Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Britovsek, George J. P.' 'Gibson, Vernon C.' 'Spitzmesser, Stefan K.' 'Tellmann, Kilian P.' 'White, Andrew J. P.' 'Williams, David J.' _publ_contact_author_name 'Vernon C Gibson' _publ_contact_author_address ; Department of Chemistry Imperial College of Science, Technology and Medicine South Kensington London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email 'V.GIBSON@IC.AC.UK' _publ_section_title ; Cationic 2,6-Bis(imino)pyridine Iron and Cobalt Complexes. Synthesis, Structures, Polymerisation and Polar Monomer Co-polymerisation Studies. ; data_VG9869 _database_code_CSD 168887 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38.50 H54 N4 Cl3 Fe Sb F6' _chemical_formula_weight 970.81 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.925(2) _cell_length_b 10.0628(5) _cell_length_c 36.759(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.553(7) _cell_angle_gamma 90.00 _cell_volume 9580.1(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 90 _cell_measurement_theta_min 10.03 _cell_measurement_theta_max 27.89 _exptl_crystal_description needles _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method ? _exptl_crystal_F_000 3960 _exptl_absorpt_coefficient_mu 8.885 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.0241 _exptl_absorpt_correction_T_max 0.1098 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7174 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 59.99 _reflns_number_total 6994 _reflns_number_observed 3810 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1022 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000059(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5972 _refine_ls_number_parameters 542 _refine_ls_number_restraints 384 _refine_ls_R_factor_all 0.1528 _refine_ls_R_factor_obs 0.0809 _refine_ls_wR_factor_all 0.2609 _refine_ls_wR_factor_obs 0.1896 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.152 _refine_ls_restrained_S_all 1.156 _refine_ls_restrained_S_obs 1.147 _refine_ls_shift/esd_max 0.148 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.35372(6) 0.94335(12) 0.11974(4) 0.0584(4) Uani 1 d . . Cl Cl 0.34886(15) 0.7351(2) 0.09906(9) 0.0962(10) Uani 1 d . . N1 N 0.3788(3) 1.1414(7) 0.1272(2) 0.061(2) Uani 1 d . . C2 C 0.4113(4) 1.1707(9) 0.1551(3) 0.063(2) Uani 1 d . . C3 C 0.4191(5) 1.2992(10) 0.1665(3) 0.082(3) Uani 1 d . . H3A H 0.4405(5) 1.3184(10) 0.1868(3) 0.099 Uiso 1 calc R . C4 C 0.3941(5) 1.4003(10) 0.1467(4) 0.089(4) Uani 1 d . . H4A H 0.3993(5) 1.4885(10) 0.1535(4) 0.107 Uiso 1 calc R . C5 C 0.3626(6) 1.3706(10) 0.1180(3) 0.084(3) Uani 1 d . . H5A H 0.3465(6) 1.4381(10) 0.1045(3) 0.100 Uiso 1 calc R . C6 C 0.3541(4) 1.2364(9) 0.1083(3) 0.067(3) Uani 1 d . . C7 C 0.4360(4) 1.0492(9) 0.1728(3) 0.062(2) Uani 1 d . . N7 N 0.4200(3) 0.9380(7) 0.1602(2) 0.060(2) Uani 1 d . . C8 C 0.4774(5) 1.0680(12) 0.2013(3) 0.087(3) Uani 1 d . . H8A H 0.4623(5) 1.0903(12) 0.2239(3) 0.131 Uiso 1 d R . H8B H 0.4998(5) 1.1386(12) 0.1943(3) 0.131 Uiso 1 d R . H8C H 0.4969(5) 0.9873(12) 0.2042(3) 0.131 Uiso 1 d R . C9 C 0.3200(5) 1.1898(9) 0.0773(3) 0.076(3) Uani 1 d . . N9 N 0.3154(4) 1.0630(7) 0.0755(2) 0.071(2) Uani 1 d . . C10 C 0.2961(7) 1.2894(12) 0.0509(4) 0.113(5) Uani 1 d . . H10A H 0.3144(7) 1.2880(12) 0.0288(4) 0.169 Uiso 1 d R . H10B H 0.2984(7) 1.3766(12) 0.0615(4) 0.169 Uiso 1 d R . H10C H 0.2606(7) 1.2672(12) 0.0457(4) 0.169 Uiso 1 d R . C11 C 0.4440(4) 0.8164(8) 0.1724(3) 0.067(3) Uani 1 d . . C12 C 0.4855(5) 0.7691(12) 0.1531(3) 0.083(3) Uani 1 d . . C13 C 0.5088(6) 0.6501(14) 0.1663(5) 0.102(5) Uani 1 d . . H13A H 0.5369(6) 0.6164(14) 0.1544(5) 0.122 Uiso 1 calc R . C14 C 0.4918(6) 0.5837(12) 0.1953(5) 0.096(4) Uani 1 d . . H14A H 0.5079(6) 0.5053(12) 0.2030(5) 0.116 Uiso 1 calc R . C15 C 0.4513(5) 0.6319(11) 0.2131(4) 0.086(4) Uani 1 d . . H15A H 0.4396(5) 0.5851(11) 0.2330(4) 0.103 Uiso 1 calc R . C16 C 0.4260(4) 0.7514(9) 0.2026(3) 0.067(3) Uani 1 d . . C17 C 0.5056(6) 0.8376(17) 0.1204(4) 0.110(5) Uani 1 d . . H17A H 0.4836(6) 0.9151(17) 0.1152(4) 0.132 Uiso 1 calc R . C18 C 0.5047(10) 0.7511(27) 0.0862(5) 0.168(9) Uani 1 d . . H18A H 0.4705(10) 0.7169(27) 0.0815(5) 0.251 Uiso 1 calc R . H18B H 0.5284(10) 0.6785(27) 0.0898(5) 0.251 Uiso 1 calc R . H18C H 0.5146(10) 0.8035(27) 0.0659(5) 0.251 Uiso 1 calc R . C19 C 0.5584(10) 0.8845(24) 0.1254(6) 0.159(8) Uani 1 d . . H19A H 0.5686(10) 0.9271(24) 0.1035(6) 0.238 Uiso 1 calc R . H19B H 0.5808(10) 0.8105(24) 0.1308(6) 0.238 Uiso 1 calc R . H19C H 0.5607(10) 0.9468(24) 0.1451(6) 0.238 Uiso 1 calc R . C20 C 0.3812(5) 0.8004(10) 0.2235(3) 0.080(3) Uani 1 d . . H20A H 0.3738(5) 0.8919(10) 0.2157(3) 0.096 Uiso 1 calc R . C21 C 0.3908(8) 0.8020(16) 0.2641(4) 0.114(5) Uani 1 d . . H21A H 0.3606(8) 0.8343(16) 0.2755(4) 0.172 Uiso 1 calc R . H21B H 0.4195(8) 0.8592(16) 0.2703(4) 0.172 Uiso 1 calc R . H21C H 0.3984(8) 0.7136(16) 0.2726(4) 0.172 Uiso 1 calc R . C22 C 0.3325(6) 0.7134(14) 0.2125(5) 0.113(5) Uani 1 d . . H22A H 0.3271(6) 0.7138(14) 0.1865(5) 0.170 Uiso 1 calc R . H22B H 0.3027(6) 0.7493(14) 0.2235(5) 0.170 Uiso 1 calc R . H22C H 0.3381(6) 0.6238(14) 0.2208(5) 0.170 Uiso 1 calc R . C23 C 0.2845(6) 1.0068(9) 0.0448(3) 0.078(3) Uani 1 d . . C24 C 0.2334(6) 0.9818(11) 0.0476(4) 0.094(4) Uani 1 d . . C25 C 0.2070(7) 0.9287(12) 0.0157(5) 0.113(6) Uani 1 d . . H25A H 0.1717(7) 0.9130(12) 0.0163(5) 0.136 Uiso 1 calc R . C26 C 0.2305(9) 0.9011(13) -0.0147(4) 0.113(6) Uani 1 d . . H26A H 0.2118(9) 0.8680(13) -0.0349(4) 0.136 Uiso 1 calc R . C27 C 0.2829(8) 0.9218(12) -0.0162(4) 0.101(4) Uani 1 d U . H27A H 0.2998(8) 0.9002(12) -0.0372(4) 0.121 Uiso 1 calc R . C28 C 0.3107(7) 0.9755(12) 0.0140(3) 0.096(4) Uani 1 d . . C29 C 0.2047(6) 1.0049(17) 0.0821(5) 0.114(5) Uani 1 d . . H29A H 0.2290(6) 1.0481(17) 0.0995(5) 0.137 Uiso 1 calc R . C30 C 0.1912(9) 0.8714(21) 0.0984(5) 0.142(7) Uani 1 d . . H30A H 0.1730(9) 0.8852(21) 0.1203(5) 0.214 Uiso 1 calc R . H30B H 0.2223(9) 0.8223(21) 0.1040(5) 0.214 Uiso 1 calc R . H30C H 0.1697(9) 0.8223(21) 0.0812(5) 0.214 Uiso 1 calc R . C31 C 0.1580(10) 1.0991(27) 0.0768(8) 0.190(11) Uani 1 d U . H31A H 0.1691(10) 1.1814(27) 0.0664(8) 0.286 Uiso 1 calc R . H31B H 0.1435(10) 1.1161(27) 0.0999(8) 0.286 Uiso 1 calc R . H31C H 0.1324(10) 1.0586(27) 0.0607(8) 0.286 Uiso 1 calc R . C32 C 0.3681(9) 0.9901(17) 0.0118(4) 0.125(6) Uani 1 d . . H32A H 0.3806(9) 1.0214(17) 0.0359(4) 0.150 Uiso 1 calc R . C33 C 0.3978(10) 0.8611(29) 0.0050(7) 0.178(10) Uani 1 d . . H33A H 0.4340(10) 0.8804(29) 0.0040(7) 0.267 Uiso 1 calc R . H33B H 0.3856(10) 0.8227(29) -0.0177(7) 0.267 Uiso 1 calc R . H33C H 0.3924(10) 0.7996(29) 0.0244(7) 0.267 Uiso 1 calc R . C34 C 0.3836(14) 1.0987(28) -0.0154(9) 0.227(15) Uani 1 d . . H34A H 0.4206(14) 1.1037(28) -0.0157(9) 0.340 Uiso 1 calc R . H34B H 0.3701(14) 1.1829(28) -0.0080(9) 0.340 Uiso 1 calc R . H34C H 0.3698(14) 1.0770(28) -0.0393(9) 0.340 Uiso 1 calc R . N40 N 0.2980(4) 0.9834(9) 0.1584(3) 0.079(2) Uani 1 d . . C41 C 0.2752(6) 1.0157(13) 0.1827(4) 0.087(3) Uani 1 d . . C42 C 0.2465(7) 1.0587(17) 0.2145(5) 0.124(6) Uani 1 d . . H42A H 0.2556(7) 1.0029(17) 0.2350(5) 0.187 Uiso 1 d R . H42B H 0.2101(7) 1.0525(17) 0.2089(5) 0.187 Uiso 1 d R . H42C H 0.2554(7) 1.1492(17) 0.2203(5) 0.187 Uiso 1 d R . Sb Sb 0.62694(4) 0.27944(8) 0.22074(3) 0.0946(4) Uani 1 d D . F11 F 0.6963(4) 0.2438(15) 0.2147(5) 0.117(5) Uani 0.60 d PD 1 F12 F 0.6299(6) 0.1429(13) 0.2578(5) 0.137(6) Uani 0.60 d PD 1 F13 F 0.6069(6) 0.1519(17) 0.1881(5) 0.163(9) Uani 0.60 d PD 1 F14 F 0.6267(7) 0.4099(16) 0.1868(5) 0.162(9) Uani 0.60 d PD 1 F15 F 0.6470(7) 0.4015(16) 0.2570(4) 0.151(8) Uani 0.60 d PD 1 F16 F 0.5587(5) 0.3095(18) 0.2313(6) 0.130(9) Uani 0.60 d PD 1 F11' F 0.6895(7) 0.2662(25) 0.1974(6) 0.120(10) Uiso 0.40 d PD 2 F12' F 0.6344(13) 0.1117(20) 0.2389(9) 0.293(36) Uiso 0.40 d PD 2 F13' F 0.5938(11) 0.2133(30) 0.1786(7) 0.235(26) Uiso 0.40 d PD 2 F14' F 0.6205(10) 0.4522(17) 0.2014(6) 0.128(10) Uiso 0.40 d PD 2 F15' F 0.6598(10) 0.3512(28) 0.2611(6) 0.166(16) Uiso 0.40 d PD 2 F16' F 0.5629(7) 0.2979(27) 0.2409(7) 0.102(9) Uiso 0.40 d PD 2 C50 C 0.2819(17) 0.9922(35) -0.1570(8) 0.178(14) Uani 0.75 d P 1 Cl1 Cl 0.2459(5) 1.0812(11) -0.1829(3) 0.195(4) Uani 0.75 d P 1 Cl2 Cl 0.2954(5) 1.0259(16) -0.1121(2) 0.228(5) Uani 0.75 d P 1 C50' C 0.3004(25) 1.1648(59) -0.1297(18) 0.097(15) Uiso 0.25 d P 2 Cl1' Cl 0.2775(15) 1.1880(36) -0.1557(10) 0.206(12) Uiso 0.25 d P 2 Cl2' Cl 0.2610(15) 0.9372(36) -0.1310(11) 0.197(11) Uiso 0.25 d P 2 C61 C 0.4916(13) 1.1521(28) 0.0733(8) 0.084(9) Uani 0.50 d PU . C62 C 0.4765(15) 1.2011(44) 0.0640(10) 0.109(11) Uani 0.50 d PU . C63 C 0.5400(23) 1.2852(67) 0.1106(15) 0.181(19) Uani 0.50 d PU . C64 C 0.4374(21) 1.4627(50) 0.0147(15) 0.171(17) Uani 0.50 d PU . C65 C 0.5213(30) 1.3634(72) 0.0946(21) 0.217(26) Uani 0.50 d PU . 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 Fe 0.0708(10) 0.0421(6) 0.0616(8) -0.0013(6) -0.0056(7) -0.0006(6) Cl 0.132(3) 0.0512(12) 0.103(2) -0.0146(12) -0.032(2) 0.0044(14) N1 0.075(5) 0.046(4) 0.061(4) 0.009(3) -0.002(4) 0.001(3) C2 0.074(7) 0.050(4) 0.065(6) -0.008(4) -0.003(5) -0.006(4) C3 0.094(8) 0.058(5) 0.093(8) -0.014(5) -0.010(6) -0.009(6) C4 0.111(10) 0.049(5) 0.106(9) -0.007(5) -0.015(8) -0.004(6) C5 0.118(10) 0.048(5) 0.083(7) 0.001(5) -0.008(7) -0.001(6) C6 0.087(7) 0.055(5) 0.058(5) 0.004(4) 0.002(5) 0.004(5) C7 0.061(6) 0.055(5) 0.069(5) -0.006(4) 0.003(4) -0.003(4) N7 0.063(5) 0.058(4) 0.060(4) 0.001(3) -0.003(4) 0.002(4) C8 0.098(9) 0.079(7) 0.082(7) -0.014(6) -0.024(7) 0.003(6) C9 0.104(9) 0.049(5) 0.074(6) 0.002(4) -0.014(6) 0.006(5) N9 0.092(6) 0.049(4) 0.069(5) 0.004(3) -0.013(4) 0.002(4) C10 0.162(14) 0.063(6) 0.109(10) 0.022(7) -0.032(10) 0.019(8) C11 0.068(7) 0.048(5) 0.084(7) -0.006(4) -0.014(5) 0.009(4) C12 0.071(7) 0.087(7) 0.090(8) -0.019(6) -0.006(6) 0.016(6) C13 0.075(9) 0.088(8) 0.141(13) -0.032(9) -0.009(9) 0.031(7) C14 0.093(10) 0.061(6) 0.131(12) -0.025(7) -0.038(9) 0.011(6) C15 0.094(9) 0.063(6) 0.099(8) -0.003(6) -0.036(7) 0.005(6) C16 0.068(6) 0.057(5) 0.074(6) -0.006(4) -0.012(5) 0.006(4) C17 0.096(11) 0.125(11) 0.111(11) 0.001(9) 0.037(9) 0.023(9) C18 0.178(21) 0.215(24) 0.112(13) -0.012(15) 0.040(14) 0.005(19) C19 0.177(22) 0.174(19) 0.127(15) -0.017(14) 0.036(14) -0.052(17) C20 0.094(9) 0.060(5) 0.083(7) 0.009(5) -0.009(6) 0.001(5) C21 0.160(15) 0.109(10) 0.074(7) 0.014(7) 0.009(8) -0.009(10) C22 0.108(11) 0.084(8) 0.148(13) 0.038(9) 0.006(9) -0.010(8) C23 0.115(11) 0.050(5) 0.065(6) 0.004(4) -0.025(6) 0.002(6) C24 0.103(11) 0.061(6) 0.114(10) -0.003(6) -0.043(8) 0.005(6) C25 0.143(14) 0.066(7) 0.124(12) -0.009(7) -0.062(11) 0.019(8) C26 0.182(19) 0.071(7) 0.082(9) 0.004(6) -0.042(11) 0.002(9) C27 0.163(13) 0.070(6) 0.069(7) 0.006(5) -0.014(8) -0.006(8) C28 0.139(13) 0.079(7) 0.068(7) 0.008(6) -0.009(8) -0.009(8) C29 0.091(10) 0.115(11) 0.134(13) -0.028(10) -0.016(9) 0.021(9) C30 0.162(19) 0.145(16) 0.122(14) -0.001(12) 0.028(13) -0.011(14) C31 0.154(18) 0.187(20) 0.228(23) -0.051(18) -0.024(17) 0.072(16) C32 0.171(19) 0.118(11) 0.089(9) -0.021(8) 0.037(10) -0.032(12) C33 0.173(22) 0.224(27) 0.141(18) -0.006(18) 0.056(16) 0.019(20) C34 0.289(39) 0.165(22) 0.232(31) 0.041(21) 0.087(28) -0.076(24) N40 0.080(7) 0.066(5) 0.090(7) 0.001(5) -0.004(6) -0.003(5) C41 0.078(9) 0.086(7) 0.098(9) -0.008(7) 0.002(7) -0.017(6) C42 0.132(14) 0.124(11) 0.122(12) -0.032(10) 0.063(11) -0.034(10) Sb 0.0850(6) 0.0679(4) 0.1320(8) -0.0157(4) 0.0171(5) -0.0046(4) F11 0.071(8) 0.128(12) 0.151(14) -0.010(11) -0.010(8) 0.008(7) F12 0.141(14) 0.082(8) 0.190(17) 0.057(10) 0.028(12) 0.030(8) F13 0.121(13) 0.144(15) 0.222(21) -0.111(15) -0.003(14) -0.010(12) F14 0.181(20) 0.137(14) 0.176(19) 0.049(14) 0.083(16) 0.030(13) F15 0.181(18) 0.096(11) 0.174(17) -0.057(11) 0.004(14) -0.033(12) F16 0.077(9) 0.117(12) 0.197(22) 0.044(13) 0.038(11) 0.024(8) C50 0.259(41) 0.164(26) 0.112(19) -0.021(18) -0.003(23) 0.072(27) Cl1 0.206(9) 0.206(9) 0.174(8) 0.031(7) 0.005(7) -0.001(7) Cl2 0.230(11) 0.334(16) 0.120(5) -0.011(8) -0.002(6) -0.016(11) C61 0.092(20) 0.081(15) 0.079(16) 0.040(12) 0.015(14) 0.004(13) C62 0.099(22) 0.138(26) 0.094(21) 0.010(19) 0.025(17) 0.021(20) C63 0.161(31) 0.219(36) 0.163(30) 0.046(29) 0.031(26) -0.022(29) C64 0.163(23) 0.161(22) 0.186(23) -0.013(18) -0.035(18) 0.007(17) C65 0.221(41) 0.200(37) 0.233(41) 0.049(32) 0.027(33) 0.040(32) _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 Fe N40 2.109(12) . ? Fe N1 2.110(7) . ? Fe N7 2.221(8) . ? Fe N9 2.223(8) . ? Fe Cl 2.231(3) . ? N1 C6 1.329(12) . ? N1 C2 1.333(12) . ? C2 C3 1.372(13) . ? C2 C7 1.514(13) . ? C3 C4 1.39(2) . ? C4 C5 1.34(2) . ? C5 C6 1.412(14) . ? C6 C9 1.487(15) . ? C7 N7 1.275(12) . ? C7 C8 1.477(14) . ? N7 C11 1.436(12) . ? C9 N9 1.283(12) . ? C9 C10 1.507(15) . ? N9 C23 1.466(13) . ? C11 C16 1.39(2) . ? C11 C12 1.40(2) . ? C12 C13 1.42(2) . ? C12 C17 1.50(2) . ? C13 C14 1.35(2) . ? C14 C15 1.35(2) . ? C15 C16 1.415(14) . ? C16 C20 1.51(2) . ? C17 C19 1.45(3) . ? C17 C18 1.53(3) . ? C20 C21 1.50(2) . ? C20 C22 1.57(2) . ? C23 C24 1.36(2) . ? C23 C28 1.38(2) . ? C24 C25 1.44(2) . ? C24 C29 1.52(2) . ? C25 C26 1.33(2) . ? C26 C27 1.38(2) . ? C27 C28 1.41(2) . ? C28 C32 1.50(3) . ? C29 C30 1.52(3) . ? C29 C31 1.54(2) . ? C32 C33 1.54(3) . ? C32 C34 1.55(3) . ? N40 C41 1.14(2) . ? C41 C42 1.48(2) . ? Sb F14 1.811(12) . ? Sb F13 1.817(10) . ? Sb F12' 1.82(2) . ? Sb F15' 1.83(2) . ? Sb F16 1.854(11) . ? Sb F16' 1.86(2) . ? Sb F11 1.857(10) . ? Sb F13' 1.86(2) . ? Sb F15 1.869(11) . ? Sb F11' 1.87(2) . ? Sb F14' 1.88(2) . ? Sb F12 1.933(11) . ? C50 Cl1 1.58(3) . ? C50 Cl2 1.71(3) . ? C50' Cl1' 1.13(6) . ? C61 C62 0.71(4) . ? C63 C65 1.08(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N40 Fe N1 87.0(3) . . ? N40 Fe N7 94.9(3) . . ? N1 Fe N7 73.2(3) . . ? N40 Fe N9 95.3(4) . . ? N1 Fe N9 73.0(3) . . ? N7 Fe N9 144.1(3) . . ? N40 Fe Cl 112.3(3) . . ? N1 Fe Cl 160.7(3) . . ? N7 Fe Cl 103.6(2) . . ? N9 Fe Cl 104.1(2) . . ? C6 N1 C2 121.1(8) . . ? C6 N1 Fe 118.3(7) . . ? C2 N1 Fe 119.3(6) . . ? N1 C2 C3 121.5(9) . . ? N1 C2 C7 113.2(7) . . ? C3 C2 C7 125.2(9) . . ? C2 C3 C4 118.1(10) . . ? C5 C4 C3 120.1(9) . . ? C4 C5 C6 119.7(10) . . ? N1 C6 C5 119.3(10) . . ? N1 C6 C9 115.4(8) . . ? C5 C6 C9 125.2(9) . . ? N7 C7 C8 125.9(9) . . ? N7 C7 C2 115.2(8) . . ? C8 C7 C2 118.8(8) . . ? C7 N7 C11 120.2(8) . . ? C7 N7 Fe 117.0(6) . . ? C11 N7 Fe 122.8(6) . . ? N9 C9 C6 113.8(9) . . ? N9 C9 C10 126.4(11) . . ? C6 C9 C10 119.7(9) . . ? C9 N9 C23 118.0(8) . . ? C9 N9 Fe 117.7(7) . . ? C23 N9 Fe 124.3(6) . . ? C16 C11 C12 122.6(9) . . ? C16 C11 N7 119.7(10) . . ? C12 C11 N7 117.7(10) . . ? C11 C12 C13 116.2(13) . . ? C11 C12 C17 123.5(11) . . ? C13 C12 C17 120.3(13) . . ? C14 C13 C12 122.7(13) . . ? C13 C14 C15 119.5(12) . . ? C14 C15 C16 122.1(14) . . ? C11 C16 C15 116.9(11) . . ? C11 C16 C20 123.3(8) . . ? C15 C16 C20 119.8(11) . . ? C19 C17 C12 114.1(15) . . ? C19 C17 C18 105.5(16) . . ? C12 C17 C18 113.8(16) . . ? C21 C20 C16 114.5(11) . . ? C21 C20 C22 111.0(12) . . ? C16 C20 C22 108.3(10) . . ? C24 C23 C28 122.4(12) . . ? C24 C23 N9 121.1(12) . . ? C28 C23 N9 116.4(13) . . ? C23 C24 C25 116.1(16) . . ? C23 C24 C29 123.4(12) . . ? C25 C24 C29 120.4(16) . . ? C26 C25 C24 123.1(18) . . ? C25 C26 C27 119.6(14) . . ? C26 C27 C28 119.9(16) . . ? C23 C28 C27 118.8(16) . . ? C23 C28 C32 123.1(12) . . ? C27 C28 C32 118.0(15) . . ? C30 C29 C24 109.0(13) . . ? C30 C29 C31 113.6(19) . . ? C24 C29 C31 113.5(17) . . ? C28 C32 C33 115.6(16) . . ? C28 C32 C34 113.0(21) . . ? C33 C32 C34 110.2(20) . . ? C41 N40 Fe 167.5(10) . . ? N40 C41 C42 179.0(14) . . ? F14 Sb F13 93.7(8) . . ? F12' Sb F15' 91.8(10) . . ? F14 Sb F16 93.0(7) . . ? F13 Sb F16 90.3(7) . . ? F12' Sb F16' 91.6(9) . . ? F15' Sb F16' 91.6(9) . . ? F14 Sb F11 91.8(7) . . ? F13 Sb F11 92.0(6) . . ? F16 Sb F11 174.6(8) . . ? F12' Sb F13' 90.6(9) . . ? F15' Sb F13' 177.5(11) . . ? F16' Sb F13' 88.9(9) . . ? F14 Sb F15 90.4(7) . . ? F13 Sb F15 175.9(8) . . ? F16 Sb F15 89.0(7) . . ? F11 Sb F15 88.4(6) . . ? F12' Sb F11' 