5) 0.118(6) 0.075(4) 0.001(3) 0.002(3) F3A 0.0357(18) 0.0426(18) 0.0313(18) 0.0085(15) 0.0133(11) -0.0047(13) F1B 0.040(3) 0.117(7) 0.092(5) -0.066(5) 0.024(3) -0.049(3) F2B 0.019(2) 0.049(2) 0.044(2) 0.0041(19) 0.0097(15) 0.0007(15) F3B 0.039(3) 0.073(5) 0.149(7) 0.078(5) 0.021(4) 0.011(3) C41 0.0248(7) 0.0219(6) 0.0222(6) -0.0015(5) -0.0018(5) 0.0016(5) C44 0.0394(9) 0.0284(8) 0.0257(8) -0.0032(6) -0.0007(7) 0.0004(7) F4A 0.153(5) 0.0292(12) 0.0345(14) 0.0002(9) 0.030(2) 0.022(2) F5A 0.097(3) 0.074(3) 0.045(2) -0.033(2) 0.042(2) -0.055(3) F6A 0.071(2) 0.137(5) 0.0295(12) -0.0175(18) -0.0175(12) 0.021(2) F4B 0.087(5) 0.080(5) 0.071(4) -0.061(4) 0.037(4) -0.055(4) F5B 0.045(2) 0.155(8) 0.044(2) -0.047(3) -0.0013(18) 0.040(3) F6B 0.199(11) 0.045(3) 0.032(2) 0.0097(19) 0.044(4) 0.037(5) _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 B1 2.2167(15) . ? Fe1 P2 2.3648(4) . ? Fe1 P1 2.3884(5) . ? Fe1 P3 2.3986(4) . ? P2 C8 1.8141(15) . ? P2 C25 1.8469(17) . ? P2 C28 1.8594(19) . ? P3 C14 1.8199(15) . ? P3 C31 1.8465(16) . ? P3 C34 1.8576(16) . ? P1 C2 1.8121(15) . ? P1 C19 1.8523(18) . ? P1 C22 1.8647(17) . ? F12 C52 1.339(2) . ? F9 C51 1.332(2) . ? C14 C15 1.402(2) . ? C14 C13 1.4145(19) . ? C63 C64 1.387(2) . ? C63 C62 1.392(2) . ? C63 C67 1.493(3) . ? C36 C34 1.527(2) . ? C8 C9 1.403(2) . ? C8 C7 1.405(2) . ? C55 C56 1.390(2) . ? C55 C54 1.393(2) . ? C55 C59 1.496(3) . ? F11 C52 1.342(2) . ? F15 C59 1.344(2) . ? F21 C67 1.325(2) . ? C58 C57 1.394(2) . ? C58 C53 1.404(2) . ? C24 C22 1.533(3) . ? C66 C65 1.394(2) . ? C66 C61 1.403(2) . ? C49 C48 1.385(2) . ? C49 C50 1.393(2) . ? C49 C52 1.494(2) . ? F24 C68 1.345(2) . ? F14 C59 1.342(2) . ? F13 C59 1.335(2) . ? C13 C18 1.414(2) . ? C13 B1 1.617(2) . ? B2 C37 1.632(2) . ? B2 C61 1.640(2) . ? B2 C53 1.643(2) . ? B2 C45 1.646(2) . ? C1 C6 1.403(2) . ? C1 C2 1.412(2) . ? C1 B1 1.597(2) . ? C37 C38 1.398(2) . ? C37 C42 1.404(2) . ? F10 C52 1.330(2) . ? F23 C68 1.334(2) . ? C61 C62 1.396(2) . ? C9 C10 1.390(2) . ? C42 C41 1.389(2) . ? C56 C57 1.382(3) . ? F8 C51 1.335(2) . ? C53 C54 1.405(2) . ? C7 C12 1.407(2) . ? C7 B1 1.602(2) . ? C50 C45 1.400(2) . ? F22 C68 1.334(2) . ? C12 C11 1.393(2) . ? C19 C21 1.521(3) . ? C19 C20 1.529(3) . ? C5 C4 1.388(3) . ? C5 C6 1.394(2) . ? C45 C46 1.401(2) . ? C18 C17 1.395(2) . ? C57 C60 1.499(3) . ? C64 C65 1.385(2) . ? C34 C35 1.534(2) . ? C65 C68 1.498(2) . ? C30 C28 1.528(3) . ? F18 C60 1.329(2) . ? C4 C3 1.385(2) . ? C3 C2 1.398(2) . ? C31 C33 1.522(3) . ? C31 C32 1.533(2) . ? C10 C11 1.384(2) . ? C47 C48 1.389(2) . ? C47 C46 1.393(2) . ? C47 C51 1.497(2) . ? F7 C51 1.340(2) . ? C15 C16 1.387(2) . ? C38 C39 1.394(2) . ? C22 C23 1.537(2) . ? F20 C67 1.336(3) . ? C17 C16 1.388(2) . ? F17 C60 1.328(2) . ? C40 C39 1.382(2) . ? C40 C41 1.393(2) . ? F19 C67 1.318(3) . ? C25 C27 1.520(3) . ? C25 C26 1.538(3) . ? F16 C60 1.329(3) . ? C29 C28 1.527(3) . ? C39 C43 1.500(2) . ? C43 F3B 1.248(8) . ? C43 F2A 1.259(7) . ? C43 F1B 1.351(6) . ? C43 F3A 1.363(5) . ? C43 F1A 1.367(5) . ? C43 F2B 1.389(6) . ? C41 C44 1.494(2) . ? C44 F4B 1.231(4) . ? C44 F6B 1.266(5) . ? C44 F5A 1.284(3) . ? C44 F4A 1.306(3) . ? C44 F6A 1.364(3) . ? C44 F5B 1.371(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 B1 Fe1 P2 86.33(4) . . ? B1 Fe1 P1 85.16(4) . . ? P2 Fe1 P1 109.214(16) . . ? B1 Fe1 P3 88.31(4) . . ? P2 Fe1 P3 136.394(17) . . ? P1 Fe1 P3 113.385(16) . . ? C8 P2 C25 104.51(8) . . ? C8 P2 C28 107.13(8) . . ? C25 P2 C28 107.54(9) . . ? C8 P2 Fe1 100.86(5) . . ? C25 P2 Fe1 125.59(6) . . ? C28 P2 Fe1 109.62(6) . . ? C14 P3 C31 106.86(7) . . ? C14 P3 C34 107.12(7) . . ? C31 P3 C34 103.59(8) . . ? C14 P3 Fe1 91.15(5) . . ? C31 P3 Fe1 110.85(6) . . ? C34 P3 Fe1 134.11(6) . . ? C2 P1 C19 107.43(8) . . ? C2 P1 C22 105.94(7) . . ? C19 P1 C22 102.83(8) . . ? C2 P1 Fe1 97.53(5) . . ? C19 P1 Fe1 115.02(6) . . ? C22 P1 Fe1 126.44(5) . . ? C15 C14 C13 121.15(13) . . ? C15 C14 P3 121.63(11) . . ? C13 C14 P3 117.04(11) . . ? C64 C63 C62 121.02(15) . . ? C64 C63 C67 120.54(16) . . ? C62 C63 C67 118.42(16) . . ? C9 C8 C7 121.02(13) . . ? C9 C8 P2 122.21(11) . . ? C7 C8 P2 116.55(10) . . ? C56 C55 C54 121.31(16) . . ? C56 C55 C59 117.82(15) . . ? C54 C55 C59 120.86(16) . . ? C57 C58 C53 122.31(16) . . ? C65 C66 C61 122.04(14) . . ? C48 C49 C50 120.99(15) . . ? C48 C49 C52 120.86(15) . . ? C50 C49 C52 117.99(15) . . ? C18 C13 C14 116.59(13) . . ? C18 C13 B1 117.09(12) . . ? C14 C13 B1 126.30(13) . . ? C37 B2 C61 113.43(12) . . ? C37 B2 C53 112.29(12) . . ? C61 B2 C53 103.04(11) . . ? C37 B2 C45 105.28(12) . . ? C61 B2 C45 111.87(12) . . ? C53 B2 C45 111.12(12) . . ? C6 C1 C2 116.93(13) . . ? C6 C1 B1 118.49(13) . . ? C2 C1 B1 124.43(13) . . ? C38 C37 C42 115.63(13) . . ? C38 C37 B2 123.67(13) . . ? C42 C37 B2 120.47(13) . . ? C62 C61 C66 115.74(14) . . ? C62 C61 B2 121.38(13) . . ? C66 C61 B2 122.39(13) . . ? C10 C9 C8 120.21(14) . . ? C41 C42 C37 122.16(14) . . ? C57 C56 C55 118.00(15) . . ? C58 C53 C54 115.84(14) . . ? C58 C53 B2 121.28(14) . . ? C54 C53 B2 122.48(13) . . ? C8 C7 C12 117.21(12) . . ? C8 C7 B1 124.14(12) . . ? C12 C7 B1 118.64(12) . . ? C49 C50 C45 122.19(15) . . ? C11 C12 C7 121.72(14) . . ? C21 C19 C20 111.41(19) . . ? C21 C19 P1 112.26(12) . . ? C20 C19 P1 109.03(13) . . ? C4 C5 C6 120.14(15) . . ? C50 C45 C46 115.64(14) . . ? C50 C45 B2 121.30(14) . . ? C46 C45 B2 122.99(14) . . ? C17 C18 C13 122.03(14) . . ? C56 C57 C58 120.88(15) . . ? C56 C57 C60 120.62(16) . . ? C58 C57 C60 118.48(17) . . ? C65 C64 C63 117.76(15) . . ? C36 C34 C35 109.47(14) . . ? C36 C34 P3 111.75(11) . . ? C35 C34 P3 112.55(13) . . ? C64 C65 C66 121.10(15) . . ? C64 C65 C68 119.45(15) . . ? C66 C65 C68 119.40(15) . . ? C5 C6 C1 121.67(15) . . ? C1 B1 C7 114.15(12) . . ? C1 B1 C13 118.54(12) . . ? C7 B1 C13 114.65(12) . . ? C1 B1 Fe1 103.64(9) . . ? C7 B1 Fe1 106.93(9) . . ? C13 B1 Fe1 95.58(9) . . ? F10 C52 F12 106.73(14) . . ? F10 C52 F11 106.48(15) . . ? F12 C52 F11 105.71(16) . . ? F10 C52 C49 113.46(16) . . ? F12 C52 C49 111.17(15) . . ? F11 C52 C49 112.78(14) . . ? C63 C62 C61 122.34(15) . . ? C3 C4 C5 119.73(15) . . ? C4 C3 C2 120.14(15) . . ? C33 C31 C32 110.23(16) . . ? C33 C31 P3 109.76(12) . . ? C32 C31 P3 110.10(13) . . ? C11 C10 C9 119.77(14) . . ? C48 C47 C46 120.57(15) . . ? C48 C47 C51 120.29(15) . . ? C46 C47 C51 119.14(16) . . ? C55 C54 C53 121.67(15) . . ? C10 C11 C12 120.04(14) . . ? C16 C15 C14 120.46(14) . . ? C39 C38 C37 122.45(15) . . ? F22 C68 F23 107.16(15) . . ? F22 C68 F24 105.81(15) . . ? F23 C68 F24 106.35(16) . . ? F22 C68 C65 112.57(16) . . ? F23 C68 C65 112.77(14) . . ? F24 C68 C65 111.71(14) . . ? C24 C22 C23 109.17(16) . . ? C24 C22 P1 111.87(11) . . ? C23 C22 P1 113.15(12) . . ? C49 C48 C47 118.09(15) . . ? C16 C17 C18 119.88(15) . . ? C39 C40 C41 117.89(15) . . ? C27 C25 C26 111.38(17) . . ? C27 C25 P2 109.74(12) . . ? C26 C25 P2 113.11(14) . . ? C15 C16 C17 119.82(16) . . ? C3 C2 C1 121.32(14) . . ? C3 C2 P1 122.97(12) . . ? C1 C2 P1 115.70(11) . . ? F17 C60 F18 105.46(17) . . ? F17 C60 F16 107.20(18) . . ? F18 C60 F16 105.6(2) . . ? F17 C60 C57 113.32(19) . . ? F18 C60 C57 112.10(15) . . ? F16 C60 C57 112.54(16) . . ? F9 C51 F8 106.12(16) . . ? F9 C51 F7 105.61(16) . . ? F8 C51 F7 106.58(16) . . ? F9 C51 C47 112.91(14) . . ? F8 C51 C47 112.98(16) . . ? F7 C51 C47 112.08(15) . . ? F19 C67 F21 106.4(2) . . ? F19 C67 F20 107.8(2) . . ? F21 C67 F20 104.49(19) . . ? F19 C67 C63 112.48(19) . . ? F21 C67 C63 113.86(17) . . ? F20 C67 C63 111.33(18) . . ? F13 C59 F14 105.99(15) . . ? F13 C59 F15 106.25(16) . . ? F14 C59 F15 105.71(14) . . ? F13 C59 C55 113.68(14) . . ? F14 C59 C55 112.29(16) . . ? F15 C59 C55 112.31(15) . . ? C47 C46 C45 122.49(15) . . ? C29 C28 C30 110.71(16) . . ? C29 C28 P2 109.67(15) . . ? C30 C28 P2 116.08(15) . . ? C40 C39 C38 120.86(15) . . ? C40 C39 C43 120.78(15) . . ? C38 C39 C43 118.35(16) . . ? F3B C43 F2A 112.4(6) . . ? F3B C43 F1B 114.2(6) . . ? F2A C43 F1B 80.0(4) . . ? F3B C43 F3A 13.8(9) . . ? F2A C43 F3A 107.2(6) . . ? F1B C43 F3A 126.9(8) . . ? F3B C43 F1A 84.2(6) . . ? F2A C43 F1A 112.8(4) . . ? F1B C43 F1A 37.7(4) . . ? F3A C43 F1A 97.9(5) . . ? F3B C43 F2B 104.7(6) . . ? F2A C43 F2B 17.9(7) . . ? F1B C43 F2B 97.9(6) . . ? F3A C43 F2B 96.2(4) . . ? F1A C43 F2B 129.4(6) . . ? F3B C43 C39 116.5(5) . . ? F2A C43 C39 116.2(4) . . ? F1B C43 C39 112.4(4) . . ? F3A C43 C39 110.5(3) . . ? F1A C43 C39 110.6(4) . . ? F2B C43 C39 109.1(4) . . ? C42 C41 C40 121.00(15) . . ? C42 C41 C44 119.67(15) . . ? C40 C41 C44 119.31(15) . . ? F4B C44 F6B 109.9(6) . . ? F4B C44 F5A 127.6(3) . . ? F6B C44 F5A 44.3(4) . . ? F4B C44 F4A 48.0(4) . . ? F6B C44 F4A 132.1(3) . . ? F5A C44 F4A 109.3(3) . . ? F4B C44 F6A 55.4(4) . . ? F6B C44 F6A 63.0(5) . . ? F5A C44 F6A 103.7(3) . . ? F4A C44 F6A 101.7(3) . . ? F4B C44 F5B 106.0(5) . . ? F6B C44 F5B 102.3(5) . . ? F5A C44 F5B 58.9(4) . . ? F4A C44 F5B 60.8(4) . . ? F6A C44 F5B 142.1(2) . . ? F4B C44 C41 116.0(3) . . ? F6B C44 C41 114.0(3) . . ? F5A C44 C41 116.31(19) . . ? F4A C44 C41 113.86(18) . . ? F6A C44 C41 110.5(2) . . ? F5B C44 C41 107.3(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 33.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.740 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.074 data_(TPB)Fe(N2H4)BArF_(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H68 B2 F24 Fe N2 P3' _chemical_formula_weight 1659.72 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.0031(7) _cell_length_b 25.7862(8) _cell_length_c 26.6970(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13770.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6776 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8361 _exptl_absorpt_correction_T_max 0.9419 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 347031 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 32.59 _reflns_number_total 25087 _reflns_number_gt 17680 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0870P)^2^+21.7122P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25087 _refine_ls_number_parameters 981 _refine_ls_number_restraints 971 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1681 _refine_ls_wR_factor_gt 0.1373 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.922 _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 Fe1 Fe 0.719608(13) 0.013844(10) 0.149305(10) 0.01649(6) Uani 1 1 d U . . F17 F 0.09896(9) 0.13847(7) 0.11509(6) 0.0442(4) Uani 1 1 d U . . P2 P 0.82064(2) 0.066807(18) 0.163897(18) 0.01773(9) Uani 1 1 d U . . C73 C 0.37788(10) 0.24967(7) 0.19627(7) 0.0196(3) Uani 1 1 d U . . P3 P 0.61780(2) 0.014697(18) 0.198814(19) 0.01762(9) Uani 1 1 d U . . F19 F 0.49579(7) 0.23882(7) 0.19230(6) 0.0378(3) Uani 1 1 d U . . P1 P 0.74793(3) -0.073590(18) 0.120688(18) 0.01837(9) Uani 1 1 d U . . F9 F 0.44938(8) 0.44000(7) -0.00722(6) 0.0445(4) Uani 1 1 d U . . C2 C 0.81495(9) -0.09167(7) 0.16243(7) 0.0178(3) Uani 1 1 d U . . F21 F 0.45832(8) 0.29487(5) 0.24426(6) 0.0376(3) Uani 1 1 d U . . C6 C 0.86385(9) -0.08113(7) 0.24376(7) 0.0197(3) Uani 1 1 d U . . H6 H 0.8643 -0.0659 0.2753 0.024 Uiso 1 1 calc R . . F18 F 0.16678(9) 0.08491(6) 0.08100(7) 0.0464(4) Uani 1 1 d U . . C1 C 0.81380(9) -0.06667(7) 0.20939(7) 0.0160(3) Uani 1 1 d U . . C56 C 0.37038(10) 0.34855(7) 0.04625(7) 0.0198(3) Uani 1 1 d U . . H56 H 0.4102 0.3306 0.0416 0.024 Uiso 1 1 calc R . . F12 F 0.16236(9) 0.41944(7) 0.11364(6) 0.0447(4) Uani 1 1 d U . . C55 