91.3(9) . . ? F15' Sb F11' 91.0(9) . . ? F16' Sb F11' 176.0(10) . . ? F13' Sb F11' 88.3(9) . . ? F12' Sb F14' 178.8(11) . . ? F15' Sb F14' 88.4(9) . . ? F16' Sb F14' 89.6(8) . . ? F13' Sb F14' 89.2(9) . . ? F11' Sb F14' 87.5(8) . . ? F14 Sb F12 177.6(8) . . ? F13 Sb F12 87.9(7) . . ? F16 Sb F12 88.7(6) . . ? F11 Sb F12 86.5(6) . . ? F15 Sb F12 88.0(7) . . ? Cl1 C50 Cl2 124.1(19) . . ? _refine_diff_density_max 0.899 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.103 data_VG9921 _database_code_CSD 168888 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36.50 H49 N4 Cl4 Co Sb F6' _chemical_formula_weight 980.28 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 25.879(5) _cell_length_b 10.073(2) _cell_length_c 36.573(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.011(12) _cell_angle_gamma 90.00 _cell_volume 9521.4(29) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 10.57 _cell_measurement_theta_max 22.47 _exptl_crystal_description prisms _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method ? _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 9.734 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.0861 _exptl_absorpt_correction_T_max 0.2282 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6502 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.1092 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 57.08 _reflns_number_total 6327 _reflns_number_observed 3496 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 864 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5463 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1477 _refine_ls_R_factor_obs 0.0755 _refine_ls_wR_factor_all 0.2333 _refine_ls_wR_factor_obs 0.1783 _refine_ls_goodness_of_fit_all 1.005 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.14730(6) 0.5480(2) 0.37964(4) 0.0443(4) Uani 1 d . . Cl Cl 0.15541(15) 0.7571(3) 0.39812(9) 0.0777(9) Uani 1 d . . N1 N 0.1244(3) 0.3544(8) 0.3723(2) 0.045(2) Uani 1 d . . C2 C 0.0905(4) 0.3259(10) 0.3441(3) 0.047(2) Uani 1 d . . C3 C 0.0821(5) 0.1951(11) 0.3337(3) 0.064(3) Uani 1 d . . H3A H 0.0595(5) 0.1747(11) 0.3139(3) 0.076 Uiso 1 calc R . C4 C 0.1078(6) 0.0956(12) 0.3532(4) 0.076(4) Uani 1 d . . H4A H 0.1030(6) 0.0077(12) 0.3461(4) 0.092 Uiso 1 calc R . C5 C 0.1402(5) 0.1251(12) 0.3828(4) 0.067(3) Uani 1 d . . H5A H 0.1562(5) 0.0583(12) 0.3968(4) 0.081 Uiso 1 calc R . C6 C 0.1483(4) 0.2577(10) 0.3914(3) 0.050(3) Uani 1 d . . C7 C 0.0656(4) 0.4476(11) 0.3272(3) 0.047(2) Uani 1 d . . N7 N 0.0805(3) 0.5573(8) 0.3405(2) 0.044(2) Uani 1 d . . C8 C 0.0247(5) 0.4293(12) 0.2982(3) 0.070(3) Uani 1 d . . H8A H 0.0013(5) 0.3614(12) 0.3054(3) 0.105 Uiso 1 d R . H8B H 0.0400(5) 0.4035(12) 0.2759(3) 0.105 Uiso 1 d R . H8C H 0.0061(5) 0.5110(12) 0.2943(3) 0.105 Uiso 1 d R . C9 C 0.1807(5) 0.3101(11) 0.4224(3) 0.058(3) Uani 1 d . . N9 N 0.1848(4) 0.4367(9) 0.4245(2) 0.054(2) Uani 1 d . . C10 C 0.2069(7) 0.2118(13) 0.4489(4) 0.095(5) Uani 1 d . . H10A H 0.2225(7) 0.1422(13) 0.4354(4) 0.143 Uiso 1 d R . H10B H 0.1817(7) 0.1745(13) 0.4643(4) 0.143 Uiso 1 d R . H10C H 0.2331(7) 0.2566(13) 0.4639(4) 0.143 Uiso 1 d R . C11 C 0.0564(3) 0.6796(10) 0.3284(3) 0.047(3) Uani 1 d . . C12 C 0.0158(4) 0.7240(14) 0.3481(3) 0.066(3) Uani 1 d . . C13 C -0.0076(5) 0.8432(16) 0.3355(5) 0.083(4) Uani 1 d . . H13A H -0.0349(5) 0.8777(16) 0.3480(5) 0.100 Uiso 1 calc R . C14 C 0.0078(6) 0.9082(14) 0.3063(5) 0.090(5) Uani 1 d . . H14A H -0.0091(6) 0.9857(14) 0.2987(5) 0.107 Uiso 1 calc R . C15 C 0.0488(6) 0.8612(12) 0.2872(4) 0.078(4) Uani 1 d . . H15A H 0.0594(6) 0.9077(12) 0.2670(4) 0.094 Uiso 1 calc R . C16 C 0.0743(4) 0.7440(10) 0.2981(3) 0.056(3) Uani 1 d . . C17 C -0.0033(6) 0.6548(18) 0.3815(5) 0.097(5) Uani 1 d . . H17A H 0.0196(6) 0.5789(18) 0.3868(5) 0.117 Uiso 1 calc R . C18 C -0.0002(9) 0.7436(28) 0.4147(6) 0.155(9) Uani 1 d . . H18A H 0.0344(9) 0.7774(28) 0.4184(6) 0.232 Uiso 1 calc R . H18B H -0.0091(9) 0.6938(28) 0.4358(6) 0.232 Uiso 1 calc R . H18C H -0.0239(9) 0.8163(28) 0.4110(6) 0.232 Uiso 1 calc R . C19 C -0.0564(8) 0.6028(24) 0.3757(7) 0.139(8) Uani 1 d . . H19A H -0.0583(8) 0.5462(24) 0.3546(7) 0.209 Uiso 1 calc R . H19B H -0.0802(8) 0.6754(24) 0.3720(7) 0.209 Uiso 1 calc R . H19C H -0.0654(8) 0.5529(24) 0.3968(7) 0.209 Uiso 1 calc R . C20 C 0.1192(4) 0.6944(12) 0.2771(3) 0.064(3) Uani 1 d . . H20A H 0.1268(4) 0.6035(12) 0.2854(3) 0.077 Uiso 1 calc R . C21 C 0.1077(7) 0.6898(17) 0.2359(4) 0.095(5) Uani 1 d . . H21A H 0.1375(7) 0.6575(17) 0.2241(4) 0.143 Uiso 1 calc R . H21B H 0.0993(7) 0.7773(17) 0.2271(4) 0.143 Uiso 1 calc R . H21C H 0.0789(7) 0.6315(17) 0.2304(4) 0.143 Uiso 1 calc R . C22 C 0.1668(6) 0.7781(16) 0.2866(4) 0.089(4) Uani 1 d . . H22A H 0.1952(6) 0.7464(16) 0.2732(4) 0.134 Uiso 1 calc R . H22B H 0.1755(6) 0.7721(16) 0.3124(4) 0.134 Uiso 1 calc R . H22C H 0.1598(6) 0.8690(16) 0.2801(4) 0.134 Uiso 1 calc R . C23 C 0.2140(6) 0.4950(11) 0.4553(3) 0.066(3) Uani 1 d . . C24 C 0.2673(5) 0.5191(12) 0.4526(4) 0.069(3) Uani 1 d . . C25 C 0.2946(8) 0.5739(14) 0.4832(5) 0.103(6) Uani 1 d . . H25A H 0.3296(8) 0.5935(14) 0.4824(5) 0.123 Uiso 1 calc R . C26 C 0.2671(10) 0.5992(14) 0.5160(5) 0.110(7) Uani 1 d . . H26A H 0.2849(10) 0.6305(14) 0.5370(5) 0.132 Uiso 1 calc R . C27 C 0.2173(9) 0.5780(14) 0.5160(4) 0.093(5) Uani 1 d . . H27A H 0.2004(9) 0.5988(14) 0.5371(4) 0.112 Uiso 1 calc R . C28 C 0.1876(7) 0.5254(12) 0.4859(3) 0.082(4) Uani 1 d . . C29 C 0.2944(7) 0.4990(20) 0.4177(5) 0.107(6) Uani 1 d . . H29A H 0.2702(7) 0.4532(20) 0.4005(5) 0.128 Uiso 1 calc R 1 C30 C 0.3084(9) 0.6313(24) 0.4003(6) 0.134(7) Uani 1 d . 1 H30A H 0.3256(9) 0.6150(24) 0.3781(6) 0.200 Uiso 1 calc R 1 H30B H 0.3308(9) 0.6806(24) 0.4170(6) 0.200 Uiso 1 calc R 1 H30C H 0.2774(9) 0.6815(24) 0.3948(6) 0.200 Uiso 1 calc R 1 C31 C 0.3410(9) 0.4091(26) 0.4246(8) 0.174(12) Uani 1 d . 1 H31A H 0.3581(9) 0.3969(26) 0.4021(8) 0.261 Uiso 1 calc R 1 H31B H 0.3298(9) 0.3246(26) 0.4334(8) 0.261 Uiso 1 calc R 1 H31C H 0.3646(9) 0.4489(26) 0.4425(8) 0.261 Uiso 1 calc R 1 C32 C 0.1305(8) 0.5048(19) 0.4885(4) 0.105(6) Uani 1 d . . H32A H 0.1184(8) 0.4728(19) 0.4642(4) 0.126 Uiso 1 calc R 1 C33 C 0.1006(11) 0.6331(29) 0.4939(8) 0.169(10) Uani 1 d . 1 H33A H 0.1110(11) 0.6984(29) 0.4766(8) 0.253 Uiso 1 calc R 1 H33B H 0.1078(11) 0.6654(29) 0.5184(8) 0.253 Uiso 1 calc R 1 H33C H 0.0642(11) 0.6164(29) 0.4902(8) 0.253 Uiso 1 calc R 1 C34 C 0.1170(13) 0.3967(30) 0.5142(10) 0.232(18) Uani 1 d . 1 H34A H 0.0800(13) 0.3889(30) 0.5145(10) 0.349 Uiso 1 calc R 1 H34B H 0.1309(13) 0.4173(30) 0.5384(10) 0.349 Uiso 1 calc R 1 H34C H 0.1313(13) 0.3143(30) 0.5063(10) 0.349 Uiso 1 calc R 1 N40 N 0.2006(4) 0.5091(10) 0.3416(3) 0.062(2) Uani 1 d . . C41 C 0.2244(5) 0.4774(14) 0.3174(4) 0.069(3) Uani 1 d . . C42 C 0.2534(7) 0.4371(19) 0.2852(5) 0.116(7) Uani 1 d . . H42A H 0.2409(7) 0.4862(19) 0.2640(5) 0.174 Uiso 1 d R . H42B H 0.2486(7) 0.3439(19) 0.2808(5) 0.174 Uiso 1 d R . H42C H 0.2895(7) 0.4552(19) 0.2900(5) 0.174 Uiso 1 d R . Sb Sb 0.12622(4) 0.78490(9) 0.72029(3) 0.0782(3) Uani 1 d . . F11 F 0.0601(3) 0.8128(10) 0.7343(4) 0.125(4) Uani 1 d . . F12 F 0.1504(6) 0.8930(16) 0.7578(4) 0.181(6) Uani 1 d . . F13 F 0.1312(5) 0.6435(12) 0.7535(6) 0.196(8) Uani 1 d . . F14 F 0.1056(7) 0.6692(19) 0.6856(5) 0.237(10) Uani 1 d . . F15 F 0.1225(5) 0.9347(14) 0.6927(5) 0.176(6) Uani 1 d . . F16 F 0.1939(4) 0.7583(14) 0.7083(4) 0.166(5) Uani 1 d . . C50 C 0.2172(14) 0.5161(31) 0.6563(7) 0.186(13) Uani 1 d . . Cl1 Cl 0.2025(4) 0.4674(16) 0.6135(2) 0.212(6) Uani 0.75 d P 1 Cl2 Cl 0.2544(4) 0.4273(10) 0.6844(3) 0.158(3) Uani 0.75 d P 1 Cl1' Cl 0.2100(19) 0.3124(45) 0.6478(14) 0.231(17) Uiso 0.25 d P 2 Cl2' Cl 0.2398(16) 0.5711(43) 0.6273(13) 0.137(12) Uiso 0.15 d P 2 Cl2" Cl 0.2361(22) 0.3386(57) 0.6708(16) 0.112(14) Uiso 0.10 d P 3 C60 C 0.0317(38) 0.1227(98) 0.4555(27) 0.125(26) Uiso 0.25 d P . C61 C -0.0172(41) 0.1986(121) 0.4245(30) 0.137(30) Uiso 0.25 d P . Cl3 Cl 0.0139(11) 0.3253(27) 0.4289(8) 0.143(8) Uiso 0.25 d P . Cl4 Cl 0.0331(23) 0.2455(62) 0.4418(16) 0.196(19) Uiso 0.17 d P . Cl5 Cl 0.0540(33) 0.0425(81) 0.4803(24) 0.187(28) Uiso 0.12 d P . Cl6 Cl -0.0298(21) 0.1499(59) 0.3941(16) 0.167(16) Uiso 0.15 d P . Cl7 Cl 0.0021(42) 0.1152(105) 0.4286(30) 0.195(33) Uiso 0.10 d P . Cl8 Cl -0.0372(29) 0.2529(76) 0.4003(22) 0.166(22) Uiso 0.11 d P . Cl9 Cl 0.0718(33) 0.0810(84) 0.4669(24) 0.161(26) Uiso 0.10 d P . 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 Co 0.0560(9) 0.0366(9) 0.0394(8) -0.0011(7) -0.0048(7) 0.0002(7) Cl 0.107(2) 0.046(2) 0.077(2) -0.0099(14) -0.028(2) 0.0030(15) N1 0.061(5) 0.039(5) 0.035(4) 0.002(4) -0.004(4) 0.001(4) C2 0.053(6) 0.042(6) 0.047(6) -0.002(4) -0.001(5) -0.001(4) C3 0.076(7) 0.048(8) 0.066(7) -0.010(6) -0.007(6) -0.004(6) C4 0.102(10) 0.037(7) 0.090(10) -0.007(6) -0.001(8) -0.017(7) C5 0.095(9) 0.043(7) 0.064(7) -0.010(6) 0.008(7) 0.003(6) C6 0.073(7) 0.032(6) 0.045(5) 0.000(4) 0.004(5) 0.000(5) C7 0.049(5) 0.044(6) 0.050(6) -0.002(5) 0.003(4) -0.005(5) N7 0.045(4) 0.049(5) 0.038(4) -0.001(4) -0.002(3) -0.006(4) C8 0.081(8) 0.057(8) 0.070(8) -0.014(6) -0.025(7) -0.008(6) C9 0.081(7) 0.039(7) 0.053(6) 0.005(5) -0.016(6) 0.003(5) N9 0.074(6) 0.040(6) 0.046(5) -0.002(4) -0.008(4) -0.001(4) C10 0.152(14) 0.039(7) 0.089(10) 0.015(7) -0.048(10) 0.020(8) C11 0.033(5) 0.048(7) 0.058(6) -0.010(5) -0.006(4) 0.008(4) C12 0.053(6) 0.077(8) 0.066(7) -0.014(6) -0.003(5) 0.016(6) C13 0.061(8) 0.088(11) 0.100(11) -0.018(9) 0.000(8) 0.018(7) C14 0.069(9) 0.056(9) 0.138(15) -0.038(9) -0.053(10) 0.012(7) C15 0.092(10) 0.042(7) 0.096(10) -0.003(7) -0.042(9) 0.001(7) C16 0.064(6) 0.045(7) 0.058(6) -0.002(5) -0.017(5) -0.001(5) C17 0.089(10) 0.113(12) 0.093(11) -0.008(9) 0.030(9) 0.012(9) C18 0.141(18) 0.231(28) 0.095(13) -0.012(17) 0.027(13) 0.017(19) C19 0.109(14) 0.165(21) 0.146(19) -0.024(16) 0.031(13) -0.017(14) C20 0.064(7) 0.048(7) 0.080(8) 0.013(6) -0.005(6) 0.011(5) C21 0.126(12) 0.106(12) 0.053(7) 0.005(8) 0.001(8) 0.017(10) C22 0.086(9) 0.092(10) 0.090(10) 0.028(9) 0.002(8) -0.016(9) C23 0.102(10) 0.044(7) 0.048(7) -0.001(5) -0.025(6) 0.006(6) C24 0.077(8) 0.051(7) 0.076(8) 0.002(6) -0.033(7) 0.009(6) C25 0.128(13) 0.066(10) 0.107(13) -0.018(9) -0.064(11) 0.017(9) C26 0.190(21) 0.051(9) 0.080(12) 0.005(8) -0.079(14) 0.000(11) C27 0.175(18) 0.061(9) 0.040(7) 0.000(6) -0.030(9) -0.002(10) C28 0.150(14) 0.043(7) 0.052(7) 0.008(6) -0.017(8) -0.010(8) C29 0.088(11) 0.126(15) 0.103(13) -0.036(11) -0.030(10) 0.018(10) C30 0.140(18) 0.160(20) 0.102(15) -0.003(14) 0.012(13) 0.001(15) C31 0.126(18) 0.174(23) 0.218(30) -0.052(21) -0.028(19) 0.055(17) C32 0.137(15) 0.122(14) 0.058(8) -0.022(9) 0.022(9) -0.040(12) C33 0.161(22) 0.195(27) 0.156(23) -0.013(20) 0.052(19) -0.002(20) C34 0.241(36) 0.185(29) 0.280(42) 0.103(28) 0.092(31) -0.058(25) N40 0.060(5) 0.062(6) 0.062(6) 0.007(5) -0.006(5) -0.002(5) C41 0.066(7) 0.076(9) 0.066(8) 0.000(7) 0.001(7) -0.015(7) C42 0.122(13) 0.131(15) 0.101(12) -0.040(11) 0.068(11) -0.040(12) Sb 0.0691(5) 0.0606(5) 0.1063(7) -0.0155(5) 0.0188(4) -0.0054(4) F11 0.072(5) 0.116(8) 0.190(11) 0.031(7) 0.037(6) 0.012(5) F12 0.195(13) 0.220(15) 0.130(10) -0.068(10) 0.009(9) -0.093(12) F13 0.143(10) 0.089(8) 0.359(24) 0.065(11) 0.041(13) 0.012(7) F14 0.184(14) 0.276(19) 0.253(19) -0.186(17) 0.024(13) -0.078(13) F15 0.128(9) 0.173(12) 0.229(16) 0.116(11) 0.028(10) 0.007(8) F16 0.096(7) 0.173(11) 0.236(15) -0.025(11) 0.073(8) 0.008(7) C50 0.256(35) 0.185(27) 0.114(18) -0.021(18) -0.020(21) 0.074(25) Cl1 0.172(8) 0.368(17) 0.096(5) -0.048(8) -0.006(5) -0.026(10) Cl2 0.183(8) 0.163(8) 0.128(6) 0.004(6) -0.004(6) 0.000(7) _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 Co N40 2.049(11) . ? Co N1 2.052(8) . ? Co N9 2.174(9) . ? Co N7 2.188(8) . ? Co Cl 2.218(3) . ? N1 C6 1.331(13) . ? N1 C2 1.349(13) . ? C2 C3 1.38(2) . ? C2 C7 1.503(15) . ? C3 C4 1.38(2) . ? C4 C5 1.37(2) . ? C5 C6 1.38(2) . ? C6 C9 1.475(15) . ? C7 N7 1.259(13) . ? C7 C8 1.472(15) . ? N7 C11 1.441(13) . ? C9 N9 1.281(14) . ? C9 C10 1.519(15) . ? N9 C23 1.448(14) . ? C11 C12 1.379(15) . ? C11 C16 1.38(2) . ? C12 C13 1.41(2) . ? C12 C17 1.51(2) . ? C13 C14 1.33(2) . ? C14 C15 1.38(2) . ? C15 C16 1.40(2) . ? C16 C20 1.51(2) . ? C17 C19 1.48(2) . ? C17 C18 1.51(3) . ? C20 C22 1.52(2) . ? C20 C21 1.52(2) . ? C23 C28 1.38(2) . ? C23 C24 1.41(2) . ? C24 C25 1.41(2) . ? C24 C29 1.50(2) . ? C25 C26 1.45(3) . ? C26 C27 1.31(3) . ? C27 C28 1.41(2) . ? C28 C32 1.50(2) . ? C29 C31 1.52(2) . ? C29 C30 1.53(3) . ? C32 C34 1.49(3) . ? C32 C33 1.53(3) . ? N40 C41 1.15(2) . ? C41 C42 1.49(2) . ? Sb F14 1.785(12) . ? Sb F15 1.816(11) . ? Sb F11 1.834(9) . ? Sb F12 1.836(11) . ? Sb F16 1.847(10) . ? Sb F13 1.871(14) . ? C50 Cl2' 1.36(5) . ? C50 Cl2 1.64(3) . ? C50 Cl1 1.66(3) . ? C50 Cl2" 1.92(6) . ? C50 Cl1' 2.08(5) . ? C60 Cl9 1.18(11) . ? C60 Cl7 1.22(12) . ? C60 Cl5 1.32(12) . ? C60 Cl4 1.34(10) . ? C60 C61 1.82(15) . ? C61 Cl7 0.98(12) . ? C61 Cl8 1.14(11) . ? C61 Cl6 1.24(11) . ? C61 Cl4 1.49(11) . ? C61 Cl3 1.51(11) . ? Cl3 Cl4 1.04(6) . ? Cl3 Cl8 1.80(8) . ? Cl3 Cl7 2.14(11) . ? Cl3 Cl6 2.42(6) . ? Cl4 Cl7 1.60(11) . ? Cl4 Cl9 2.12(11) . ? Cl4 Cl8 2.31(10) . ? Cl5 Cl9 0.79(11) . ? Cl5 Cl7 2.38(14) . ? Cl6 Cl8 1.08(8) . ? Cl6 Cl7 1.51(12) . ? Cl7 Cl8 1.98(13) . ? Cl7 Cl9 2.25(14) . ? 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 N40 Co N1 85.9(4) . . ? N40 Co N9 97.2(4) . . ? N1 Co N9 73.9(3) . . ? N40 Co N7 95.8(3) . . ? N1 Co N7 75.1(3) . . ? N9 Co N7 145.2(3) . . ? N40 Co Cl 109.4(3) . . ? N1 Co Cl 164.6(3) . . ? N9 Co Cl 103.2(2) . . ? N7 Co Cl 102.6(2) . . ? C6 N1 C2 120.6(9) . . ? C6 N1 Co 120.3(7) . . ? C2 N1 Co 118.3(6) . . ? N1 C2 C3 119.9(9) . . ? N1 C2 C7 112.8(8) . . ? C3 C2 C7 127.3(10) . . ? C4 C3 C2 119.1(11) . . ? C5 C4 C3 120.6(11) . . ? C4 C5 C6 117.8(12) . . ? N1 C6 C5 121.9(11) . . ? N1 C6 C9 111.8(9) . . ? C5 C6 C9 126.3(10) . . ? N7 C7 C8 125.6(10) . . ? N7 C7 C2 116.2(9) . . ? C8 C7 C2 118.1(9) . . ? C7 N7 C11 120.9(8) . . ? C7 N7 Co 115.5(7) . . ? C11 N7 Co 123.5(6) . . ? N9 C9 C6 116.3(9) . . ? N9 C9 C10 125.3(11) . . ? C6 C9 C10 118.4(10) . . ? C9 N9 C23 119.2(9) . . ? C9 N9 Co 115.9(7) . . ? C23 N9 Co 124.9(7) . . ? C12 C11 C16 124.2(10) . . ? C12 C11 N7 116.5(10) . . ? C16 C11 N7 119.3(9) . . ? C11 C12 C13 115.5(12) . . ? C11 C12 C17 124.2(12) . . ? C13 C12 C17 120.3(12) . . ? C14 C13 C12 122.7(14) . . ? C13 C14 C15 120.4(14) . . ? C14 C15 C16 120.4(15) . . ? C11 C16 C15 116.8(12) . . ? C11 C16 C20 123.4(9) . . ? C15 C16 C20 119.8(12) . . ? C19 C17 C18 109.6(16) . . ? C19 C17 C12 112.9(16) . . ? C18 C17 C12 111.8(16) . . ? C16 C20 C22 109.7(11) . . ? C16 C20 C21 113.5(10) . . ? C22 C20 C21 110.9(12) . . ? C28 C23 C24 123.4(12) . . ? C28 C23 N9 117.4(13) . . ? C24 C23 N9 119.2(12) . . ? C25 C24 C23 117.6(16) . . ? C25 C24 C29 119.4(15) . . ? C23 C24 C29 122.8(12) . . ? C24 C25 C26 118.7(18) . . ? C27 C26 C25 119.8(14) . . ? C26 C27 C28 124.0(18) . . ? C23 C28 C27 116.3(17) . . ? C23 C28 C32 123.6(12) . . ? C27 C28 C32 120.1(16) . . ? C24 C29 C31 110.1(18) . . ? C24 C29 C30 111.6(15) . . ? C31 C29 C30 112.7(20) . . ? C34 C32 C28 113.9(20) . . ? C34 C32 C33 113.6(21) . . ? C28 C32 C33 113.5(16) . . ? C41 N40 Co 169.6(10) . . ? N40 C41 C42 177.8(15) . . ? F14 Sb F15 98.1(10) . . ? F14 Sb F11 92.9(7) . . ? F15 Sb F11 90.3(5) . . ? F14 Sb F12 175.4(10) . . ? F15 Sb F12 85.9(8) . . ? F11 Sb F12 89.2(6) . . ? F14 Sb F16 89.3(7) . . ? F15 Sb F16 90.7(6) . . ? F11 Sb F16 177.4(7) . . ? F12 Sb F16 88.5(7) . . ? F14 Sb F13 88.4(10) . . ? F15 Sb F13 173.3(8) . . ? F11 Sb F13 88.2(5) . . ? F12 Sb F13 87.6(8) . . ? F16 Sb F13 90.6(6) . . ? Cl2 C50 Cl1 121.9(18) . . ? Cl2' C50 Cl1' 109.0(28) . . ? Cl9 C60 Cl7 140.3(100) . . ? Cl9 C60 Cl5 36.4(58) . . ? Cl7 C60 Cl5 138.5(100) . . ? Cl9 C60 Cl4 114.9(98) . . ? Cl7 C60 Cl4 77.5(81) . . ? Cl5 C60 Cl4 143.3(100) . . ? Cl9 C60 C61 160.2(100) . . ? Cl7 C60 C61 30.3(63) . . ? Cl5 C60 C61 161.0(96) . . ? Cl4 C60 C61 53.9(53) . . ? Cl7 C61 Cl8 137.2(100) . . ? Cl7 C61 Cl6 84.7(100) . . ? Cl8 C61 Cl6 53.8(64) . . ? Cl7 C61 Cl4 77.5(100) . . ? Cl8 C61 Cl4 121.9(100) . . ? Cl6 