C 0.31092(10) 0.32056(7) 0.05087(7) 0.0179(3) Uani 1 1 d U . . F20 F 0.44643(8) 0.21399(6) 0.25968(6) 0.0404(4) Uani 1 1 d U . . F7 F 0.48925(7) 0.40368(6) 0.05868(7) 0.0413(4) Uani 1 1 d U . . F22 F 0.16345(8) 0.21351(6) 0.23190(6) 0.0395(3) Uani 1 1 d U . . C18 C 0.70591(9) -0.08994(7) 0.28978(7) 0.0184(3) Uani 1 1 d U . . H18 H 0.7492 -0.1019 0.2951 0.022 Uiso 1 1 calc R . . F11 F 0.14400(9) 0.42236(9) 0.03514(7) 0.0618(6) Uani 1 1 d U . . C71 C 0.31335(10) 0.25086(7) 0.11862(7) 0.0184(3) Uani 1 1 d U . . C12 C 0.78378(10) 0.02640(7) 0.30788(7) 0.0201(3) Uani 1 1 d U . . H12 H 0.7626 -0.0006 0.3247 0.024 Uiso 1 1 calc R . . C8 C 0.82074(10) 0.06653(7) 0.23190(7) 0.0183(3) Uani 1 1 d U . . C72 C 0.37472(10) 0.24868(7) 0.14394(7) 0.0190(3) Uani 1 1 d U . . H72 H 0.4141 0.2465 0.1256 0.023 Uiso 1 1 calc R . . C5 C 0.91273(10) -0.11764(8) 0.23178(8) 0.0226(4) Uani 1 1 d U . . H5 H 0.9447 -0.1268 0.2554 0.027 Uiso 1 1 calc R . . F15 F 0.08265(9) 0.30604(6) -0.04890(6) 0.0433(4) Uani 1 1 d U . . C13 C 0.69498(9) -0.05108(7) 0.25376(7) 0.0153(3) Uani 1 1 d U . . C63 C 0.23737(10) 0.23295(7) 0.03640(7) 0.0186(3) Uani 1 1 d U . . C38 C 0.39689(10) 0.24305(7) -0.01643(7) 0.0208(3) Uani 1 1 d U . . H38 H 0.3853 0.2756 -0.0286 0.025 Uiso 1 1 calc R . . C7 C 0.78765(9) 0.02451(7) 0.25549(7) 0.0160(3) Uani 1 1 d U . . F24 F 0.15210(8) 0.29253(7) 0.20830(6) 0.0430(4) Uani 1 1 d U . . C22 C 0.69251(10) -0.13226(7) 0.11993(8) 0.0225(4) Uani 1 1 d U . . H22 H 0.6537 -0.1241 0.0990 0.027 Uiso 1 1 calc R . . B1 B 0.75776(10) -0.02492(7) 0.22550(7) 0.0156(3) Uani 1 1 d U . . C37 C 0.36750(9) 0.22571(7) 0.02809(7) 0.0171(3) Uani 1 1 d U . . C42 C 0.38808(10) 0.17638(7) 0.04440(7) 0.0187(3) Uani 1 1 d U . . H42 H 0.3701 0.1631 0.0738 0.022 Uiso 1 1 calc R . . N1 N 0.67577(11) 0.04249(8) 0.07876(7) 0.0288(4) Uani 1 1 d U . . H1N1 H 0.7095(15) 0.0428(12) 0.0527(12) 0.035 Uiso 1 1 d . . . H2N1 H 0.6395(16) 0.0159(12) 0.0655(12) 0.035 Uiso 1 1 d . . . C60 C 0.25281(10) 0.35026(7) 0.05819(7) 0.0201(3) Uani 1 1 d U . . H60 H 0.2120 0.3333 0.0616 0.024 Uiso 1 1 calc R . . F8 F 0.43820(9) 0.47663(6) 0.06412(8) 0.0481(4) Uani 1 1 d U . . C58 C 0.31363(11) 0.43117(7) 0.05540(7) 0.0228(4) Uani 1 1 d U . . H58 H 0.3145 0.4672 0.0566 0.027 Uiso 1 1 calc R . . F23 F 0.20419(8) 0.27476(7) 0.27686(5) 0.0391(3) Uani 1 1 d U . . C76 C 0.25605(10) 0.25445(7) 0.14860(7) 0.0202(3) Uani 1 1 d U . . H76 H 0.2144 0.2561 0.1332 0.024 Uiso 1 1 calc R . . C41 C 0.43434(10) 0.14685(7) 0.01800(8) 0.0212(3) Uani 1 1 d U A . C31 C 0.58684(11) 0.07094(8) 0.23571(8) 0.0245(4) Uani 1 1 d U . . H31 H 0.5467 0.0591 0.2534 0.029 Uiso 1 1 calc R . . C66 C 0.11488(10) 0.18830(8) 0.00238(8) 0.0236(4) Uani 1 1 d U . . H66 H 0.0747 0.1739 -0.0083 0.028 Uiso 1 1 calc R . . C14 C 0.62853(9) -0.03504(7) 0.24636(7) 0.0172(3) Uani 1 1 d U . . C57 C 0.37195(11) 0.40271(7) 0.04842(7) 0.0212(3) Uani 1 1 d U . . C75 C 0.25944(11) 0.25564(7) 0.20073(7) 0.0208(3) Uani 1 1 d U . . C15 C 0.57624(10) -0.05577(8) 0.27477(8) 0.0218(4) Uani 1 1 d U . . H15 H 0.5328 -0.0441 0.2697 0.026 Uiso 1 1 calc R . . C17 C 0.65388(10) -0.11104(7) 0.31777(7) 0.0206(3) Uani 1 1 d U . . H17 H 0.6626 -0.1367 0.3413 0.025 Uiso 1 1 calc R . . C16 C 0.58899(10) -0.09356(8) 0.31036(8) 0.0236(4) Uani 1 1 d U . . H16 H 0.5541 -0.1072 0.3293 0.028 Uiso 1 1 calc R . . C64 C 0.20071(10) 0.25435(7) -0.00342(7) 0.0198(3) Uani 1 1 d U . . H64 H 0.2168 0.2841 -0.0191 0.024 Uiso 1 1 calc R . . C59 C 0.25427(11) 0.40419(7) 0.06051(7) 0.0211(3) Uani 1 1 d U . . F14 F 0.13953(9) 0.26435(8) -0.10301(6) 0.0483(4) Uani 1 1 d U . . C74 C 0.32035(11) 0.25306(7) 0.22516(7) 0.0221(4) Uani 1 1 d U . . H74 H 0.3227 0.2536 0.2600 0.026 Uiso 1 1 calc R . . C28 C 0.80967(11) 0.13596(8) 0.14668(8) 0.0237(4) Uani 1 1 d U . . H28 H 0.8472 0.1553 0.1611 0.028 Uiso 1 1 calc R . . F10 F 0.19724(10) 0.48352(6) 0.07148(8) 0.0513(5) Uani 1 1 d U . . C11 C 0.81044(11) 0.06715(8) 0.33580(8) 0.0244(4) Uani 1 1 d U . . H11 H 0.8069 0.0670 0.3705 0.029 Uiso 1 1 calc R . . F13 F 0.04812(9) 0.23271(7) -0.07529(7) 0.0530(5) Uani 1 1 d U . . C69 C 0.10304(11) 0.25856(9) -0.06165(8) 0.0258(4) Uani 1 1 d U . . C23 C 0.66657(11) -0.14526(8) 0.17232(8) 0.0247(4) Uani 1 1 d U . . H23A H 0.6373 -0.1747 0.1705 0.037 Uiso 1 1 calc R . . H23B H 0.6425 -0.1161 0.1855 0.037 Uiso 1 1 calc R . . H23C H 0.7036 -0.1531 0.1939 0.037 Uiso 1 1 calc R . . C39 C 0.44281(11) 0.21348(8) -0.04313(8) 0.0236(4) Uani 1 1 d U B . C4 C 0.91371(10) -0.14036(8) 0.18446(8) 0.0240(4) Uani 1 1 d U . . H4 H 0.9469 -0.1641 0.1761 0.029 Uiso 1 1 calc R . . C34 C 0.54438(10) 0.00121(8) 0.15752(8) 0.0248(4) Uani 1 1 d U . . H34 H 0.5441 0.0292 0.1327 0.030 Uiso 1 1 calc R . . F16 F 0.07135(10) 0.09875(7) 0.04764(7) 0.0532(5) Uani 1 1 d U . . C68 C 0.21073(10) 0.18761(8) 0.05773(7) 0.0214(3) Uani 1 1 d U . . H68 H 0.2339 0.1713 0.0835 0.026 Uiso 1 1 calc R . . C25 C 0.90837(10) 0.05551(8) 0.14272(8) 0.0240(4) Uani 1 1 d U . . H25 H 0.9075 0.0520 0.1062 0.029 Uiso 1 1 calc R . . C61 C 0.43687(12) 0.43055(8) 0.04146(9) 0.0283(4) Uani 1 1 d U . . C27 C 0.93749(11) 0.00537(8) 0.16401(9) 0.0261(4) Uani 1 1 d U . . H27A H 0.9820 0.0006 0.1515 0.039 Uiso 1 1 calc R . . H27B H 0.9101 -0.0234 0.1540 0.039 Uiso 1 1 calc R . . H27C H 0.9386 0.0074 0.1999 0.039 Uiso 1 1 calc R . . C67 C 0.15062(11) 0.16649(8) 0.04140(8) 0.0227(4) Uani 1 1 d U . . C65 C 0.14083(10) 0.23247(8) -0.02032(7) 0.0213(3) Uani 1 1 d U . . C9 C 0.84746(12) 0.10765(8) 0.25989(8) 0.0259(4) Uani 1 1 d U . . H9 H 0.8688 0.1349 0.2436 0.031 Uiso 1 1 calc R . . C62 C 0.19015(12) 0.43233(8) 0.07011(8) 0.0263(4) Uani 1 1 d U . . C3 C 0.86489(10) -0.12739(7) 0.15002(8) 0.0214(3) Uani 1 1 d U . . H3 H 0.8653 -0.1425 0.1184 0.026 Uiso 1 1 calc R . . C70 C 0.12174(12) 0.12223(9) 0.07072(9) 0.0293(4) Uani 1 1 d U . . C78 C 0.19524(12) 0.25942(8) 0.22951(8) 0.0266(4) Uani 1 1 d U . . C40 C 0.46225(10) 0.16479(8) -0.02619(8) 0.0239(4) Uani 1 1 d U . . H40 H 0.4930 0.1449 -0.0439 0.029 Uiso 1 1 calc R . . C19 C 0.78398(11) -0.07501(9) 0.05649(8) 0.0261(4) Uani 1 1 d U . . H19 H 0.8071 -0.1082 0.0524 0.031 Uiso 1 1 calc R . . C21 C 0.72811(13) -0.07273(10) 0.01719(8) 0.0333(5) Uani 1 1 d U . . H21A H 0.7009 -0.0426 0.0230 0.050 Uiso 1 1 calc R . . H21B H 0.7010 -0.1033 0.0196 0.050 Uiso 1 1 calc R . . H21C H 0.7474 -0.0708 -0.0157 0.050 Uiso 1 1 calc R . . C26 C 0.95622(12) 0.09999(10) 0.15536(11) 0.0345(5) Uani 1 1 d U . . H26A H 0.9551 0.1065 0.1907 0.052 Uiso 1 1 calc R . . H26B H 0.9428 0.1307 0.1376 0.052 Uiso 1 1 calc R . . H26C H 1.0008 0.0907 0.1456 0.052 Uiso 1 1 calc R . . C24 C 0.72603(12) -0.18057(8) 0.09782(10) 0.0304(5) Uani 1 1 d U . . H24A H 0.7656 -0.1886 0.1167 0.046 Uiso 1 1 calc R . . H24B H 0.7379 -0.1741 0.0636 0.046 Uiso 1 1 calc R . . H24C H 0.6956 -0.2093 0.0994 0.046 Uiso 1 1 calc R . . C10 C 0.84230(13) 0.10811(8) 0.31163(8) 0.0293(4) Uani 1 1 d U . . H10 H 0.8599 0.1355 0.3300 0.035 Uiso 1 1 calc R . . C29 C 0.81279(12) 0.14278(9) 0.08950(9) 0.0307(5) Uani 1 1 d U . . H29A H 0.7769 0.1238 0.0742 0.046 Uiso 1 1 calc R . . H29B H 0.8548 0.1299 0.0773 0.046 Uiso 1 1 calc R . . H29C H 0.8087 0.1789 0.0813 0.046 Uiso 1 1 calc R . . N2 N 0.65055(12) 0.09518(8) 0.07873(9) 0.0356(5) Uani 1 1 d U . . H1N2 H 0.6245(17) 0.1030(13) 0.0494(13) 0.043 Uiso 1 1 d . . . H2N2 H 0.6218(17) 0.0971(13) 0.1092(13) 0.043 Uiso 1 1 d . . . C77 C 0.44409(11) 0.24920(8) 0.22263(8) 0.0241(4) Uani 1 1 d U . . C30 C 0.74554(13) 0.15869(9) 0.16837(9) 0.0318(5) Uani 1 1 d U . . H30A H 0.7431 0.1950 0.1605 0.048 Uiso 1 1 calc R . . H30B H 0.7454 0.1543 0.2041 0.048 Uiso 1 1 calc R . . H30C H 0.7077 0.1411 0.1542 0.048 Uiso 1 1 calc R . . C33 C 0.63702(12) 0.08739(8) 0.27574(9) 0.0292(4) Uani 1 1 d U . . H33A H 0.6777 0.0986 0.2600 0.044 Uiso 1 1 calc R . . H33B H 0.6463 0.0586 0.2974 0.044 Uiso 1 1 calc R . . H33C H 0.6187 0.1154 0.2950 0.044 Uiso 1 1 calc R . . C20 C 0.83555(13) -0.03194(10) 0.04922(8) 0.0324(5) Uani 1 1 d U . . H20A H 0.8536 -0.0339 0.0160 0.049 Uiso 1 1 calc R . . H20B H 0.8709 -0.0360 0.0732 0.049 Uiso 1 1 calc R . . H20C H 0.8145 0.0012 0.0539 0.049 Uiso 1 1 calc R . . C32 C 0.56551(13) 0.11731(9) 0.20332(10) 0.0316(5) Uani 1 1 d U . . H32A H 0.5487 0.1444 0.2245 0.047 Uiso 1 1 calc R . . H32B H 0.5312 0.1066 0.1804 0.047 Uiso 1 1 calc R . . H32C H 0.6034 0.1299 0.1848 0.047 Uiso 1 1 calc R . . C35 C 0.47544(12) 0.00217(11) 0.18156(10) 0.0359(5) Uani 1 1 d U . . H35A H 0.4418 0.0001 0.1560 0.054 Uiso 1 1 calc R . . H35B H 0.4700 0.0338 0.2001 0.054 Uiso 1 1 calc R . . H35C H 0.4710 -0.0268 0.2038 0.054 Uiso 1 1 calc R . . C36 C 0.55257(13) -0.04875(10) 0.12751(11) 0.0380(6) Uani 1 1 d U . . H36A H 0.5472 -0.0780 0.1493 0.057 Uiso 1 1 calc R . . H36B H 0.5963 -0.0496 0.1127 0.057 Uiso 1 1 calc R . . H36C H 0.5193 -0.0500 0.1016 0.057 Uiso 1 1 calc R . . B2 B 0.30800(11) 0.25718(8) 0.05740(8) 0.0178(3) Uani 1 1 d U . . C44 C 0.45456(12) 0.09490(9) 0.03822(10) 0.0319(5) Uani 1 1 d U . . F4 F 0.47785(19) 0.10097(11) 0.08748(10) 0.0505(10) Uani 0.660(6) 1 d PU A 1 F5 F 0.5070(2) 0.07489(17) 0.01557(14) 0.0463(10) Uani 0.660(6) 1 d PU A 1 F6 F 0.40758(15) 0.06203(13) 0.0423(2) 0.0651(17) Uani 0.660(6) 1 d PU A 1 F4A F 0.4367(5) 0.0559(2) -0.0013(3) 0.082(3) Uani 0.340(6) 1 d PU A 2 F5A F 0.5130(4) 0.0844(4) 0.0395(6) 0.099(5) Uani 0.340(6) 1 d PU A 2 F6A F 0.4214(6) 0.0760(3) 0.0725(4) 0.097(5) Uani 0.340(6) 1 d PU A 2 C43 C 0.47272(14) 0.23471(11) -0.09045(10) 0.0370(5) Uani 1 1 d U . . F1 F 0.5225(3) 0.2634(3) -0.08375(14) 0.107(3) Uani 0.693(9) 1 d PU B 1 F2 F 0.4270(2) 0.25988(15) -0.11868(16) 0.0538(11) Uani 0.693(9) 1 d PU B 1 F3 F 0.4894(2) 0.19555(13) -0.12248(9) 0.0545(11) Uani 0.693(9) 1 d PU B 1 F1A F 0.5333(7) 0.2180(4) -0.1000(6) 0.114(6) Uani 0.307(9) 1 d PU B 2 F2A F 0.4346(7) 0.2443(7) -0.1244(4) 0.112(5) Uani 0.307(9) 1 d PU B 2 F3A F 0.4926(5) 0.2878(3) -0.0813(4) 0.056(2) Uani 0.307(9) 1 d PU B 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 0.01668(12) 0.01720(11) 0.01560(12) 0.00065(9) -0.00032(9) 0.00153(9) F17 0.0533(10) 0.0486(9) 0.0308(8) 0.0019(6) 0.0176(7) -0.0113(8) P2 0.0189(2) 0.0173(2) 0.0169(2) 0.00244(15) 0.00157(16) -0.00221(16) C73 0.0273(9) 0.0129(7) 0.0187(8) -0.0005(6) -0.0025(7) -0.0017(6) P3 0.0153(2) 0.01740(19) 0.0202(2) 0.00099(16) 0.00070(16) 0.00271(15) F19 0.0274(7) 0.0534(9) 0.0325(7) -0.0030(6) -0.0045(6) 0.0092(6) P1 0.0209(2) 0.0188(2) 0.0155(2) -0.00292(15) -0.00213(17) 0.00394(16) F9 0.0364(8) 0.0595(10) 0.0376(8) 0.0138(7) 0.0073(7) -0.0105(7) C2 0.0170(8) 0.0163(7) 0.0202(8) -0.0002(6) -0.0018(6) -0.0002(6) F21 0.0356(8) 0.0257(6) 0.0517(9) -0.0097(6) -0.0108(7) -0.0064(5) C6 0.0174(8) 0.0212(8) 0.0205(8) 0.0009(6) -0.0024(6) -0.0018(6) F18 0.0466(9) 0.0332(8) 0.0594(11) 0.0196(7) 0.0095(8) -0.0025(7) C1 0.0155(7) 0.0157(7) 0.0167(7) 0.0007(6) 0.0000(6) -0.0023(6) C56 0.0224(9) 0.0179(7) 0.0190(8) 0.0001(6) 0.0007(7) -0.0001(6) F12 0.0427(9) 0.0554(10) 0.0360(8) 0.0100(7) 0.0148(7) 0.0203(7) C55 0.0209(8) 0.0183(7) 0.0146(7) -0.0014(6) -0.0011(6) 0.0008(6) F20 0.0428(8) 0.0400(8) 0.0383(8) 0.0207(6) -0.0175(7) -0.0148(7) F7 0.0276(7) 0.0339(7) 0.0624(11) 0.0110(7) -0.0107(7) -0.0075(6) F22 0.0381(8) 0.0338(7) 0.0466(9) -0.0048(6) 0.0156(7) -0.0103(6) C18 0.0183(8) 0.0184(7) 0.0184(8) 0.0020(6) -0.0012(6) -0.0015(6) F11 0.0462(10) 0.0924(15) 0.0466(10) -0.0378(10) -0.0263(8) 0.0401(10) C71 0.0235(9) 0.0142(7) 0.0176(8) -0.0013(6) 0.0015(7) -0.0008(6) C12 0.0249(9) 0.0180(7) 0.0174(8) 0.0015(6) 0.0001(7) -0.0043(6) C8 0.0212(8) 0.0165(7) 0.0171(8) 0.0018(6) 0.0012(6) -0.0029(6) C72 0.0245(9) 0.0139(7) 0.0185(8) -0.0002(6) 0.0012(7) -0.0023(6) C5 0.0163(8) 0.0225(8) 0.0289(10) 0.0043(7) -0.0037(7) -0.0001(6) F15 0.0488(9) 0.0338(8) 0.0471(9) -0.0033(6) -0.0093(7) 0.0171(7) C13 0.0152(7) 0.0149(7) 0.0157(7) -0.0016(5) -0.0003(6) -0.0013(5) C63 0.0198(8) 0.0183(7) 0.0177(8) -0.0022(6) 0.0032(6) 0.0000(6) C38 0.0253(9) 0.0208(8) 0.0162(8) 0.0010(6) -0.0010(7) -0.0013(7) C7 0.0166(8) 0.0146(7) 0.0169(7) 0.0013(6) -0.0001(6) -0.0012(6) F24 0.0414(9) 0.0506(9) 0.0371(8) 0.0054(7) 0.0116(7) 0.0217(7) C22 0.0219(9) 0.0212(8) 0.0244(9) -0.0079(7) -0.0074(7) 0.0040(7) B1 0.0149(8) 0.0164(8) 0.0154(8) 0.0011(6) -0.0014(6) -0.0007(6) C37 0.0177(8) 0.0177(7) 0.0158(8) -0.0006(6) -0.0016(6) -0.0011(6) C42 0.0196(8) 0.0187(7) 0.0179(8) 0.0007(6) 0.0006(6) -0.0004(6) N1 0.0339(10) 0.0301(9) 0.0223(8) 0.0017(7) -0.0049(7) 0.0064(7) C60 0.0225(9) 0.0199(8) 0.0178(8) -0.0012(6) -0.0001(7) 0.0008(6) F8 0.0452(9) 0.0262(7) 0.0729(12) -0.0127(7) 0.0063(8) -0.0140(6) C58 0.0325(10) 0.0170(8) 0.0190(8) -0.0008(6) -0.0014(7) 0.0012(7) F23 0.0411(8) 0.0515(9) 0.0246(7) -0.0119(6) 0.0095(6) -0.0002(7) C76 0.0243(9) 0.0174(7) 0.0191(8) -0.0018(6) 0.0007(7) 0.0002(6) C41 0.0205(8) 0.0196(8) 0.0235(9) -0.0002(6) 0.0014(7) 0.0023(6) C31 0.0243(9) 0.0212(8) 0.0280(10) 0.0003(7) 0.0055(8) 0.0070(7) C66 0.0204(9) 0.0271(9) 0.0233(9) -0.0037(7) 0.0012(7) -0.0027(7) C14 0.0167(8) 0.0151(7) 0.0197(8) -0.0008(6) 0.0006(6) 0.0002(6) C57 0.0276(9) 0.0174(8) 0.0184(8) 0.0012(6) -0.0007(7) -0.0026(7) C75 0.0282(9) 0.0156(7) 0.0186(8) -0.0023(6) 0.0032(7) -0.0012(6) C15 0.0155(8) 0.0218(8) 0.0281(10) 0.0004(7) 0.0041(7) -0.0006(6) C17 0.0231(9) 0.0177(7) 0.0209(8) 0.0016(6) 0.0008(7) -0.0037(6) C16 0.0210(9) 0.0239(9) 0.0259(9) 0.0020(7) 0.0041(7) -0.0049(7) C64 0.0206(8) 0.0198(8) 0.0189(8) -0.0010(6) 0.0017(6) 0.0001(6) C59 0.0279(9) 0.0201(8) 0.0152(8) -0.0007(6) -0.0004(7) 0.0050(7) F14 0.0410(9) 0.0783(12) 0.0257(7) 0.0166(7) 0.0063(6) 0.0245(8) C74 0.0328(10) 0.0170(7) 0.0164(8) -0.0009(6) 0.0012(7) -0.0024(7) C28 0.0268(10) 0.0204(8) 0.0239(9) 0.0051(7) 0.0018(7) -0.0020(7) F10 0.0534(10) 0.0248(7) 0.0756(13) 0.0023(7) 0.0162(9) 0.0166(7) C11 0.0344(11) 0.0222(8) 0.0165(8) -0.0016(6) -0.0010(7) -0.0040(7) F13 0.0448(10) 0.0509(10) 0.0632(11) 0.0197(8) -0.0320(9) -0.0182(8) C69 0.0205(9) 0.0296(10) 0.0274(10) -0.0002(8) -0.0028(7) 0.0019(7) C23 0.0251(9) 0.0201(8) 0.0290(10) -0.0050(7) -0.0020(8) -0.0032(7) C39 0.0252(9) 0.0274(9) 0.0182(8) 0.0004(7) 0.0040(7) -0.0010(7) C4 0.0193(9) 0.0196(8) 0.0331(10) -0.0002(7) 0.0009(8) 0.0024(6) C34 0.0179(8) 0.0261(9) 0.0305(10) 0.0032(7) -0.0028(7) 0.0027(7) F16 0.0598(11) 0.0540(10) 0.0457(9) 0.0137(8) -0.0167(8) -0.0390(9) C68 0.0241(9) 0.0211(8) 0.0189(8) -0.0010(6) 0.0003(7) -0.0020(7) C25 0.0207(9) 0.0280(9) 0.0234(9) 0.0055(7) 0.0042(7) -0.0023(7) C61 0.0314(11) 0.0229(9) 0.0306(11) 0.0015(8) -0.0018(8) -0.0049(8) C27 0.0196(9) 0.0285(10) 0.0302(10) 0.0047(8) 0.0021(8) -0.0009(7) C67 0.0254(9) 0.0229(8) 0.0199(9) -0.0014(7) 0.0045(7) -0.0050(7) C65 0.0200(8) 0.0243(8) 0.0197(8) -0.0029(6) 0.0006(7) 0.0022(7) C9 0.0369(11) 0.0169(8) 0.0239(9) 0.0012(6) -0.0009(8) -0.0090(7) C62 0.0327(11) 0.0260(9) 0.0200(9) -0.0025(7) -0.0021(8) 0.0080(8) C3 0.0208(9) 0.0189(8) 0.0246(9) -0.0031(7) 0.0016(7) 0.0013(6) C70 0.0309(11) 0.0319(10) 0.0250(10) 0.0020(8) 0.0007(8) -0.0094(8) C78 0.0321(11) 0.0244(9) 0.0232(9) -0.0028(7) 0.0069(8) 0.0003(8) C40 0.0218(9) 0.0260(9) 0.0240(9) -0.0030(7) 0.0042(7) 0.0020(7) C19 0.0315(11) 0.0309(10) 0.0157(8) -0.0044(7) 0.0004(7) 0.0061(8) C21 0.0416(13) 0.0401(12) 0.0182(9) -0.0051(8) -0.0058(9) 0.0083(10) C26 0.0236(10) 0.0311(11) 0.0488(15) 0.0105(10) 0.0012(10) -0.0082(8) C24 0.0309(11) 0.0233(9) 0.0368(12) -0.0138(8) -0.0022(9) 0.0016(8) C10 0.0441(13) 0.0200(9) 0.0239(10) -0.0031(7) -0.0023(9) -0.0083(8) C29 0.0334(11) 0.0312(10) 0.0275(10) 0.0125(8) 0.0021(9) -0.0002(9) N2 0.0401(12) 0.0341(10) 0.0326(11) 0.0023(8) -0.0097(9) 0.0097(9) C77 0.0315(10) 0.0173(8) 0.0236(9) 0.0016(6) -0.0030(8) -0.0021(7) C30 0.0369(12) 0.0242(9) 0.0344(12) 0.0018(8) 0.0015(10) 0.0044(8) C33 0.0354(11) 0.0230(9) 0.0292(11) -0.0042(8) 0.0034(9) 0.0038(8) C20 0.0392(13) 0.0387(12) 0.0193(9) -0.0011(8) 0.0054(9) 0.0005(10) C32 0.0340(12) 0.0230(9) 0.0379(12) 0.0040(8) 0.0033(9) 0.0105(8) C35 0.0189(10) 0.0506(14) 0.0384(13) 0.0078(11) -0.0019(9) -0.0005(9) C36 0.0265(11) 0.0330(11) 0.0544(16) -0.0116(11) -0.0146(11) 0.0033(9) B2 0.0193(9) 0.0155(8) 0.0186(9) -0.0013(6) 0.0005(7) 0.0002(6) C44 0.0272(11) 0.0256(10) 0.0428(13) 0.0055(9) 0.0054(9) 0.0070(8) F4 0.078(2) 0.0401(15) 0.0330(13) 0.0065(10) -0.0125(13) 0.0281(15) F5 0.051(2) 0.0388(16) 0.0489(17) 0.0035(13) 0.0187(15) 0.0275(15) F6 0.0267(14) 0.0294(15) 0.139(5) 0.038(2) -0.022(2) -0.0091(11) F4A 0.145(8) 0.023(2) 0.077(5) -0.007(3) -0.038(5) 0.020(3) F5A 0.024(3) 0.057(6) 0.214(14) 0.067(8) -0.020(6) 0.001(3) F6A 0.146(11) 0.045(5) 0.099(6) 0.044(5) 0.091(7) 0.051(6) C43 0.0388(13) 0.0456(13) 0.0265(11) 0.0038(9) 0.0114(10) -0.0023(10) F1 0.093(4) 0.201(7) 0.0281(15) 0.005(3) -0.001(2) -0.118(5) F2 0.072(2) 0.0502(17) 0.0387(18) 0.0246(13) 0.0239(15) 0.0263(18) F3 0.089(3) 0.0498(17) 0.0247(12) 0.0024(10) 0.0255(14) 0.0173(17) F1A 0.129(8) 0.073(6) 0.141(11) 0.061(7) 0.126(8) 0.056(7) F2A 0.118(8) 0.198(12) 0.020(3) 0.036(5) -0.036(5) -0.135(8) F3A 0.066(5) 0.055(4) 0.047(4) 0.013(3) 0.026(4) -0.021(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 Fe1 N1 2.2050(19) . ? Fe1 B1 2.392(2) . ? Fe1 P3 2.4279(6) . ? Fe1 P1 2.4470(5) . ? Fe1 P2 2.4701(6) . ? F17 C70 1.336(3) . ? P2 C8 1.8154(19) . ? P2 C28 1.854(2) . ? P2 C25 1.867(2) . ? C73 C74 1.388(3) . ? C73 C72 1.399(3) . ? C73 C77 1.500(3) . ? P3 C14 1.8172(19) . ? P3 C31 1.859(2) . ? P3 C34 1.869(2) . ? F19 C77 1.340(3) . ? P1 C2 1.8046(19) . ? P1 C19 1.860(2) . ? P1 C22 1.876(2) . ? F9 C61 1.346(3) . ? C2 C3 1.399(3) . ? C2 C1 1.410(3) . ? F21 C77 1.342(2) . ? C6 C5 1.394(3) . ? C6 C1 1.408(3) . ? F18 C70 1.347(3) . ? C1 B1 1.613(3) . ? C56 C55 1.397(3) . ? C56 C57 1.398(3) . ? F12 C62 1.330(3) . ? C55 C60 1.406(3) . ? C55 B2 1.645(3) . ? F20 C77 1.343(2) . ? F7 C61 1.338(3) . ? F22 C78 1.346(3) . ? C18 C17 1.392(3) . ? C18 C13 1.406(2) . ? F11 C62 1.338(3) . ? C71 C76 1.401(3) . ? C71 C72 1.402(3) . ? C71 B2 1.646(3) . ? C12 C11 1.395(3) . ? C12 C7 1.402(3) . ? C8 C9 1.403(3) . ? C8 C7 1.417(2) . ? C5 C4 1.393(3) . ? F15 C69 1.335(3) . ? C13 C14 1.406(2) . ? C13 B1 1.613(3) . ? C63 C64 1.404(3) . ? C63 C68 1.406(3) . ? C63 B2 1.643(3) . ? C38 C39 1.390(3) . ? C38 C37 1.399(3) . ? C7 B1 1.620(3) . ? F24 C78 1.339(3) . ? C22 C23 1.529(3) . ? C22 C24 1.533(3) . ? C37 C42 1.406(3) . ? C37 B2 1.639(3) . ? C42 C41 1.390(3) . ? N1 N2 1.449(3) . ? C60 C59 1.392(3) . ? F8 C61 1.334(3) . ? C58 C59 1.383(3) . ? C58 C57 1.391(3) . ? F23 C78 1.337(3) . ? C76 C75 1.394(3) . ? C41 C40 1.385(3) . ? C41 C44 1.500(3) . ? C31 C33 1.526(3) . ? C31 C32 1.536(3) . ? C66 C67 1.383(3) . ? C66 C65 1.391(3) . ? C14 C15 1.398(3) . ? C57 C61 1.495(3) . ? C75 C74 1.384(3) . ? C75 C78 1.500(3) . ? C15 C16 1.385(3) . ? C17 C16 1.388(3) . ? C64 C65 1.399(3) . ? C59 C62 1.496(3) . ? F14 C69 1.332(3) . ? C28 C30 1.525(3) . ? C28 C29 1.538(3) . ? F10 C62 1.328(3) . ? C11 C10 1.392(3) . ? F13 C69 1.336(3) . ? C69 C65 1.497(3) . ? C39 C40 1.390(3) . ? C39 C43 1.501(3) . ? C4 C3 1.382(3) . ? C34 C35 1.521(3) . ? C34 C36 1.526(3) . ? F16 C70 1.327(3) . ? C68 C67 1.390(3) . ? C25 C27 1.528(3) . ? C25 C26 1.531(3) . ? C67 C70 1.500(3) . ? C9 C10 1.385(3) . ? C19 C20 1.528(3) . ? C19 C21 1.534(3) . ? C44 F5A 1.201(9) . ? C44 F6A 1.231(7) . ? C44 F6 1.270(4) . ? C44 F5 1.316(4) . ? C44 F4 1.404(4) . ? C44 F4A 1.502(7) . ? C43 F2A 1.210(11) . ? C43 F1 1.252(4) . ? C43 F1A 1.312(9) . ? C43 F3 1.364(4) . ? C43 F2 1.352(5) . ? C43 F3A 1.445(9) . ? 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 B1 173.45(8) . . ? N1 Fe1 P3 97.38(6) . . ? B1 Fe1 P3 78.95(5) . . ? N1 Fe1 P1 97.70(5) . . ? B1 Fe1 P1 78.85(5) . . ? P3 Fe1 P1 111.869(19) . . ? N1 Fe1 P2 105.95(6) . . ? B1 Fe1 P2 80.55(5) . . ? P3 Fe1 P2 126.54(2) . . ? P1 Fe1 P2 111.67(2) . . ? C8 P2 C28 104.58(9) . . ? C8 P2 C25 107.53(9) . . ? C28 P2 C25 100.73(9) . . ? C8 P2 Fe1 99.00(6) . . ? C28 P2 Fe1 113.31(7) . . ? C25 P2 Fe1 129.43(7) . . ? C74 C73 C72 121.24(19) . . ? C74 C73 C77 118.16(17) . . ? C72 C73 C77 120.56(18) . . ? C14 P3 C31 102.70(9) . . ? C14 P3 C34 111.93(9) . . ? C31 P3 C34 101.29(10) . . ? C14 P3 Fe1 105.95(6) . . ? C31 P3 Fe1 125.09(7) . . ? C34 P3 Fe1 109.65(7) . . ? C2 P1 C19 106.02(9) . . ? C2 P1 C22 103.73(9) . . ? C19 P1 C22 101.73(10) . . ? C2 P1 Fe1 102.55(6) . . ? C19 P1 Fe1 113.31(7) . . ? C22 P1 Fe1 127.57(7) . . ? C3 C2 C1 121.56(17) . . ? C3 C2 P1 123.67(15) . . ? C1 C2 P1 114.76(13) . . ? C5 C6 C1 121.84(18) . . ? C6 C1 C2 116.54(17) . . ? C6 C1 B1 119.80(16) . . ? C2 C1 B1 123.62(16) . . ? C55 C56 C57 122.12(18) . . ? C56 C55 C60 115.78(17) . . ? C56 C55 B2 123.58(17) . . ? C60 C55 B2 119.82(17) . . ? C17 C18 C13 121.98(17) . . ? C76 C71 C72 116.32(17) . . ? C76 C71 B2 120.49(17) . . ? C72 C71 B2 122.65(17) . . ? C11 C12 C7 122.59(17) . . ? C9 C8 C7 121.26(17) . . ? C9 C8 P2 122.02(14) . . ? C7 C8 P2 116.54(13) . . ? C73 C72 C71 121.35(18) . . ? C4 C5 C6 120.13(18) . . ? C14 C13 C18 116.92(16) . . ? C14 C13 B1 123.18(15) . . ? C18 C13 B1 119.80(16) . . ? C64 C63 C68 115.82(18) . . ? C64 C63 B2 123.91(16) . . ? C68 C63 B2 120.26(17) . . ? C39 C38 C37 122.53(18) . . ? C12 C7 C8 116.27(16) . . ? C12 C7 B1 120.01(15) . . ? C8 C7 B1 123.67(16) . . ? C23 C22 C24 108.81(18) . . ? C23 C22 P1 111.56(13) . . ? C24 C22 P1 113.65(15) . . ? C13 B1 C1 112.76(14) . . ? C13 B1 C7 112.67(15) . . ? C1 B1 C7 113.61(15) . . ? C13 B1 Fe1 108.92(12) . . ? C1 B1 Fe1 105.90(12) . . ? C7 B1 Fe1 102.08(11) . . ? C38 C37 C42 115.42(17) . . ? C38 C37 B2 123.52(16) . . ? C42 C37 B2 120.83(16) . . ? C41 C42 C37 122.22(18) . . ? N2 N1 Fe1 116.92(14) . . ? C59 C60 C55 122.20(19) . . ? C59 C58 C57 117.90(17) . . ? C75 C76 C71 122.15(19) . . ? C40 C41 C42 121.16(18) . . ? C40 C41 C44 119.75(18) . . ? C42 C41 C44 119.09(18) . . ? C33 C31 C32 111.11(18) . . ? C33 C31 P3 111.64(14) . . ? C32 C31 P3 113.68(16) . . ? C67 C66 C65 117.94(19) . . ? C15 C14 C13 121.23(17) . . ? C15 C14 P3 124.08(14) . . ? C13 C14 P3 114.67(13) . . ? C58 C57 C56 120.91(19) . . ? C58 C57 C61 119.46(18) . . ? C56 C57 C61 119.59(19) . . ? C74 C75 C76 120.83(19) . . ? C74 C75 C78 121.05(18) . . ? C76 C75 C78 118.13(19) . . ? C16 C15 C14 120.23(18) . . ? C16 C17 C18 119.71(18) . . ? C15 C16 C17 119.90(18) . . ? C65 C64 C63 122.20(18) . . ? C58 C59 C60 121.08(19) . . ? C58 C59 C62 120.60(18) . . ? C60 C59 C62 118.30(19) . . ? C75 C74 C73 118.11(18) . . ? C30 C28 C29 111.54(19) . . ? C30 C28 P2 112.03(14) . . ? C29 C28 P2 110.56(15) . . ? C10 C11 C12 119.93(19) . . ? F14 C69 F13 106.3(2) . . ? F14 C69 F15 106.03(19) . . ? F13 C69 F15 106.03(19) . . ? F14 C69 C65 112.61(18) . . ? F13 C69 C65 113.07(19) . . ? F15 C69 C65 112.25(18) . . ? C40 C39 C38 120.89(18) . . ? C40 C39 C43 119.4(2) . . ? C38 C39 C43 119.7(2) . . ? C3 C4 C5 119.44(18) . . ? C35 C34 C36 109.4(2) . . ? C35 C34 P3 117.41(17) . . ? C36 C34 P3 112.49(15) . . ? C67 C68 C63 