C61 Cl4 133.4(88) . . ? Cl7 C61 Cl3 116.2(100) . . ? Cl8 C61 Cl3 84.1(89) . . ? Cl6 C61 Cl3 122.9(90) . . ? Cl4 C61 Cl3 40.6(37) . . ? Cl7 C61 C60 38.5(86) . . ? Cl8 C61 C60 163.0(100) . . ? Cl6 C61 C60 122.2(99) . . ? Cl4 C61 C60 46.2(46) . . ? Cl3 C61 C60 86.5(61) . . ? Cl4 Cl3 C61 68.7(54) . . ? Cl4 Cl3 Cl8 105.6(45) . . ? C61 Cl3 Cl8 39.1(45) . . ? Cl4 Cl3 Cl7 46.0(44) . . ? C61 Cl3 Cl7 24.4(48) . . ? Cl8 Cl3 Cl7 59.6(39) . . ? Cl4 Cl3 Cl6 82.8(39) . . ? C61 Cl3 Cl6 25.5(44) . . ? Cl8 Cl3 Cl6 24.4(26) . . ? Cl7 Cl3 Cl6 38.1(32) . . ? Cl3 Cl4 C60 149.3(76) . . ? Cl3 Cl4 C61 70.7(59) . . ? C60 Cl4 C61 79.9(70) . . ? Cl3 Cl4 Cl7 106.0(62) . . ? C60 Cl4 Cl7 47.9(52) . . ? C61 Cl4 Cl7 36.9(49) . . ? Cl3 Cl4 Cl9 178.6(57) . . ? C60 Cl4 Cl9 30.2(51) . . ? C61 Cl4 Cl9 108.5(65) . . ? Cl7 Cl4 Cl9 73.0(55) . . ? Cl3 Cl4 Cl8 48.6(35) . . ? C60 Cl4 Cl8 103.8(59) . . ? C61 Cl4 Cl8 24.8(50) . . ? Cl7 Cl4 Cl8 57.5(49) . . ? Cl9 Cl4 Cl8 130.4(41) . . ? Cl9 Cl5 C60 61.6(94) . . ? Cl9 Cl5 Cl7 71.4(100) . . ? C60 Cl5 Cl7 19.9(55) . . ? Cl8 Cl6 C61 58.4(65) . . ? Cl8 Cl6 Cl7 98.2(71) . . ? C61 Cl6 Cl7 40.4(60) . . ? Cl8 Cl6 Cl3 43.4(51) . . ? C61 Cl6 Cl3 31.6(56) . . ? Cl7 Cl6 Cl3 60.7(45) . . ? C61 Cl7 C60 111.2(100) . . ? C61 Cl7 Cl6 54.9(91) . . ? C60 Cl7 Cl6 162.3(100) . . ? C61 Cl7 Cl4 65.6(90) . . ? C60 Cl7 Cl4 54.5(64) . . ? Cl6 Cl7 Cl4 107.8(74) . . ? C61 Cl7 Cl8 23.1(83) . . ? C60 Cl7 Cl8 131.5(97) . . ? Cl6 Cl7 Cl8 32.7(35) . . ? Cl4 Cl7 Cl8 79.6(57) . . ? C61 Cl7 Cl3 39.4(80) . . ? C60 Cl7 Cl3 81.4(74) . . ? Cl6 Cl7 Cl3 81.2(54) . . ? Cl4 Cl7 Cl3 28.0(29) . . ? Cl8 Cl7 Cl3 51.6(36) . . ? C61 Cl7 Cl9 127.5(100) . . ? C60 Cl7 Cl9 19.5(60) . . ? Cl6 Cl7 Cl9 159.9(70) . . ? Cl4 Cl7 Cl9 64.2(51) . . ? Cl8 Cl7 Cl9 143.6(63) . . ? Cl3 Cl7 Cl9 92.2(47) . . ? C61 Cl7 Cl5 130.1(100) . . ? C60 Cl7 Cl5 21.7(62) . . ? Cl6 Cl7 Cl5 174.9(75) . . ? Cl4 Cl7 Cl5 76.0(55) . . ? Cl8 Cl7 Cl5 152.3(65) . . ? Cl3 Cl7 Cl5 103.0(50) . . ? Cl9 Cl7 Cl5 19.5(28) . . ? Cl6 Cl8 C61 67.9(74) . . ? Cl6 Cl8 Cl3 112.2(69) . . ? C61 Cl8 Cl3 56.8(71) . . ? Cl6 Cl8 Cl7 49.1(52) . . ? C61 Cl8 Cl7 19.7(69) . . ? Cl3 Cl8 Cl7 68.8(43) . . ? Cl6 Cl8 Cl4 87.9(61) . . ? C61 Cl8 Cl4 33.3(66) . . ? Cl3 Cl8 Cl4 25.8(19) . . ? Cl7 Cl8 Cl4 43.0(36) . . ? Cl5 Cl9 C60 82.0(100) . . ? Cl5 Cl9 Cl4 111.8(100) . . ? C60 Cl9 Cl4 34.8(60) . . ? Cl5 Cl9 Cl7 89.1(100) . . ? C60 Cl9 Cl7 20.2(63) . . ? Cl4 Cl9 Cl7 42.8(33) . . ? _refine_diff_density_max 0.542 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.098 data_VG0029 _database_code_CSD 168889 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H55 N3 O Cl5 Co Sb F6' _chemical_formula_weight 1053.79 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.982(3) _cell_length_b 14.094(3) _cell_length_c 17.000(3) _cell_angle_alpha 88.863(14) _cell_angle_beta 86.75(2) _cell_angle_gamma 83.77(2) _cell_volume 2373.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.82 _cell_measurement_theta_max 12.52 _exptl_crystal_description prisms _exptl_crystal_colour Green _exptl_crystal_size_max 0.83 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method ? _exptl_crystal_F_000 1070 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.66 _diffrn_reflns_number 8887 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8361 _reflns_number_observed 6404 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 549 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+0.6870P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7812 _refine_ls_number_parameters 551 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_obs 0.0523 _refine_ls_wR_factor_all 0.1464 _refine_ls_wR_factor_obs 0.1276 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.074 _refine_ls_restrained_S_all 1.087 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co Co 0.32510(5) 0.29186(4) 0.24371(3) 0.02750(14) Uani 1 d . . Cl Cl 0.53649(12) 0.30881(11) 0.20111(9) 0.0530(3) Uani 1 d . . O O 0.2789(6) 0.3922(3) 0.3318(3) 0.0646(12) Uani 1 d D . N1 N 0.1357(4) 0.2483(3) 0.2619(2) 0.0311(7) Uani 1 d . . C2 C 0.0345(4) 0.2913(4) 0.2225(3) 0.0355(9) Uani 1 d . . C3 C -0.0984(5) 0.2733(5) 0.2411(3) 0.0491(13) Uani 1 d . . H3A H -0.1709(5) 0.3041(5) 0.2131(3) 0.059 Uiso 1 calc R . C4 C -0.1214(6) 0.2089(5) 0.3021(4) 0.063(2) Uani 1 d . . H4A H -0.2110(6) 0.1965(5) 0.3172(4) 0.075 Uiso 1 calc R . C5 C -0.0134(6) 0.1625(5) 0.3411(4) 0.0531(14) Uani 1 d . . H5A H -0.0278(6) 0.1177(5) 0.3824(4) 0.064 Uiso 1 calc R . C6 C 0.1154(5) 0.1833(3) 0.3181(3) 0.0358(9) Uani 1 d . . C7 C 0.0777(4) 0.3534(3) 0.1567(3) 0.0334(9) Uani 1 d . . N7 N 0.2044(4) 0.3631(3) 0.1505(2) 0.0303(7) Uani 1 d . . C8 C -0.0263(5) 0.3936(5) 0.1010(3) 0.0536(14) Uani 1 d . . H8A H -0.0939(29) 0.4380(28) 0.1292(8) 0.080 Uiso 1 calc R . H8B H -0.0705(36) 0.3415(6) 0.0800(23) 0.080 Uiso 1 calc R . H8C H 0.0175(9) 0.4275(32) 0.0576(17) 0.080 Uiso 1 calc R . C9 C 0.2431(5) 0.1357(3) 0.3490(3) 0.0335(9) Uani 1 d . . N9 N 0.3525(4) 0.1658(2) 0.3190(2) 0.0295(7) Uani 1 d . . C10 C 0.2348(6) 0.0564(4) 0.4083(3) 0.0505(13) Uani 1 d . . H10A H 0.1952(46) 0.0037(15) 0.3849(10) 0.076 Uiso 1 calc R . H10B H 0.1783(41) 0.0797(10) 0.4544(13) 0.076 Uiso 1 calc R . H10C H 0.3256(8) 0.0339(24) 0.4245(22) 0.076 Uiso 1 calc R . C11 C 0.2574(4) 0.4141(3) 0.0829(3) 0.0313(9) Uani 1 d . . C12 C 0.3161(5) 0.3593(4) 0.0193(3) 0.0384(10) Uani 1 d . . C13 C 0.3612(5) 0.4077(4) -0.0480(3) 0.0428(11) Uani 1 d . . H13A H 0.3984(5) 0.3724(4) -0.0925(3) 0.051 Uiso 1 calc R . C14 C 0.3525(5) 0.5066(4) -0.0506(3) 0.0435(11) Uani 1 d . . H14A H 0.3836(5) 0.5386(4) -0.0967(3) 0.052 Uiso 1 calc R . C15 C 0.2993(5) 0.5579(4) 0.0130(3) 0.0401(10) Uani 1 d . . H15A H 0.2961(5) 0.6255(4) 0.0107(3) 0.048 Uiso 1 calc R . C16 C 0.2492(4) 0.5144(4) 0.0817(3) 0.0354(9) Uani 1 d . . C17 C 0.3284(6) 0.2508(4) 0.0218(3) 0.0446(11) Uani 1 d . . H17A H 0.3151(6) 0.2308(4) 0.0782(3) 0.053 Uiso 1 calc R . C18 C 0.4679(7) 0.2070(5) -0.0075(4) 0.0607(15) Uani 1 d . . H18A H 0.4715(7) 0.1372(5) -0.0049(4) 0.091 Uiso 1 calc R . H18B H 0.5359(7) 0.2279(5) 0.0257(4) 0.091 Uiso 1 calc R . H18C H 0.4861(7) 0.2275(5) -0.0621(4) 0.091 Uiso 1 calc R . C19 C 0.2183(9) 0.2124(6) -0.0231(6) 0.082(2) Uani 1 d . . H19A H 0.2290(9) 0.1425(6) -0.0204(6) 0.124 Uiso 1 calc R . H19B H 0.2255(9) 0.2335(6) -0.0784(6) 0.124 Uiso 1 calc R . H19C H 0.1296(9) 0.2365(6) 0.0005(6) 0.124 Uiso 1 calc R . C20 C 0.1928(5) 0.5750(4) 0.1507(3) 0.0431(11) Uani 1 d . . H20A H 0.1720(5) 0.5316(4) 0.1960(3) 0.052 Uiso 1 calc R . C21 C 0.0616(7) 0.6378(5) 0.1317(4) 0.064(2) Uani 1 d . . H21A H 0.0285(7) 0.6759(5) 0.1778(4) 0.095 Uiso 1 calc R . H21B H -0.0068(7) 0.5970(5) 0.1181(4) 0.095 Uiso 1 calc R . H21C H 0.0801(7) 0.6805(5) 0.0871(4) 0.095 Uiso 1 calc R . C22 C 0.2971(7) 0.6400(5) 0.1759(4) 0.0587(14) Uani 1 d . . H22A H 0.2587(7) 0.6786(5) 0.2207(4) 0.088 Uiso 1 calc R . H22B H 0.3202(7) 0.6821(5) 0.1318(4) 0.088 Uiso 1 calc R . H22C H 0.3786(7) 0.6006(5) 0.1914(4) 0.088 Uiso 1 calc R . C23 C 0.4816(5) 0.1168(3) 0.3399(3) 0.0331(9) Uani 1 d . . C24 C 0.5423(4) 0.1427(3) 0.4066(3) 0.0343(9) Uani 1 d . . C25 C 0.6636(5) 0.0920(4) 0.4257(3) 0.0437(11) Uani 1 d . . H25A H 0.7061(5) 0.1088(4) 0.4713(3) 0.052 Uiso 1 calc R . C26 C 0.7235(6) 0.0182(4) 0.3800(4) 0.0575(15) Uani 1 d . . H26A H 0.8054(6) -0.0166(4) 0.3946(4) 0.069 Uiso 1 calc R . C27 C 0.6641(8) -0.0048(5) 0.3130(4) 0.075(2) Uani 1 d . . H27A H 0.7065(8) -0.0555(5) 0.2813(4) 0.090 Uiso 1 calc R . C28 C 0.5432(7) 0.0442(4) 0.2901(4) 0.059(2) Uani 1 d . . C29 C 0.4841(6) 0.2243(5) 0.4582(4) 0.064(2) Uani 1 d . . H29A H 0.3937(6) 0.2487(5) 0.4391(4) 0.077 Uiso 1 calc R . C30 C 0.5760(11) 0.3053(5) 0.4486(7) 0.108(4) Uani 1 d . . H30A H 0.5866(11) 0.3231(5) 0.3928(7) 0.162 Uiso 1 calc R . H30B H 0.6647(11) 0.2835(5) 0.4684(7) 0.162 Uiso 1 calc R . H30C H 0.5353(11) 0.3608(5) 0.4786(7) 0.162 Uiso 1 calc R . C31 C 0.4648(10) 0.1944(10) 0.5432(5) 0.117(4) Uani 1 d . . H31A H 0.4268(10) 0.2498(10) 0.5743(5) 0.176 Uiso 1 calc R . H31B H 0.5520(10) 0.1692(10) 0.5630(5) 0.176 Uiso 1 calc R . H31C H 0.4029(10) 0.1449(10) 0.5476(5) 0.176 Uiso 1 calc R . C32 C 0.4811(11) 0.0182(6) 0.2155(5) 0.093(3) Uani 1 d . . H32A H 0.4029(11) 0.0669(6) 0.2062(5) 0.112 Uiso 1 calc R . C33 C 0.5816(18) 0.0210(8) 0.1449(5) 0.137(6) Uani 1 d . . H33A H 0.6144(18) 0.0841(8) 0.1409(5) 0.205 Uiso 1 calc R . H33B H 0.5372(18) 0.0086(8) 0.0968(5) 0.205 Uiso 1 calc R . H33C H 0.6578(18) -0.0279(8) 0.1517(5) 0.205 Uiso 1 calc R . C34 C 0.4287(12) -0.0776(11) 0.2235(7) 0.121(4) Uani 1 d . . H34A H 0.3891(12) -0.0926(11) 0.1744(7) 0.182 Uiso 1 calc R . H34B H 0.3596(12) -0.0764(11) 0.2670(7) 0.182 Uiso 1 calc R . H34C H 0.5031(12) -0.1265(11) 0.2345(7) 0.182 Uiso 1 calc R . C35 C 0.3826(16) 0.4678(9) 0.3273(8) 0.054(3) Uani 0.50 d PDU 1 H35A H 0.4762(16) 0.4365(9) 0.3279(8) 0.065 Uiso 0.50 calc PR 1 H35B H 0.3732(16) 0.5078(9) 0.2790(8) 0.065 Uiso 0.50 calc PR 1 C36 C 0.3468(16) 0.5264(11) 0.3997(10) 0.073(4) Uani 0.50 d PDU 1 H36A H 0.3097(16) 0.5920(11) 0.3852(10) 0.087 Uiso 0.50 calc PR 1 H36B H 0.4275(16) 0.5300(11) 0.4304(10) 0.087 Uiso 0.50 calc PR 1 C37 C 0.2395(17) 0.4749(11) 0.4482(8) 0.061(4) Uani 0.50 d PDU 1 H37A H 0.2818(17) 0.4308(11) 0.4880(8) 0.073 Uiso 0.50 calc PR 1 H37B H 0.1712(17) 0.5213(11) 0.4750(8) 0.073 Uiso 0.50 calc PR 1 C38 C 0.1776(16) 0.4207(12) 0.3859(10) 0.068(5) Uani 0.50 d PDU 1 H38A H 0.1380(16) 0.3648(12) 0.4098(10) 0.081 Uiso 0.50 calc PR 1 H38B H 0.1055(16) 0.4624(12) 0.3607(10) 0.081 Uiso 0.50 calc PR 1 C35' C 0.3238(15) 0.4773(9) 0.3518(8) 0.055(3) Uani 0.50 d PDU 2 H35C H 0.2815(15) 0.5296(9) 0.3187(8) 0.066 Uiso 0.50 calc PR 2 H35D H 0.4228(15) 0.4736(9) 0.3412(8) 0.066 Uiso 0.50 calc PR 2 C36' C 0.2905(17) 0.4986(11) 0.4355(9) 0.060(4) Uani 0.50 d PDU 2 H36C H 0.2885(17) 0.5677(11) 0.4455(9) 0.072 Uiso 0.50 calc PR 2 H36D H 0.3561(17) 0.4628(11) 0.4696(9) 0.072 Uiso 0.50 calc PR 2 C37' C 0.1477(18) 0.4646(11) 0.4493(8) 0.071(4) Uani 0.50 d PDU 2 H37C H 0.1311(18) 0.4436(11) 0.5045(8) 0.085 Uiso 0.50 calc PR 2 H37D H 0.0761(18) 0.5155(11) 0.4355(8) 0.085 Uiso 0.50 calc PR 2 C38' C 0.1559(17) 0.3830(12) 0.3941(9) 0.067(4) Uani 0.50 d PDU 2 H38C H 0.0708(17) 0.3843(12) 0.3666(9) 0.080 Uiso 0.50 calc PR 2 H38D H 0.1699(17) 0.3218(12) 0.4237(9) 0.080 Uiso 0.50 calc PR 2 Sb Sb 0.96102(3) 0.22139(3) 0.60241(2) 0.04691(13) Uani 1 d . . F1 F 0.9743(5) 0.1059(3) 0.5485(3) 0.0800(13) Uani 1 d . . F2 F 1.0213(11) 0.1598(6) 0.6906(4) 0.171(4) Uani 1 d . . F3 F 0.7814(5) 0.2135(5) 0.6293(5) 0.122(2) Uani 1 d . . F4 F 0.9080(7) 0.2872(4) 0.5098(3) 0.110(2) Uani 1 d . . F5 F 1.1371(5) 0.2333(5) 0.5684(4) 0.113(2) Uani 1 d . . F6 F 0.9480(5) 0.3385(3) 0.6545(3) 0.0854(13) Uani 1 d . . C40 C -0.0594(16) 0.0711(12) -0.1278(9) 0.146(6) Uani 1 d . . H40A H -0.0871(16) 0.1136(12) -0.1724(9) 0.175 Uiso 1 calc R . H40B H 0.0360(16) 0.0783(12) -0.1185(9) 0.175 Uiso 1 calc R . Cl1 Cl -0.1621(4) 0.1031(3) -0.0427(2) 0.1367(12) Uani 1 d . . Cl2 Cl -0.0760(7) -0.0472(4) -0.1503(3) 0.204(3) Uani 1 d . . C50 C -0.2347(10) 0.6165(7) 0.3033(8) 0.114(4) Uani 1 d D . H50A H -0.2241(10) 0.6473(7) 0.3541(8) 0.137 Uiso 0.70 calc PR 1 H50B H -0.1651(10) 0.6373(7) 0.2649(8) 0.137 Uiso 0.70 calc PR 1 H50C H -0.2544(10) 0.6284(7) 0.3584(8) 0.137 Uiso 0.30 d PR 2 H50D H -0.1385(10) 0.6057(7) 0.2942(8) 0.137 Uiso 0.30 d PR 2 Cl3 Cl -0.3920(5) 0.6557(4) 0.2707(3) 0.1195(15) Uani 0.70 d PD 1 Cl4 Cl -0.2062(7) 0.4926(3) 0.3163(5) 0.160(3) Uani 0.70 d PD 1 Cl3' Cl -0.3152(17) 0.7042(11) 0.2447(9) 0.153(5) Uiso 0.30 d PD 2 Cl4' Cl -0.2795(19) 0.5079(10) 0.2843(10) 0.156(5) Uiso 0.30 d PD 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 Co 0.0255(3) 0.0291(3) 0.0289(3) 0.0056(2) -0.0028(2) -0.0077(2) Cl 0.0279(5) 0.0710(8) 0.0617(8) 0.0303(7) -0.0058(5) -0.0169(5) O 0.107(4) 0.035(2) 0.054(2) -0.006(2) -0.020(2) -0.005(2) N1 0.028(2) 0.038(2) 0.028(2) 0.0025(14) 0.0013(13) -0.0078(14) C2 0.022(2) 0.046(2) 0.037(2) 0.002(2) 0.002(2) -0.004(2) C3 0.025(2) 0.069(3) 0.053(3) 0.017(3) 0.002(2) -0.009(2) C4 0.031(3) 0.088(5) 0.070(4) 0.031(3) 0.004(2) -0.018(3) C5 0.038(3) 0.067(4) 0.055(3) 0.021(3) 0.005(2) -0.019(2) C6 0.035(2) 0.040(2) 0.033(2) 0.009(2) 0.002(2) -0.009(2) C7 0.025(2) 0.044(2) 0.031(2) 0.007(2) -0.003(2) -0.004(2) N7 0.027(2) 0.037(2) 0.028(2) 0.0037(14) -0.0022(13) -0.0054(14) C8 0.031(2) 0.078(4) 0.052(3) 0.028(3) -0.011(2) -0.010(2) C9 0.039(2) 0.030(2) 0.032(2) 0.005(2) -0.003(2) -0.008(2) N9 0.034(2) 0.028(2) 0.027(2) 0.0040(13) 0.0006(14) -0.0072(14) C10 0.051(3) 0.048(3) 0.053(3) 0.024(2) 0.003(2) -0.011(2) C11 0.022(2) 0.042(2) 0.031(2) 0.011(2) -0.003(2) -0.006(2) C12 0.029(2) 0.048(3) 0.038(2) 0.006(2) -0.001(2) -0.006(2) C13 0.036(2) 0.062(3) 0.029(2) 0.005(2) 0.002(2) -0.006(2) C14 0.034(2) 0.064(3) 0.033(2) 0.021(2) -0.003(2) -0.009(2) C15 0.034(2) 0.047(3) 0.042(3) 0.017(2) -0.008(2) -0.011(2) C16 0.025(2) 0.047(3) 0.035(2) 0.012(2) -0.005(2) -0.006(2) C17 0.050(3) 0.045(3) 0.037(2) 0.001(2) 0.005(2) 0.001(2) C18 0.058(4) 0.060(4) 0.062(4) -0.012(3) 0.012(3) -0.001(3) C19 0.073(5) 0.062(4) 0.116(7) -0.007(4) -0.021(5) -0.015(4) C20 0.045(3) 0.043(3) 0.041(3) 0.005(2) 0.003(2) -0.007(2) C21 0.049(3) 0.066(4) 0.071(4) -0.004(3) 0.005(3) 0.008(3) C22 0.065(4) 0.056(3) 0.057(3) -0.006(3) 0.003(3) -0.021(3) C23 0.037(2) 0.026(2) 0.034(2) 0.011(2) 0.004(2) 0.001(2) C24 0.024(2) 0.038(2) 0.042(2) 0.010(2) 0.000(2) -0.007(2) C25 0.033(2) 0.044(3) 0.054(3) 0.020(2) -0.004(2) -0.007(2) C26 0.048(3) 0.049(3) 0.071(4) 0.023(3) -0.001(3) 0.013(2) C27 0.086(5) 0.060(4) 0.069(4) -0.007(3) -0.006(4) 0.038(4) C28 0.075(4) 0.048(3) 0.048(3) -0.006(2) -0.005(3) 0.022(3) C29 0.037(3) 0.078(4) 0.078(4) -0.035(3) -0.025(3) 0.011(3) C30 0.124(8) 0.044(4) 0.165(10) -0.022(5) -0.089(7) 0.001(4) C31 0.074(5) 0.203(13) 0.073(5) -0.063(7) 0.004(4) 0.001(7) C32 0.117(7) 0.082(5) 0.072(5) -0.038(4) -0.032(5) 0.049(5) C33 0.265(18) 0.086(6) 0.056(5) -0.008(4) 0.007(7) -0.009(9) C34 0.105(8) 0.176(13) 0.089(7) -0.040(8) -0.018(6) -0.027(8) C35 0.066(7) 0.040(5) 0.059(6) -0.018(5) -0.011(6) -0.010(5) C36 0.073(7) 0.060(7) 0.088(8) -0.030(6) -0.005(6) -0.013(6) C37 0.059(8) 0.064(7) 0.057(7) -0.027(6) -0.006(6) 0.006(6) C38 0.082(8) 0.048(7) 0.072(8) -0.031(6) -0.003(6) 0.003(6) C35' 0.057(7) 0.043(6) 0.065(7) -0.013(5) -0.011(6) -0.005(5) C36' 0.067(8) 0.054(7) 0.059(7) -0.017(6) -0.007(6) -0.004(6) C37' 0.086(8) 0.067(7) 0.059(6) -0.016(6) 0.001(6) -0.004(6) C38' 0.083(8) 0.057(8) 0.057(7) -0.028(6) 0.004(6) 0.011(6) Sb 0.0338(2) 0.0456(2) 0.0611(2) -0.0084(2) -0.00411(14) -0.00143(13) F1 0.080(3) 0.048(2) 0.112(3) -0.026(2) 0.020(2) -0.018(2) F2 0.262(11) 0.151(6) 0.076(4) 0.014(4) -0.042(5) 0.096(7) F3 0.060(3) 0.136(5) 0.171(6) -0.045(5) 0.034(3) -0.026(3) F4 0.141(5) 0.092(4) 0.091(3) 0.001(3) -0.028(3) 0.024(3) F5 0.052(2) 0.117(4) 0.174(6) -0.053(4) 0.022(3) -0.030(3) F6 0.082(3) 0.068(3) 0.107(3) -0.036(2) -0.017(3) 0.000(2) C40 0.134(11) 0.160(13) 0.149(12) -0.048(10) 0.020(9) -0.054(10) Cl1 0.148(3) 0.138(3) 0.121(2) -0.012(2) 0.003(2) -0.004(2) Cl2 0.291(7) 0.141(3) 0.179(4) -0.070(3) -0.063(5) 0.017(4) C50 0.078(6) 0.095(7) 0.173(12) -0.034(7) -0.012(7) -0.018(5) Cl3 0.105(3) 0.160(4) 0.096(2) -0.038(3) -0.042(2) -0.001(3) Cl4 0.157(5) 0.078(2) 0.250(7) -0.037(3) -0.066(5) 0.002(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 Co N1 2.056(4) . ? Co O 2.079(4) . ? Co N9 2.171(3) . ? Co N7 2.205(4) . ? Co Cl 2.2279(14) . ? O C38 1.360(15) . ? O C35' 1.381(12) . ? O C35 1.562(13) . ? O C38' 1.589(15) . ? N1 C2 1.328(6) . ? N1 C6 1.332(6) . ? C2 C3 1.396(7) . ? C2 C7 1.480(6) . ? C3 C4 1.390(8) . ? C4 C5 1.393(9) . ? C5 C6 1.383(7) . ? C6 C9 1.493(6) . ? C7 N7 1.285(6) . ? C7 C8 1.503(6) . ? N7 C11 1.448(5) . ? C9 N9 1.289(6) . ? C9 C10 1.496(6) . ? N9 C23 1.454(6) . ? C11 C12 1.404(7) . ? C11 C16 1.407(7) . ? C12 C13 1.398(7) . ? C12 C17 1.520(7) . ? C13 C14 1.387(8) . ? C14 C15 1.362(8) . ? C15 C16 1.400(7) . ? C16 C20 1.512(7) . ? C17 C18 1.522(8) . ? C17 C19 1.525(9) . ? C20 C22 1.543(8) . ? C20 C21 1.545(8) . ? C23 C24 1.388(7) . ? C23 C28 1.408(7) . ? C24 C25 1.389(7) . ? C24 C29 1.506(7) . ? C25 C26 1.374(9) . ? C26 C27 1.375(11) . ? C27 C28 1.395(9) . ? C28 C32 1.510(10) . ? C29 C31 1.504(13) . ? C29 C30 1.542(12) . ? C32 C34 1.50(2) . ? C32 C33 1.52(2) . ? C35 C36 1.50(2) . ? C36 C37 1.55(2) . ? C37 C38 1.51(2) . ? C35' C36' 1.47(2) . ? C36' C37' 1.56(2) . ? C37' C38' 1.49(2) . ? Sb F2 1.817(5) . ? Sb F3 1.840(5) . ? Sb F5 1.843(5) . ? Sb F1 1.873(4) . ? Sb F6 1.877(4) . ? Sb F4 1.883(5) . ? C40 Cl2 1.746(15) . ? C40 Cl1 1.762(14) . ? C50 Cl4' 1.68(2) . ? C50 Cl3 1.725(10) . ? C50 Cl3' 1.729(15) . ? C50 Cl4 1.751(10) . ? 