121.80(19) . . ? C27 C25 C26 108.28(18) . . ? C27 C25 P2 112.19(14) . . ? C26 C25 P2 113.82(16) . . ? F8 C61 F7 106.85(19) . . ? F8 C61 F9 105.84(19) . . ? F7 C61 F9 106.3(2) . . ? F8 C61 C57 112.9(2) . . ? F7 C61 C57 112.89(17) . . ? F9 C61 C57 111.62(19) . . ? C66 C67 C68 121.60(19) . . ? C66 C67 C70 120.23(19) . . ? C68 C67 C70 117.89(19) . . ? C66 C65 C64 120.62(19) . . ? C66 C65 C69 120.06(18) . . ? C64 C65 C69 119.26(18) . . ? C10 C9 C8 120.61(18) . . ? F10 C62 F12 105.59(18) . . ? F10 C62 F11 106.5(2) . . ? F12 C62 F11 105.9(2) . . ? F10 C62 C59 113.3(2) . . ? F12 C62 C59 112.75(17) . . ? F11 C62 C59 112.26(17) . . ? C4 C3 C2 120.42(18) . . ? F16 C70 F17 107.2(2) . . ? F16 C70 F18 106.1(2) . . ? F17 C70 F18 105.7(2) . . ? F16 C70 C67 113.42(19) . . ? F17 C70 C67 110.83(19) . . ? F18 C70 C67 113.11(19) . . ? F23 C78 F24 107.31(18) . . ? F23 C78 F22 106.20(18) . . ? F24 C78 F22 106.0(2) . . ? F23 C78 C75 112.90(19) . . ? F24 C78 C75 112.12(18) . . ? F22 C78 C75 111.83(17) . . ? C41 C40 C39 117.77(18) . . ? C20 C19 C21 112.15(19) . . ? C20 C19 P1 111.38(15) . . ? C21 C19 P1 110.31(16) . . ? C9 C10 C11 119.34(19) . . ? F19 C77 F21 105.74(18) . . ? F19 C77 F20 106.44(18) . . ? F21 C77 F20 105.60(17) . . ? F19 C77 C73 113.55(17) . . ? F21 C77 C73 112.46(17) . . ? F20 C77 C73 112.44(17) . . ? C37 B2 C63 105.85(14) . . ? C37 B2 C55 114.56(15) . . ? C63 B2 C55 111.84(15) . . ? C37 B2 C71 112.20(15) . . ? C63 B2 C71 110.92(15) . . ? C55 B2 C71 101.62(14) . . ? F5A C44 F6A 114.5(8) . . ? F5A C44 F6 124.6(5) . . ? F6A C44 F6 43.4(6) . . ? F5A C44 F5 31.7(7) . . ? F6A C44 F5 128.1(4) . . ? F6 C44 F5 111.6(4) . . ? F5A C44 F4 71.0(8) . . ? F6A C44 F4 61.7(7) . . ? F6 C44 F4 103.9(3) . . ? F5 C44 F4 102.1(3) . . ? F5A C44 C41 118.3(5) . . ? F6A C44 C41 118.4(4) . . ? F6 C44 C41 115.3(2) . . ? F5 C44 C41 113.6(3) . . ? F4 C44 C41 109.1(2) . . ? F5A C44 F4A 95.8(8) . . ? F6A C44 F4A 97.5(7) . . ? F6 C44 F4A 55.8(4) . . ? F5 C44 F4A 66.7(4) . . ? F4 C44 F4A 144.3(3) . . ? C41 C44 F4A 106.3(3) . . ? F2A C43 F1 119.2(6) . . ? F2A C43 F1A 120.2(9) . . ? F1 C43 F1A 59.1(7) . . ? F2A C43 F3 80.5(9) . . ? F1 C43 F3 109.4(4) . . ? F1A C43 F3 53.8(8) . . ? F2A C43 F2 19.6(10) . . ? F1 C43 F2 109.6(5) . . ? F1A C43 F2 132.5(6) . . ? F3 C43 F2 99.9(3) . . ? F2A C43 F3A 96.2(8) . . ? F1 C43 F3A 36.8(4) . . ? F1A C43 F3A 95.2(7) . . ? F3 C43 F3A 137.7(4) . . ? F2 C43 F3A 80.0(5) . . ? F2A C43 C39 117.0(6) . . ? F1 C43 C39 114.3(3) . . ? F1A C43 C39 114.3(5) . . ? F3 C43 C39 110.8(2) . . ? F2 C43 C39 112.0(3) . . ? F3A C43 C39 108.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 32.59 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.295 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.096 data_(TPB)Fe(NH3)BArF_(4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H80 B4 F24 Fe N2 O2 P3' _chemical_formula_weight 1605.34 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' 'B' 'B' 0.0013 0.0007 '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' 'P' 'P' 0.1023 0.0942 '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' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.846(4) _cell_length_b 25.821(5) _cell_length_c 26.862(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13765(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max .25 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6600 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 155016 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0077 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.18 _reflns_number_total 12232 _reflns_number_gt 11720 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0900P)^2^+25.0844P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12232 _refine_ls_number_parameters 961 _refine_ls_number_restraints 972 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1692 _refine_ls_wR_factor_gt 0.1680 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.022 _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 0.78978(2) 0.013636(17) 0.646628(18) 0.03786(14) Uani 1 1 d U . . P2 P 0.76070(4) -0.07276(3) 0.61750(3) 0.03023(17) Uani 1 1 d U . . P3 P 0.68675(4) 0.06689(3) 0.65970(3) 0.03181(18) Uani 1 1 d U . . P1 P 0.88943(4) 0.01365(3) 0.69885(3) 0.03546(19) Uani 1 1 d U . . F16 F 0.63625(10) -0.25072(8) 1.10374(7) 0.0475(5) Uani 1 1 d U . . F9 F 0.96305(11) -0.20508(8) 0.75280(9) 0.0554(5) Uani 1 1 d U . . F8 F 1.00233(10) -0.25841(9) 0.80580(7) 0.0505(5) Uani 1 1 d U . . F13 F 0.67273(11) -0.41772(8) 0.92144(9) 0.0563(5) Uani 1 1 d U . . F23 F 0.99238(10) -0.09454(8) 0.94014(9) 0.0548(5) Uani 1 1 d U . . F22 F 0.94006(12) -0.02246(8) 0.93535(11) 0.0675(7) Uani 1 1 d U . . F15 F 0.60376(13) -0.36644(9) 0.88543(8) 0.0652(6) Uani 1 1 d U . . F19 F 0.69788(13) -0.01819(8) 0.92177(10) 0.0663(7) Uani 1 1 d U . . F7 F 0.95324(11) -0.28645(9) 0.73997(8) 0.0579(6) Uani 1 1 d U . . F12 F 0.66694(12) -0.28750(9) 0.76713(9) 0.0612(6) Uani 1 1 d U . . C41 C 0.94099(15) -0.35144(11) 0.97934(11) 0.0332(6) Uani 1 1 d U B . F17 F 0.60722(13) -0.19017(9) 1.05467(9) 0.0671(7) Uani 1 1 d U . . F21 F 0.65990(12) -0.08484(10) 0.88664(10) 0.0705(7) Uani 1 1 d U . . C45 C 0.88366(15) -0.24974(10) 0.80152(11) 0.0305(6) Uani 1 1 d U . . C44 C 0.87973(15) -0.25087(10) 0.85341(10) 0.0280(6) Uani 1 1 d U . . H44 H 0.9193 -0.2526 0.8718 0.034 Uiso 1 1 calc R . . C48 C 0.76003(15) -0.24655(10) 0.84857(10) 0.0301(6) Uani 1 1 d U . . H48 H 0.7179 -0.2455 0.8637 0.036 Uiso 1 1 calc R . . F11 F 0.65595(12) -0.20818(10) 0.78755(9) 0.0654(6) Uani 1 1 d U . . F24 F 0.95074(11) -0.05978(10) 1.00542(8) 0.0631(6) Uani 1 1 d U . . C37 C 0.87264(13) -0.27348(10) 0.96864(10) 0.0263(5) Uani 1 1 d U . . C49 C 0.74144(14) -0.26768(11) 0.96051(10) 0.0282(6) Uani 1 1 d U . . C11 C 0.64081(14) -0.08077(11) 0.73838(11) 0.0319(6) Uani 1 1 d U . . H11 H 0.6396 -0.0661 0.7700 0.038 Uiso 1 1 calc R . . C68 C 0.93920(18) -0.06882(12) 0.95707(13) 0.0415(7) Uani 1 1 d U . . F20 F 0.64862(14) -0.07486(13) 0.96496(11) 0.0904(10) Uani 1 1 d U . . F10 F 0.70828(11) -0.22867(10) 0.72038(7) 0.0580(6) Uani 1 1 d U . . C25 C 0.81562(15) -0.13164(11) 0.61758(11) 0.0336(6) Uani 1 1 d U . . H25 H 0.8559 -0.1235 0.5979 0.040 Uiso 1 1 calc R . . C43 C 0.81779(14) -0.24942(10) 0.87860(10) 0.0269(5) Uani 1 1 d U . . F14 F 0.57579(13) -0.40296(10) 0.95363(10) 0.0710(7) Uani 1 1 d U . . C17 C 0.72092(15) 0.02822(11) 0.80398(10) 0.0316(6) Uani 1 1 d U . . H17 H 0.7410 0.0011 0.8213 0.038 Uiso 1 1 calc R . . C8 C 0.64168(15) -0.12520(11) 0.64487(11) 0.0330(6) Uani 1 1 d U . . H8 H 0.6416 -0.1395 0.6131 0.040 Uiso 1 1 calc R . . C55 C 0.81380(14) -0.17959(10) 0.94556(10) 0.0276(5) Uani 1 1 d U . . C1 C 0.87677(14) -0.03503(10) 0.74681(10) 0.0283(5) Uani 1 1 d U . . C58 C 0.81568(16) -0.06918(11) 0.94187(10) 0.0341(6) Uani 1 1 d U . . H58 H 0.8163 -0.0332 0.9407 0.041 Uiso 1 1 calc R . . F18 F 0.54429(10) -0.25663(12) 1.06314(9) 0.0715(7) Uani 1 1 d U . . C50 C 0.71480(14) -0.31331(11) 0.94039(11) 0.0304(6) Uani 1 1 d U . . H50 H 0.7377 -0.3297 0.9146 0.036 Uiso 1 1 calc R . . C27 C 0.83889(15) -0.14510(12) 0.67006(11) 0.0361(6) Uani 1 1 d U . . H27A H 0.8006 -0.1541 0.6901 0.054 Uiso 1 1 calc R . . H27B H 0.8613 -0.1158 0.6845 0.054 Uiso 1 1 calc R . . H27C H 0.8695 -0.1739 0.6687 0.054 Uiso 1 1 calc R . . C60 C 0.87348(15) -0.15114(11) 0.95092(10) 0.0287(6) Uani 1 1 d U . . H60 H 0.9138 -0.1688 0.9557 0.034 Uiso 1 1 calc R . . C5 C 0.79746(14) -0.09015(11) 0.78788(10) 0.0286(6) Uani 1 1 d U . . H5 H 0.7537 -0.1024 0.7919 0.034 Uiso 1 1 calc R . . C52 C 0.61964(15) -0.31278(13) 0.99637(11) 0.0362(6) Uani 1 1 d U . . H52 H 0.5798 -0.3275 1.0079 0.043 Uiso 1 1 calc R . . C13 C 0.68668(14) 0.06786(10) 0.72741(11) 0.0286(6) Uani 1 1 d U . . C57 C 0.75611(16) -0.09642(11) 0.93622(10) 0.0321(6) Uani 1 1 d U . . C7 C 0.69195(14) -0.09005(10) 0.65811(10) 0.0281(6) Uani 1 1 d U . . C64 C 0.69909(18) -0.24228(13) 0.76798(12) 0.0420(7) Uani 1 1 d U . . C56 C 0.75538(15) -0.15059(11) 0.93820(10) 0.0302(6) Uani 1 1 d U . . H56 H 0.7145 -0.1678 0.9345 0.036 Uiso 1 1 calc R . . C54 C 0.70499(14) -0.24602(11) 1.00006(11) 0.0304(6) Uani 1 1 d U . . H54 H 0.7213 -0.2161 1.0151 0.037 Uiso 1 1 calc R . . C18 C 0.71817(13) 0.02573(10) 0.75157(10) 0.0257(5) Uani 1 1 d U . . C14 C 0.66095(17) 0.10978(11) 0.75457(12) 0.0368(7) Uani 1 1 d U . . H14 H 0.6409 0.1373 0.7379 0.044 Uiso 1 1 calc R . . C42 C 0.89416(14) -0.32252(10) 0.95286(10) 0.0287(6) Uani 1 1 d U . . H42 H 0.8764 -0.3362 0.9236 0.034 Uiso 1 1 calc R . . C16 C 0.69489(16) 0.06950(12) 0.83075(11) 0.0370(7) Uani 1 1 d U . . H16 H 0.6974 0.0696 0.8653 0.044 Uiso 1 1 calc R . . C28 C 0.72671(17) -0.07268(14) 0.55319(11) 0.0405(7) Uani 1 1 d U . . H28 H 0.7037 -0.1058 0.5478 0.049 Uiso 1 1 calc R . . C51 C 0.65502(15) -0.33498(12) 0.95777(11) 0.0343(6) Uani 1 1 d U . . C4 C 0.84852(15) -0.11108(11) 0.81673(11) 0.0326(6) Uani 1 1 d U . . H4 H 0.8387 -0.1369 0.8398 0.039 Uiso 1 1 calc R . . C36 C 0.56760(16) 0.00777(13) 0.66065(13) 0.0405(7) Uani 1 1 d U . . H36A H 0.5672 0.0098 0.6963 0.061 Uiso 1 1 calc R . . H36B H 0.5942 -0.0214 0.6504 0.061 Uiso 1 1 calc R . . H36C H 0.5223 0.0037 0.6486 0.061 Uiso 1 1 calc R . . C10 C 0.59193(15) -0.11708(12) 0.72530(12) 0.0364(7) Uani 1 1 d U . . H10 H 0.5591 -0.1266 0.7483 0.044 Uiso 1 1 calc R . . C38 C 0.90152(15) -0.25573(11) 1.01300(10) 0.0309(6) Uani 1 1 d U . . H38 H 0.8885 -0.2236 1.0253 0.037 Uiso 1 1 calc R . . C34 C 0.59779(16) 0.05710(13) 0.63935(12) 0.0395(7) Uani 1 1 d U . . H34 H 0.5980 0.0537 0.6030 0.047 Uiso 1 1 calc R . . C6 C 0.80970(13) -0.05112(10) 0.75278(10) 0.0251(5) Uani 1 1 d U . . C9 C 0.59209(15) -0.13895(12) 0.67829(12) 0.0363(6) Uani 1 1 d U . . H9 H 0.5590 -0.1627 0.6693 0.044 Uiso 1 1 calc R . . C12 C 0.69197(13) -0.06572(10) 0.70505(10) 0.0263(5) Uani 1 1 d U . . B1 B 0.74783(16) -0.02469(12) 0.72337(12) 0.0292(6) Uani 1 1 d U . . C62 C 0.96269(18) -0.40341(13) 0.96027(15) 0.0468(8) Uani 1 1 d U . . C47 C 0.76398(16) -0.24518(10) 0.79654(11) 0.0326(6) Uani 1 1 d U . . C59 C 0.87429(16) -0.09725(11) 0.94927(10) 0.0321(6) Uani 1 1 d U . . C39 C 0.94903(16) -0.28447(12) 1.03945(11) 0.0360(6) Uani 1 1 d U A . C3 C 0.91382(16) -0.09372(12) 0.81131(12) 0.0379(7) Uani 1 1 d U . . H3 H 0.9480 -0.1074 0.8310 0.045 Uiso 1 1 calc R . . C46 C 0.82530(16) -0.24705(10) 0.77287(10) 0.0322(6) Uani 1 1 d U . . H46 H 0.8278 -0.2465 0.7383 0.039 Uiso 1 1 calc R . . C22 C 0.96372(18) 0.00073(17) 0.65912(14) 0.0500(8) Uani 1 1 d U . . H22 H 0.9660 0.0299 0.6359 0.060 Uiso 1 1 calc R . . B2 B 0.81224(16) -0.24291(12) 0.93938(12) 0.0273(6) Uani 1 1 d U . . C40 C 0.96926(16) -0.33272(12) 1.02283(12) 0.0374(7) Uani 1 1 d U . . H40 H 1.0009 -0.3520 1.0404 0.045 Uiso 1 1 calc R B . C53 C 0.64502(15) -0.26772(12) 1.01769(11) 0.0334(6) Uani 1 1 d U . . C2 C 0.92814(15) -0.05590(12) 0.77638(11) 0.0349(6) Uani 1 1 d U . . H2 H 0.9722 -0.0443 0.7725 0.042 Uiso 1 1 calc R . . C66 C 0.60870(15) -0.24175(13) 1.05934(12) 0.0404(7) Uani 1 1 d U . . C31 C 0.7011(2) 0.13510(13) 0.64066(13) 0.0466(8) Uani 1 1 d U . . H31 H 0.6658 0.1561 0.6562 0.056 Uiso 1 1 calc R . . C63 C 0.95001(17) -0.25013(11) 0.77555(11) 0.0363(6) Uani 1 1 d U . . C65 C 0.62681(17) -0.38057(14) 0.93026(13) 0.0447(8) Uani 1 1 d U . . C61 C 0.9782(2) -0.26258(16) 1.08609(13) 0.0521(9) Uani 1 1 d U . . C15 C 0.66503(17) 0.11059(12) 0.80588(12) 0.0398(7) Uani 1 1 d U . . H15 H 0.6479 0.1385 0.8237 