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 Co O 89.6(2) . . ? N1 Co N9 74.98(14) . . ? O Co N9 97.85(15) . . ? N1 Co N7 74.39(14) . . ? O Co N7 98.9(2) . . ? N9 Co N7 144.78(14) . . ? N1 Co Cl 165.05(12) . . ? O Co Cl 105.3(2) . . ? N9 Co Cl 101.94(11) . . ? N7 Co Cl 103.15(10) . . ? C38 O C35 108.7(9) . . ? C35' O C38' 102.8(10) . . ? C38 O Co 140.0(7) . . ? C35' O Co 136.5(7) . . ? C35 O Co 110.5(6) . . ? C38' O Co 120.6(6) . . ? C2 N1 C6 121.6(4) . . ? C2 N1 Co 119.4(3) . . ? C6 N1 Co 118.8(3) . . ? N1 C2 C3 121.0(4) . . ? N1 C2 C7 114.0(4) . . ? C3 C2 C7 125.0(4) . . ? C4 C3 C2 117.9(5) . . ? C3 C4 C5 120.2(5) . . ? C6 C5 C4 118.2(5) . . ? N1 C6 C5 121.0(5) . . ? N1 C6 C9 113.3(4) . . ? C5 C6 C9 125.6(4) . . ? N7 C7 C2 115.6(4) . . ? N7 C7 C8 126.2(4) . . ? C2 C7 C8 118.1(4) . . ? C7 N7 C11 119.1(4) . . ? C7 N7 Co 115.3(3) . . ? C11 N7 Co 125.5(3) . . ? N9 C9 C6 115.4(4) . . ? N9 C9 C10 125.9(4) . . ? C6 C9 C10 118.7(4) . . ? C9 N9 C23 118.9(3) . . ? C9 N9 Co 115.5(3) . . ? C23 N9 Co 125.5(3) . . ? C12 C11 C16 122.0(4) . . ? C12 C11 N7 117.2(4) . . ? C16 C11 N7 120.8(4) . . ? C13 C12 C11 117.8(5) . . ? C13 C12 C17 120.3(5) . . ? C11 C12 C17 121.8(4) . . ? C14 C13 C12 120.9(5) . . ? C15 C14 C13 120.0(4) . . ? C14 C15 C16 122.3(5) . . ? C15 C16 C11 117.0(5) . . ? C15 C16 C20 119.9(5) . . ? C11 C16 C20 123.1(4) . . ? C12 C17 C18 112.1(5) . . ? C12 C17 C19 111.5(5) . . ? C18 C17 C19 111.2(5) . . ? C16 C20 C22 110.7(4) . . ? C16 C20 C21 112.1(5) . . ? C22 C20 C21 108.9(5) . . ? C24 C23 C28 121.6(5) . . ? C24 C23 N9 120.4(4) . . ? C28 C23 N9 118.1(5) . . ? C23 C24 C25 118.5(5) . . ? C23 C24 C29 123.0(4) . . ? C25 C24 C29 118.5(5) . . ? C26 C25 C24 121.3(5) . . ? C25 C26 C27 119.5(5) . . ? C26 C27 C28 121.8(6) . . ? C27 C28 C23 117.2(6) . . ? C27 C28 C32 120.7(6) . . ? C23 C28 C32 122.1(6) . . ? C31 C29 C24 112.5(7) . . ? C31 C29 C30 111.4(7) . . ? C24 C29 C30 108.8(6) . . ? C34 C32 C28 111.3(8) . . ? C34 C32 C33 110.9(8) . . ? C28 C32 C33 110.9(10) . . ? C36 C35 O 104.0(10) . . ? C35 C36 C37 105.8(9) . . ? C38 C37 C36 102.8(10) . . ? O C38 C37 106.7(11) . . ? O C35' C36' 111.0(11) . . ? C35' C36' C37' 102.7(10) . . ? C38' C37' C36' 101.6(10) . . ? C37' C38' O 108.3(11) . . ? F2 Sb F3 94.9(5) . . ? F2 Sb F5 89.4(4) . . ? F3 Sb F5 175.8(4) . . ? F2 Sb F1 90.9(3) . . ? F3 Sb F1 91.3(2) . . ? F5 Sb F1 88.3(2) . . ? F2 Sb F6 90.2(3) . . ? F3 Sb F6 89.1(3) . . ? F5 Sb F6 91.2(2) . . ? F1 Sb F6 178.8(2) . . ? F2 Sb F4 176.9(4) . . ? F3 Sb F4 88.2(4) . . ? F5 Sb F4 87.6(3) . . ? F1 Sb F4 89.7(2) . . ? F6 Sb F4 89.2(2) . . ? Cl2 C40 Cl1 109.0(9) . . ? Cl4' C50 Cl3' 111.7(10) . . ? Cl3 C50 Cl4 114.0(6) . . ? _refine_diff_density_max 0.869 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.096 data_VG9859 _database_code_CSD 168890 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H49 N3 O Cl5 Fe Sb F6' _chemical_formula_weight 996.62 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.938(2) _cell_length_b 24.269(3) _cell_length_c 18.711(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.90(2) _cell_angle_gamma 90.00 _cell_volume 4361.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 10.81 _cell_measurement_theta_max 24.96 _exptl_crystal_description needles _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method ? _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 10.886 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1442 _exptl_absorpt_correction_T_max 0.6163 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6684 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 60.02 _reflns_number_total 6269 _reflns_number_observed 3729 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 821 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+1.0096P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5448 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_obs 0.0646 _refine_ls_wR_factor_all 0.2526 _refine_ls_wR_factor_obs 0.1508 _refine_ls_goodness_of_fit_all 1.078 _refine_ls_goodness_of_fit_obs 1.123 _refine_ls_restrained_S_all 1.422 _refine_ls_restrained_S_obs 1.123 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.29821(14) 0.59771(5) 0.74291(6) 0.0292(3) Uani 1 d . . Cl Cl 0.0667(3) 0.59637(11) 0.70254(12) 0.0489(6) Uani 1 d . . O1 O 0.3733(8) 0.5445(2) 0.8344(3) 0.044(2) Uani 1 d . . N1 N 0.5038(8) 0.6218(3) 0.7590(3) 0.029(2) Uani 1 d . . C2 C 0.5909(10) 0.5954(3) 0.7246(4) 0.032(2) Uani 1 d . . C3 C 0.7273(12) 0.6070(4) 0.7374(5) 0.045(2) Uani 1 d . . H3A H 0.7827(12) 0.5886(4) 0.7111(5) 0.054 Uiso 1 calc R . C4 C 0.7852(12) 0.6465(4) 0.7900(5) 0.046(2) Uani 1 d . . H4A H 0.8812(12) 0.6540(4) 0.8017(5) 0.055 Uiso 1 calc R . C5 C 0.6989(10) 0.6747(4) 0.8251(5) 0.037(2) Uani 1 d . . H5A H 0.7349(10) 0.7024(4) 0.8599(5) 0.044 Uiso 1 calc R . C6 C 0.5589(10) 0.6614(3) 0.8081(4) 0.034(2) Uani 1 d . . C7 C 0.5098(10) 0.5574(3) 0.6653(5) 0.035(2) Uani 1 d . . N7 N 0.3790(8) 0.5544(3) 0.6583(3) 0.032(2) Uani 1 d . . C8 C 0.5887(11) 0.5284(4) 0.6183(5) 0.046(2) Uani 1 d . . H8A H 0.6693(11) 0.5108(4) 0.6493(5) 0.069 Uiso 1 d R . H8B H 0.6173(11) 0.5549(4) 0.5870(5) 0.069 Uiso 1 d R . H8C H 0.5301(11) 0.5012(4) 0.5883(5) 0.069 Uiso 1 d R . C9 C 0.4478(10) 0.6895(3) 0.8377(4) 0.029(2) Uani 1 d . . N9 N 0.3270(8) 0.6731(3) 0.8130(3) 0.030(2) Uani 1 d . . C10 C 0.4926(13) 0.7370(4) 0.8901(5) 0.052(3) Uani 1 d . . H10A H 0.5126(13) 0.7684(4) 0.8634(5) 0.078 Uiso 1 d R . H10B H 0.5744(13) 0.7269(4) 0.9278(5) 0.078 Uiso 1 d R . H10C H 0.4188(13) 0.7459(4) 0.9127(5) 0.078 Uiso 1 d R . C11 C 0.2943(9) 0.5230(3) 0.5961(4) 0.030(2) Uani 1 d . . C12 C 0.2500(12) 0.5499(4) 0.5284(5) 0.042(2) Uani 1 d . . C13 C 0.1663(11) 0.5190(4) 0.4685(5) 0.042(2) Uani 1 d . . H13A H 0.1305(11) 0.5359(4) 0.4223(5) 0.050 Uiso 1 calc R . C14 C 0.1380(11) 0.4646(4) 0.4782(5) 0.042(2) Uani 1 d . . H14A H 0.0884(11) 0.4438(4) 0.4376(5) 0.051 Uiso 1 calc R . C15 C 0.1804(11) 0.4404(4) 0.5453(5) 0.042(2) Uani 1 d . . H15A H 0.1552(11) 0.4036(4) 0.5506(5) 0.050 Uiso 1 calc R . C16 C 0.2598(11) 0.4680(3) 0.6067(5) 0.036(2) Uani 1 d . . C17 C 0.2826(12) 0.6095(4) 0.5170(5) 0.045(3) Uani 1 d . . H17A H 0.3622(12) 0.6196(4) 0.5589(5) 0.054 Uiso 1 calc R . C18 C 0.1681(19) 0.6467(5) 0.5206(9) 0.097(6) Uani 1 d . . H18A H 0.1942(19) 0.6843(5) 0.5129(9) 0.145 Uiso 1 calc R . H18B H 0.1491(19) 0.6436(5) 0.5687(9) 0.145 Uiso 1 calc R . H18C H 0.0854(19) 0.6368(5) 0.4824(9) 0.145 Uiso 1 calc R . C19 C 0.3301(24) 0.6192(6) 0.4472(9) 0.133(9) Uani 1 d . . H19A H 0.4056(24) 0.5941(6) 0.4461(9) 0.199 Uiso 1 calc R . H19B H 0.3621(24) 0.6569(6) 0.4465(9) 0.199 Uiso 1 calc R . H19C H 0.2529(24) 0.6127(6) 0.4042(9) 0.199 Uiso 1 calc R . C20 C 0.3054(13) 0.4403(4) 0.6821(5) 0.047(3) Uani 1 d . . H20A H 0.3668(13) 0.4662(4) 0.7166(5) 0.057 Uiso 1 calc R . C21 C 0.3870(19) 0.3872(5) 0.6802(8) 0.094(6) Uani 1 d . . H21A H 0.4136(19) 0.3711(5) 0.7293(8) 0.141 Uiso 1 calc R . H21B H 0.4700(19) 0.3954(5) 0.6639(8) 0.141 Uiso 1 calc R . H21C H 0.3293(19) 0.3613(5) 0.6462(8) 0.141 Uiso 1 calc R . C22 C 0.1778(16) 0.4292(6) 0.7112(7) 0.079(4) Uani 1 d . . H22A H 0.2066(16) 0.4115(6) 0.7592(7) 0.118 Uiso 1 calc R . H22B H 0.1139(16) 0.4053(6) 0.6770(7) 0.118 Uiso 1 calc R . H22C H 0.1319(16) 0.4638(6) 0.7159(7) 0.118 Uiso 1 calc R . C23 C 0.2133(10) 0.7022(3) 0.8312(4) 0.033(2) Uani 1 d . . C24 C 0.1687(11) 0.6870(3) 0.8941(4) 0.036(2) Uani 1 d . . C25 C 0.0610(11) 0.7165(4) 0.9098(5) 0.045(2) Uani 1 d . . H25A H 0.0292(11) 0.7069(4) 0.9513(5) 0.054 Uiso 1 calc R . C26 C -0.0016(13) 0.7603(4) 0.8655(6) 0.055(3) Uani 1 d . . H26A H -0.0722(13) 0.7809(4) 0.8780(6) 0.066 Uiso 1 calc R . C27 C 0.0414(13) 0.7730(4) 0.8027(6) 0.054(3) Uani 1 d . . H27A H -0.0027(13) 0.8019(4) 0.7721(6) 0.064 Uiso 1 calc R . C28 C 0.1476(11) 0.7443(4) 0.7838(5) 0.041(2) Uani 1 d . . C29 C 0.2358(13) 0.6388(4) 0.9419(5) 0.048(3) Uani 1 d . . H29A H 0.3214(13) 0.6280(4) 0.9276(5) 0.058 Uiso 1 calc R . C30 C 0.1344(16) 0.5897(4) 0.9281(7) 0.070(4) Uani 1 d . . H30A H 0.1767(16) 0.5588(4) 0.9585(7) 0.105 Uiso 1 calc R . H30B H 0.1134(16) 0.5793(4) 0.8764(7) 0.105 Uiso 1 calc R . H30C H 0.0491(16) 0.6001(4) 0.9407(7) 0.105 Uiso 1 calc R . C31 C 0.2745(17) 0.6533(6) 1.0239(5) 0.081(4) Uani 1 d . . H31A H 0.3169(17) 0.6216(6) 1.0525(5) 0.121 Uiso 1 calc R . H31B H 0.1913(17) 0.6638(6) 1.0386(5) 0.121 Uiso 1 calc R . H31C H 0.3399(17) 0.6838(6) 1.0328(5) 0.121 Uiso 1 calc R . C32 C 0.1901(12) 0.7595(4) 0.7144(5) 0.048(3) Uani 1 d . . H32A H 0.2607(12) 0.7322(4) 0.7086(5) 0.058 Uiso 1 calc R . C33 C 0.0713(17) 0.7562(5) 0.6461(6) 0.074(4) Uani 1 d . . H33A H 0.0295(17) 0.7199(5) 0.6427(6) 0.111 Uiso 1 calc R . H33B H 0.1056(17) 0.7628(5) 0.6028(6) 0.111 Uiso 1 calc R . H33C H 0.0021(17) 0.7838(5) 0.6487(6) 0.111 Uiso 1 calc R . C34 C 0.2592(18) 0.8154(6) 0.7224(7) 0.093(5) Uani 1 d . . H34A H 0.3352(18) 0.8160(6) 0.7669(7) 0.139 Uiso 1 calc R . H34B H 0.1916(18) 0.8435(6) 0.7257(7) 0.139 Uiso 1 calc R . H34C H 0.2952(18) 0.8225(6) 0.6798(7) 0.139 Uiso 1 calc R . Sb Sb 0.73594(8) 0.59996(3) 1.03579(3) 0.0481(2) Uani 1 d . . F11 F 0.7873(10) 0.6631(3) 0.9939(4) 0.105(3) Uani 1 d . . F12 F 0.5940(14) 0.5860(4) 0.9532(5) 0.140(5) Uani 1 d . . F13 F 0.8539(15) 0.5587(4) 1.0001(8) 0.158(5) Uani 1 d . . F14 F 0.8743(14) 0.6167(4) 1.1180(4) 0.134(5) Uani 1 d . . F15 F 0.6233(15) 0.6411(4) 1.0747(8) 0.170(6) Uani 1 d . . F16 F 0.6865(11) 0.5388(3) 1.0798(4) 0.106(3) Uani 1 d . . C40 C -0.1676(18) 0.4706(6) 0.8563(7) 0.087(4) Uani 1 d . . H40A H -0.1379(18) 0.5016(6) 0.8903(7) 0.104 Uiso 1 calc R . H40B H -0.1318(18) 0.4368(6) 0.8830(7) 0.104 Uiso 1 calc R . Cl1 Cl -0.3474(4) 0.4680(2) 0.8313(2) 0.0921(11) Uani 1 d . . Cl2 Cl -0.0953(6) 0.4778(2) 0.7835(3) 0.124(2) Uani 1 d . . C50 C 0.3135(19) 0.2720(6) 0.3887(9) 0.098(5) Uani 1 d . . H50A H 0.2400(19) 0.2745(6) 0.3425(9) 0.117 Uiso 1 calc R . H50B H 0.3021(19) 0.2366(6) 0.4118(9) 0.117 Uiso 1 calc R . Cl3 Cl 0.4728(6) 0.2719(2) 0.3676(3) 0.124(2) Uani 1 d . . Cl4 Cl 0.2906(6) 0.3235(2) 0.4458(2) 0.118(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0278(8) 0.0312(6) 0.0303(6) -0.0033(5) 0.0105(5) -0.0009(7) Cl 0.0312(14) 0.0671(14) 0.0475(11) -0.0141(11) 0.0087(10) -0.0024(13) O1 0.057(5) 0.036(3) 0.043(3) 0.003(3) 0.017(3) -0.003(3) N1 0.029(4) 0.028(3) 0.033(3) 0.003(3) 0.010(3) 0.003(3) C2 0.036(6) 0.029(4) 0.038(4) 0.000(3) 0.022(4) 0.002(4) C3 0.048(7) 0.047(5) 0.048(5) 0.001(4) 0.027(5) -0.004(5) C4 0.035(7) 0.052(5) 0.051(5) -0.007(4) 0.011(5) -0.008(5) C5 0.024(6) 0.045(5) 0.039(4) -0.007(4) 0.003(4) -0.005(4) C6 0.035(6) 0.037(4) 0.033(4) -0.004(3) 0.012(4) 0.001(4) C7 0.030(6) 0.035(4) 0.041(4) 0.002(3) 0.011(4) 0.002(4) N7 0.034(5) 0.030(3) 0.033(3) -0.003(3) 0.011(3) 0.001(3) C8 0.037(7) 0.053(5) 0.052(5) -0.021(4) 0.016(5) -0.005(5) C9 0.028(6) 0.030(4) 0.029(4) -0.005(3) 0.007(4) 0.000(4) N9 0.027(5) 0.033(3) 0.030(3) 0.005(3) 0.004(3) 0.005(4) C10 0.059(9) 0.052(5) 0.045(5) -0.028(4) 0.013(5) -0.011(6) C11 0.021(5) 0.042(4) 0.028(4) -0.007(3) 0.007(4) 0.000(4) C12 0.046(7) 0.045(5) 0.039(4) -0.003(4) 0.018(4) -0.002(5) C13 0.028(6) 0.063(6) 0.032(4) -0.009(4) 0.003(4) -0.004(5) C14 0.030(6) 0.056(6) 0.044(5) -0.015(4) 0.016(4) -0.005(5) C15 0.043(7) 0.040(5) 0.046(5) -0.011(4) 0.017(5) -0.007(5) C16 0.034(6) 0.037(4) 0.041(4) 0.000(4) 0.016(4) 0.004(4) C17 0.051(7) 0.044(5) 0.034(4) 0.005(4) -0.001(4) -0.015(5) C18 0.116(16) 0.058(7) 0.145(13) 0.021(8) 0.083(12) 0.019(9) C19 0.242(27) 0.078(9) 0.123(13) -0.017(9) 0.129(17) -0.069(13) C20 0.067(9) 0.033(4) 0.045(5) 0.006(4) 0.018(5) 0.000(5) C21 0.134(17) 0.075(9) 0.083(9) 0.015(7) 0.046(10) 0.050(10) C22 0.090(12) 0.095(9) 0.061(7) 0.017(7) 0.037(8) -0.011(9) C23 0.034(6) 0.032(4) 0.032(4) -0.007(3) 0.009(4) -0.001(4) C24 0.036(6) 0.038(4) 0.038(4) -0.010(4) 0.014(4) -0.003(4) C25 0.040(7) 0.057(6) 0.043(5) -0.012(4) 0.020(4) 0.003(5) C26 0.064(9) 0.041(5) 0.069(6) -0.020(5) 0.032(6) 0.006(6) C27 0.057(9) 0.034(5) 0.072(6) 0.001(5) 0.019(6) 0.004(5) C28 0.028(6) 0.037(4) 0.059(5) -0.001(4) 0.014(5) 0.005(4) C29 0.057(8) 0.056(6) 0.041(5) 0.009(4) 0.026(5) 0.013(5) C30 0.080(11) 0.046(6) 0.087(8) 0.010(6) 0.026(7) -0.001(6) C31 0.103(13) 0.098(10) 0.039(6) 0.005(6) 0.014(6) 0.014(9) C32 0.043(7) 0.048(5) 0.055(6) 0.019(4) 0.012(5) 0.010(5) C33 0.111(13) 0.060(7) 0.048(6) 0.005(5) 0.016(7) 0.002(8) C34 0.114(15) 0.109(11) 0.059(7) 0.013(7) 0.028(8) -0.053(10) Sb 0.0539(5) 0.0446(3) 0.0453(3) 0.0090(3) 0.0121(3) 0.0028(4) F11 0.109(8) 0.096(5) 0.087(5) 0.037(4) -0.016(5) -0.043(5) F12 0.179(13) 0.114(7) 0.085(5) 0.017(5) -0.043(6) -0.058(7) F13 0.161(13) 0.125(8) 0.238(13) -0.052(8) 0.140(11) -0.006(8) F14 0.185(13) 0.112(7) 0.074(5) 0.024(5) -0.024(6) -0.036(7) F15 0.144(13) 0.104(7) 0.293(15) -0.076(9) 0.112(12) 0.006(7) F16 0.137(10) 0.083(5) 0.100(5) 0.027(4) 0.031(6) -0.033(6) C40 0.094(13) 0.097(10) 0.078(8) 0.006(8) 0.038(8) -0.005(9) Cl1 0.064(3) 0.099(2) 0.115(3) 0.025(2) 0.027(2) 0.010(2) Cl2 0.119(4) 0.144(4) 0.136(3) 0.067(3) 0.081(3) 0.057(3) C50 0.081(13) 0.092(10) 0.127(13) 0.043(10) 0.038(10) 0.016(10) Cl3 0.116(5) 0.108(3) 0.154(4) 0.059(3) 0.046(3) 0.016(3) Cl4 0.139(5) 0.094(3) 0.112(3) 0.001(2) 0.016(3) 0.000(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 Fe N1 2.072(8) . ? Fe O1 2.121(6) . ? Fe N7 2.217(7) . ? Fe N9 2.227(7) . ? Fe Cl 2.230(3) . ? N1 C6 1.343(11) . ? N1 C2 1.364(11) . ? C2 C3 1.344(14) . ? C2 C7 1.507(12) . ? C3 C4 1.389(13) . ? C4 C5 1.388(13) . ? C5 C6 1.383(13) . ? C6 C9 1.519(12) . ? C7 N7 1.274(12) . ? C7 C8 1.497(12) . ? N7 C11 1.462(10) . ? C9 N9 1.236(11) . ? C9 C10 1.504(11) . ? N9 C23 1.445(11) . ? C11 C12 1.391(12) . ? C11 C16 1.404(12) . ? C12 C13 1.425(13) . ? C12 C17 1.509(12) . ? C13 C14 1.372(13) . ? C14 C15 1.351(13) . ? C15 C16 1.388(13) . ? C16 C20 1.524(12) . ? C17 C18 1.47(2) . ? C17 C19 1.517(15) . ? C20 C22 1.53(2) . ? C20 C21 1.528(15) . ? C23 C28 1.400(12) . ? C23 C24 1.410(11) . ? C24 C25 1.382(13) . ? C24 C29 1.518(13) . ? C25 C26 1.392(14) . ? C26 C27 1.385(14) . ? C27 C28 1.383(14) . ? C28 C32 1.511(13) . ? C29 C31 1.523(13) . ? C29 C30 1.54(2) . ? C32 C33 1.50(2) . ? C32 C34 1.51(2) . ? Sb F15 1.789(10) . ? Sb F13 1.796(9) . ? Sb F16 1.825(7) . ? Sb F14 1.826(9) . ? Sb F12 1.836(9) . ? Sb F11 1.852(7) . ? C40 Cl2 1.704(13) . ? C40 Cl1 1.73(2) . ? C50 Cl4 1.70(2) . ? C50 Cl3 1.73(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 N1 Fe O1 85.7(3) . . ? N1 Fe N7 73.3(3) . . ? O1 Fe N7 99.8(2) . . ? N1 Fe N9 73.1(3) . . ? O1 Fe N9 93.5(2) . . ? N7 Fe N9 142.7(3) . . ? N1 Fe Cl 161.2(2) . . ? O1 Fe Cl 112.5(2) . . ? N7 Fe Cl 106.4(2) . . ? N9 Fe Cl 100.2(2) . . ? C6 N1 C2 117.5(8) . . ? C6 N1 Fe 121.0(6) . . ? C2 N1 Fe 121.4(6) . . ? C3 C2 N1 123.5(8) . . ? C3 C2 C7 125.7(8) . . ? N1 C2 C7 110.5(8) . . ? C2 C3 C4 119.0(9) . . ? C5 C4 C3 118.8(10) . . ? C6 C5 C4 118.9(8) . . ? N1 C6 C5 122.3(8) . . ? N1 C6 C9 111.3(8) . . ? C5 C6 C9 126.3(8) . . ? N7 C7 C8 125.9(8) . . ? N7 C7 C2 116.8(7) . . ? C8 C7 C2 117.3(8) . . ? C7 N7 C11 118.4(7) . . ? C7 N7 Fe 116.4(6) . . ? C11 N7 Fe 125.1(6) . . ? N9 C9 C10 125.9(8) . . ? N9 C9 C6 116.5(7) . . ? C10 C9 C6 117.5(8) . . ? C9 N9 C23 119.8(7) . . ? C9 N9 Fe 116.7(6) . . ? C23 N9 Fe 123.4(6) . . ? C12 C11 C16 122.9(8) . . ? C12 C11 N7 117.6(7) . . ? C16 C11 N7 119.6(7) . . ? C11 C12 C13 116.9(8) . . ? C11 C12 C17 123.3(8) . . ? C13 C12 C17 119.7(8) . . ? C14 C13 C12 120.0(9) . . ? C15 C14 C13 121.0(9) . . ? C14 C15 C16 122.2(9) . . ? C15 C16 C11 116.8(8) . . ? C15 C16 C20 121.5(8) . . ? C11 C16 C20 121.7(8) . . ? C18 C17 C12 112.7(10) . . ? C18 C17 C19 111.1(12) . . ? C12 C17 C19 113.4(8) . . ? C16 C20 C22 109.3(10) . . ? C16 C20 C21 112.6(8) . . ? C22 C20 C21 110.8(10) . . ? C28 C23 C24 121.6(8) . . ? C28 C23 N9 118.3(7) . . ? C24 C23 N9 120.1(7) . . ? C25 C24 C23 117.9(8) . . ? C25 C24 C29 121.5(8) . . ? C23 C24 C29 120.6(8) . . ? C24 C25 C26 121.5(9) . . ? C27 C26 C25 119.2(10) . . ? C28 C27 C26 121.8(10) . . ? C27 C28 C23 117.9(9) . . ? C27 C28 C32 119.8(9) . . ? C23 C28 C32 122.2(8) . . ? C24 C29 C31 112.0(8) . . ? C24 C29 C30 109.1(9) . . ? C31 C29 C30 109.4(9) . . ? C33 C32 C34 111.7(9) . . ? C33 C32 C28 112.7(10) . . ? C34 C32 C28 110.7(9) . . ? F15 Sb F13 177.8(7) . . ? F15 Sb F16 90.0(5) . . ? F13 Sb F16 89.6(5) . . ? F15 Sb F14 86.9(6) . . ? F13 Sb F14 90.9(7) . . ? F16 Sb F14 91.9(4) . . ? F15 Sb F12 91.1(7) . . ? F13 Sb F12 91.0(7) . . ? F16 Sb F12 89.5(4) . . ? F14 Sb F12 177.7(5) . . ? F15 Sb F11 88.8(5) . . ? F13 Sb F11 91.5(5) . . ? F16 Sb F11 178.2(4) . . ? F14 Sb F11 86.7(4) . . ? F12 Sb F11 91.9(4) . . ? Cl2 C40 Cl1 114.0(9) . . ? Cl4 C50 Cl3 115.1(11) . . ? _refine_diff_density_max 0.810 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.121 data_VG9844 _database_code_CSD 168891 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34.50 H50 N3 O2 Cl4 Fe F6 Sb' _chemical_formula_weight 972.17 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.075(2) _cell_length_b 13.265(3) _cell_length_c 18.925(3) _cell_angle_alpha 84.223(15) _cell_angle_beta 78.89(2) _cell_angle_gamma 68.341(15) _cell_volume 2305.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5.18 _cell_measurement_theta_max 12.47 _exptl_crystal_description prisms _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method ? _exptl_crystal_F_000 986 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.7358 _exptl_absorpt_correction_T_max 0.8176 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 19.40 _diffrn_reflns_number 8617 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.1338 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8112 _reflns_number_observed 4073 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1364 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6748 _refine_ls_number_parameters 519 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1711 _refine_ls_R_factor_obs 0.0820 _refine_ls_wR_factor_all 0.2485 _refine_ls_wR_factor_obs 0.1854 _refine_ls_goodness_of_fit_all 1.031 _refine_ls_goodness_of_fit_obs 1.175 _refine_ls_restrained_S_all 1.095 _refine_ls_restrained_S_obs 1.174 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.31547(14) 0.80940(11) 0.74166(7) 0.0414(4) Uani 1 d . . Cl Cl 0.5372(3) 0.8157(3) 0.7053(2) 0.0822(11) Uani 1 d . . O1 O 0.2007(9) 0.9375(6) 0.8094(4) 0.064(2) Uani 1 d D . H1A H 0.1496(82) 0.9345(71) 0.8536(20) 0.036(24) Uiso 1 d D . H1B H 0.2263(114) 0.9955(55) 0.8103(60) 0.068(35) Uiso 1 d D . N1 N 0.1341(8) 0.7631(6) 0.7610(4) 0.042(2) Uani 1 d . . C2 C 0.0331(10) 0.8029(8) 0.7193(5) 0.048(2) Uani 1 d . . C3 C -0.0987(11) 0.7879(10) 0.7366(6) 0.066(3) Uani 1 d . . H3A H -0.1696(11) 0.8177(10) 0.7076(6) 0.079 Uiso 1 calc R . C4 C -0.1209(12) 0.7272(10) 0.7980(6) 0.065(3) Uani 1 d . . H4A H -0.2084(12) 0.7161(10) 0.8110(6) 0.078 Uiso 1 calc R . C5 C -0.0150(12) 0.6826(10) 0.8407(6) 0.066(3) Uani 1 d . . H5A H -0.0313(12) 0.6436(10) 0.8830(6) 0.079 Uiso 1 calc R . C6 C 0.1170(11) 0.6977(8) 0.8188(5) 0.048(2) Uani 1 d . . C7 C 0.0765(10) 0.8633(9) 0.6537(5) 0.049(2) Uani 1 d . . N7 N 0.2010(8) 0.8717(6) 0.6481(4) 0.043(2) Uani 1 d . . C8 C -0.0222(14) 0.9058(13) 0.6003(7) 0.083(4) Uani 1 d . . H8A H -0.0446(88) 0.8477(20) 0.5853(41) 0.125 Uiso 1 calc R . H8B H 0.0239(46) 0.9364(76) 0.5592(25) 0.125 Uiso 1 calc R . H8C H -0.1100(48) 0.9607(59) 0.6216(19) 0.125 Uiso 1 calc R . C9 C 0.2458(11) 0.6509(8) 0.8534(5) 0.048(2) Uani 1 d . . N9 N 0.3537(8) 0.6807(6) 0.8273(4) 0.040(2) Uani 1 d . . C10 C 0.2450(12) 0.5703(10) 0.9151(6) 0.070(3) Uani 1 d . . H10A H 0.2103(93) 0.5172(43) 0.9024(19) 0.105 Uiso 1 calc R . H10B H 0.1827(77) 0.6072(14) 0.9569(14) 0.105 Uiso 1 calc R . H10C H 0.3416(20) 0.5347(53) 0.9252(33) 0.105 Uiso 1 calc R . C11 C 0.2541(10) 0.9229(8) 0.5838(5) 0.048(2) Uani 1 d . . C12 C 0.3424(12) 0.8571(10) 0.5281(5) 0.059(3) Uani 1 d . . C13 C 0.3906(14) 0.9071(12) 0.4648(6) 0.072(3) Uani 1 d . . H13A H 0.4479(14) 0.8644(12) 0.4263(6) 0.086 Uiso 1 calc R . C14 C 0.3554(12) 1.0172(12) 0.4584(6) 0.070(4) Uani 1 d . . H14A H 0.3858(12) 1.0492(12) 0.4154(6) 0.084 Uiso 1 calc R . C15 C 0.2747(13) 1.0799(10) 0.5161(7) 0.069(3) Uani 1 d . . H15A H 0.2552(13) 1.1543(10) 0.5125(7) 0.082 Uiso 1 calc R . C16 C 0.2198(12) 1.0336(10) 0.5815(7) 0.066(3) Uani 1 d . . C17 C 0.3845(17) 0.7354(11) 0.5329(7) 0.083(4) Uani 1 d . . H17A H 0.3435(17) 0.7148(11) 0.5810(7) 0.099 Uiso 1 calc R . C18 C 0.5526(21) 0.6817(13) 0.5231(12) 0.134(7) Uani 1 d . . H18A H 0.5875(21) 0.7087(13) 0.5581(12) 0.201 Uiso 1 calc R . H18B H 0.5941(21) 0.6989(13) 0.4755(12) 0.201 Uiso 1 calc R . H18C H 0.5797(21) 0.6044(13) 0.5296(12) 0.201 Uiso 1 calc R . C19 C 0.3333(28) 0.6924(19) 0.4784(14) 0.163(10) Uani 1 d . . H19A H 0.3635(28) 0.6148(19) 0.4843(14) 0.244 Uiso 1 calc R . H19B H 0.3737(28) 0.7111(19) 0.4310(14) 0.244 Uiso 1 calc R . H19C H 0.2295(28) 0.7233(19) 0.4845(14) 0.244 Uiso 1 calc R . C20 C 0.1326(16) 1.1037(11) 0.6432(8) 0.084(4) Uani 1 d . . H20A H 0.1052(16) 1.0567(11) 0.6820(8) 0.100 Uiso 1 calc R . C21 C -0.0063(23) 1.1909(15) 0.6260(12) 0.142(8) Uani 1 d . . H21A H -0.0568(23) 1.2328(15) 0.6679(12) 0.212 Uiso 1 calc R . H21B H -0.0665(23) 1.1575(15) 0.6119(12) 0.212 Uiso 1 calc R . H21C H 0.0168(23) 1.2376(15) 0.5874(12) 0.212 Uiso 1 calc R . C22 C 0.2300(25) 1.1540(17) 0.6717(9) 0.128(7) Uani 1 d . . H22A H 0.1742(25) 1.1993(17) 0.7115(9) 0.192 Uiso 1 calc R . H22B H 0.2642(25) 1.1967(17) 0.6338(9) 0.192 Uiso 1 calc R . H22C H 0.3112(25) 1.0968(17) 0.6873(9) 0.192 Uiso 1 calc R . C23 C 0.4890(9) 0.6327(7) 0.8540(5) 0.043(2) Uani 1 d . . C24 C 0.5078(11) 0.6740(9) 0.9140(6) 0.054(3) Uani 1 d . . C25 C 0.6434(12) 0.6231(11) 0.9373(6) 0.067(3) Uani 1 d . . H25A H 0.6614(12) 0.6494(11) 0.9768(6) 0.080 Uiso 1 calc R . C26 C 0.7486(12) 0.5356(11) 0.9024(8) 0.077(4) Uani 1 d . . H26A H 0.8353(12) 0.5018(11) 0.9197(8) 0.093 Uiso 1 calc R . C27 C 0.7281(13) 0.4974(10) 0.8428(7) 0.071(3) Uani 1 d . . H27A H 0.8012(13) 0.4387(10) 0.8194(7) 0.086 Uiso 1 calc R . C28 C 0.5972(12) 0.5463(9) 0.8167(6) 0.059(3) Uani 1 d . . C29 C 0.3942(14) 0.7692(12) 0.9527(7) 0.077(4) Uani 1 d . . H29A H 0.3055(14) 0.7871(12) 0.9325(7) 0.093 Uiso 1 calc R . C30 C 0.4409(21) 0.8688(12) 0.9407(10) 0.110(6) Uani 1 d . . H30A H 0.3668(21) 0.9291(12) 0.9659(10) 0.166 Uiso 1 calc R . H30B H 0.4552(21) 0.8872(12) 0.8902(10) 0.166 Uiso 1 calc R . H30C H 0.5297(21) 0.8523(12) 0.9587(10) 0.166 Uiso 1 calc R . C31 C 0.3598(20) 0.7410(17) 1.0352(8) 0.114(6) Uani 1 d . . H31A H 0.2868(20) 0.8031(17) 1.0589(8) 0.171 Uiso 1 calc R . H31B H 0.4463(20) 0.7209(17) 1.0559(8) 0.171 Uiso 1 calc R . H31C H 0.3255(20) 0.6816(17) 1.0413(8) 0.171 Uiso 1 calc R . C32 C 0.5752(16) 0.5017(10) 0.7506(7) 0.082(4) Uani 1 d . . H32A H 0.4838(16) 0.5510(10) 0.7366(7) 0.099 Uiso 1 calc R . C33 C 0.6933(20) 0.4926(15) 0.6871(8) 0.115(6) Uani 1 d . . H33A H 0.7019(20) 0.5623(15) 0.6755(8) 0.173 Uiso 1 calc R . H33B H 0.6704(20) 0.4682(15) 0.6465(8) 0.173 Uiso 1 calc R . H33C H 0.7833(20) 0.4416(15) 0.6986(8) 0.173 Uiso 1 calc R . C34 C 0.5628(27) 0.3907(16) 0.7683(12) 0.145(8) Uani 1 d . . H34A H 0.4874(27) 0.3957(16) 0.8090(12) 0.217 Uiso 1 calc R . H34B H 0.6531(27) 0.3399(16) 0.7796(12) 0.217 Uiso 1 calc R . H34C H 0.5400(27) 0.3666(16) 0.7276(12) 0.217 Uiso 1 calc R . Sb Sb 0.15741(10) 1.24577(8) 0.90828(5) 0.0693(3) Uani 1 d . . F1 F 0.2355(13) 1.1198(8) 0.8555(6) 0.131(4) Uani 1 d . . F2 F 0.3385(17) 1.2524(21) 0.9004(12) 0.118(7) Uani 0.55 d P 1 F3 F 0.1097(24) 1.3369(14) 0.8284(9) 0.114(6) Uani 0.55 d P 1 F4 F -0.0185(26) 1.2299(34) 0.9308(24) 0.186(17) Uani 0.55 d P 1 F5 F 0.1869(36) 1.1654(25) 0.9939(15) 0.159(11) Uani 0.55 d P 1 F6 F 0.0814(12) 1.3703(8) 0.9622(6) 0.129(4) Uani 1 d . . F2' F 0.3185(37) 1.2741(28) 0.8640(17) 0.135(12) Uiso 0.45 d P 2 F3' F 0.0383(44) 1.3030(34) 0.8471(22) 0.181(16) Uiso 0.45 d P 2 F4' F 0.0059(86) 1.2294(75) 0.9536(49) 0.297(40) Uiso 0.45 d P 2 F5' F 0.2526(37) 1.1669(31) 0.9822(20) 0.122(11) Uiso 0.45 d P 2 O40 O 0.0100(17) 0.9299(16) 0.9330(8) 0.174(7) Uani 1 d . . C50 C -0.3761(29) 1.0846(26) 0.8076(14) 0.176(11) Uani 1 d . . Cl1 Cl -0.3882(15) 1.0971(11) 0.7193(6) 0.155(4) Uani 0.55 d P 1 Cl2 Cl -0.1840(11) 1.0718(12) 0.8025(8) 0.156(5) Uani 0.55 d P 1 Cl1' Cl -0.4170(36) 1.0316(27) 0.7587(19) 0.164(10) Uiso 0.25 d P 2 Cl2' Cl -0.3364(34) 0.9976(24) 0.8692(15) 0.155(9) Uiso 0.25 d P 2 Cl1" Cl -0.2699(46) 1.0953(32) 0.7290(21) 0.168(12) Uiso 0.20 d P 3 Cl2" Cl -0.2407(67) 1.0213(44) 0.8394(29) 0.203(19) Uiso 0.20 d P 3 C60 C 0.1092(53) 0.4900(30) 0.6657(25) 0.137(15) Uani 0.50 d P . Cl3 Cl 0.2445(15) 0.5162(11) 0.6631(8) 0.158(5) Uani 0.50 d P . Cl4 Cl -0.0007(30) 0.5957(23) 0.5789(14) 0.179(9) Uiso 0.30 d P 1 Cl4' Cl 0.0642(38) 0.5031(29) 0.5889(19) 0.151(10) Uiso 0.20 d P 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 Fe 0.0382(7) 0.0505(8) 0.0420(7) 0.0130(6) -0.0147(6) -0.0231(6) Cl 0.052(2) 0.116(3) 0.091(2) 0.048(2) -0.027(2) -0.051(2) O1 0.088(6) 0.054(4) 0.056(5) -0.008(4) -0.008(4) -0.034(4) N1 0.036(4) 0.046(4) 0.047(4) 0.001(3) -0.006(3) -0.018(3) C2 0.045(5) 0.057(6) 0.050(5) 0.003(4) -0.024(4) -0.023(5) C3 0.043(6) 0.085(8) 0.074(8) 0.010(6) -0.018(5) -0.027(6) C4 0.046(6) 0.086(8) 0.079(8) 0.012(6) -0.009(5) -0.046(6) C5 0.055(7) 0.081(8) 0.069(7) 0.019(6) -0.010(6) -0.040(6) C6 0.048(5) 0.061(6) 0.047(5) 0.013(5) -0.007(4) -0.035(5) C7 0.043(5) 0.067(6) 0.041(5) 0.007(5) -0.011(4) -0.024(5) N7 0.035(4) 0.055(5) 0.038(4) 0.003(3) -0.004(3) -0.017(4) C8 0.067(8) 0.125(12) 0.073(8) 0.027(8) -0.043(7) -0.046(8) C9 0.053(6) 0.052(6) 0.045(5) 0.010(4) -0.009(4) -0.028(5) N9 0.039(4) 0.048(4) 0.033(4) 0.007(3) -0.010(3) -0.016(4) C10 0.058(7) 0.084(8) 0.072(7) 0.045(6) -0.023(6) -0.038(6) C11 0.045(5) 0.064(6) 0.039(5) 0.016(5) -0.013(4) -0.026(5) C12 0.056(6) 0.076(7) 0.044(6) 0.006(5) -0.013(5) -0.022(6) C13 0.070(8) 0.104(10) 0.048(6) 0.009(6) -0.015(6) -0.038(7) C14 0.052(7) 0.111(11) 0.054(7) 0.031(7) -0.022(6) -0.041(7) C15 0.062(7) 0.073(8) 0.076(8) 0.042(7) -0.025(6) -0.034(6) C16 0.051(6) 0.072(8) 0.071(7) 0.020(6) -0.018(6) -0.020(6) C17 0.104(11) 0.071(8) 0.064(8) -0.010(6) 0.006(7) -0.030(8) C18 0.123(15) 0.068(10) 0.185(20) 0.014(11) -0.048(14) 0.002(10) C19 0.188(25) 0.141(19) 0.200(24) -0.029(18) -0.067(20) -0.083(19) C20 0.090(10) 0.067(8) 0.085(9) 0.025(7) -0.007(8) -0.028(8) C21 0.129(17) 0.097(13) 0.155(18) 0.002(12) -0.009(14) 0.001(12) C22 0.184(21) 0.141(16) 0.079(11) -0.010(10) 0.000(12) -0.091(16) C23 0.035(5) 0.047(5) 0.045(5) 0.022(4) -0.015(4) -0.014(4) C24 0.054(6) 0.058(6) 0.055(6) 0.018(5) -0.017(5) -0.027(5) C25 0.057(7) 0.087(9) 0.070(7) 0.036(6) -0.033(6) -0.039(7) C26 0.042(6) 0.073(8) 0.110(11) 0.052(8) -0.028(7) -0.020(6) C27 0.052(7) 0.058(7) 0.088(9) 0.010(6) -0.004(6) -0.008(6) C28 0.058(6) 0.057(6) 0.058(6) 0.009(5) -0.011(5) -0.018(5) C29 0.066(8) 0.102(10) 0.068(8) -0.014(7) -0.035(6) -0.020(7) C30 0.139(15) 0.071(9) 0.124(13) 0.002(9) -0.067(12) -0.021(10) C31 0.112(13) 0.162(17) 0.082(10) -0.026(11) -0.016(9) -0.060(13) C32 0.085(9) 0.061(7) 0.084(9) -0.005(6) -0.014(7) -0.007(7) C33 0.118(14) 0.127(14) 0.078(10) -0.017(10) -0.004(10) -0.019(12) C34 0.186(23) 0.118(15) 0.145(18) 0.002(13) -0.011(16) -0.081(16) Sb 0.0539(5) 0.0673(5) 0.0894(7) -0.0088(4) -0.0162(4) -0.0212(4) F1 0.153(10) 0.090(6) 0.160(9) -0.045(6) -0.043(8) -0.036(6) F2 0.051(9) 0.202(22) 0.114(15) -0.053(15) 0.003(9) -0.056(11) F3 0.134(16) 0.092(11) 0.088(11) 0.031(9) -0.048(11) 0.000(11) F4 0.068(12) 0.255(34) 0.281(39) -0.031(27) -0.002(16) -0.117(18) F5 0.160(28) 0.148(20) 0.142(20) 0.067(15) -0.020(19) -0.046(20) F6 0.111(8) 0.109(7) 0.147(9) -0.044(6) 0.000(6) -0.019(6) O40 0.129(12) 0.234(18) 0.140(12) -0.028(12) 0.039(10) -0.068(13) C50 0.128(19) 0.224(29) 0.133(19) -0.037(20) 0.013(16) -0.022(20) Cl1 0.175(11) 0.173(11) 0.129(8) -0.032(8) -0.053(8) -0.055(9) Cl2 0.089(6) 0.183(11) 0.183(11) -0.087(9) -0.003(6) -0.024(7) C60 0.153(39) 0.083(23) 0.161(38) -0.045(23) 0.011(30) -0.035(25) Cl3 0.148(11) 0.154(10) 0.180(12) -0.058(9) -0.017(9) -0.056(9) _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 Fe O1 2.070(8) . ? Fe N1 2.092(7) . ? Fe N9 2.210(7) . ? Fe N7 2.222(7) . ? Fe Cl 2.237(3) . ? N1 C2 1.329(12) . ? N1 C6 1.351(11) . ? C2 C3 1.388(14) . ? C2 C7 1.491(13) . ? C3 C4 1.38(2) . ? C4 C5 1.38(2) . ? C5 C6 1.396(14) . ? C6 C9 1.467(14) . ? C7 N7 1.284(12) . ? C7 C8 1.479(14) . ? N7 C11 1.442(11) . ? C9 N9 1.286(12) . ? C9 C10 1.502(13) . ? N9 C23 1.442(11) . ? C11 C16 1.38(2) . ? C11 C12 1.383(15) . ? C12 C13 1.40(2) . ? C12 C17 1.51(2) . ? C13 C14 1.37(2) . ? C14 C15 1.37(2) . ? C15 C16 1.43(2) . ? C16 C20 1.49(2) . ? C17 C19 1.48(2) . ? C17 C18 1.56(2) . ? C20 C21 1.52(2) . ? C20 C22 1.57(2) . ? C23 C24 1.383(15) . ? C23 C28 1.394(15) . ? C24 C25 1.417(14) . ? C24 C29 1.50(2) . ? C25 C26 1.37(2) . ? C26 C27 1.36(2) . ? C27 C28 1.40(2) . ? C28 C32 1.52(2) . ? C29 C30 1.54(2) . ? C29 C31 1.57(2) . ? C32 C33 1.50(2) . ? C32 C34 1.52(2) . ? Sb F4' 1.68(8) . ? Sb F3' 1.74(4) . ? Sb F4 1.83(2) . ? Sb F2' 1.83(3) . ? Sb F2 1.836(15) . ? Sb F5 1.86(2) . ? Sb F5' 1.86(4) . ? Sb F3 1.860(14) . ? Sb F6 1.860(9) . ? Sb F1 1.862(9) . ? C50 Cl1' 1.42(4) . ? C50 Cl2" 1.52(6) . ? C50 Cl2' 1.56(4) . ? C50 Cl1 1.69(3) . ? C50 Cl1" 1.68(4) . ? C50 Cl2 1.86(3) . ? Cl1' Cl2' 2.33(4) . ? Cl1" Cl2" 2.24(6) . ? C60 Cl3 1.52(5) . ? C60 Cl4' 1.58(6) . ? C60 Cl4 2.23(6) . ? 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 Fe N1 88.6(3) . . ? O1 Fe N9 96.4(3) . . ? N1 Fe N9 73.8(3) . . ? O1 Fe N7 98.7(3) . . ? N1 Fe N7 73.3(3) . . ? N9 Fe N7 143.2(3) . . ? O1 Fe Cl 107.1(3) . . ? N1 Fe Cl 164.2(2) . . ? N9 Fe Cl 101.8(2) . . ? N7 Fe Cl 105.4(2) . . ? C2 N1 C6 120.6(8) . . ? C2 N1 Fe 120.1(6) . . ? C6 N1 Fe 119.1(6) . . ? N1 C2 C3 121.9(9) . . ? N1 C2 C7 113.5(8) . . ? C3 C2 C7 124.6(9) . . ? C4 C3 C2 117.7(10) . . ? C3 C4 C5 121.0(9) . . ? C4 C5 C6 118.3(10) . . ? N1 C6 C5 120.0(9) . . ? N1 C6 C9 113.2(8) . . ? C5 C6 C9 126.7(9) . . ? N7 C7 C8 125.4(9) . . ? N7 C7 C2 115.6(8) . . ? C8 C7 C2 119.0(9) . . ? C7 N7 C11 118.6(8) . . ? C7 N7 Fe 116.3(6) . . ? C11 N7 Fe 125.0(6) . . ? N9 C9 C6 116.9(8) . . ? N9 C9 C10 124.5(9) . . ? C6 C9 C10 118.6(8) . . ? C9 N9 C23 120.9(7) . . ? C9 N9 Fe 115.7(6) . . ? C23 N9 Fe 123.4(5) . . ? C16 C11 C12 123.1(9) . . ? C16 C11 N7 119.0(10) . . ? C12 C11 N7 117.9(9) . . ? C11 C12 C13 117.9(11) . . ? C11 C12 C17 122.4(10) . . ? C13 C12 C17 119.7(11) . . ? C14 C13 C12 121.6(12) . . ? C13 C14 C15 119.2(10) . . ? C14 C15 C16 121.7(12) . . ? C11 C16 C15 116.4(12) . . ? C11 C16 C20 123.2(10) . . ? C15 C16 C20 120.4(11) . . ? C19 C17 C12 113.6(14) . . ? C19 C17 C18 108.4(15) . . ? C12 C17 C18 109.1(12) . . ? C16 C20 C21 113.9(14) . . ? C16 C20 C22 109.1(12) . . ? C21 C20 C22 111.4(15) . . ? C24 C23 C28 122.7(9) . . ? C24 C23 N9 119.7(9) . . ? C28 C23 N9 117.6(9) . . ? C23 C24 C25 116.7(11) . . ? C23 C24 C29 122.9(9) . . ? C25 C24 C29 120.3(11) . . ? C26 C25 C24 120.9(12) . . ? C27 C26 C25 121.2(11) . . ? C26 C27 C28 120.1(12) . . ? C23 C28 C27 118.3(11) . . ? C23 C28 C32 122.2(10) . . ? C27 C28 C32 119.4(11) . . ? C24 C29 C30 110.6(12) . . ? C24 C29 C31 111.0(12) . . ? C30 C29 C31 111.1(12) . . ? C33 C32 C34 108.9(14) . . ? C33 C32 C28 113.5(13) . . ? C34 C32 C28 110.4(13) . . ? F4' Sb F3' 78.7(32) . . ? F4' Sb F2' 174.8(33) . . ? F3' Sb F2' 102.3(17) . . ? F4 Sb F2 170.7(16) . . ? F4 Sb F5 82.3(18) . . ? F2 Sb F5 88.5(13) . . ? F4' Sb F5' 88.1(32) . . ? F3' Sb F5' 165.7(16) . . ? F2' Sb F5' 91.3(14) . . ? F4 Sb F3 94.0(16) . . ? F2 Sb F3 95.0(12) . . ? F5 Sb F3 173.7(12) . . ? F4' Sb F6 80.6(31) . . ? F3' Sb F6 92.4(14) . . ? F4 Sb F6 88.9(13) . . ? F2' Sb F6 94.3(11) . . ? F2 Sb F6 89.2(7) . . ? F5 Sb F6 87.9(11) . . ? F5' Sb F6 90.8(12) . . ? F3 Sb F6 86.9(7) . . ? F4' Sb F1 99.5(31) . . ? F3' Sb F1 88.6(14) . . ? F4 Sb F1 91.4(13) . . ? F2' Sb F1 85.7(11) . . ? F2 Sb F1 90.3(7) . . ? F5 Sb F1 91.2(11) . . ? F5' Sb F1 88.2(12) . . ? F3 Sb F1 94.1(7) . . ? F6 Sb F1 179.0(5) . . ? Cl1' C50 Cl2' 103.0(29) . . ? Cl2" C50 Cl1" 88.8(29) . . ? Cl1 C50 Cl2 100.5(14) . . ? C50 Cl1' Cl2' 40.6(18) . . ? C50 Cl2' Cl1' 36.4(16) . . ? C50 Cl1" Cl2" 42.5(19) . . ? C50 Cl2" Cl1" 48.6(21) . . ? Cl3 C60 Cl4' 111.7(32) . . ? Cl3 C60 Cl4 104.8(25) . . ? _refine_diff_density_max 0.733 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.108 data_VG9902 _database_code_CSD 168892 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H54 N3 O2 Fe Sb F6 Cl4' _chemical_formula_weight 1042.26 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.005(2) _cell_length_b 16.903(2) _cell_length_c 18.815(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.950(9) _cell_angle_gamma 90.00 _cell_volume 4754.