0.048 Uiso 1 1 calc R . . C26 C 0.78242(17) -0.17923(13) 0.59409(14) 0.0438(8) Uani 1 1 d U . . H26A H 0.8128 -0.2081 0.5958 0.066 Uiso 1 1 calc R . . H26B H 0.7718 -0.1720 0.5599 0.066 Uiso 1 1 calc R . . H26C H 0.7418 -0.1874 0.6118 0.066 Uiso 1 1 calc R . . C29 C 0.78494(19) -0.06913(17) 0.51571(12) 0.0514(9) Uani 1 1 d U . . H29A H 0.7671 -0.0677 0.4825 0.077 Uiso 1 1 calc R . . H29B H 0.8133 -0.0990 0.5190 0.077 Uiso 1 1 calc R . . H29C H 0.8108 -0.0385 0.5222 0.077 Uiso 1 1 calc R . . C67 C 0.69093(17) -0.06890(12) 0.92740(12) 0.0400(7) Uani 1 1 d U . . C30 C 0.67488(19) -0.02942(15) 0.54639(12) 0.0473(8) Uani 1 1 d U . . H30A H 0.6963 0.0035 0.5513 0.071 Uiso 1 1 calc R . . H30B H 0.6393 -0.0336 0.5702 0.071 Uiso 1 1 calc R . . H30C H 0.6566 -0.0310 0.5133 0.071 Uiso 1 1 calc R . . C33 C 0.6939(2) 0.14114(16) 0.58420(14) 0.0567(10) Uani 1 1 d U . . H33A H 0.6990 0.1769 0.5754 0.085 Uiso 1 1 calc R . . H33B H 0.6502 0.1292 0.5740 0.085 Uiso 1 1 calc R . . H33C H 0.7280 0.1210 0.5678 0.085 Uiso 1 1 calc R . . C24 C 1.03192(19) -0.0010(2) 0.68442(16) 0.0668(12) Uani 1 1 d U . . H24A H 1.0357 -0.0323 0.7035 0.100 Uiso 1 1 calc R . . H24B H 1.0365 0.0284 0.7061 0.100 Uiso 1 1 calc R . . H24C H 1.0668 -0.0001 0.6597 0.100 Uiso 1 1 calc R . . C19 C 0.9214(2) 0.06989(14) 0.73443(15) 0.0560(9) Uani 1 1 d U . . H19 H 0.9620 0.0582 0.7519 0.067 Uiso 1 1 calc R . . C20 C 0.8727(3) 0.08734(15) 0.77345(16) 0.0644(11) Uani 1 1 d U . . H20A H 0.8920 0.1154 0.7920 0.097 Uiso 1 1 calc R . . H20B H 0.8630 0.0591 0.7955 0.097 Uiso 1 1 calc R . . H20C H 0.8318 0.0987 0.7578 0.097 Uiso 1 1 calc R . . C35 C 0.55100(19) 0.10261(15) 0.65255(17) 0.0571(10) Uani 1 1 d U . . H35A H 0.5060 0.0949 0.6418 0.086 Uiso 1 1 calc R . . H35B H 0.5666 0.1334 0.6362 0.086 Uiso 1 1 calc R . . H35C H 0.5513 0.1079 0.6879 0.086 Uiso 1 1 calc R . . C21 C 0.9432(2) 0.11493(16) 0.70003(19) 0.0698(12) Uani 1 1 d U . . H21A H 0.9063 0.1244 0.6788 0.105 Uiso 1 1 calc R . . H21B H 0.9807 0.1042 0.6800 0.105 Uiso 1 1 calc R . . H21C H 0.9561 0.1442 0.7199 0.105 Uiso 1 1 calc R . . C32 C 0.7681(2) 0.15546(15) 0.65883(16) 0.0592(10) Uani 1 1 d U . . H32A H 0.8038 0.1353 0.6446 0.089 Uiso 1 1 calc R . . H32B H 0.7699 0.1530 0.6945 0.089 Uiso 1 1 calc R . . H32C H 0.7730 0.1910 0.6490 0.089 Uiso 1 1 calc R . . C23 C 0.9560(2) -0.04636(18) 0.62739(19) 0.0654(11) Uani 1 1 d U . . H23A H 0.9905 -0.0466 0.6024 0.098 Uiso 1 1 calc R . . H23B H 0.9126 -0.0459 0.6117 0.098 Uiso 1 1 calc R . . H23C H 0.9600 -0.0768 0.6477 0.098 Uiso 1 1 calc R . . N1 N 0.83698(14) 0.04983(11) 0.57749(12) 0.0469(7) Uani 1 1 d U . . H1A H 0.8506 0.0818 0.5845 0.070 Uiso 1 1 calc R . . H1B H 0.8066 0.0509 0.5531 0.070 Uiso 1 1 calc R . . H1C H 0.8721 0.0309 0.5679 0.070 Uiso 1 1 calc R . . F1 F 1.0460(3) -0.2754(3) 1.0915(3) 0.085(3) Uani 0.444(7) 1 d PU A 1 F2 F 0.9456(5) -0.2617(4) 1.1222(3) 0.088(3) Uani 0.444(7) 1 d PU A 1 F3 F 0.9957(3) -0.2077(2) 1.0793(2) 0.0486(14) Uani 0.444(7) 1 d PU A 1 F1A F 0.9934(3) -0.30192(19) 1.11915(13) 0.0711(19) Uani 0.556(7) 1 d PU A 2 F2A F 0.9276(2) -0.24000(17) 1.11633(18) 0.0488(12) Uani 0.556(7) 1 d PU A 2 F3A F 1.0243(4) -0.2340(4) 1.0814(2) 0.093(2) Uani 0.556(7) 1 d PU A 2 F4 F 0.9979(12) -0.4309(5) 0.9893(5) 0.084(4) Uani 0.381(18) 1 d PU B 1 F5 F 1.0251(5) -0.4095(4) 0.9545(6) 0.068(3) Uani 0.381(18) 1 d PU B 1 F6 F 0.9206(9) -0.4292(9) 0.9361(10) 0.082(5) Uani 0.381(18) 1 d PU B 1 F4A F 0.9551(6) -0.44064(19) 0.9984(2) 0.076(2) Uani 0.619(18) 1 d PU B 2 F5A F 1.0169(6) -0.3980(4) 0.9302(6) 0.118(4) Uani 0.619(18) 1 d PU B 2 F6A F 0.9241(7) -0.4223(5) 0.9253(5) 0.077(3) Uani 0.619(18) 1 d PU B 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 0.0349(3) 0.0319(2) 0.0468(3) -0.00076(18) -0.00411(19) -0.00337(17) P2 0.0333(4) 0.0302(4) 0.0272(3) -0.0026(3) 0.0010(3) -0.0056(3) P3 0.0363(4) 0.0289(4) 0.0302(4) 0.0053(3) -0.0039(3) 0.0011(3) P1 0.0350(4) 0.0364(4) 0.0350(4) 0.0011(3) -0.0003(3) -0.0115(3) F16 0.0501(11) 0.0564(12) 0.0360(9) -0.0029(8) -0.0010(8) 0.0176(9) F9 0.0522(12) 0.0410(11) 0.0731(14) 0.0174(10) 0.0160(10) -0.0065(9) F8 0.0428(10) 0.0624(13) 0.0465(11) -0.0010(9) 0.0059(8) 0.0075(9) F13 0.0551(12) 0.0431(11) 0.0708(14) -0.0139(10) -0.0064(11) -0.0096(9) F23 0.0427(11) 0.0439(11) 0.0779(15) -0.0129(10) 0.0103(10) -0.0101(9) F22 0.0649(14) 0.0358(11) 0.1020(19) 0.0157(11) -0.0089(13) -0.0174(10) F15 0.0729(15) 0.0674(14) 0.0553(13) 0.0016(11) -0.0291(11) -0.0180(12) F19 0.0750(15) 0.0349(11) 0.0889(18) 0.0041(11) -0.0180(13) 0.0197(10) F7 0.0611(13) 0.0580(13) 0.0547(12) -0.0281(10) 0.0205(10) -0.0143(10) F12 0.0618(13) 0.0572(13) 0.0646(14) 0.0114(10) -0.0248(11) -0.0232(11) C41 0.0310(14) 0.0286(14) 0.0401(15) 0.0042(12) -0.0005(12) 0.0012(11) F17 0.0856(17) 0.0494(12) 0.0663(14) 0.0128(11) 0.0262(12) 0.0337(12) F21 0.0629(14) 0.0697(15) 0.0789(16) -0.0236(13) -0.0341(12) 0.0296(12) C45 0.0441(16) 0.0158(12) 0.0317(14) -0.0002(10) 0.0027(12) -0.0021(11) C44 0.0373(14) 0.0179(12) 0.0287(13) -0.0010(10) -0.0032(11) -0.0018(11) C48 0.0374(15) 0.0223(13) 0.0308(14) 0.0028(10) -0.0039(11) -0.0013(11) F11 0.0604(14) 0.0772(16) 0.0585(13) -0.0050(11) -0.0221(11) 0.0268(12) F24 0.0549(13) 0.0803(16) 0.0541(13) -0.0210(11) -0.0102(10) -0.0164(11) C37 0.0264(13) 0.0269(13) 0.0255(12) 0.0037(10) 0.0007(10) -0.0034(10) C49 0.0296(13) 0.0272(13) 0.0277(13) 0.0052(10) -0.0050(11) 0.0009(11) C11 0.0284(14) 0.0351(15) 0.0323(14) -0.0010(11) 0.0024(11) 0.0066(11) C68 0.0468(18) 0.0308(15) 0.0468(18) -0.0037(13) -0.0006(15) -0.0046(13) F20 0.0716(17) 0.117(2) 0.0829(18) 0.0511(17) 0.0370(14) 0.0561(16) F10 0.0617(13) 0.0754(15) 0.0370(10) 0.0160(10) -0.0170(9) -0.0082(11) C25 0.0296(14) 0.0335(15) 0.0376(15) -0.0111(12) 0.0076(12) -0.0022(12) C43 0.0352(14) 0.0162(11) 0.0292(13) 0.0014(10) -0.0037(11) -0.0015(10) F14 0.0684(15) 0.0671(15) 0.0776(16) -0.0140(12) 0.0209(12) -0.0406(13) C17 0.0362(15) 0.0287(14) 0.0298(14) 0.0013(11) -0.0029(11) 0.0084(12) C8 0.0321(14) 0.0281(14) 0.0387(15) -0.0056(12) -0.0035(12) 0.0027(11) C55 0.0345(14) 0.0254(13) 0.0230(12) 0.0005(10) -0.0004(11) 0.0013(11) C1 0.0282(13) 0.0259(13) 0.0307(13) -0.0051(11) 0.0004(11) -0.0015(11) C58 0.0494(17) 0.0253(14) 0.0276(14) -0.0014(11) -0.0003(12) 0.0017(12) F18 0.0319(10) 0.114(2) 0.0691(15) -0.0231(14) 0.0121(10) -0.0042(12) C50 0.0309(14) 0.0299(14) 0.0303(14) 0.0046(11) -0.0034(11) -0.0008(11) C27 0.0348(15) 0.0316(15) 0.0417(16) -0.0084(12) 0.0032(13) 0.0060(12) C60 0.0339(14) 0.0262(13) 0.0261(13) -0.0008(10) -0.0011(11) 0.0009(11) C5 0.0270(13) 0.0277(14) 0.0311(14) 0.0010(11) 0.0000(11) 0.0015(11) C52 0.0271(14) 0.0449(17) 0.0367(15) 0.0092(13) -0.0043(12) -0.0032(12) C13 0.0304(14) 0.0233(13) 0.0322(14) 0.0025(10) -0.0026(11) 0.0010(11) C57 0.0435(16) 0.0274(14) 0.0254(13) 0.0001(11) -0.0012(12) 0.0066(12) C7 0.0292(13) 0.0240(13) 0.0312(13) -0.0013(10) -0.0005(11) 0.0051(11) C64 0.0516(19) 0.0383(17) 0.0360(16) 0.0062(13) -0.0118(14) -0.0046(14) C56 0.0348(14) 0.0290(14) 0.0268(13) 0.0016(11) -0.0015(11) 0.0018(11) C54 0.0297(14) 0.0298(14) 0.0318(14) 0.0048(11) -0.0054(11) 0.0028(11) C18 0.0250(13) 0.0226(12) 0.0294(13) 0.0016(10) -0.0019(10) 0.0002(10) C14 0.0467(17) 0.0242(13) 0.0395(15) 0.0021(12) -0.0020(13) 0.0099(12) C42 0.0303(14) 0.0255(13) 0.0304(14) 0.0022(11) -0.0021(11) -0.0018(11) C16 0.0459(17) 0.0359(16) 0.0293(14) -0.0040(12) -0.0008(13) 0.0062(13) C28 0.0456(18) 0.0488(18) 0.0270(14) -0.0042(13) -0.0003(13) -0.0062(14) C51 0.0328(15) 0.0348(15) 0.0353(15) 0.0075(12) -0.0063(12) -0.0040(12) C4 0.0395(15) 0.0265(14) 0.0318(14) 0.0017(11) -0.0012(12) 0.0063(12) C36 0.0316(15) 0.0463(18) 0.0437(17) 0.0013(14) -0.0060(13) 0.0044(13) C10 0.0254(14) 0.0388(16) 0.0451(17) 0.0048(13) 0.0043(12) 0.0038(12) C38 0.0339(14) 0.0306(14) 0.0281(13) 0.0011(11) 0.0013(11) -0.0002(11) C34 0.0337(15) 0.0467(18) 0.0383(16) 0.0063(14) -0.0074(13) 0.0047(13) C6 0.0250(13) 0.0219(12) 0.0284(13) -0.0045(10) -0.0004(10) 0.0036(10) C9 0.0266(14) 0.0312(15) 0.0510(18) -0.0032(13) -0.0027(12) 0.0007(11) C12 0.0257(13) 0.0243(13) 0.0290(13) 0.0001(10) -0.0037(10) 0.0067(10) B1 0.0284(15) 0.0283(15) 0.0309(15) -0.0010(12) -0.0030(12) 0.0063(12) C62 0.0429(18) 0.0351(17) 0.063(2) 0.0015(15) -0.0078(15) 0.0096(14) C47 0.0457(16) 0.0215(13) 0.0305(14) 0.0031(11) -0.0080(12) -0.0030(12) C59 0.0422(16) 0.0278(14) 0.0264(13) -0.0023(11) -0.0006(12) -0.0030(12) C39 0.0370(15) 0.0417(16) 0.0291(14) 0.0026(12) -0.0056(12) -0.0008(13) C3 0.0331(15) 0.0410(17) 0.0396(16) -0.0034(13) -0.0107(13) 0.0123(13) C46 0.0511(17) 0.0193(12) 0.0263(13) 0.0008(10) -0.0039(12) -0.0020(12) C22 0.0368(17) 0.066(2) 0.0471(19) 0.0081(17) 0.0014(14) -0.0042(16) B2 0.0284(15) 0.0239(14) 0.0296(15) 0.0016(12) -0.0016(12) -0.0012(12) C40 0.0340(15) 0.0398(16) 0.0385(16) 0.0103(13) -0.0063(12) 0.0038(13) C53 0.0288(14) 0.0400(15) 0.0315(14) 0.0077(12) -0.0028(11) 0.0060(12) C2 0.0245(13) 0.0417(16) 0.0386(16) -0.0036(13) -0.0046(11) 0.0002(12) C66 0.0304(15) 0.0490(18) 0.0418(17) 0.0081(14) 0.0020(13) 0.0082(13) C31 0.063(2) 0.0337(16) 0.0433(18) 0.0140(14) -0.0035(16) 0.0010(15) C63 0.0469(17) 0.0275(14) 0.0346(15) -0.0015(12) 0.0021(13) -0.0033(13) C65 0.0399(17) 0.0499(19) 0.0442(18) 0.0031(15) -0.0016(14) -0.0146(15) C61 0.051(2) 0.069(2) 0.0356(17) 0.0024(16) -0.0112(15) -0.0076(18) C15 0.0518(19) 0.0263(14) 0.0414(16) -0.0068(12) 0.0011(14) 0.0097(13) C26 0.0390(17) 0.0388(17) 0.0536(19) -0.0194(15) 0.0034(14) -0.0014(14) C29 0.054(2) 0.070(2) 0.0301(16) -0.0020(16) 0.0042(15) -0.0078(18) C67 0.0489(18) 0.0344(16) 0.0365(16) 0.0028(12) 0.0001(14) 0.0104(14) C30 0.054(2) 0.055(2) 0.0326(16) 0.0000(14) -0.0062(14) 0.0018(16) C33 0.070(2) 0.051(2) 0.050(2) 0.0232(17) -0.0024(18) 0.0018(18) C24 0.0368(19) 0.105(4) 0.058(2) 0.020(2) 0.0000(17) 0.001(2) C19 0.064(2) 0.0424(19) 0.062(2) 0.0030(16) -0.0142(18) -0.0248(17) C20 0.093(3) 0.041(2) 0.059(2) -0.0092(17) -0.012(2) -0.013(2) C35 0.045(2) 0.047(2) 0.080(3) 0.0115(19) -0.0106(18) 0.0128(16) C21 0.074(3) 0.045(2) 0.091(3) 0.010(2) 0.001(2) -0.024(2) C32 0.074(3) 0.0393(19) 0.064(2) 0.0105(17) -0.004(2) -0.0152(18) C23 0.043(2) 0.066(3) 0.088(3) -0.010(2) 0.013(2) 0.0006(18) N1 0.0326(14) 0.0365(14) 0.0717(19) -0.0014(13) 0.0029(13) -0.0092(11) F1 0.077(4) 0.074(4) 0.104(5) -0.039(4) -0.070(4) 0.026(3) F2 0.093(4) 0.112(5) 0.060(3) -0.002(3) 0.008(3) -0.044(4) F3 0.058(3) 0.043(3) 0.044(3) -0.015(2) -0.014(2) -0.006(2) F1A 0.114(4) 0.072(3) 0.0274(19) -0.0005(18) -0.032(2) 0.032(3) F2A 0.064(3) 0.041(2) 0.041(2) -0.0174(18) -0.0178(18) 0.0141(19) F3A 0.091(4) 0.127(4) 0.062(3) -0.004(3) 0.002(3) -0.064(3) F4 0.129(11) 0.060(6) 0.065(5) 0.000(3) -0.031(5) 0.051(6) F5 0.025(3) 0.043(4) 0.135(9) -0.003(5) 0.000(4) 0.011(3) F6 0.046(5) 0.037(6) 0.164(15) -0.032(7) -0.021(6) -0.005(5) F4A 0.108(6) 0.035(2) 0.087(3) 0.0206(19) 0.016(3) 0.018(3) F5A 0.100(5) 0.058(5) 0.196(10) -0.063(5) 0.087(6) -0.020(4) F6A 0.092(6) 0.045(4) 0.093(4) -0.031(3) -0.052(4) 0.037(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 N1 2.280(3) . ? Fe1 P1 2.4247(10) . ? Fe1 B1 2.433(3) . ? Fe1 P2 2.4335(9) . ? Fe1 P3 2.4891(10) . ? P2 C7 1.803(3) . ? P2 C28 1.854(3) . ? P2 C25 1.871(3) . ? P3 C13 1.819(3) . ? P3 C31 1.856(3) . ? P3 C34 1.865(3) . ? P1 C1 1.817(3) . ? P1 C22 1.850(4) . ? P1 C19 1.851(4) . ? F16 C66 1.332(4) . ? F9 C63 1.339(4) . ? F8 C63 1.336(4) . ? F13 C65 1.344(4) . ? F23 C68 