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 12.53 _exptl_crystal_description prisms _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.73 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method ? _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.4865 _exptl_absorpt_correction_T_max 0.5531 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.42 _diffrn_reflns_number 8638 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8301 _reflns_number_observed 4802 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1092 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7209 _refine_ls_number_parameters 550 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1253 _refine_ls_R_factor_obs 0.0656 _refine_ls_wR_factor_all 0.1920 _refine_ls_wR_factor_obs 0.1513 _refine_ls_goodness_of_fit_all 1.003 _refine_ls_goodness_of_fit_obs 1.104 _refine_ls_restrained_S_all 1.053 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.67698(6) 0.31807(5) 0.07440(5) 0.0411(2) Uani 1 d . . O1 O 0.6152(3) 0.3780(3) 0.1446(3) 0.0535(12) Uani 1 d . . O2 O 0.5900(3) 0.3494(3) -0.0027(2) 0.0479(11) Uani 1 d . . N1 N 0.7839(4) 0.2427(3) 0.1078(3) 0.0446(13) Uani 1 d . . C2 C 0.7672(5) 0.1679(4) 0.1258(4) 0.052(2) Uani 1 d . . C3 C 0.8343(6) 0.1225(5) 0.1616(5) 0.071(2) Uani 1 d . . H3A H 0.8232(6) 0.0709(5) 0.1754(5) 0.085 Uiso 1 calc R . C4 C 0.9166(6) 0.1555(6) 0.1759(6) 0.079(3) Uani 1 d . . H4A H 0.9619(6) 0.1260(6) 0.2001(6) 0.095 Uiso 1 calc R . C5 C 0.9342(6) 0.2312(5) 0.1554(5) 0.071(2) Uani 1 d . . H5A H 0.9908(6) 0.2532(5) 0.1648(5) 0.085 Uiso 1 calc R . C6 C 0.8663(5) 0.2734(4) 0.1209(4) 0.049(2) Uani 1 d . . C7 C 0.6743(5) 0.1406(4) 0.1033(4) 0.051(2) Uani 1 d . . N7 N 0.6211(4) 0.1951(3) 0.0795(3) 0.0467(13) Uani 1 d . . C8 C 0.6555(6) 0.0533(4) 0.1041(6) 0.072(3) Uani 1 d . . H8A H 0.5949(16) 0.0438(6) 0.0853(35) 0.108 Uiso 1 calc R . H8B H 0.6639(45) 0.0341(9) 0.1523(7) 0.108 Uiso 1 calc R . H8C H 0.6957(31) 0.0263(6) 0.0754(30) 0.108 Uiso 1 calc R . C9 C 0.8735(4) 0.3565(5) 0.0930(4) 0.051(2) Uani 1 d . . N9 N 0.8006(4) 0.3885(3) 0.0703(3) 0.0453(13) Uani 1 d . . C10 C 0.9651(6) 0.3924(6) 0.0936(6) 0.078(3) Uani 1 d . . H10A H 1.0020(16) 0.3597(25) 0.0665(35) 0.117 Uiso 1 calc R . H10B H 0.9912(22) 0.3962(43) 0.1418(6) 0.117 Uiso 1 calc R . H10C H 0.9605(8) 0.4443(19) 0.0728(38) 0.117 Uiso 1 calc R . C11 C 0.5308(5) 0.1767(4) 0.0503(4) 0.047(2) Uani 1 d . . C12 C 0.5202(5) 0.1540(4) -0.0224(4) 0.057(2) Uani 1 d . . C13 C 0.4323(7) 0.1430(6) -0.0524(5) 0.072(2) Uani 1 d . . H13A H 0.4222(7) 0.1277(6) -0.0999(5) 0.087 Uiso 1 calc R . C14 C 0.3610(6) 0.1544(6) -0.0126(6) 0.082(3) Uani 1 d . . H14A H 0.3031(6) 0.1470(6) -0.0334(6) 0.098 Uiso 1 calc R . C15 C 0.3743(6) 0.1766(6) 0.0576(5) 0.074(2) Uani 1 d . . H15A H 0.3254(6) 0.1839(6) 0.0840(5) 0.089 Uiso 1 calc R . C16 C 0.4600(5) 0.1882(4) 0.0897(4) 0.054(2) Uani 1 d . . C17 C 0.5967(7) 0.1423(6) -0.0679(4) 0.076(2) Uani 1 d . . H17A H 0.6524(7) 0.1527(6) -0.0383(4) 0.091 Uiso 1 calc R . C18 C 0.5918(9) 0.1999(6) -0.1312(5) 0.094(3) Uani 1 d . . H18A H 0.6416(9) 0.1908(6) -0.1590(5) 0.141 Uiso 1 calc R . H18B H 0.5939(9) 0.2533(6) -0.1138(5) 0.141 Uiso 1 calc R . H18C H 0.5370(9) 0.1917(6) -0.1605(5) 0.141 Uiso 1 calc R . C19 C 0.5998(9) 0.0554(7) -0.0953(6) 0.100(4) Uani 1 d . . H19A H 0.6491(9) 0.0494(7) -0.1242(6) 0.150 Uiso 1 calc R . H19B H 0.5450(9) 0.0433(7) -0.1233(6) 0.150 Uiso 1 calc R . H19C H 0.6073(9) 0.0200(7) -0.0554(6) 0.150 Uiso 1 calc R . C20 C 0.4729(6) 0.2120(5) 0.1688(5) 0.063(2) Uani 1 d . . H20A H 0.5251(6) 0.2469(5) 0.1752(5) 0.076 Uiso 1 calc R . C21 C 0.4921(8) 0.1383(7) 0.2158(5) 0.091(3) Uani 1 d . . H21A H 0.5425(8) 0.1104(7) 0.2001(5) 0.136 Uiso 1 calc R . H21B H 0.4407(8) 0.1042(7) 0.2121(5) 0.136 Uiso 1 calc R . H21C H 0.5050(8) 0.1543(7) 0.2646(5) 0.136 Uiso 1 calc R . C22 C 0.3926(7) 0.2566(6) 0.1936(6) 0.089(3) Uani 1 d . . H22A H 0.4040(7) 0.2699(6) 0.2431(6) 0.134 Uiso 1 calc R . H22B H 0.3404(7) 0.2238(6) 0.1872(6) 0.134 Uiso 1 calc R . H22C H 0.3831(7) 0.3041(6) 0.1660(6) 0.134 Uiso 1 calc R . C23 C 0.7980(5) 0.4688(4) 0.0421(4) 0.051(2) Uani 1 d . . C24 C 0.8016(5) 0.5334(4) 0.0880(4) 0.055(2) Uani 1 d . . C25 C 0.7963(6) 0.6088(5) 0.0573(6) 0.076(3) Uani 1 d . . H25A H 0.7983(6) 0.6532(5) 0.0866(6) 0.092 Uiso 1 calc R . C26 C 0.7884(8) 0.6183(5) -0.0145(7) 0.085(3) Uani 1 d . . H26A H 0.7871(8) 0.6690(5) -0.0336(7) 0.103 Uiso 1 calc R . C27 C 0.7824(7) 0.5553(6) -0.0585(5) 0.078(3) Uani 1 d . . H27A H 0.7743(7) 0.5636(6) -0.1075(5) 0.093 Uiso 1 calc R . C28 C 0.7880(5) 0.4776(5) -0.0325(4) 0.059(2) Uani 1 d . . C29 C 0.8101(5) 0.5240(5) 0.1686(4) 0.062(2) Uani 1 d . . H29A H 0.8130(5) 0.4675(5) 0.1800(4) 0.074 Uiso 1 calc R . C30 C 0.7299(7) 0.5595(7) 0.2014(5) 0.084(3) Uani 1 d . . H30A H 0.7370(7) 0.5528(7) 0.2522(5) 0.126 Uiso 1 calc R . H30B H 0.6763(7) 0.5332(7) 0.1824(5) 0.126 Uiso 1 calc R . H30C H 0.7257(7) 0.6148(7) 0.1901(5) 0.126 Uiso 1 calc R . C31 C 0.8947(7) 0.5641(9) 0.2033(6) 0.108(4) Uani 1 d . . H31A H 0.8977(7) 0.5569(9) 0.2541(6) 0.162 Uiso 1 calc R . H31B H 0.8928(7) 0.6196(9) 0.1924(6) 0.162 Uiso 1 calc R . H31C H 0.9465(7) 0.5408(9) 0.1851(6) 0.162 Uiso 1 calc R . C32 C 0.7886(7) 0.4077(6) -0.0823(5) 0.071(2) Uani 1 d . . H32A H 0.7790(7) 0.3597(6) -0.0547(5) 0.085 Uiso 1 calc R . C33 C 0.7138(7) 0.4129(7) -0.1431(5) 0.087(3) Uani 1 d . . H33A H 0.7165(7) 0.3675(7) -0.1735(5) 0.130 Uiso 1 calc R . H33B H 0.7213(7) 0.4601(7) -0.1703(5) 0.130 Uiso 1 calc R . H33C H 0.6569(7) 0.4144(7) -0.1234(5) 0.130 Uiso 1 calc R . C34 C 0.8787(8) 0.4005(8) -0.1125(7) 0.102(4) Uani 1 d . . H34A H 0.8780(8) 0.3558(8) -0.1441(7) 0.153 Uiso 1 calc R . H34B H 0.9245(8) 0.3934(8) -0.0742(7) 0.153 Uiso 1 calc R . H34C H 0.8905(8) 0.4478(8) -0.1384(7) 0.153 Uiso 1 calc R . C35 C 0.5377(5) 0.4079(4) 0.1339(4) 0.053(2) Uani 1 d . . C36 C 0.4878(5) 0.4089(4) 0.0685(4) 0.055(2) Uani 1 d . . H36A H 0.4312(5) 0.4316(4) 0.0671(4) 0.066 Uiso 1 calc R . C37 C 0.5136(5) 0.3798(4) 0.0060(4) 0.051(2) Uani 1 d . . C38 C 0.5006(7) 0.4445(5) 0.1978(5) 0.074(2) Uani 1 d . . H38A H 0.5155(44) 0.4120(24) 0.2390(9) 0.111 Uiso 1 calc R . H38B H 0.4368(8) 0.4486(41) 0.1895(17) 0.111 Uiso 1 calc R . H38C H 0.5258(38) 0.4962(19) 0.2058(24) 0.111 Uiso 1 calc R . C39 C 0.4489(6) 0.3817(6) -0.0604(5) 0.075(3) Uani 1 d . . H39A H 0.4069(33) 0.4241(29) -0.0567(19) 0.113 Uiso 1 calc R . H39B H 0.4174(38) 0.3324(18) -0.0652(23) 0.113 Uiso 1 calc R . H39C H 0.4815(8) 0.3900(46) -0.1015(6) 0.113 Uiso 1 calc R . Sb Sb 0.83701(5) 0.85942(4) 0.21159(3) 0.0705(2) Uani 1 d . . F11 F 0.8390(18) 0.8105(14) 0.3008(10) 0.141(9) Uani 0.70 d P 1 F12 F 0.7586(9) 0.7821(6) 0.1756(5) 0.118(4) Uani 0.70 d P 1 F13 F 0.9302(12) 0.7931(12) 0.1915(13) 0.189(8) Uani 0.70 d P 1 F14 F 0.9246(13) 0.9300(12) 0.2418(10) 0.192(7) Uani 0.70 d PU 1 F15 F 0.7431(13) 0.9240(9) 0.2355(8) 0.167(7) Uani 0.70 d PU 1 F16 F 0.8310(12) 0.9128(9) 0.1243(6) 0.117(5) Uani 0.70 d P 1 F11' F 0.8382(43) 0.8313(35) 0.3010(32) 0.132(19) Uiso 0.30 d P 2 F12' F 0.8501(64) 0.7885(55) 0.1419(44) 0.335(38) Uiso 0.30 d P 2 F13' F 0.9454(29) 0.8439(29) 0.2181(22) 0.156(14) Uiso 0.30 d P 2 F14' F 0.8722(18) 0.9542(16) 0.2623(14) 0.096(7) Uiso 0.30 d P 2 F15' F 0.7314(22) 0.8926(20) 0.2047(17) 0.122(10) Uiso 0.30 d P 2 F16' F 0.8542(49) 0.8917(43) 0.1336(35) 0.210(30) Uiso 0.30 d P 2 C40 C 0.9000(19) 0.3419(17) 0.3718(13) 0.223(11) Uani 1 d U . H40A H 0.9472(19) 0.3046(17) 0.3637(13) 0.268 Uiso 1 calc R . H40B H 0.9265(19) 0.3942(17) 0.3767(13) 0.268 Uiso 1 calc R . Cl1 Cl 0.8550(5) 0.3181(5) 0.4474(3) 0.207(3) Uani 1 d . . Cl2 Cl 0.8179(6) 0.3410(6) 0.2964(4) 0.245(4) Uani 1 d U . C45 C 0.8999(24) 0.6047(24) 0.4706(17) 0.246(13) Uani 1 d U . Cl5 Cl 0.8627(6) 0.6683(7) 0.4034(7) 0.188(4) Uani 0.60 d PU . Cl6 Cl 0.8474(17) 0.5162(16) 0.4524(13) 0.257(10) Uiso 0.40 d P . Cl7 Cl 0.9118(17) 0.6999(17) 0.4897(14) 0.267(10) Uiso 0.40 d P . Cl8 Cl 0.8518(22) 0.5729(23) 0.3973(18) 0.255(13) Uiso 0.30 d P . Cl9 Cl 0.9703(24) 0.5402(22) 0.4440(17) 0.269(13) Uiso 0.30 d P . 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 Fe 0.0395(5) 0.0343(4) 0.0476(5) 0.0021(4) -0.0077(4) -0.0002(4) O1 0.061(3) 0.049(3) 0.049(3) -0.002(2) -0.007(2) 0.003(2) O2 0.048(3) 0.049(3) 0.045(2) 0.003(2) -0.008(2) 0.002(2) N1 0.045(3) 0.039(3) 0.048(3) 0.002(2) -0.009(2) 0.001(2) C2 0.060(4) 0.042(3) 0.051(4) 0.009(3) -0.009(3) 0.006(3) C3 0.070(5) 0.056(5) 0.084(6) 0.017(4) -0.012(4) 0.020(4) C4 0.057(5) 0.071(6) 0.103(7) 0.021(5) -0.026(5) 0.014(4) C5 0.052(4) 0.064(5) 0.091(6) 0.005(5) -0.026(4) 0.003(4) C6 0.045(4) 0.050(4) 0.052(4) -0.007(3) -0.005(3) 0.001(3) C7 0.060(4) 0.035(3) 0.055(4) 0.003(3) -0.005(3) -0.001(3) N7 0.058(3) 0.031(3) 0.049(3) 0.006(2) -0.007(3) -0.004(2) C8 0.072(5) 0.034(4) 0.109(7) 0.019(4) -0.007(5) -0.003(4) C9 0.040(3) 0.053(4) 0.056(4) 0.001(3) -0.009(3) -0.006(3) N9 0.046(3) 0.041(3) 0.047(3) -0.002(2) -0.005(2) -0.003(2) C10 0.052(5) 0.070(5) 0.108(7) 0.006(5) -0.012(5) -0.007(4) C11 0.055(4) 0.028(3) 0.055(4) 0.004(3) -0.006(3) -0.008(3) C12 0.064(5) 0.046(4) 0.061(4) -0.001(3) -0.006(4) -0.011(3) C13 0.081(6) 0.067(5) 0.065(5) 0.001(4) -0.020(4) -0.017(5) C14 0.062(5) 0.082(6) 0.095(7) 0.011(5) -0.027(5) -0.023(5) C15 0.053(4) 0.074(5) 0.093(6) 0.002(5) -0.001(4) -0.005(4) C16 0.062(4) 0.037(3) 0.061(4) 0.004(3) -0.001(3) -0.008(3) C17 0.102(7) 0.068(5) 0.056(4) -0.008(4) -0.004(4) -0.016(5) C18 0.146(11) 0.074(6) 0.067(6) -0.006(5) 0.034(6) -0.013(7) C19 0.132(10) 0.085(7) 0.085(7) -0.021(6) 0.020(7) 0.008(7) C20 0.063(5) 0.055(4) 0.072(5) 0.001(4) 0.006(4) -0.008(4) C21 0.116(8) 0.078(6) 0.077(6) 0.025(5) 0.000(6) -0.001(6) C22 0.078(6) 0.076(6) 0.116(8) -0.004(6) 0.015(6) -0.003(5) C23 0.040(3) 0.042(3) 0.068(4) 0.001(3) -0.002(3) -0.009(3) C24 0.052(4) 0.042(4) 0.071(5) -0.006(3) -0.003(3) -0.005(3) C25 0.072(6) 0.042(4) 0.115(8) -0.007(5) 0.010(5) -0.008(4) C26 0.098(7) 0.047(5) 0.114(8) 0.022(5) 0.021(6) -0.010(5) C27 0.094(7) 0.064(5) 0.076(6) 0.018(5) 0.011(5) -0.004(5) C28 0.060(4) 0.053(4) 0.065(5) 0.011(4) 0.003(4) -0.009(3) C29 0.055(4) 0.054(4) 0.074(5) -0.010(4) -0.007(4) -0.007(4) C30 0.078(6) 0.098(7) 0.076(6) -0.013(5) 0.004(5) -0.004(6) C31 0.067(6) 0.144(11) 0.108(9) -0.030(8) -0.026(6) -0.017(7) C32 0.086(6) 0.069(5) 0.058(5) 0.009(4) 0.007(4) -0.009(5) C33 0.099(7) 0.091(7) 0.067(5) 0.005(5) -0.009(5) -0.026(6) C34 0.100(8) 0.103(8) 0.105(8) -0.017(7) 0.020(7) 0.002(7) C35 0.062(4) 0.036(3) 0.060(4) -0.001(3) 0.002(3) 0.002(3) C36 0.054(4) 0.053(4) 0.058(4) 0.009(3) -0.001(3) 0.016(3) C37 0.052(4) 0.043(4) 0.056(4) 0.014(3) -0.011(3) -0.001(3) C38 0.088(6) 0.062(5) 0.074(5) -0.002(4) 0.021(5) 0.020(5) C39 0.075(6) 0.080(6) 0.066(5) 0.012(4) -0.020(4) 0.003(5) Sb 0.0794(4) 0.0632(3) 0.0656(3) 0.0024(3) -0.0131(3) 0.0049(3) F11 0.200(17) 0.126(14) 0.088(8) 0.060(9) -0.033(8) -0.013(11) F12 0.160(10) 0.086(6) 0.103(7) -0.014(5) -0.014(6) -0.054(6) F13 0.123(11) 0.169(15) 0.283(23) 0.010(15) 0.060(13) 0.090(11) F14 0.186(13) 0.188(14) 0.190(13) 0.011(11) -0.052(11) -0.101(11) F15 0.245(16) 0.134(10) 0.127(10) -0.016(8) 0.043(10) 0.117(11) F16 0.166(12) 0.117(9) 0.065(5) 0.041(6) -0.008(6) 0.004(8) C40 0.245(19) 0.237(19) 0.189(16) 0.010(15) 0.030(15) -0.015(16) Cl1 0.240(7) 0.232(7) 0.157(5) 0.033(5) 0.068(5) -0.030(6) Cl2 0.258(8) 0.317(10) 0.172(5) 0.049(6) 0.089(6) 0.031(7) C45 0.267(20) 0.248(20) 0.226(19) -0.007(17) 0.045(16) -0.001(17) Cl5 0.138(6) 0.199(9) 0.238(10) 0.066(8) 0.068(6) 0.040(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 Fe O2 1.940(4) . ? Fe O1 1.960(5) . ? Fe N1 2.101(5) . ? Fe N9 2.211(6) . ? Fe N7 2.247(5) . ? O1 C35 1.267(9) . ? O2 C37 1.279(9) . ? N1 C2 1.338(9) . ? N1 C6 1.345(9) . ? C2 C3 1.393(10) . ? C2 C7 1.495(10) . ? C3 C4 1.360(13) . ? C4 C5 1.368(13) . ? C5 C6 1.361(10) . ? C6 C9 1.507(10) . ? C7 N7 1.274(9) . ? C7 C8 1.502(9) . ? N7 C11 1.450(8) . ? C9 N9 1.261(9) . ? C9 C10 1.502(11) . ? N9 C23 1.457(9) . ? C11 C16 1.361(11) . ? C11 C12 1.417(10) . ? C12 C13 1.402(11) . ? C12 C17 1.502(13) . ? C13 C14 1.372(15) . ? C14 C15 1.371(14) . ? C15 C16 1.386(11) . ? C16 C20 1.537(11) . ? C17 C18 1.536(13) . ? C17 C19 1.559(14) . ? C20 C22 1.527(14) . ? C20 C21 1.540(12) . ? C23 C24 1.389(10) . ? C23 C28 1.407(11) . ? C24 C25 1.400(12) . ? C24 C29 1.520(11) . ? C25 C26 1.354(15) . ? C26 C27 1.347(14) . ? C27 C28 1.402(12) . ? C28 C32 1.508(12) . ? C29 C30 1.521(13) . ? C29 C31 1.534(11) . ? C32 C34 1.515(15) . ? C32 C33 1.534(12) . ? C35 C36 1.385(10) . ? C35 C38 1.501(11) . ? C36 C37 1.361(11) . ? C37 C39 1.516(9) . ? Sb F16' 1.61(7) . ? Sb F13' 1.64(4) . ? Sb F15' 1.68(3) . ? Sb F11' 1.75(6) . ? Sb F12' 1.80(9) . ? Sb F14 1.829(13) . ? Sb F12 1.848(8) . ? Sb F13 1.856(12) . ? Sb F15 1.868(12) . ? Sb F11 1.869(15) . ? Sb F16 1.869(10) . ? Sb F14' 1.92(3) . ? F12' F16' 1.75(10) . ? C40 Cl1 1.67(2) . ? C40 Cl2 1.80(3) . ? C45 Cl8 1.59(4) . ? C45 Cl9 1.63(4) . ? C45 Cl7 1.65(4) . ? C45 Cl6 1.71(4) . ? C45 Cl5 1.72(4) . ? Cl5 Cl8 1.62(4) . ? Cl5 Cl7 1.80(3) . ? Cl6 Cl8 1.42(4) . ? Cl6 Cl9 1.91(4) . ? Cl8 Cl9 1.99(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 O2 Fe O1 92.0(2) . . ? O2 Fe N1 146.8(2) . . ? O1 Fe N1 120.3(2) . . ? O2 Fe N9 109.8(2) . . ? O1 Fe N9 101.1(2) . . ? N1 Fe N9 73.5(2) . . ? O2 Fe N7 93.2(2) . . ? O1 Fe N7 104.5(2) . . ? N1 Fe N7 72.8(2) . . ? N9 Fe N7 144.8(2) . . ? C35 O1 Fe 125.4(5) . . ? C37 O2 Fe 124.5(4) . . ? C2 N1 C6 120.5(6) . . ? C2 N1 Fe 119.6(5) . . ? C6 N1 Fe 119.2(5) . . ? N1 C2 C3 120.0(7) . . ? N1 C2 C7 114.2(6) . . ? C3 C2 C7 125.8(7) . . ? C4 C3 C2 118.4(8) . . ? C3 C4 C5 121.5(7) . . ? C6 C5 C4 118.0(8) . . ? N1 C6 C5 121.6(7) . . ? N1 C6 C9 112.8(6) . . ? C5 C6 C9 125.6(7) . . ? N7 C7 C2 114.7(6) . . ? N7 C7 C8 126.9(7) . . ? C2 C7 C8 118.1(6) . . ? C7 N7 C11 121.0(6) . . ? C7 N7 Fe 117.3(5) . . ? C11 N7 Fe 121.4(4) . . ? N9 C9 C10 126.6(7) . . ? N9 C9 C6 115.6(6) . . ? C10 C9 C6 117.8(6) . . ? C9 N9 C23 121.2(6) . . ? C9 N9 Fe 117.6(5) . . ? C23 N9 Fe 121.2(4) . . ? C16 C11 C12 122.5(7) . . ? C16 C11 N7 120.7(6) . . ? C12 C11 N7 116.6(7) . . ? C13 C12 C11 116.7(8) . . ? C13 C12 C17 119.4(8) . . ? C11 C12 C17 123.9(7) . . ? C14 C13 C12 120.8(8) . . ? C15 C14 C13 120.7(8) . . ? C14 C15 C16 120.7(9) . . ? C11 C16 C15 118.8(8) . . ? C11 C16 C20 121.8(7) . . ? C15 C16 C20 119.5(8) . . ? C12 C17 C18 111.8(9) . . ? C12 C17 C19 111.0(8) . . ? C18 C17 C19 110.0(8) . . ? C22 C20 C16 112.8(8) . . ? C22 C20 C21 109.7(9) . . ? C16 C20 C21 110.3(7) . . ? C24 C23 C28 122.2(7) . . ? C24 C23 N9 120.5(7) . . ? C28 C23 N9 117.3(6) . . ? C23 C24 C25 117.5(8) . . ? C23 C24 C29 122.3(7) . . ? C25 C24 C29 120.2(8) . . ? C26 C25 C24 121.1(9) . . ? C27 C26 C25 121.0(9) . . ? C26 C27 C28 121.8(9) . . ? C27 C28 C23 116.4(8) . . ? C27 C28 C32 121.3(8) . . ? C23 C28 C32 122.1(7) . . ? C24 C29 C30 111.2(7) . . ? C24 C29 C31 112.0(8) . . ? C30 C29 C31 108.0(8) . . ? C28 C32 C34 110.5(8) . . ? C28 C32 C33 112.0(8) . . ? C34 C32 C33 110.1(9) . . ? O1 C35 C36 124.4(7) . . ? O1 C35 C38 115.8(7) . . ? C36 C35 C38 119.8(7) . . ? C37 C36 C35 126.2(7) . . ? O2 C37 C36 125.5(6) . . ? O2 C37 C39 114.8(7) . . ? C36 C37 C39 119.7(7) . . ? F16' Sb F13' 83.5(29) . . ? F16' Sb F15' 92.4(27) . . ? F13' Sb F15' 169.6(21) . . ? F16' Sb F11' 169.3(35) . . ? F13' Sb F11' 87.5(26) . . ? F15' Sb F11' 95.5(23) . . ? F16' Sb F12' 61.6(33) . . ? F13' Sb F12' 77.2(31) . . ? F15' Sb F12' 109.2(32) . . ? F11' Sb F12' 121.9(36) . . ? F14 Sb F12 173.3(9) . . ? F14 Sb F13 85.7(10) . . ? F12 Sb F13 88.0(9) . . ? F14 Sb F15 94.6(10) . . ? F12 Sb F15 91.8(8) . . ? F13 Sb F15 177.6(8) . . ? F14 Sb F11 93.1(10) . . ? F12 Sb F11 88.7(9) . . ? F13 Sb F11 87.8(11) . . ? F15 Sb F11 89.8(10) . . ? F14 Sb F16 86.4(7) . . ? F12 Sb F16 92.2(6) . . ? F13 Sb F16 95.3(9) . . ? F15 Sb F16 87.1(7) . . ? F11 Sb F16 176.8(10) . . ? F16' Sb F14' 96.4(28) . . ? F13' Sb F14' 82.4(18) . . ? F15' Sb F14' 88.7(13) . . ? F11' Sb F14' 76.6(23) . . ? F12' Sb F14' 151.3(31) . . ? F16' F12' Sb 53.8(35) . . ? Sb F16' F12' 64.6(38) . . ? Cl1 C40 Cl2 111.7(16) . . ? Cl8 C45 Cl9 76.4(23) . . ? Cl8 C45 Cl7 123.3(30) . . ? Cl9 C45 Cl7 131.1(29) . . ? Cl8 C45 Cl6 50.6(17) . . ? Cl9 C45 Cl6 69.7(21) . . ? Cl7 C45 Cl6 158.8(29) . . ? Cl8 C45 Cl5 58.7(19) . . ? Cl9 C45 Cl5 111.8(23) . . ? Cl7 C45 Cl5 64.7(18) . . ? Cl6 C45 Cl5 106.6(22) . . ? Cl8 Cl5 C45 56.9(16) . . ? Cl8 Cl5 Cl7 112.8(16) . . ? C45 Cl5 Cl7 56.0(14) . . ? Cl8 Cl6 C45 60.4(18) . . ? Cl8 Cl6 Cl9 71.8(20) . . ? C45 Cl6 Cl9 53.1(15) . . ? C45 Cl7 Cl5 59.3(15) . . ? Cl6 Cl8 C45 69.0(22) . . ? Cl6 Cl8 Cl5 129.1(27) . . ? C45 Cl8 Cl5 64.4(20) . . ? Cl6 Cl8 Cl9 65.6(19) . . ? C45 Cl8 Cl9 52.6(17) . . ? Cl5 Cl8 Cl9 99.4(21) . . ? C45 Cl9 Cl6 57.2(18) . . ? C45 Cl9 Cl8 51.0(17) . . ? Cl6 Cl9 Cl8 42.5(13) . . ? _refine_diff_density_max 0.645 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.085 data_VG0003 _database_code_CSD 168893 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H44 N3 O2 F12 Fe Sb' _chemical_formula_weight 980.36 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.518(3) _cell_length_b 37.750(4) _cell_length_c 9.275(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.099(14) _cell_angle_gamma 90.00 _cell_volume 4349.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 5.04 _cell_measurement_theta_max 11.00 _exptl_crystal_description blocks _exptl_crystal_colour Red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method ? _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 22.46 _diffrn_reflns_number 6088 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5676 _reflns_number_observed 3821 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 562 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5114 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_obs 0.0563 _refine_ls_wR_factor_all 0.1452 _refine_ls_wR_factor_obs 0.1204 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.100 _refine_ls_restrained_S_all 1.068 _refine_ls_restrained_S_obs 1.100 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.25564(8) 0.38061(3) 0.60498(11) 0.0332(3) Uani 1 d . . O1 O 0.2024(4) 0.32997(13) 0.5837(6) 0.0408(12) Uani 1 d . . O2 O 0.2765(5) 0.37241(14) 0.8204(6) 0.0453(13) Uani 1 d . . N1 N 0.2830(5) 0.41517(15) 0.4357(6) 0.0327(14) Uani 1 d . . C2 C 0.3832(6) 0.4211(2) 0.4048(8) 0.035(2) Uani 1 d . . C3 C 0.4049(6) 0.4459(2) 0.3044(9) 0.042(2) Uani 1 d . . H3A H 0.4752(6) 0.4499(2) 0.2858(9) 0.051 Uiso 1 calc R . C4 C 0.3204(7) 0.4650(2) 0.2311(9) 0.049(2) Uani 1 d . . H4A H 0.3334(7) 0.4813(2) 0.1602(9) 0.059 Uiso 1 calc R . C5 C 0.2165(7) 0.4596(2) 0.2641(9) 0.041(2) Uani 1 d . . H5A H 0.1592(7) 0.4725(2) 0.2172(9) 0.049 Uiso 1 calc R . C6 C 0.1994(6) 0.4342(2) 0.3695(8) 0.034(2) Uani 1 d . . C7 C 0.4673(6) 0.3995(2) 0.4952(9) 0.041(2) Uani 1 d . . N7 N 0.4309(4) 0.37866(15) 0.5875(6) 0.0303(13) Uani 1 d . . C8 C 0.5809(7) 0.4045(3) 0.4699(12) 0.064(3) Uani 1 d . . H8A H 0.6030(7) 0.4283(3) 0.4950(12) 0.096 Uiso 1 d R . H8B H 0.5875(7) 0.4003(3) 0.3693(12) 0.096 Uiso 1 d R . H8C H 0.6257(7) 0.3881(3) 0.5289(12) 0.096 Uiso 1 d R . C9 C 0.0926(6) 0.4249(2) 0.4136(8) 0.036(2) Uani 1 d . . N9 N 0.0942(5) 0.4003(2) 0.5098(6) 0.0319(13) Uani 1 d . . C10 C -0.0041(7) 0.4437(2) 0.3477(10) 0.050(2) Uani 1 d . . H10A H -0.0050(7) 0.4443(2) 0.2441(10) 0.075 Uiso 1 d R . H10B H -0.0032(7) 0.4675(2) 0.3844(10) 0.075 Uiso 1 d R . H10C H -0.0672(7) 0.4317(2) 0.3717(10) 0.075 Uiso 1 d R . C11 C 0.5038(5) 0.3571(2) 0.6861(8) 0.036(2) Uani 1 d . . C12 C 0.5556(6) 0.3724(2) 0.8117(8) 0.038(2) Uani 1 d . . C13 C 0.6157(7) 0.3498(3) 0.9096(10) 0.054(2) Uani 1 d . . H13A H 0.6518(7) 0.3592(3) 0.9947(10) 0.065 Uiso 1 calc R . C14 C 0.6227(8) 0.3149(3) 0.8848(11) 0.065(3) Uani 1 d . . H14A H 0.6618(8) 0.3005(3) 0.9537(11) 0.077 Uiso 1 calc R . C15 C 0.5724(7) 0.3000(2) 0.7573(12) 0.061(3) Uani 1 d . . H15A H 0.5796(7) 0.2759(2) 0.7406(12) 0.073 Uiso 1 calc R . C16 C 0.5115(7) 0.3208(2) 0.6547(10) 0.048(2) Uani 1 d . . C17 C 0.5512(7) 0.4119(2) 0.8459(10) 0.051(2) Uani 1 d . . H17A H 0.5040(7) 0.4232(2) 0.7670(10) 0.061 Uiso 1 calc R . C18 C 0.5052(10) 0.4197(3) 0.9884(12) 0.069(3) Uani 1 d . . H18A H 0.5045(10) 0.4449(3) 1.0040(12) 0.104 Uiso 1 calc R . H18B H 0.5492(10) 0.4086(3) 1.0677(12) 0.104 Uiso 1 calc R . H18C H 0.4331(10) 0.4107(3) 0.9827(12) 0.104 Uiso 1 calc R . C19 C 0.6636(10) 0.4291(3) 0.8516(16) 0.093(4) Uani 1 d . . H19A H 0.6585(10) 0.4539(3) 0.8733(16) 0.139 Uiso 1 calc R . H19B H 0.6898(10) 0.4263(3) 0.7592(16) 0.139 Uiso 1 calc R . H19C H 0.7123(10) 0.4179(3) 0.9257(16) 0.139 Uiso 1 calc R . C20 C 0.4600(8) 0.3049(3) 0.5104(12) 0.063(3) Uani 1 d . . H20A H 0.3979(8) 0.3196(3) 0.4745(12) 0.076 Uiso 1 calc R . C21 C 0.5415(11) 0.3069(4) 0.3977(13) 0.092(4) Uani 1 d . . H21A H 0.5657(11) 0.3308(4) 0.3903(13) 0.137 Uiso 1 calc R . H21B H 0.5072(11) 0.2991(4) 0.3048(13) 0.137 Uiso 1 calc R . H21C H 0.6019(11) 0.2918(4) 0.4283(13) 0.137 Uiso 1 calc R . C22 C 0.4205(10) 0.2674(3) 0.5243(17) 0.095(4) Uani 1 d . . H22A H 0.3893(10) 0.2590(3) 0.4308(17) 0.142 Uiso 1 calc R . H22B H 0.3672(10) 0.2670(3) 0.5904(17) 0.142 Uiso 1 calc R . H22C H 0.4798(10) 0.2525(3) 0.5607(17) 0.142 Uiso 1 calc R . C23 C -0.0032(6) 0.3844(2) 0.5498(8) 0.038(2) Uani 1 d . . C24 C -0.0635(6) 0.3612(2) 0.4518(10) 0.046(2) Uani 1 d . . C25 C -0.1464(7) 0.3423(3) 0.5042(10) 0.056(2) Uani 1 d . . H25A H -0.1858(7) 0.3261(3) 0.4438(10) 0.067 Uiso 1 calc R . C26 C -0.1716(8) 0.3473(3) 0.6467(12) 0.067(3) Uani 1 d . . H26A H -0.2266(8) 0.3344(3) 0.6805(12) 0.080 Uiso 1 calc R . C27 C -0.1140(7) 0.3716(3) 0.7347(10) 0.056(2) Uani 1 d . . H27A H -0.1315(7) 0.3751(3) 0.8282(10) 0.067 Uiso 1 calc R . C28 C -0.0310(6) 0.3909(2) 0.6890(9) 0.043(2) Uani 1 d . . C29 C -0.0433(7) 0.3557(3) 0.2958(10) 0.055(2) Uani 1 d . . H29A H 0.0124(7) 0.3724(3) 0.2737(10) 0.066 Uiso 1 calc R . C30 C -0.0053(12) 0.3183(3) 0.2689(13) 0.094(4) Uani 1 d . . H30A H 0.0065(12) 0.3159(3) 0.1690(13) 0.141 Uiso 1 calc R . H30B H -0.0591(12) 0.3016(3) 0.2902(13) 0.141 Uiso 1 calc R . H30C H 0.0607(12) 0.3137(3) 0.3304(13) 0.141 Uiso 1 calc R . C31 C -0.1479(9) 0.3635(3) 0.1931(12) 0.079(3) Uani 1 d . . H31A H -0.1352(9) 0.3600(3) 0.0942(12) 0.118 Uiso 1 calc R . H31B H -0.1695(9) 0.3876(3) 0.2061(12) 0.118 Uiso 1 calc R . H31C H -0.2039(9) 0.3478(3) 0.2155(12) 0.118 Uiso 1 calc R . C32 C 0.0240(7) 0.4205(3) 0.7851(9) 0.052(2) Uani 1 d . . H32A H 0.0959(7) 0.4241(3) 0.7561(9) 0.062 Uiso 1 calc R . C33 C 0.0380(11) 0.4114(4) 0.9453(12) 0.091(4) Uani 1 d . . H33A H 0.0767(11) 0.3894(4) 0.9603(12) 0.136 Uiso 1 calc R . H33B H -0.0314(11) 0.4089(4) 0.9782(12) 0.136 Uiso 1 calc R . H33C H 0.0775(11) 0.4299(4) 0.9991(12) 0.136 Uiso 1 calc R . C34 C -0.0372(9) 0.4551(3) 0.7592(15) 0.084(3) Uani 1 d . . H34A H -0.0456(9) 0.4606(3) 0.6574(15) 0.126 Uiso 1 calc R . H34B H 0.0021(9) 0.4738(3) 0.8125(15) 0.126 Uiso 1 calc R . H34C H -0.1069(9) 0.4528(3) 0.7915(15) 0.126 Uiso 1 calc R . C35 C 0.1865(7) 0.3091(2) 0.6843(10) 0.049(2) Uani 1 d . . C36 C 0.2129(8) 0.3138(2) 0.8318(10) 0.054(2) Uani 1 d . . H36A H 0.2011(8) 0.2955(2) 0.8949(10) 0.065 Uiso 1 calc R . C37 C 0.2566(7) 0.3453(2) 0.8882(9) 0.046(2) Uani 1 d . . C38 C 0.1314(11) 0.2738(3) 0.6364(12) 0.074(3) Uani 1 d . . F1 F 0.0324(7) 0.2740(2) 0.6545(16) 0.159(5) Uani 1 d . . F2 F 0.1764(8) 0.2466(2) 0.7080(9) 0.109(3) Uani 1 d . . F3 F 0.1428(9) 0.2659(2) 0.4993(7) 0.120(3) Uani 1 d . . C39 C 0.2899(10) 0.3465(3) 1.0557(11) 0.067(3) Uani 1 d . . F4 F 0.2769(8) 0.3782(2) 1.1075(7) 0.108(3) Uani 1 d . . F5 F 0.3917(9) 0.3393(3) 1.0865(9) 0.153(4) Uani 1 d . . F6 F 0.2381(11) 0.3249(3) 1.1253(8) 0.173(6) Uani 1 d . . Sb Sb 0.28769(4) 0.495184(13) 0.73002(6) 0.0442(2) Uani 1 d . . F11 F 0.2949(5) 0.44527(13) 0.7243(7) 0.0665(14) Uani 1 d . . F12 F 0.3688(6) 0.4972(2) 0.5754(8) 0.099(2) Uani 1 d . . F13 F 0.1630(4) 0.4920(2) 0.5983(7) 0.074(2) Uani 1 d . . F14 F 0.2071(6) 0.4923(2) 0.8857(7) 0.098(2) Uani 1 d . . F15 F 0.4128(5) 0.4974(2) 0.8583(8) 0.102(2) Uani 1 d . . F16 F 0.2778(6) 0.54443(14) 0.7297(8) 0.087(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0317(5) 0.0381(6) 0.0295(6) 0.0090(4) 0.0029(4) -0.0016(4) O1 0.052(3) 0.036(3) 0.034(3) 0.003(2) 0.004(2) -0.008(2) O2 0.056(3) 0.046(3) 0.032(3) 0.003(3) -0.001(3) -0.008(3) N1 0.037(4) 0.032(3) 0.030(3) 0.003(3) 0.007(3) -0.004(3) C2 0.036(4) 0.042(4) 0.027(4) -0.002(3) 0.005(3) -0.005(3) C3 0.042(4) 0.047(5) 0.040(5) 0.008(4) 0.013(4) 0.002(4) C4 0.064(6) 0.051(5) 0.033(4) 0.008(4) 0.010(4) -0.014(4) C5 0.050(5) 0.034(4) 0.038(4) 0.006(4) 0.001(3) 0.007(4) C6 0.038(4) 0.032(4) 0.029(4) 0.001(3) -0.003(3) 0.007(3) C7 0.044(5) 0.047(5) 0.032(4) 0.002(4) 0.008(4) -0.004(3) N7 0.032(3) 0.031(3) 0.028(3) -0.001(3) 0.003(3) -0.003(2) C8 0.039(5) 0.087(7) 0.068(7) 0.027(5) 0.013(5) 0.004(5) C9 0.041(4) 0.041(4) 0.025(4) 0.002(3) 0.003(3) 0.003(3) N9 0.033(3) 0.034(3) 0.028(3) -0.001(3) 0.001(3) -0.005(2) C10 0.044(5) 0.052(5) 0.053(5) 0.014(4) 0.002(4) 0.010(4) C11 0.023(4) 0.051(5) 0.034(4) 0.009(3) 0.007(3) -0.001(3) C12 0.030(4) 0.051(5) 0.033(4) 0.007(4) 0.002(3) -0.002(3) C13 0.049(5) 0.069(6) 0.040(5) 0.007(4) -0.016(4) 0.002(4) C14 0.063(6) 0.068(7) 0.062(7) 0.023(5) 0.002(5) 0.010(5) C15 0.055(5) 0.041(5) 0.087(8) 0.011(5) 0.003(5) 0.002(4) C16 0.045(5) 0.035(4) 0.063(6) 0.011(4) 0.004(4) 0.006(3) C17 0.045(5) 0.052(5) 0.053(5) -0.014(4) -0.005(4) 0.001(4) C18 0.076(6) 0.069(7) 0.062(6) -0.021(5) 0.007(5) -0.003(5) C19 0.098(9) 0.059(7) 0.123(11) -0.010(7) 0.020(8) -0.026(6) C20 0.059(6) 0.056(6) 0.074(7) -0.017(5) 0.004(5) 0.009(4) C21 0.109(10) 0.102(9) 0.060(7) -0.029(7) -0.005(7) -0.013(7) C22 0.090(9) 0.052(6) 0.140(12) -0.035(7) 0.005(8) -0.014(6) C23 0.028(4) 0.044(4) 0.041(5) 0.004(4) 0.001(3) 0.004(3) C24 0.025(4) 0.060(5) 0.052(5) 0.003(4) 0.002(4) 0.007(4) C25 0.042(5) 0.068(6) 0.056(6) -0.005(5) 0.000(4) -0.019(4) C26 0.049(6) 0.075(7) 0.080(8) 0.010(6) 0.024(5) -0.017(5) C27 0.050(5) 0.075(6) 0.046(5) 0.010(5) 0.014(4) -0.007(5) C28 0.039(4) 0.053(5) 0.038(5) 0.004(4) 0.006(4) 0.006(4) C29 0.052(5) 0.071(6) 0.039(5) -0.011(4) -0.007(4) -0.009(4) C30 0.121(11) 0.099(9) 0.063(7) -0.019(7) 0.012(7) 0.022(8) C31 0.081(7) 0.100(8) 0.051(6) 0.007(6) -0.011(5) -0.016(6) C32 0.045(5) 0.076(6) 0.035(5) -0.010(4) 0.010(4) -0.004(4) C33 0.086(8) 0.131(11) 0.052(7) -0.020(7) -0.002(6) -0.007(8) C34 0.073(7) 0.069(7) 0.109(10) -0.015(6) 0.010(7) -0.007(6) C35 0.055(5) 0.037(4) 0.055(6) 0.000(4) 0.001(4) -0.002(4) C36 0.085(7) 0.038(5) 0.039(5) 0.009(4) 0.003(5) -0.013(4) C37 0.063(5) 0.046(5) 0.031(4) 0.008(4) 0.008(4) -0.011(4) C38 0.110(10) 0.051(6) 0.059(7) -0.002(5) 0.000(6) -0.025(6) F1 0.087(6) 0.102(6) 0.290(15) -0.065(8) 0.032(7) -0.050(5) F2 0.180(8) 0.038(3) 0.102(5) 0.006(3) -0.010(5) -0.017(4) F3 0.227(10) 0.073(4) 0.058(4) -0.017(3) 0.003(5) -0.042(5) C39 0.088(8) 0.069(7) 0.039(5) 0.011(5) -0.003(5) -0.033(6) F4 0.182(8) 0.098(5) 0.040(3) -0.014(3) -0.001(4) -0.014(5) F5 0.150(9) 0.225(12) 0.070(5) 0.014(6) -0.038(6) 0.049(8) F6 0.296(14) 0.186(9) 0.039(4) 0.006(5) 0.023(6) -0.153(10) Sb 0.0453(3) 0.0408(3) 0.0456(3) -0.0056(3) 0.0019(2) -0.0047(3) F11 0.068(3) 0.052(3) 0.075(4) -0.005(3) -0.007(3) 0.004(3) F12 0.102(5) 0.105(5) 0.101(5) -0.022(4) 0.058(4) -0.024(4) F13 0.059(3) 0.077(4) 0.081(4) -0.016(3) -0.015(3) 0.010(3) F14 0.123(6) 0.114(5) 0.067(4) -0.024(4) 0.049(4) -0.027(4) F15 0.085(4) 0.082(4) 0.124(6) -0.015(4) -0.049(4) -0.011(4) F16 0.113(5) 0.050(3) 0.098(5) -0.006(3) 0.010(4) -0.001(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 Fe O2 2.006(5) . ? Fe O1 2.026(5) . ? Fe N1 2.102(6) . ? Fe N7 2.222(6) . ? Fe N9 2.230(6) . ? O1 C35 1.257(10) . ? O2 C37 1.243(10) . ? N1 C2 1.340(10) . ? N1 C6 1.352(9) . ? C2 C3 1.371(11) . ? C2 C7 1.501(11) . ? C3 C4 1.386(12) . ? C4 C5 1.389(13) . ? C5 C6 1.404(11) . ? C6 C9 1.487(11) . ? C7 N7 1.287(10) . ? C7 C8 1.481(12) . ? N7 C11 1.458(10) . ? C9 N9 1.285(10) . ? C9 C10 1.471(11) . ? N9 C23 1.448(10) . ? C11 C12 1.388(11) . ? C11 C16 1.406(11) . ? C12 C13 1.397(12) . ? C12 C17 1.525(12) . ? C13 C14 1.341(14) . ? C14 C15 1.388(15) . ? C15 C16 1.386(13) . ? C16 C20 1.534(13) . ? C17 C18 1.534(14) . ? C17 C19 1.545(14) . ? C20 C22 1.509(15) . ? C20 C21 1.55(2) . ? C23 C28 1.399(12) . ? C23 C24 1.412(12) . ? C24 C25 1.395(12) . ? C24 C29 1.514(13) . ? C25 C26 1.409(15) . ? C26 C27 1.371(14) . ? C27 C28 1.378(12) . ? C28 C32 1.539(12) . ? C29 C30 1.520(15) . ? C29 C31 1.549(13) . ? C32 C33 1.515(15) . ? C32 C34 1.518(15) . ? C35 C36 1.379(13) . ? C35 C38 1.540(13) . ? C36 C37 1.383(12) . ? C37 C39 1.559(13) . ? C38 F1 1.27(2) . ? C38 F2 1.311(13) . ? C38 F3 1.331(14) . ? C39 F6 1.266(12) . ? C39 F5 1.299(15) . ? C39 F4 1.308(13) . ? Sb F15 1.848(6) . ? Sb F12 1.858(6) . ? Sb F16 1.863(5) . ? Sb F13 1.863(5) . ? Sb F14 1.865(6) . ? Sb F11 1.887(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 O2 Fe O1 87.3(2) . . ? O2 Fe N1 145.7(2) . . ? O1 Fe N1 126.5(2) . . ? O2 Fe N7 93.4(2) . . ? O1 Fe N7 106.1(2) . . ? N1 Fe N7 73.3(2) . . ? O2 Fe N9 116.5(2) . . ? O1 Fe N9 90.3(2) . . ? N1 Fe N9 73.8(2) . . ? N7 Fe N9 146.8(2) . . ? C35 O1 Fe 126.9(5) . . ? C37 O2 Fe 128.4(5) . . ? C2 N1 C6 120.5(6) . . ? C2 N1 Fe 120.4(5) . . ? C6 N1 Fe 118.7(5) . . ? N1 C2 C3 121.9(7) . . ? N1 C2 C7 113.6(6) . . ? C3 C2 C7 124.5(7) . . ? C2 C3 C4 119.1(7) . . ? C3 C4 C5 119.6(7) . . ? C4 C5 C6 118.8(7) . . ? N1 C6 C5 120.2(7) . . ? N1 C6 C9 114.9(6) . . ? C5 C6 C9 124.9(7) . . ? N7 C7 C8 127.4(7) . . ? N7 C7 C2 115.0(7) . . ? C8 C7 C2 117.6(7) . . ? C7 N7 C11 121.0(6) . . ? C7 N7 Fe 117.5(5) . . ? C11 N7 Fe 121.3(4) . . ? N9 C9 C10 125.4(7) . . ? N9 C9 C6 115.1(6) . . ? C10 C9 C6 119.5(7) . . ? C9 N9 C23 122.4(6) . . ? C9 N9 Fe 116.8(5) . . ? C23 N9 Fe 120.7(4) . . ? C12 C11 C16 122.9(7) . . ? C12 C11 N7 119.0(7) . . ? C16 C11 N7 117.9(7) . . ? C11 C12 C13 116.6(8) . . ? C11 C12 C17 123.9(7) . . ? C13 C12 C17 119.5(7) . . ? C14 C13 C12 122.0(9) . . ? C13 C14 C15 120.7(9) . . ? C16 C15 C14 120.6(9) . . ? C15 C16 C11 117.0(8) . . ? C15 C16 C20 120.9(8) . . ? C11 C16 C20 121.9(7) . . ? C12 C17 C18 113.3(8) . . ? C12 C17 C19 111.3(8) . . ? C18 C17 C19 109.0(9) . . ? C22 C20 C16 113.5(10) . . ? C22 C20 C21 110.6(9) . . ? C16 C20 C21 109.3(8) . . ? C28 C23 C24 121.8(7) . . ? C28 C23 N9 118.6(7) . . ? C24 C23 N9 119.5(7) . . ? C25 C24 C23 117.0(8) . . ? C25 C24 C29 118.7(8) . . ? C23 C24 C29 124.2(8) . . ? C24 C25 C26 121.4(8) . . ? C27 C26 C25 119.0(8) . . ? C26 C27 C28 122.1(9) . . ? C27 C28 C23 118.3(8) . . ? C27 C28 C32 120.5(8) . . ? C23 C28 C32 121.1(7) . . ? C24 C29 C30 112.2(9) . . ? C24 C29 C31 109.4(8) . . ? C30 C29 C31 109.5(9) . . ? C33 C32 C34 110.2(9) . . ? C33 C32 C28 113.0(9) . . ? C34 C32 C28 110.7(8) . . ? O1 C35 C36 127.9(8) . . ? O1 C35 C38 115.8(8) . . ? C36 C35 C38 116.3(8) . . ? C35 C36 C37 121.5(8) . . ? O2 C37 C36 127.6(8) . . ? O2 C37 C39 115.8(7) . . ? C36 C37 C39 116.5(7) . . ? F1 C38 F2 107.6(11) . . ? F1 C38 F3 110.4(11) . . ? F2 C38 F3 102.7(10) . . ? F1 C38 C35 111.5(10) . . ? F2 C38 C35 112.4(9) . . ? F3 C38 C35 111.7(9) . . ? F6 C39 F5 107.7(12) . . ? F6 C39 F4 107.9(11) . . ? F5 C39 F4 105.8(9) . . ? F6 C39 C37 113.5(8) . . ? F5 C39 C37 110.3(10) . . ? F4 C39 C37 111.2(8) . . ? F15 Sb F12 89.7(4) . . ? F15 Sb F16 90.3(3) . . ? F12 Sb F16 90.0(3) . . ? F15 Sb F13 178.6(3) . . ? F12 Sb F13 89.4(3) . . ? F16 Sb F13 90.8(3) . . ? F15 Sb F14 90.0(4) . . ? F12 Sb F14 179.0(3) . . ? F16 Sb F14 91.0(3) . . ? F13 Sb F14 90.8(3) . . ? F15 Sb F11 91.4(3) . . ? F12 Sb F11 89.2(3) . . ? F16 Sb F11 178.1(3) . . ? F13 Sb F11 87.5(3) . . ? F14 Sb F11 89.8(3) . . ? _refine_diff_density_max 0.499 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.089 data_VG9982 _database_code_CSD 168894 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H44 N3 O2 F12 Fe Sb' _chemical_formula_weight 980.36 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.214(2) _cell_length_b 12.567(2) _cell_length_c 19.096(2) _cell_angle_alpha 87.526(7) _cell_angle_beta 78.494(10) _cell_angle_gamma 83.307(11) _cell_volume 2151.