1.327(4) . ? F22 C68 1.332(4) . ? F15 C65 1.339(4) . ? F19 C67 1.325(4) . ? F7 C63 1.340(4) . ? F12 C64 1.331(4) . ? C41 C40 1.383(4) . ? C41 C42 1.388(4) . ? C41 C62 1.499(4) . ? F17 C66 1.338(4) . ? F21 C67 1.322(4) . ? C45 C46 1.392(4) . ? C45 C44 1.396(4) . ? C45 C63 1.490(4) . ? C44 C43 1.404(4) . ? C48 C47 1.400(4) . ? C48 C43 1.404(4) . ? F11 C64 1.336(4) . ? F24 C68 1.340(4) . ? C37 C38 1.399(4) . ? C37 C42 1.402(4) . ? C37 B2 1.636(4) . ? C49 C50 1.400(4) . ? C49 C54 1.402(4) . ? C49 B2 1.645(4) . ? C11 C10 1.394(4) . ? C11 C12 1.408(4) . ? C68 C59 1.497(4) . ? F20 C67 1.322(4) . ? F10 C64 1.339(4) . ? C25 C27 1.523(4) . ? C25 C26 1.531(4) . ? C43 B2 1.645(4) . ? F14 C65 1.324(4) . ? C17 C16 1.386(4) . ? C17 C18 1.410(4) . ? C8 C9 1.379(4) . ? C8 C7 1.395(4) . ? C55 C56 1.394(4) . ? C55 C60 1.401(4) . ? C55 B2 1.644(4) . ? C1 C2 1.400(4) . ? C1 C6 1.404(4) . ? C58 C57 1.384(5) . ? C58 C59 1.385(4) . ? F18 C66 1.339(4) . ? C50 C51 1.392(4) . ? C60 C59 1.392(4) . ? C5 C4 1.386(4) . ? C5 C6 1.401(4) . ? C52 C51 1.377(5) . ? C52 C53 1.391(5) . ? C13 C14 1.402(4) . ? C13 C18 1.413(4) . ? C57 C56 1.400(4) . ? C57 C67 1.495(4) . ? C7 C12 1.409(4) . ? C64 C47 1.501(4) . ? C54 C53 1.398(4) . ? C18 B1 1.617(4) . ? C14 C15 1.381(4) . ? C16 C15 1.387(4) . ? C28 C30 1.529(5) . ? C28 C29 1.536(5) . ? C51 C65 1.498(5) . ? C4 C3 1.379(5) . ? C36 C34 1.520(5) . ? C10 C9 1.383(5) . ? C38 C39 1.394(4) . ? C34 C35 1.539(5) . ? C6 B1 1.612(4) . ? C12 B1 1.610(4) . ? C62 F6 1.250(17) . ? C62 F5 1.257(11) . ? C62 F4 1.266(8) . ? C62 F6A 1.306(10) . ? C62 F5A 1.354(8) . ? C62 F4A 1.413(6) . ? C47 C46 1.374(5) . ? C39 C40 1.383(5) . ? C39 C61 1.491(5) . ? C3 C2 1.384(5) . ? C22 C23 1.493(6) . ? C22 C24 1.515(5) . ? C53 C66 1.490(4) . ? C31 C32 1.510(6) . ? C31 C33 1.531(5) . ? C61 F2 1.166(9) . ? C61 F3A 1.183(6) . ? C61 F1A 1.383(6) . ? C61 F1 1.394(7) . ? C61 F2A 1.417(6) . ? C61 F3 1.471(7) . ? C19 C20 1.496(6) . ? C19 C21 1.547(5) . ? F4 F5 1.21(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 N1 Fe1 P1 97.82(8) . . ? N1 Fe1 B1 175.64(11) . . ? P1 Fe1 B1 77.82(8) . . ? N1 Fe1 P2 102.19(8) . . ? P1 Fe1 P2 112.31(3) . . ? B1 Fe1 P2 79.54(8) . . ? N1 Fe1 P3 103.06(8) . . ? P1 Fe1 P3 126.04(3) . . ? B1 Fe1 P3 79.87(8) . . ? P2 Fe1 P3 110.91(3) . . ? C7 P2 C28 106.77(14) . . ? C7 P2 C25 103.82(13) . . ? C28 P2 C25 102.36(15) . . ? C7 P2 Fe1 102.24(9) . . ? C28 P2 Fe1 112.64(11) . . ? C25 P2 Fe1 127.33(10) . . ? C13 P3 C31 105.22(15) . . ? C13 P3 C34 107.11(14) . . ? C31 P3 C34 101.15(16) . . ? C13 P3 Fe1 98.58(9) . . ? C31 P3 Fe1 111.05(13) . . ? C34 P3 Fe1 131.40(11) . . ? C1 P1 C22 113.23(16) . . ? C1 P1 C19 102.94(15) . . ? C22 P1 C19 99.53(19) . . ? C1 P1 Fe1 107.29(9) . . ? C22 P1 Fe1 108.43(12) . . ? C19 P1 Fe1 125.37(14) . . ? C40 C41 C42 121.1(3) . . ? C40 C41 C62 119.0(3) . . ? C42 C41 C62 119.9(3) . . ? C46 C45 C44 120.4(3) . . ? C46 C45 C63 118.5(3) . . ? C44 C45 C63 121.1(3) . . ? C45 C44 C43 122.0(3) . . ? C47 C48 C43 122.0(3) . . ? C38 C37 C42 115.4(2) . . ? C38 C37 B2 123.4(2) . . ? C42 C37 B2 120.9(2) . . ? C50 C49 C54 115.7(3) . . ? C50 C49 B2 121.1(2) . . ? C54 C49 B2 123.2(2) . . ? C10 C11 C12 121.8(3) . . ? F23 C68 F22 106.8(3) . . ? F23 C68 F24 106.5(3) . . ? F22 C68 F24 105.4(3) . . ? F23 C68 C59 113.0(3) . . ? F22 C68 C59 113.0(3) . . ? F24 C68 C59 111.6(3) . . ? C27 C25 C26 109.2(3) . . ? C27 C25 P2 111.30(19) . . ? C26 C25 P2 113.6(2) . . ? C48 C43 C44 116.1(3) . . ? C48 C43 B2 120.7(3) . . ? C44 C43 B2 122.7(2) . . ? C16 C17 C18 122.6(3) . . ? C9 C8 C7 120.8(3) . . ? C56 C55 C60 115.8(3) . . ? C56 C55 B2 120.3(2) . . ? C60 C55 B2 123.2(2) . . ? C2 C1 C6 120.8(3) . . ? C2 C1 P1 124.6(2) . . ? C6 C1 P1 114.6(2) . . ? C57 C58 C59 117.8(3) . . ? C51 C50 C49 122.1(3) . . ? C59 C60 C55 122.0(3) . . ? C4 C5 C6 122.0(3) . . ? C51 C52 C53 118.3(3) . . ? C14 C13 C18 121.1(3) . . ? C14 C13 P3 122.1(2) . . ? C18 C13 P3 116.7(2) . . ? C58 C57 C56 120.8(3) . . ? C58 C57 C67 121.0(3) . . ? C56 C57 C67 118.2(3) . . ? C8 C7 C12 121.2(3) . . ? C8 C7 P2 123.2(2) . . ? C12 C7 P2 115.5(2) . . ? F12 C64 F11 106.1(3) . . ? F12 C64 F10 106.2(3) . . ? F11 C64 F10 106.9(3) . . ? F12 C64 C47 112.1(3) . . ? F11 C64 C47 112.4(3) . . ? F10 C64 C47 112.6(3) . . ? C55 C56 C57 122.2(3) . . ? C53 C54 C49 122.4(3) . . ? C17 C18 C13 116.2(2) . . ? C17 C18 B1 119.4(2) . . ? C13 C18 B1 124.4(2) . . ? C15 C14 C13 120.7(3) . . ? C41 C42 C37 122.3(3) . . ? C17 C16 C15 119.9(3) . . ? C30 C28 C29 112.6(3) . . ? C30 C28 P2 110.9(2) . . ? C29 C28 P2 109.7(2) . . ? C52 C51 C50 121.3(3) . . ? C52 C51 C65 120.5(3) . . ? C50 C51 C65 118.0(3) . . ? C3 C4 C5 120.1(3) . . ? C9 C10 C11 120.2(3) . . ? C39 C38 C37 122.4(3) . . ? C36 C34 C35 108.4(3) . . ? C36 C34 P3 112.1(2) . . ? C35 C34 P3 113.6(3) . . ? C5 C6 C1 117.0(2) . . ? C5 C6 B1 120.2(2) . . ? C1 C6 B1 122.8(2) . . ? C8 C9 C10 119.4(3) . . ? C11 C12 C7 116.5(3) . . ? C11 C12 B1 118.9(2) . . ? C7 C12 B1 124.5(2) . . ? C12 B1 C6 113.3(2) . . ? C12 B1 C18 115.0(2) . . ? C6 B1 C18 112.9(2) . . ? C12 B1 Fe1 104.14(18) . . ? C6 B1 Fe1 109.07(19) . . ? C18 B1 Fe1 101.19(18) . . ? F6 C62 F5 121.8(14) . . ? F6 C62 F4 112.9(12) . . ? F5 C62 F4 57.5(16) . . ? F6 C62 F6A 15.4(16) . . ? F5 C62 F6A 116.3(10) . . ? F4 C62 F6A 123.8(9) . . ? F6 C62 F5A 106.0(14) . . ? F5 C62 F5A 32.5(7) . . ? F4 C62 F5A 89.3(18) . . ? F6A C62 F5A 94.3(11) . . ? F6 C62 F4A 86.7(12) . . ? F5 C62 F4A 96.2(9) . . ? F4 C62 F4A 39.6(9) . . ? F6A C62 F4A 101.8(7) . . ? F5A C62 F4A 126.0(11) . . ? F6 C62 C41 117.6(11) . . ? F5 C62 C41 115.9(6) . . ? F4 C62 C41 116.7(5) . . ? F6A C62 C41 114.3(7) . . ? F5A C62 C41 109.9(5) . . ? F4A C62 C41 109.3(4) . . ? C46 C47 C48 120.7(3) . . ? C46 C47 C64 121.7(3) . . ? C48 C47 C64 117.6(3) . . ? C58 C59 C60 121.2(3) . . ? C58 C59 C68 119.1(3) . . ? C60 C59 C68 119.7(3) . . ? C40 C39 C38 120.7(3) . . ? C40 C39 C61 120.0(3) . . ? C38 C39 C61 119.3(3) . . ? C4 C3 C2 119.6(3) . . ? C47 C46 C45 118.9(3) . . ? C23 C22 C24 108.9(4) . . ? C23 C22 P1 113.2(3) . . ? C24 C22 P1 117.3(3) . . ? C37 B2 C55 114.7(2) . . ? C37 B2 C49 105.8(2) . . ? C55 B2 C49 111.6(2) . . ? C37 B2 C43 112.2(2) . . ? C55 B2 C43 101.6(2) . . ? C49 B2 C43 111.1(2) . . ? C41 C40 C39 118.0(3) . . ? C52 C53 C54 120.3(3) . . ? C52 C53 C66 120.7(3) . . ? C54 C53 C66 119.1(3) . . ? C3 C2 C1 120.4(3) . . ? F16 C66 F17 105.4(3) . . ? F16 C66 F18 105.9(3) . . ? F17 C66 F18 105.8(3) . . ? F16 C66 C53 113.3(2) . . ? F17 C66 C53 112.8(3) . . ? F18 C66 C53 113.0(3) . . ? C32 C31 C33 111.5(3) . . ? C32 C31 P3 112.1(2) . . ? C33 C31 P3 110.8(3) . . ? F8 C63 F9 105.5(3) . . ? F8 C63 F7 106.5(3) . . ? F9 C63 F7 105.8(3) . . ? F8 C63 C45 113.8(2) . . ? F9 C63 C45 112.2(3) . . ? F7 C63 C45 112.4(3) . . ? F14 C65 F15 106.5(3) . . ? F14 C65 F13 106.9(3) . . ? F15 C65 F13 105.5(3) . . ? F14 C65 C51 113.3(3) . . ? F15 C65 C51 110.9(3) . . ? F13 C65 C51 113.2(3) . . ? F2 C61 F3A 120.3(6) . . ? F2 C61 F1A 66.5(6) . . ? F3A C61 F1A 111.0(6) . . ? F2 C61 F1 117.0(7) . . ? F3A C61 F1 54.0(5) . . ? F1A C61 F1 63.1(4) . . ? F2 C61 F2A 28.6(6) . . ? F3A C61 F2A 110.6(6) . . ? F1A C61 F2A 95.1(4) . . ? F1 C61 F2A 136.3(4) . . ? F2 C61 F3 102.4(6) . . ? F3A C61 F3 37.0(5) . . ? F1A C61 F3 137.4(4) . . ? F1 C61 F3 90.8(4) . . ? F2A C61 F3 80.9(4) . . ? F2 C61 C39 119.5(5) . . ? F3A C61 C39 116.6(4) . . ? F1A C61 C39 110.2(4) . . ? F1 C61 C39 111.8(4) . . ? F2A C61 C39 111.3(3) . . ? F3 C61 C39 110.6(3) . . ? C14 C15 C16 119.6(3) . . ? F20 C67 F21 107.5(3) . . ? F20 C67 F19 105.6(3) . . ? F21 C67 F19 105.2(3) . . ? F20 C67 C57 111.9(3) . . ? F21 C67 C57 112.7(3) . . ? F19 C67 C57 113.4(3) . . ? C20 C19 C21 111.9(4) . . ? C20 C19 P1 112.1(3) . . ? C21 C19 P1 112.2(3) . . ? F5 F4 C62 60.9(8) . . ? F4 F5 C62 61.6(11) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.741 _refine_diff_density_min -1.346 _refine_diff_density_rms 0.110 data_(TPB)Fe(NH2)_(5) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H56 B Fe N P3' _chemical_formula_weight 662.39 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' 'B' 'B' 0.0013 0.0007 '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' 'P' 'P' 0.1023 0.0942 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9229(9) _cell_length_b 11.2493(13) _cell_length_c 16.5084(15) _cell_angle_alpha 77.268(7) _cell_angle_beta 84.862(5) _cell_angle_gamma 61.117(4) _cell_volume 1732.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8715 _exptl_absorpt_correction_T_max 0.9134 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52847 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8561 _reflns_number_gt 6447 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0259P)^2^+5.8225P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8561 _refine_ls_number_parameters 397 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _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 Fe1 Fe 0.85565(5) 0.22752(5) 0.31569(3) 0.01097(11) Uani 1 1 d . . . P2 P 0.82041(8) 0.45954(8) 0.28942(5) 0.01204(17) Uani 1 1 d . . . P1 P 0.63606(8) 0.24405(8) 0.27912(5) 0.01157(17) Uani 1 1 d . . . P3 P 1.07553(8) 0.07249(8) 0.27303(5) 0.01111(16) Uani 1 1 d . . . C13 C 1.1195(3) 0.1429(3) 0.17188(19) 0.0122(6) Uani 1 1 d . . . C28 C 0.9532(3) 0.5214(3) 0.2704(2) 0.0160(7) Uani 1 1 d . . . H28 H 1.0177 0.4777 0.3200 0.019 Uiso 1 1 calc R . . C6 C 0.7909(3) 0.1863(3) 0.1406(2) 0.0118(6) Uani 1 1 d . . . C18 C 0.9998(3) 0.2493(3) 0.12658(19) 0.0118(6) Uani 1 1 d . . . C32 C 1.1011(4) -0.1871(3) 0.3504(2) 0.0166(7) Uani 1 1 d . . . H32A H 1.0797 -0.2611 0.3471 0.025 Uiso 1 1 calc R . . H32B H 1.0390 -0.1327 0.3901 0.025 Uiso 1 1 calc R . . H32C H 1.1986 -0.2281 0.3688 0.025 Uiso 1 1 calc R . . C17 C 1.0211(3) 0.3163(3) 0.0483(2) 0.0139(6) Uani 1 1 d . . . H17 H 0.9424 0.3865 0.0150 0.017 Uiso 1 1 calc R . . C27 C 0.5891(4) 0.5323(4) 0.3931(2) 0.0208(7) Uani 1 1 d . . . H27A H 0.6210 0.4336 0.4156 0.031 Uiso 1 1 calc R . . H27B H 0.5315 0.5620 0.3430 0.031 Uiso 1 1 calc R . . H27C H 0.5336 0.5863 0.4347 0.031 Uiso 1 1 calc R . . C14 C 1.2536(3) 0.1048(3) 0.1406(2) 0.0148(6) Uani 1 1 d . . . H14 H 1.3327 0.0297 0.1714 0.018 Uiso 1 1 calc R . . C11 C 0.6472(3) 0.5067(3) 0.0706(2) 0.0139(6) Uani 1 1 d . . . H11 H 0.6599 0.4491 0.0329 0.017 Uiso 1 1 calc R . . C8 C 0.6100(3) 0.6815(3) 0.1763(2) 0.0146(6) Uani 1 1 d . . . H8 H 0.5985 0.7414 0.2122 0.017 Uiso 1 1 calc R . . C1 C 0.6882(3) 0.1641(3) 0.1884(2) 0.0130(6) Uani 1 1 d . . . C22 C 0.4667(3) 0.4076(3) 0.2444(2) 0.0151(6) Uani 1 1 d . . . H22 H 0.4902 0.4853 0.2304 0.018 Uiso 1 1 calc R . . C25 C 0.7156(4) 0.5559(3) 0.3714(2) 0.0167(7) Uani 1 1 d . . . H25 H 0.6808 0.6571 0.3489 0.020 Uiso 1 1 calc R . . N1 N 0.8827(3) 0.1579(3) 0.43329(19) 0.0181(6) Uani 1 1 d D . . H1N H 0.833(4) 0.187(4) 0.4751(18) 0.022 Uiso 1 1 d D . . H2N H 0.964(3) 0.110(4) 0.459(2) 0.022 Uiso 1 1 d D . . C29 C 1.0417(4) 0.4770(4) 0.1946(2) 0.0185(7) Uani 1 1 d . . . H29A H 0.9801 0.5093 0.1459 0.028 Uiso 1 1 calc R . . H29B H 1.0968 0.3757 0.2050 0.028 Uiso 1 1 calc R . . H29C H 1.1047 0.5176 0.1842 0.028 Uiso 1 1 calc R . . C12 C 0.7317(3) 0.4491(3) 0.1429(2) 0.0121(6) Uani 1 1 d . . . C15 C 1.2710(3) 0.1767(3) 0.0647(2) 0.0152(6) Uani 1 1 d . . . H15 H 1.3623 0.1538 0.0444 0.018 Uiso 1 1 calc R . . C31 C 1.0793(3) -0.0922(3) 0.2642(2) 0.0146(6) Uani 1 1 d . . . H31 H 0.9831 -0.0647 0.2453 0.018 Uiso 1 1 calc R . . C19 C 0.5872(3) 0.1253(3) 0.3555(2) 0.0159(7) Uani 1 1 d . . . H19 H 0.5034 0.1278 0.3336 0.019 Uiso 1 1 calc R . . C36 C 1.3655(3) -0.0864(4) 0.3340(2) 0.0183(7) Uani 1 1 d . . . H36A H 1.4099 -0.0417 0.2938 0.027 Uiso 1 1 calc R . . H36B H 1.3624 -0.1590 0.3121 0.027 Uiso 1 1 calc R . . H36C H 1.4196 -0.1276 0.3864 0.027 Uiso 1 1 calc R . . B1 B 0.8458(4) 0.2848(4) 0.1636(2) 0.0115(7) Uani 1 1 d . . . C7 C 0.7116(3) 0.5408(3) 0.1953(2) 0.0123(6) Uani 1 1 d . . . C10 C 0.5454(3) 0.6455(3) 0.0525(2) 0.0156(6) Uani 1 1 d . . . H10 H 0.4886 0.6804 0.0037 0.019 Uiso 1 1 calc R . . C34 C 1.2160(3) 0.0221(3) 0.3496(2) 0.0148(6) Uani 1 1 d . . . H34 H 1.1884 -0.0199 0.4031 0.018 Uiso 1 1 calc R . . C33 C 1.1784(4) -0.1689(3) 0.1994(2) 0.0192(7) Uani 1 1 d . . . H33A H 1.2755 -0.2068 0.2176 0.029 Uiso 1 1 calc R . . H33B H 1.1613 -0.1041 0.1459 0.029 Uiso 1 1 calc R . . H33C H 1.1616 -0.2446 0.1934 0.029 Uiso 1 1 calc R . . C16 C 1.1550(3) 0.2820(3) 0.0184(2) 0.0158(7) Uani 1 1 d . . . H16 H 1.1667 0.3310 -0.0338 0.019 Uiso 1 1 calc R . . C21 C 0.5544(4) 0.1641(4) 0.4414(2) 0.0185(7) Uani 1 1 d . . . H21A H 0.5288 0.0992 0.4789 0.028 Uiso 1 1 calc R . . H21B H 0.4764 0.2586 0.4362 0.028 Uiso 1 1 calc R . . H21C H 0.6371 0.1593 0.4639 0.028 Uiso 1 1 calc R . . C5 C 0.8401(3) 0.1209(3) 0.0721(2) 0.0153(6) Uani 1 1 d . . . H5 H 0.9102 0.1330 0.0386 0.018 Uiso 1 1 calc R . . C35 C 1.2147(4) 0.1511(4) 0.3658(2) 0.0195(7) Uani 1 1 d . . . H35A H 1.2798 0.1245 0.4117 0.029 Uiso 1 1 calc R . . H35B H 1.1201 0.2157 0.3804 0.029 Uiso 1 1 calc R . . H35C H 1.2434 0.1961 0.3157 0.029 Uiso 1 1 calc R . . C2 C 0.6339(3) 0.0845(4) 0.1670(2) 0.0166(7) Uani 1 1 d . . . H2 H 0.5613 0.0745 0.1988 0.020 Uiso 1 1 calc R . . C26 C 0.8064(4) 0.5134(4) 0.4481(2) 0.0250(8) Uani 1 1 d . . . H26A H 0.7479 0.5573 0.4925 0.038 Uiso 1 1 calc R . . H26B H 0.8778 0.5433 0.4345 0.038 Uiso 1 1 calc R . . H26C H 0.8518 0.4124 0.4666 0.038 Uiso 1 1 calc R . . C24 C 0.3539(3) 0.4446(3) 0.3111(2) 0.0172(7) Uani 1 1 d . . . H24A H 0.2710 0.5315 0.2885 0.026 Uiso 1 1 calc R . . H24B H 0.3904 0.4556 0.3595 0.026 Uiso 1 1 calc R . . H24C H 0.3286 0.3702 0.3278 0.026 Uiso 1 1 calc R . . C9 C 0.5266(3) 0.7328(3) 0.1054(2) 0.0156(6) Uani 1 1 d . . . H9 H 0.4569 0.8274 0.0931 0.019 Uiso 1 1 calc R . . C3 C 0.6857(4) 0.0203(3) 0.0997(2) 0.0164(7) Uani 1 1 d . . . H3 H 0.6509 -0.0360 0.0863 0.020 Uiso 1 1 calc R . . C23 C 0.4042(3) 0.4071(4) 0.1652(2) 0.0190(7) Uani 1 1 d . . . H23A H 0.3727 0.3370 0.1770 0.028 Uiso 1 1 calc R . . H23B H 0.4754 0.3853 0.1223 0.028 Uiso 1 1 calc R . . H23C H 0.3246 0.4987 0.1456 0.028 Uiso 1 1 calc R . . C30 C 0.8897(4) 0.6789(4) 0.2595(3) 0.0241(8) Uani 1 1 d . . . H30A H 0.9641 0.7050 0.2481 0.036 Uiso 1 1 calc R . . H30B H 0.8422 0.7076 0.3104 0.036 Uiso 1 1 calc R . . H30C H 0.8221 0.7248 0.2129 0.036 Uiso 1 1 calc R . . C20 C 0.7087(4) -0.0232(4) 0.3672(2) 0.0225(8) Uani 1 1 d . . . H20A H 0.7902 -0.0273 0.3908 0.034 Uiso 1 1 calc R . . H20B H 0.7326 -0.0512 0.3133 0.034 Uiso 1 1 calc R . . H20C H 0.6809 -0.0861 0.4050 0.034 Uiso 1 1 calc R . . C4 C 0.7888(3) 0.0389(3) 0.0520(2) 0.0163(7) Uani 1 1 d . . . H4 H 0.8244 -0.0044 0.0056 0.020 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 0.0080(2) 0.0090(2) 0.0160(2) -0.00354(17) 0.00180(17) -0.00398(17) P2 0.0109(4) 0.0096(4) 0.0168(4) -0.0039(3) 0.0013(3) -0.0054(3) P1 0.0088(4) 0.0102(4) 0.0167(4) -0.0041(3) 0.0024(3) -0.0051(3) P3 0.0088(4) 0.0090(4) 0.0154(4) -0.0024(3) 0.0016(3) -0.0043(3) C13 0.0123(15) 0.0107(15) 0.0142(15) -0.0035(12) 0.0018(12) -0.0057(12) C28 0.0136(15) 0.0134(16) 0.0218(17) -0.0041(13) -0.0023(13) -0.0065(13) C6 0.0083(14) 0.0070(14) 0.0162(15) -0.0017(12) -0.0009(11) -0.0008(11) C18 0.0108(14) 0.0090(14) 0.0154(15) -0.0032(12) 0.0007(12) -0.0044(12) C32 0.0200(17) 0.0138(16) 0.0191(17) -0.0016(13) 0.0030(13) -0.0117(14) C17 0.0119(15) 0.0124(15) 0.0153(15) -0.0027(12) -0.0001(12) -0.0040(12) C27 0.0199(17) 0.0180(17) 0.0235(18) -0.0077(14) 0.0077(14) -0.0081(15) C14 0.0110(15) 0.0131(15) 0.0200(17) -0.0033(13) 0.0011(12) -0.0055(13) C11 0.0138(15) 0.0138(16) 0.0165(16) -0.0043(12) 0.0021(12) -0.0081(13) C8 0.0126(15) 0.0112(15) 0.0215(17) -0.0054(13) 0.0042(12) -0.0068(13) C1 0.0092(14) 0.0117(15) 0.0170(16) -0.0045(12) 0.0002(12) -0.0035(12) C22 0.0112(15) 0.0124(15) 0.0194(17) -0.0033(13) 0.0013(12) -0.0040(13) C25 0.0199(17) 0.0115(15) 0.0190(17) -0.0070(13) 0.0037(13) -0.0065(13) N1 0.0115(13) 0.0209(15) 0.0189(15) -0.0050(12) 0.0018(11) -0.0052(12) C29 0.0146(16) 0.0174(17) 0.0265(18) -0.0040(14) 0.0020(13) -0.0105(14) C12 0.0072(14) 0.0099(14) 0.0194(16) -0.0028(12) 0.0027(12) -0.0047(12) C15 0.0115(15) 0.0156(16) 0.0196(17) -0.0064(13) 0.0055(12) -0.0071(13) C31 0.0121(15) 0.0107(15) 0.0197(16) -0.0026(12) 0.0016(12) -0.0048(13) C19 0.0129(15) 0.0152(16) 0.0218(17) -0.0038(13) 0.0024(13) -0.0088(13) C36 0.0087(15) 0.0185(17) 0.0226(18) -0.0030(14) 0.0001(13) -0.0030(13) B1 0.0069(15) 0.0100(16) 0.0154(17) -0.0036(13) 0.0012(13) -0.0020(13) C7 0.0098(14) 0.0107(15) 0.0169(16) -0.0025(12) 0.0020(12) -0.0056(12) C10 0.0113(15) 0.0154(16) 0.0183(16) -0.0019(13) 0.0000(12) -0.0055(13) C34 0.0120(15) 0.0142(16) 0.0173(16) -0.0030(13) 0.0014(12) -0.0058(13) C33 0.0232(18) 0.0126(16) 0.0232(18) -0.0059(13) 0.0061(14) -0.0095(14) C16 0.0178(16) 0.0150(16) 0.0164(16) -0.0020(13) 0.0040(13) -0.0103(14) C21 0.0183(17) 0.0176(17) 0.0199(17) -0.0040(13) 0.0044(13) -0.0093(14) C5 0.0142(15) 0.0135(16) 0.0161(16) -0.0043(12) 0.0035(12) -0.0049(13) C35 0.0169(17) 0.0179(17) 0.0256(18) -0.0056(14) -0.0023(14) -0.0090(14) C2 0.0126(15) 0.0179(17) 0.0207(17) -0.0055(13) 0.0034(13) -0.0080(13) C26 0.030(2) 0.026(2) 0.0217(19) -0.0106(15) 0.0021(15) -0.0134(17) C24 0.0108(15) 0.0144(16) 0.0233(18) -0.0051(13) 0.0053(13) -0.0039(13) C9 0.0119(15) 0.0097(15) 0.0216(17) -0.0015(13) 0.0012(12) -0.0032(12) C3 0.0194(16) 0.0092(15) 0.0251(18) -0.0055(13) 0.0013(13) -0.0095(13) C23 0.0128(16) 0.0203(18) 0.0226(18) -0.0037(14) 0.0008(13) -0.0073(14) C30 0.0199(18) 0.0151(17) 0.042(2) -0.0112(16) 0.0053(16) -0.0109(15) C20 0.0240(18) 0.0137(17) 0.0252(19) -0.0013(14) 0.0056(15) -0.0075(15) C4 0.0179(16) 0.0140(16) 0.0182(16) -0.0067(13) 0.0023(13) -0.0073(13) _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 1.918(3) . ? Fe1 P3 2.3447(9) . ? Fe1 P2 2.3894(10) . ? Fe1 P1 2.4353(9) . ? Fe1 B1 2.449(4) . ? P2 C7 1.821(3) . ? P2 C28 1.866(3) . ? P2 C25 1.867(3) . ? P1 C1 1.823(3) . ? P1 C19 1.866(3) . ? P1 C22 1.890(3) . ? P3 C13 1.813(3) . ? P3 C34 1.862(3) . ? P3 C31 1.871(3) . ? C13 C14 1.396(4) . ? C13 C18 1.404(4) . ? C28 C29 1.531(5) . ? C28 C30 1.532(5) . ? C6 C1 1.403(4) . ? C6 C5 1.409(4) . ? C6 B1 1.614(5) . ? C18 C17 1.407(4) . ? C18 B1 1.623(5) . ? C32 C31 1.538(5) . ? C17 C16 1.393(4) . ? C27 C25 1.526(5) . ? C14 C15 1.387(5) . ? C11 C10 1.393(4) . ? C11 C12 1.406(4) . ? C8 C9 1.384(5) . ? C8 C7 1.408(4) . ? C1 C2 1.403(4) . ? C22 C23 1.531(5) . ? C22 C24 1.538(4) . ? C25 C26 1.522(5) . ? C12 C7 1.415(4) . ? C12 B1 1.630(5) . ? C15 C16 1.384(5) . ? C31 C33 1.535(4) . ? C19 C20 1.533(5) . ? C19 C21 1.537(5) . ? C36 C34 1.537(4) . ? C10 C9 1.387(5) . ? C34 C35 1.526(5) . ? C5 C4 1.393(5) . ? C2 C3 1.387(5) . ? C3 C4 1.389(5) . ? 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 P3 98.64(9) . . ? N1 Fe1 P2 107.36(10) . . ? P3 Fe1 P2 112.30(3) . . ? N1 Fe1 P1 106.70(9) . . ? P3 Fe1 P1 124.07(3) . . ? P2 Fe1 P1 106.36(3) . . ? N1 Fe1 B1 172.21(12) . . ? P3 Fe1 B1 74.28(8) . . ? P2 Fe1 B1 78.74(9) . . ? P1 Fe1 B1 75.51(8) . . ? C7 P2 C28 104.11(15) . . ? C7 P2 C25 106.41(15) . . ? C28 P2 C25 100.21(15) . . ? C7 P2 Fe1 102.84(10) . . ? C28 P2 Fe1 128.90(11) . . ? C25 P2 Fe1 112.54(11) . . ? C1 P1 C19 103.55(15) . . ? C1 P1 C22 103.69(15) . . ? C19 P1 C22 106.04(15) . . ? C1 P1 Fe1 100.56(10) . . ? C19 P1 Fe1 112.75(11) . . ? C22 P1 Fe1 127.20(11) . . ? C13 P3 C34 109.25(15) . . ? C13 P3 C31 106.70(15) . . ? C34 P3 C31 106.16(15) . . ? C13 P3 Fe1 111.98(11) . . ? C34 P3 Fe1 111.65(11) . . ? C31 P3 Fe1 110.82(10) . . ? C14 C13 C18 121.6(3) . . ? C14 C13 P3 126.7(3) . . ? C18 C13 P3 111.6(2) . . ? C29 C28 C30 108.4(3) . . ? C29 C28 P2 112.1(2) . . ? C30 C28 P2 113.4(2) . . ? C1 C6 C5 116.8(3) . . ? C1 C6 B1 120.5(3) . . ? C5 C6 B1 122.7(3) . . ? C13 C18 C17 116.9(3) . . ? C13 C18 B1 119.8(3) . . ? C17 C18 B1 123.3(3) . . ? C16 C17 C18 121.5(3) . . ? C15 C14 C13 119.9(3) . . ? C10 C11 C12 122.2(3) . . ? C9 C8 C7 120.2(3) . . ? C2 C1 C6 121.4(3) . . ? C2 C1 P1 124.1(2) . . ? C6 C1 P1 114.5(2) . . ? C23 C22 C24 109.4(3) . . ? C23 C22 P1 112.8(2) . . ? C24 C22 P1 114.9(2) . . ? C26 C25 C27 111.0(3) . . ? C26 C25 P2 110.5(2) . . ? C27 C25 P2 110.7(2) . . ? C11 C12 C7 116.5(3) . . ? C11 C12 B1 120.7(3) . . ? C7 C12 B1 122.9(3) . . ? C16 C15 C14 119.8(3) . . ? C33 C31 C32 112.5(3) . . ? C33 C31 P3 116.0(2) . . ? C32 C31 P3 110.4(2) . . ? C20 C19 C21 107.4(3) . . ? C20 C19 P1 109.7(2) . . ? C21 C19 P1 112.7(2) . . ? C6 B1 C18 111.5(3) . . ? C6 B1 C12 113.5(3) . . ? C18 B1 C12 114.3(3) . . ? C6 B1 Fe1 102.8(2) . . ? C18 B1 Fe1 110.7(2) . . ? C12 B1 Fe1 103.2(2) . . ? C8 C7 C12 121.3(3) . . ? C8 C7 P2 124.1(2) . . ? C12 C7 P2 114.5(2) . . ? C9 C10 C11 120.2(3) . . ? C35 C34 C36 110.6(3) . . ? C35 C34 P3 110.2(2) . . ? C36 C34 P3 118.4(2) . . ? C15 C16 C17 120.2(3) . . ? C4 C5 C6 121.9(3) . . ? C3 C2 C1 120.3(3) . . ? C8 C9 C10 119.6(3) . . ? C2 C3 C4 119.5(3) . . ? C3 C4 C5 120.1(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.541 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.096 data_(TPB)Fe(OH)_(6) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H56 B Fe N O P3' _chemical_formula_weight 678.39 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' 'B' 'B' 0.0013 0.0007 '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' 'P' 'P' 0.1023 0.0942 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9554(4) _cell_length_b 11.3311(4) _cell_length_c 16.6454(7) _cell_angle_alpha 77.466(2) _cell_angle_beta 78.105(2) _cell_angle_gamma 61.338(2) _cell_volume 1757.30(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 10.00 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 726 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.0661 _exptl_absorpt_correction_T_max 0.9056 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 142106 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 37.78 _reflns_number_total 18846 _reflns_number_gt 15096 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0361P)^2^+0.4967P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18846 _refine_ls_number_parameters 382 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Fe1 Fe 0.396905(12) 0.180273(11) 0.318876(7) 0.00992(3) Uani 1 1 d . . . P2 P 0.56109(2) 0.01446(2) 0.230903(13) 0.01086(4) Uani 1 1 d . . . P3 P 0.17382(2) 0.18870(2) 0.330854(13) 0.01113(4) Uani 1 1 d . . . P1 P 0.41142(2) 0.38806(2) 0.310151(13) 0.01149(4) Uani 1 1 d . . . C13 C 0.13938(8) 0.19674(8) 0.22758(5) 0.01282(13) Uani 1 1 d . . . C14 C 0.21364(8) 0.25092(8) 0.16452(5) 0.01225(12) Uani 1 1 d . . . C7 C 0.46656(8) 0.24715(8) 0.12025(5) 0.01078(12) Uani 1 1 d . . . C1 C 0.28560(8) 0.51481(8) 0.24252(5) 0.01128(12) Uani 1 1 d . . . C2 C 0.25033(8) 0.46109(8) 0.18714(5) 0.01058(12) Uani 1 1 d . . . C8 C 0.58250(8) 0.11889(8) 0.13528(5) 0.01175(12) Uani 1 1 d . . . C28 C 0.73357(8) -0.07252(8) 0.27187(5) 0.01446(14) Uani 1 1 d . . . H28A H 0.8068 -0.1222 0.2279 0.017 Uiso 1 1 calc R . . C25 C 0.55462(9) -0.12976(8) 0.19719(5) 0.01463(14) Uani 1 1 d . . . H25A H 0.5308 -0.1834 0.2484 0.018 Uiso 1 1 calc R . . C12 C 0.48159(9) 0.32996(9) 0.04635(5) 0.01384(13) Uani 1 1 d . . . H12A H 0.4053 0.4165 0.0335 0.017 Uiso 1 1 calc R . . O1 O 0.45054(9) 0.10054(8) 0.42624(5) 0.02304(14) Uani 1 1 d D . . H1O H 0.4661(16) 0.0266(13) 0.4500(9) 0.028 Uiso 1 1 d D . . B1 B 0.32189(9) 0.29870(9) 0.18314(5) 0.01084(13) Uani 1 1 d . . . C19 C 0.57454(9) 0.40852(8) 0.27738(6) 0.01457(14) Uani 1 1 d . . . H19A H 0.6477 0.3346 0.3113 0.017 Uiso 1 1 calc R . . C6 C 0.22217(9) 0.65455(9) 0.24664(6) 0.01535(14) Uani 1 1 d . . . H6A H 0.2481 0.6873 0.2849 0.018 Uiso 1 1 calc R . . C3 C 0.14887(9) 0.55632(9) 0.13519(5) 0.01437(13) Uani 1 1 d . . . H3A H 0.1227 0.5249 0.0963 0.017 Uiso 1 1 calc R . . C31 C 0.00814(8) 0.32747(9) 0.37453(5) 0.01360(13) Uani 1 1 d . . . H31A H 0.0260 0.3402 0.4278 0.016 Uiso 1 1 calc R . . C30 C 0.77170(9) 0.02887(9) 0.29373(6) 0.01835(16) Uani 1 1 d . . . H30A H 0.8629 -0.0201 0.3150 0.028 Uiso 1 1 calc R . . H30B H 0.7002 0.0797 0.3362 0.028 Uiso 1 1 calc R . . H30C H 0.7765 0.0921 0.2440 0.028 Uiso 1 1 calc R . . C10 C 0.71778(9) 0.16331(9) 0.00869(6) 0.01734(15) Uani 1 1 d . . . H10A H 0.8021 0.1357 -0.0283 0.021 Uiso 1 1 calc R . . C4 C 0.08596(9) 0.69494(9) 0.13924(6) 0.01627(15) Uani 1 1 d . . . H4A H 0.0178 0.7561 0.1034 0.020 Uiso 1 1 calc R . . C34 C 0.16324(9) 0.03622(9) 0.39454(6) 0.01573(14) Uani 1 1 d . . . H34A H 0.0724 0.0403 0.3882 0.019 Uiso 1 1 calc R . . C18 C 0.04806(9) 0.15450(10) 0.20970(6) 0.01830(16) Uani 1 1 d . . . H18A H 0.0007 0.1169 0.2535 0.022 Uiso 1 1 calc R . . C9 C 0.70656(9) 0.07821(9) 0.08046(6) 0.01562(14) Uani 1 1 d . . . H9A H 0.7835 -0.0082 0.0925 0.019 Uiso 1 1 calc R . . C33 C -0.02944(9) 0.46146(9) 0.31633(6) 0.01760(15) Uani 1 1 d . . . H33A H -0.1161 0.5328 0.3402 0.026 Uiso 1 1 calc R . . H33B H -0.0429 0.4509 0.2624 0.026 Uiso 1 1 calc R . . H33C H 0.0466 0.4866 0.3092 0.026 Uiso 1 1 calc R . . C5 C 0.12172(9) 0.74502(9) 0.19513(6) 0.01621(14) Uani 1 1 d . . . H5A H 0.0780 0.8397 0.1980 0.019 Uiso 1 1 calc R . . C36 C 0.16409(11) 0.03788(10) 0.48620(6) 0.02174(18) Uani 1 1 d . . . H36A H 0.1586 -0.0426 0.5193 0.033 Uiso 1 1 calc R . . H36B H 0.0834 0.1198 0.5045 0.033 Uiso 1 1 calc R . . H36C H 0.2508 0.0375 0.4935 0.033 Uiso 1 1 calc R . . C32 C -0.11912(9) 0.29904(10) 0.39354(7) 0.02136(18) Uani 1 1 d . . . H32A H -0.2006 0.3764 0.4161 0.032 Uiso 1 1 calc R . . H32B H -0.0990 0.2171 0.4342 0.032 Uiso 1 1 calc R . . H32C H -0.1391 0.2855 0.3424 0.032 Uiso 1 1 calc R . . C21 C 0.55981(11) 0.54367(10) 0.29260(6) 0.01988(16) Uani 1 1 d . . . H21A H 0.6491 0.5472 0.2741 0.030 Uiso 1 1 calc R . . H21B H 0.5343 0.5513 0.3519 0.030 Uiso 1 1 calc R . . H21C H 0.4867 0.6190 0.2616 0.030 Uiso 1 1 calc R . . C29 C 0.73237(10) -0.17642(9) 0.34791(6) 0.01968(16) Uani 1 1 d . . . H29A H 0.8237 -0.2216 0.3689 0.030 Uiso 1 1 calc R . . H29B H 0.7136 -0.2442 0.3323 0.030 Uiso 1 1 calc R . . H29C H 0.6591 -0.1299 0.3911 0.030 Uiso 1 1 calc R . . C20 C 0.63014(9) 0.39094(10) 0.18651(6) 0.01794(15) Uani 1 1 d . . . H20A H 0.7155 0.4024 0.1722 0.027 Uiso 1 1 calc R . . H20B H 0.5592 0.4592 0.1513 0.027 Uiso 1 1 calc R . . H20C H 0.6514 0.2999 0.1777 0.027 Uiso 1 1 calc R . . C15 C 0.18897(10) 0.26263(11) 0.08297(6) 0.01838(16) Uani 1 1 d . . . H15A H 0.2367 0.2990 0.0387 0.022 Uiso 1 1 calc R . . C11 C 0.60422(9) 0.28948(9) -0.00851(5) 0.01581(14) Uani 1 1 d . . . H11A H 0.6105 0.3481 -0.0578 0.019 Uiso 1 1 calc R . . C35 C 0.28223(10) -0.09566(9) 0.36624(7) 0.02110(17) Uani 1 1 d . . . H35A H 0.2732 -0.1733 0.4012 0.032 Uiso 1 1 calc R . . H35B H 0.3724 -0.1009 0.3710 0.032 Uiso 1 1 calc R . . H35C H 0.2774 -0.0973 0.3084 0.032 Uiso 1 1 calc R . . C23 C 0.21445(11) 0.44245(11) 0.45073(6) 0.02246(18) Uani 1 1 d . . . H23A H 0.1846 0.4737 0.5052 0.034 Uiso 1 1 calc R . . H23B H 0.2278 0.3492 0.4567 0.034 Uiso 1 1 calc R . . H23C H 0.1425 0.5018 0.4139 0.034 Uiso 1 1 calc R . . C26 C 0.43864(10) -0.07911(10) 0.14214(7) 0.02088(17) Uani 1 1 d . . . H26A H 0.4384 -0.1569 0.1257 0.031 Uiso 1 1 calc R . . H26B H 0.4553 -0.0214 0.0926 0.031 Uiso 1 1 calc R . . H26C H 0.3478 -0.0265 0.1729 0.031 Uiso 1 1 calc R . . C27 C 0.69284(10) -0.22814(10) 0.15316(6) 0.02032(17) Uani 1 1 d . . . H27A H 0.6802 -0.2999 0.1377 0.030 Uiso 1 1 calc R . . H27B H 0.7656 -0.2687 0.1904 0.030 Uiso 1 1 calc R . . H27C H 0.7211 -0.1787 0.1032 0.030 Uiso 1 1 calc R . . C24 C 0.46544(12) 0.35906(11) 0.47196(6) 0.02223(18) Uani 1 1 d . . . H24A H 0.4330 0.3911 0.5262 0.033 Uiso 1 1 calc R . . H24B H 0.5519 0.3659 0.4485 0.033 Uiso 1 1 calc R . . H24C H 0.4835 0.2642 0.4783 0.033 Uiso 1 1 calc R . . C22 C 0.35258(10) 0.44670(9) 0.41376(6) 0.01690(15) Uani 1 1 d . . . H22A H 0.3368 0.5427 0.4069 0.020 Uiso 1 1 calc R . . C16 C 0.09666(11) 0.22251(12) 0.06509(6) 0.02375(19) Uani 1 1 d . . . H16A H 0.0815 0.2330 0.0092 0.029 Uiso 1 1 calc R . . C17 C 0.02640(10) 0.16720(12) 0.12851(7) 0.02334(19) Uani 1 1 d . . . H17A H -0.0355 0.1386 0.1163 0.028 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 0.01152(5) 0.00914(5) 0.01035(5) -0.00175(3) -0.00134(3) -0.00551(4) P2 0.01000(8) 0.00963(8) 0.01237(8) -0.00129(6) 0.00011(6) -0.00465(6) P3 0.00999(8) 0.01108(8) 0.01269(8) -0.00270(6) 0.00082(6) -0.00550(6) P1 0.01485(9) 0.01002(8) 0.01199(8) -0.00107(6) -0.00489(7) -0.00646(7) C13 0.0119(3) 0.0138(3) 0.0149(3) -0.0054(3) 0.0004(2) -0.0069(2) C14 0.0124(3) 0.0139(3) 0.0123(3) -0.0045(2) -0.0007(2) -0.0066(2) C7 0.0123(3) 0.0115(3) 0.0105(3) -0.0022(2) -0.0014(2) -0.0066(2) C1 0.0113(3) 0.0107(3) 0.0120(3) -0.0019(2) -0.0020(2) -0.0047(2) C2 0.0094(3) 0.0118(3) 0.0105(3) -0.0020(2) -0.0009(2) -0.0048(2) C8 0.0113(3) 0.0117(3) 0.0125(3) -0.0018(2) 0.0001(2) -0.0060(2) C28 0.0114(3) 0.0121(3) 0.0171(3) -0.0011(3) -0.0015(3) -0.0035(2) C25 0.0155(3) 0.0115(3) 0.0170(3) -0.0049(3) 0.0023(3) -0.0067(3) C12 0.0156(3) 0.0137(3) 0.0119(3) -0.0009(2) -0.0016(3) -0.0068(3) O1 0.0344(4) 0.0190(3) 0.0160(3) 0.0028(2) -0.0091(3) -0.0122(3) B1 0.0116(3) 0.0117(3) 0.0103(3) -0.0019(3) -0.0019(3) -0.0058(3) C19 0.0159(3) 0.0122(3) 0.0190(4) -0.0002(3) -0.0076(3) -0.0078(3) C6 0.0172(3) 0.0116(3) 0.0172(3) -0.0032(3) -0.0036(3) -0.0054(3) C3 0.0134(3) 0.0147(3) 0.0146(3) -0.0014(3) -0.0043(3) -0.0053(3) C31 0.0107(3) 0.0147(3) 0.0161(3) -0.0052(3) 0.0016(2) -0.0063(2) C30 0.0150(3) 0.0173(4) 0.0239(4) 0.0005(3) -0.0065(3) -0.0080(3) C10 0.0158(3) 0.0183(4) 0.0157(3) -0.0019(3) 0.0033(3) -0.0083(3) C4 0.0125(3) 0.0149(3) 0.0179(4) 0.0005(3) -0.0042(3) -0.0036(3) C34 0.0157(3) 0.0139(3) 0.0181(4) -0.0024(3) 0.0026(3) -0.0089(3) C18 0.0156(3) 0.0231(4) 0.0222(4) -0.0094(3) 0.0020(3) -0.0127(3) C9 0.0132(3) 0.0139(3) 0.0169(3) -0.0016(3) 0.0023(3) -0.0057(3) C33 0.0145(3) 0.0141(3) 0.0201(4) -0.0033(3) 0.0010(3) -0.0040(3) C5 0.0153(3) 0.0111(3) 0.0185(4) -0.0025(3) -0.0017(3) -0.0030(3) C36 0.0271(4) 0.0217(4) 0.0164(4) 0.0003(3) 0.0031(3) -0.0145(4) C32 0.0120(3) 0.0215(4) 0.0324(5) -0.0096(4) 0.0042(3) -0.0093(3) C21 0.0250(4) 0.0170(4) 0.0245(4) -0.0027(3) -0.0063(3) -0.0137(3) C29 0.0206(4) 0.0125(3) 0.0212(4) 0.0015(3) -0.0047(3) -0.0045(3) C20 0.0165(3) 0.0179(4) 0.0219(4) -0.0038(3) -0.0022(3) -0.0095(3) C15 0.0191(4) 0.0282(4) 0.0137(3) -0.0064(3) -0.0010(3) -0.0142(3) C11 0.0185(3) 0.0165(3) 0.0126(3) -0.0010(3) 0.0003(3) -0.0093(3) C35 0.0225(4) 0.0133(3) 0.0249(4) -0.0028(3) 0.0034(3) -0.0084(3) C23 0.0253(4) 0.0284(5) 0.0178(4) -0.0098(3) 0.0009(3) -0.0142(4) C26 0.0215(4) 0.0196(4) 0.0243(4) -0.0095(3) -0.0033(3) -0.0086(3) C27 0.0195(4) 0.0158(4) 0.0237(4) -0.0089(3) 0.0055(3) -0.0071(3) C24 0.0314(5) 0.0267(5) 0.0161(4) -0.0007(3) -0.0099(3) -0.0174(4) C22 0.0239(4) 0.0170(4) 0.0145(3) -0.0042(3) -0.0045(3) -0.0113(3) C16 0.0224(4) 0.0394(6) 0.0186(4) -0.0119(4) -0.0018(3) -0.0184(4) C17 0.0196(4) 0.0354(5) 0.0257(5) -0.0150(4) 0.0006(3) -0.0179(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 O1 1.8916(7) . ? Fe1 P3 2.3676(3) . ? Fe1 P2 2.4034(3) . ? Fe1 P1 2.4065(2) . ? Fe1 B1 2.4438(9) . ? P2 C8 1.8121(8) . ? P2 C28 1.8601(9) . ? P2 C25 1.8752(9) . ? P3 C13 1.8090(9) . ? P3 C34 1.8624(9) . ? P3 C31 1.8735(8) . ? P1 C1 1.8080(8) . ? P1 C22 1.8600(9) . ? P1 C19 1.8669(9) . ? C13 C18 1.4009(12) . ? C13 C14 1.4099(11) . ? C14 C15 1.4041(12) . ? C14 B1 1.6236(12) . ? C7 C12 1.4087(11) . ? C7 C8 1.4109(11) . ? C7 B1 1.6255(11) . ? C1 C6 1.4025(11) . ? C1 C2 1.4091(11) . ? C2 C3 1.4100(11) . ? C2 B1 1.6287(12) . ? C8 C9 1.4010(11) . ? C28 C30 1.5269(13) . ? C28 C29 1.5328(12) . ? C25 C26 1.5282(14) . ? C25 C27 1.5331(12) . ? C12 C11 1.3907(12) . ? C19 C20 1.5275(13) . ? C19 C21 1.5329(12) . ? C6 C5 1.3864(12) . ? C3 C4 1.3911(12) . ? C31 C33 1.5295(12) . ? C31 C32 1.5338(12) . ? C10 C9 1.3876(12) . ? C10 C11 1.3916(13) . ? C4 C5 1.3905(14) . ? C34 C35 1.5290(13) . ? C34 C36 1.5319(14) . ? C18 C17 1.3850(15) . ? C15 C16 1.3935(13) . ? C23 C22 1.5310(14) . ? C24 C22 1.5336(14) . ? C16 C17 1.3930(15) . ? 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 Fe1 P3 102.35(3) . . ? O1 Fe1 P2 104.36(3) . . ? P3 Fe1 P2 109.319(9) . . ? O1 Fe1 P1 99.05(3) . . ? P3 Fe1 P1 119.056(9) . . ? P2 Fe1 P1 119.271(9) . . ? O1 Fe1 B1 176.02(3) . . ? P3 Fe1 B1 78.12(2) . . ? P2 Fe1 B1 79.08(2) . . ? P1 Fe1 B1 77.38(2) . . ? C8 P2 C28 105.81(4) . . ? C8 P2 C25 104.74(4) . . ? C28 P2 C25 101.64(4) . . ? C8 P2 Fe1 102.61(3) . . ? C28 P2 Fe1 108.47(3) . . ? C25 P2 Fe1 131.40(3) . . ? C13 P3 C34 107.34(4) . . ? C13 P3 C31 103.15(4) . . ? C34 P3 C31 100.63(4) . . ? C13 P3 Fe1 107.43(3) . . ? C34 P3 Fe1 113.50(3) . . ? C31 P3 Fe1 123.48(3) . . ? C1 P1 C22 106.36(4) . . ? C1 P1 C19 105.91(4) . . ? C22 P1 C19 102.05(4) . . ? C1 P1 Fe1 106.87(3) . . ? C22 P1 Fe1 109.17(3) . . ? C19 P1 Fe1 125.17(3) . . ? C18 C13 C14 121.80(8) . . ? C18 C13 P3 124.59(7) . . ? C14 C13 P3 113.61(6) . . ? C15 C14 C13 116.34(8) . . ? C15 C14 B1 120.69(7) . . ? C13 C14 B1 122.97(7) . . ? C12 C7 C8 116.28(7) . . ? C12 C7 B1 120.82(7) . . ? C8 C7 B1 122.90(7) . . ? C6 C1 C2 122.04(7) . . ? C6 C1 P1 123.66(6) . . ? C2 C1 P1 114.23(6) . . ? C1 C2 C3 116.06(7) . . ? C1 C2 B1 122.23(7) . . ? C3 C2 B1 121.72(7) . . ? C9 C8 C7 121.53(7) . . ? C9 C8 P2 122.93(6) . . ? C7 C8 P2 115.51(6) . . ? C30 C28 C29 110.25(8) . . ? C30 C28 P2 111.52(6) . . ? C29 C28 P2 110.18(6) . . ? C26 C25 C27 108.93(8) . . ? C26 C25 P2 111.67(6) . . ? C27 C25 P2 114.84(6) . . ? C11 C12 C7 122.32(8) . . ? C14 B1 C7 112.30(7) . . ? C14 B1 C2 112.88(6) . . ? C7 B1 C2 112.28(6) . . ? C14 B1 Fe1 107.28(5) . . ? C7 B1 Fe1 103.83(5) . . ? C2 B1 Fe1 107.61(5) . . ? C20 C19 C21 108.81(7) . . ? C20 C19 P1 112.39(6) . . ? C21 C19 P1 114.04(6) . . ? C5 C6 C1 120.25(8) . . ? C4 C3 C2 121.92(8) . . ? C33 C31 C32 108.64(7) . . ? C33 C31 P3 110.59(6) . . ? C32 C31 P3 114.96(6) . . ? C9 C10 C11 119.30(8) . . ? C5 C4 C3 120.80(8) . . ? C35 C34 C36 110.42(8) . . ? C35 C34 P3 111.92(6) . . ? C36 C34 P3 109.94(6) . . ? C17 C18 C13 120.35(8) . . ? C10 C9 C8 120.44(8) . . ? C6 C5 C4 118.94(8) . . ? C16 C15 C14 121.98(9) . . ? C12 C11 C10 120.11(8) . . ? C23 C22 C24 110.52(8) . . ? C23 C22 P1 110.31(6) . . ? C24 C22 P1 110.39(7) . . ? C17 C16 C15 120.47(9) . . ? C18 C17 C16 119.04(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 37.78 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.810 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.066