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.62 _cell_measurement_theta_max 12.47 _exptl_crystal_description plates _exptl_crystal_colour Orange _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method ? _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.052 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10.34 _diffrn_reflns_number 8065 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.1217 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _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 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7553 _reflns_number_observed 4293 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1023 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6530 _refine_ls_number_parameters 538 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.1469 _refine_ls_R_factor_obs 0.0756 _refine_ls_wR_factor_all 0.2048 _refine_ls_wR_factor_obs 0.1631 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.130 _refine_ls_restrained_S_all 1.048 _refine_ls_restrained_S_obs 1.120 _refine_ls_shift/esd_max 0.055 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.69741(14) 0.25281(10) 0.25636(7) 0.0417(3) Uani 1 d . . O1 O 0.7095(10) 0.3030(6) 0.1532(4) 0.070(2) Uani 1 d . . O2 O 0.9219(7) 0.2382(6) 0.2355(4) 0.062(2) Uani 1 d . . N1 N 0.5036(7) 0.2245(6) 0.3313(3) 0.037(2) Uani 1 d . . C2 C 0.4710(8) 0.1241(7) 0.3451(5) 0.037(2) Uani 1 d . . C3 C 0.3472(10) 0.1040(8) 0.3981(5) 0.045(2) Uani 1 d . . H3A H 0.3257(10) 0.0340(8) 0.4091(5) 0.055 Uiso 1 calc R . C4 C 0.2590(10) 0.1869(8) 0.4332(5) 0.053(2) Uani 1 d . . H4A H 0.1734(10) 0.1748(8) 0.4663(5) 0.063 Uiso 1 calc R . C5 C 0.2982(10) 0.2894(8) 0.4191(5) 0.048(2) Uani 1 d . . H5A H 0.2419(10) 0.3468(8) 0.4443(5) 0.057 Uiso 1 calc R . C6 C 0.4215(10) 0.3066(7) 0.3672(5) 0.043(2) Uani 1 d . . C7 C 0.5755(9) 0.0414(7) 0.3032(5) 0.039(2) Uani 1 d . . N7 N 0.6854(8) 0.0773(5) 0.2586(4) 0.040(2) Uani 1 d . . C8 C 0.5511(12) -0.0736(8) 0.3181(6) 0.064(3) Uani 1 d . . H8A H 0.4579(12) -0.0861(8) 0.3065(6) 0.096 Uiso 1 d R . H8B H 0.5492(12) -0.0902(8) 0.3678(6) 0.096 Uiso 1 d R . H8C H 0.6307(12) -0.1184(8) 0.2896(6) 0.096 Uiso 1 d R . C9 C 0.4734(10) 0.4121(7) 0.3464(5) 0.042(2) Uani 1 d . . N9 N 0.5887(8) 0.4119(5) 0.2963(4) 0.044(2) Uani 1 d . . C10 C 0.3921(12) 0.5106(9) 0.3853(7) 0.068(3) Uani 1 d . . H10A H 0.4030(12) 0.5054(9) 0.4344(7) 0.102 Uiso 1 d R . H10B H 0.2883(12) 0.5156(9) 0.3832(7) 0.102 Uiso 1 d R . H10C H 0.4335(12) 0.5733(9) 0.3632(7) 0.102 Uiso 1 d R . C11 C 0.7963(10) 0.0060(6) 0.2151(5) 0.039(2) Uani 1 d . . C12 C 0.9192(10) -0.0437(7) 0.2450(5) 0.047(2) Uani 1 d . . C13 C 1.0306(12) -0.1028(8) 0.1994(6) 0.058(3) Uani 1 d . . H13A H 1.1097(12) -0.1384(8) 0.2177(6) 0.069 Uiso 1 calc R . C14 C 1.0303(13) -0.1117(9) 0.1290(8) 0.074(3) Uani 1 d . . H14A H 1.1110(13) -0.1492(9) 0.0996(8) 0.089 Uiso 1 calc R . C15 C 0.9104(15) -0.0653(9) 0.1006(6) 0.071(3) Uani 1 d . . H15A H 0.9097(15) -0.0739(9) 0.0526(6) 0.085 Uiso 1 calc R . C16 C 0.7899(12) -0.0053(7) 0.1435(5) 0.052(2) Uani 1 d . . C17 C 0.9229(12) -0.0383(9) 0.3236(6) 0.058(3) Uani 1 d . . H17A H 0.8339(12) 0.0065(9) 0.3473(6) 0.069 Uiso 1 calc R . C18 C 1.0617(14) 0.0103(11) 0.3347(8) 0.088(4) Uani 1 d . . H18A H 1.0612(14) 0.0127(11) 0.3850(8) 0.132 Uiso 1 calc R . H18B H 1.0612(14) 0.0816(11) 0.3145(8) 0.132 Uiso 1 calc R . H18C H 1.1495(14) -0.0331(11) 0.3117(8) 0.132 Uiso 1 calc R . C19 C 0.9258(17) -0.1501(12) 0.3593(7) 0.096(4) Uani 1 d . . H19A H 0.9281(17) -0.1442(12) 0.4090(7) 0.144 Uiso 1 calc R . H19B H 1.0128(17) -0.1945(12) 0.3365(7) 0.144 Uiso 1 calc R . H19C H 0.8382(17) -0.1816(12) 0.3547(7) 0.144 Uiso 1 calc R . C20 C 0.6526(14) 0.0420(9) 0.1148(6) 0.068(3) Uani 1 d . . H20A H 0.6059(14) 0.1042(9) 0.1434(6) 0.082 Uiso 1 calc R . C21 C 0.5402(16) -0.0416(12) 0.1236(8) 0.094(4) Uani 1 d . . H21A H 0.5180(16) -0.0649(12) 0.1727(8) 0.140 Uiso 1 calc R . H21B H 0.5823(16) -0.1019(12) 0.0941(8) 0.140 Uiso 1 calc R . H21C H 0.4503(16) -0.0100(12) 0.1093(8) 0.140 Uiso 1 calc R . C22 C 0.6860(22) 0.0779(13) 0.0376(8) 0.119(6) Uani 1 d . . H22A H 0.5951(22) 0.1066(13) 0.0231(8) 0.179 Uiso 1 calc R . H22B H 0.7313(22) 0.0178(13) 0.0085(8) 0.179 Uiso 1 calc R . H22C H 0.7530(22) 0.1321(13) 0.0318(8) 0.179 Uiso 1 calc R . C23 C 0.6444(9) 0.5099(7) 0.2631(5) 0.043(2) Uani 1 d . . C24 C 0.5688(12) 0.5699(8) 0.2148(6) 0.058(3) Uani 1 d . . C25 C 0.6360(13) 0.6527(9) 0.1781(7) 0.073(3) Uani 1 d . . H25A H 0.5892(13) 0.6924(9) 0.1450(7) 0.087 Uiso 1 calc R . C26 C 0.7717(14) 0.6789(10) 0.1886(7) 0.075(3) Uani 1 d . . H26A H 0.8165(14) 0.7334(10) 0.1611(7) 0.091 Uiso 1 calc R . C27 C 0.8411(12) 0.6255(8) 0.2392(7) 0.067(3) Uani 1 d . . H27A H 0.9288(12) 0.6470(8) 0.2482(7) 0.081 Uiso 1 calc R . C28 C 0.7785(10) 0.5378(7) 0.2776(6) 0.052(2) Uani 1 d . . C29 C 0.4122(13) 0.5509(9) 0.2047(8) 0.077(4) Uani 1 d . . H29A H 0.3753(13) 0.4956(9) 0.2392(8) 0.093 Uiso 1 calc R . C30 C 0.4159(19) 0.5125(15) 0.1300(9) 0.125(6) Uani 1 d . . H30A H 0.3170(19) 0.5014(15) 0.1253(9) 0.187 Uiso 1 calc R . H30B H 0.4797(19) 0.4464(15) 0.1221(9) 0.187 Uiso 1 calc R . H30C H 0.4532(19) 0.5654(15) 0.0954(9) 0.187 Uiso 1 calc R . C31 C 0.3089(14) 0.6562(12) 0.2215(11) 0.131(7) Uani 1 d . . H31A H 0.3099(14) 0.6775(12) 0.2691(11) 0.196 Uiso 1 calc R . H31B H 0.2092(14) 0.6453(12) 0.2180(11) 0.196 Uiso 1 calc R . H31C H 0.3434(14) 0.7112(12) 0.1880(11) 0.196 Uiso 1 calc R . C32 C 0.8486(12) 0.4815(8) 0.3383(7) 0.066(3) Uani 1 d . . H32A H 0.8133(12) 0.4106(8) 0.3470(7) 0.079 Uiso 1 calc R . C33 C 1.0176(14) 0.4660(14) 0.3166(9) 0.109(5) Uani 1 d . . H33A H 1.0459(14) 0.4257(14) 0.2735(9) 0.163 Uiso 1 calc R . H33B H 1.0587(14) 0.4279(14) 0.3541(9) 0.163 Uiso 1 calc R . H33C H 1.0547(14) 0.5347(14) 0.3086(9) 0.163 Uiso 1 calc R . C34 C 0.7960(18) 0.5450(11) 0.4063(7) 0.096(4) Uani 1 d . . H34A H 0.6891(18) 0.5530(11) 0.4179(7) 0.144 Uiso 1 calc R . H34B H 0.8309(18) 0.6145(11) 0.3992(7) 0.144 Uiso 1 calc R . H34C H 0.8348(18) 0.5077(11) 0.4447(7) 0.144 Uiso 1 calc R . C35 C 0.8260(21) 0.3165(11) 0.1063(6) 0.090(4) Uani 1 d . . C36 C 0.9735(18) 0.2952(12) 0.1169(9) 0.097(5) Uani 1 d . . H36A H 1.0508(18) 0.3096(12) 0.0795(9) 0.116 Uiso 1 calc R . C37 C 1.0072(13) 0.2549(10) 0.1783(8) 0.076(3) Uani 1 d . . C38 C 0.7908(21) 0.3709(12) 0.0364(9) 0.156(11) Uani 1 d D . F1 F 0.7767(23) 0.4764(8) 0.0403(7) 0.161(9) Uani 0.80 d PDU 1 F2 F 0.9103(18) 0.3407(12) -0.0148(6) 0.155(6) Uani 0.80 d PDU 1 F3 F 0.6684(18) 0.3440(11) 0.0204(7) 0.138(6) Uani 0.80 d PDU 1 F1' F 0.8408(102) 0.4653(43) 0.0310(42) 0.197(38) Uiso 0.20 d PDU 2 F2' F 0.8133(66) 0.3279(46) -0.0276(19) 0.130(19) Uiso 0.20 d PDU 2 F3' F 0.6430(35) 0.3852(78) 0.0597(43) 0.269(41) Uiso 0.20 d PDU 2 C39 C 1.1776(17) 0.2231(12) 0.1795(9) 0.120(7) Uani 1 d D . F4 F 1.2108(13) 0.2435(15) 0.2412(9) 0.150(7) Uani 0.70 d PDU 1 F5 F 1.2105(15) 0.1174(10) 0.1700(12) 0.149(6) Uani 0.70 d PDU 1 F6 F 1.2608(15) 0.2697(17) 0.1252(10) 0.173(8) Uani 0.70 d PDU 1 F4' F 1.2105(71) 0.1690(39) 0.2340(22) 0.220(25) Uiso 0.30 d PDU 2 F5' F 1.2123(66) 0.1686(37) 0.1199(20) 0.196(20) Uiso 0.30 d PDU 2 F6' F 1.2415(50) 0.3131(23) 0.1699(24) 0.149(16) Uiso 0.30 d PDU 2 Sb Sb 0.73904(8) 0.21697(5) 0.48912(4) 0.0494(2) Uani 1 d . . F11 F 0.7759(7) 0.2135(5) 0.3887(3) 0.073(2) Uani 1 d . . F12 F 0.5855(10) 0.1309(7) 0.4923(4) 0.108(3) Uani 1 d . . F13 F 0.6038(8) 0.3387(5) 0.4832(4) 0.079(2) Uani 1 d . . F14 F 0.8934(8) 0.3028(7) 0.4853(4) 0.099(2) Uani 1 d . . F15 F 0.8736(10) 0.0972(6) 0.4935(4) 0.108(3) Uani 1 d . . F16 F 0.6983(9) 0.2217(6) 0.5891(4) 0.089(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0368(7) 0.0359(7) 0.0494(8) 0.0011(6) 0.0000(6) -0.0064(6) O1 0.097(6) 0.062(5) 0.046(4) 0.007(4) -0.009(4) -0.001(4) O2 0.035(4) 0.058(4) 0.087(5) 0.001(4) 0.007(4) -0.012(3) N1 0.034(4) 0.045(4) 0.035(4) -0.004(3) -0.006(3) -0.008(3) C2 0.025(4) 0.040(5) 0.047(5) 0.010(4) -0.010(4) -0.006(4) C3 0.044(5) 0.049(5) 0.043(5) 0.013(4) -0.008(4) -0.014(4) C4 0.030(5) 0.064(7) 0.061(6) -0.010(5) 0.003(4) -0.007(5) C5 0.037(5) 0.060(6) 0.044(5) -0.008(4) -0.003(4) -0.002(4) C6 0.039(5) 0.049(5) 0.043(5) 0.001(4) -0.015(4) 0.001(4) C7 0.033(5) 0.039(5) 0.049(5) 0.003(4) -0.013(4) -0.009(4) N7 0.039(4) 0.036(4) 0.044(4) 0.002(3) -0.005(3) -0.012(3) C8 0.058(7) 0.049(6) 0.083(8) 0.003(5) -0.002(6) -0.017(5) C9 0.034(5) 0.047(5) 0.043(5) -0.012(4) -0.006(4) 0.011(4) N9 0.045(4) 0.032(4) 0.059(5) 0.004(3) -0.020(4) 0.000(3) C10 0.056(7) 0.061(7) 0.085(8) -0.021(6) -0.013(6) 0.006(5) C11 0.044(5) 0.028(4) 0.042(5) 0.005(4) 0.000(4) -0.009(4) C12 0.034(5) 0.045(5) 0.060(6) -0.011(4) 0.001(4) -0.005(4) C13 0.053(6) 0.045(6) 0.069(7) -0.009(5) 0.005(5) -0.007(5) C14 0.056(7) 0.052(6) 0.103(10) -0.013(6) 0.010(7) 0.004(5) C15 0.100(10) 0.059(7) 0.049(6) -0.012(5) 0.001(6) -0.009(7) C16 0.072(7) 0.033(5) 0.045(6) 0.000(4) -0.007(5) 0.000(5) C17 0.053(6) 0.062(6) 0.059(6) -0.016(5) -0.017(5) 0.006(5) C18 0.067(8) 0.094(10) 0.117(11) -0.025(8) -0.038(8) -0.020(7) C19 0.110(12) 0.108(11) 0.066(8) 0.009(8) -0.023(8) 0.007(9) C20 0.098(9) 0.057(6) 0.052(6) -0.003(5) -0.024(6) -0.004(6) C21 0.090(10) 0.103(11) 0.099(11) 0.003(8) -0.042(8) -0.016(8) C22 0.180(18) 0.099(11) 0.083(10) 0.003(8) -0.052(11) 0.010(12) C23 0.036(5) 0.032(4) 0.059(6) 0.002(4) -0.003(4) -0.006(4) C24 0.055(6) 0.046(6) 0.076(7) 0.003(5) -0.021(5) -0.002(5) C25 0.070(8) 0.051(6) 0.098(9) 0.027(6) -0.025(7) -0.005(6) C26 0.078(8) 0.062(7) 0.088(9) 0.013(6) -0.008(7) -0.033(6) C27 0.054(6) 0.044(6) 0.109(9) 0.012(6) -0.026(6) -0.014(5) C28 0.041(5) 0.041(5) 0.069(7) 0.002(5) -0.003(5) -0.004(4) C29 0.064(7) 0.058(7) 0.116(11) 0.032(7) -0.038(7) -0.010(6) C30 0.114(13) 0.159(17) 0.129(15) 0.018(12) -0.074(11) -0.051(12) C31 0.044(7) 0.101(11) 0.236(21) 0.061(13) -0.025(10) 0.014(7) C32 0.057(6) 0.052(6) 0.101(9) 0.020(6) -0.037(6) -0.028(5) C33 0.054(8) 0.135(14) 0.143(14) 0.010(11) -0.034(9) -0.013(8) C34 0.127(13) 0.085(9) 0.080(9) -0.003(8) -0.022(9) -0.025(9) C35 0.145(14) 0.077(9) 0.044(7) 0.010(6) -0.006(8) -0.022(9) C36 0.084(11) 0.097(11) 0.094(11) 0.012(9) 0.020(9) -0.019(9) C37 0.053(7) 0.067(7) 0.097(10) -0.005(7) 0.015(7) -0.014(6) C38 0.295(34) 0.086(13) 0.057(11) 0.002(9) 0.037(16) -0.025(17) F1 0.295(26) 0.069(7) 0.095(9) 0.038(6) -0.007(11) 0.011(10) F2 0.233(18) 0.162(13) 0.052(6) 0.010(7) -0.003(9) 0.008(13) F3 0.251(18) 0.106(9) 0.065(7) 0.023(6) -0.058(9) -0.012(10) C39 0.060(10) 0.118(15) 0.168(19) 0.016(14) 0.024(11) -0.037(10) F4 0.046(7) 0.152(14) 0.258(22) -0.011(14) -0.049(10) 0.005(8) F5 0.076(8) 0.099(10) 0.249(20) -0.001(12) 0.007(11) 0.020(7) F6 0.069(9) 0.230(19) 0.204(18) 0.022(15) 0.040(10) -0.070(11) Sb 0.0514(4) 0.0469(4) 0.0532(4) 0.0018(3) -0.0191(3) -0.0046(3) F11 0.081(4) 0.075(4) 0.063(4) 0.000(3) -0.022(3) 0.008(3) F12 0.118(6) 0.118(6) 0.110(6) 0.029(5) -0.048(5) -0.070(5) F13 0.077(4) 0.077(4) 0.084(5) -0.017(4) -0.032(4) 0.025(4) F14 0.080(5) 0.114(6) 0.120(6) 0.019(5) -0.040(5) -0.054(5) F15 0.133(7) 0.083(5) 0.107(6) 0.004(4) -0.050(5) 0.038(5) F16 0.100(5) 0.105(6) 0.061(4) 0.001(4) -0.019(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O2 2.015(6) . ? Fe O1 2.027(7) . ? Fe N1 2.109(7) . ? Fe N7 2.220(7) . ? Fe N9 2.223(7) . ? O1 C35 1.28(2) . ? O2 C37 1.236(14) . ? N1 C6 1.333(11) . ? N1 C2 1.334(10) . ? C2 C3 1.405(12) . ? C2 C7 1.477(12) . ? C3 C4 1.357(13) . ? C4 C5 1.380(14) . ? C5 C6 1.381(13) . ? C6 C9 1.473(13) . ? C7 N7 1.297(11) . ? C7 C8 1.495(13) . ? N7 C11 1.432(11) . ? C9 N9 1.280(11) . ? C9 C10 1.513(13) . ? N9 C23 1.459(11) . ? C11 C16 1.394(13) . ? C11 C12 1.435(13) . ? C12 C13 1.373(13) . ? C12 C17 1.513(14) . ? C13 C14 1.35(2) . ? C14 C15 1.38(2) . ? C15 C16 1.403(15) . ? C16 C20 1.526(15) . ? C17 C19 1.54(2) . ? C17 C18 1.534(15) . ? C20 C22 1.50(2) . ? C20 C21 1.54(2) . ? C23 C28 1.405(13) . ? C23 C24 1.406(13) . ? C24 C25 1.368(15) . ? C24 C29 1.540(15) . ? C25 C26 1.38(2) . ? C26 C27 1.37(2) . ? C27 C28 1.412(14) . ? C28 C32 1.542(14) . ? C29 C30 1.52(2) . ? C29 C31 1.54(2) . ? C32 C34 1.52(2) . ? C32 C33 1.52(2) . ? C35 C36 1.41(2) . ? C35 C38 1.55(2) . ? C36 C37 1.34(2) . ? C37 C39 1.58(2) . ? C38 F1' 1.32(2) . ? C38 F3 1.31(2) . ? C38 F1 1.32(2) . ? C38 F2' 1.33(2) . ? C38 F3' 1.34(2) . ? C38 F2 1.35(2) . ? C39 F4' 1.29(2) . ? C39 F4 1.32(2) . ? C39 F5' 1.32(2) . ? C39 F6 1.320(15) . ? C39 F6' 1.32(2) . ? C39 F5 1.34(2) . ? Sb F15 1.846(7) . ? Sb F12 1.868(7) . ? Sb F13 1.871(6) . ? Sb F14 1.871(6) . ? Sb F16 1.874(7) . ? Sb F11 1.881(6) . ? 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 O2 Fe O1 86.7(3) . . ? O2 Fe N1 145.9(3) . . ? O1 Fe N1 127.0(3) . . ? O2 Fe N7 93.9(3) . . ? O1 Fe N7 106.7(3) . . ? N1 Fe N7 73.6(3) . . ? O2 Fe N9 114.9(3) . . ? O1 Fe N9 91.7(3) . . ? N1 Fe N9 73.3(3) . . ? N7 Fe N9 146.8(3) . . ? C35 O1 Fe 128.0(9) . . ? C37 O2 Fe 128.4(8) . . ? C6 N1 C2 121.3(7) . . ? C6 N1 Fe 119.3(6) . . ? C2 N1 Fe 119.3(5) . . ? N1 C2 C3 119.6(8) . . ? N1 C2 C7 115.1(7) . . ? C3 C2 C7 125.2(8) . . ? C4 C3 C2 119.9(9) . . ? C3 C4 C5 118.9(9) . . ? C4 C5 C6 119.8(9) . . ? N1 C6 C5 120.4(8) . . ? N1 C6 C9 114.7(8) . . ? C5 C6 C9 124.9(8) . . ? N7 C7 C2 115.1(7) . . ? N7 C7 C8 126.4(8) . . ? C2 C7 C8 118.4(8) . . ? C7 N7 C11 121.2(7) . . ? C7 N7 Fe 116.8(6) . . ? C11 N7 Fe 121.9(5) . . ? N9 C9 C6 115.8(8) . . ? N9 C9 C10 124.9(9) . . ? C6 C9 C10 119.3(9) . . ? C9 N9 C23 123.0(8) . . ? C9 N9 Fe 116.7(6) . . ? C23 N9 Fe 120.2(6) . . ? C16 C11 N7 119.4(8) . . ? C16 C11 C12 121.9(8) . . ? N7 C11 C12 118.5(8) . . ? C13 C12 C11 116.6(9) . . ? C13 C12 C17 120.9(9) . . ? C11 C12 C17 122.4(8) . . ? C14 C13 C12 122.9(11) . . ? C13 C14 C15 120.2(11) . . ? C14 C15 C16 120.8(11) . . ? C11 C16 C15 117.5(10) . . ? C11 C16 C20 120.5(9) . . ? C15 C16 C20 121.9(10) . . ? C12 C17 C19 111.4(9) . . ? C12 C17 C18 111.3(10) . . ? C19 C17 C18 107.5(10) . . ? C22 C20 C16 114.0(12) . . ? C22 C20 C21 108.8(11) . . ? C16 C20 C21 109.3(9) . . ? C28 C23 C24 121.8(8) . . ? C28 C23 N9 118.1(8) . . ? C24 C23 N9 120.0(8) . . ? C25 C24 C23 117.6(10) . . ? C25 C24 C29 119.0(10) . . ? C23 C24 C29 123.4(9) . . ? C24 C25 C26 121.9(11) . . ? C27 C26 C25 120.9(10) . . ? C26 C27 C28 119.6(10) . . ? C23 C28 C27 118.0(9) . . ? C23 C28 C32 121.3(8) . . ? C27 C28 C32 120.5(9) . . ? C30 C29 C24 111.4(12) . . ? C30 C29 C31 112.3(13) . . ? C24 C29 C31 107.9(11) . . ? C34 C32 C33 112.2(11) . . ? C34 C32 C28 109.5(10) . . ? C33 C32 C28 110.7(10) . . ? O1 C35 C36 125.3(12) . . ? O1 C35 C38 113.2(15) . . ? C36 C35 C38 121.2(14) . . ? C37 C36 C35 122.7(12) . . ? O2 C37 C36 128.6(13) . . ? O2 C37 C39 114.4(13) . . ? C36 C37 C39 117.0(12) . . ? F3 C38 F1 107.5(17) . . ? F1' C38 F2' 110.0(25) . . ? F1' C38 F3' 108.1(25) . . ? F2' C38 F3' 106.4(24) . . ? F3 C38 F2 111.1(14) . . ? F1 C38 F2 108.3(14) . . ? F1' C38 C35 107.2(45) . . ? F3 C38 C35 113.2(14) . . ? F1 C38 C35 111.4(13) . . ? F2' C38 C35 127.6(30) . . ? F3' C38 C35 95.4(44) . . ? F2 C38 C35 105.4(15) . . ? F4' C39 F5' 113.4(22) . . ? F4 C39 F6 112.3(14) . . ? F4' C39 F6' 111.4(22) . . ? F5' C39 F6' 109.3(20) . . ? F4 C39 F5 106.8(15) . . ? F6 C39 F5 106.1(14) . . ? F4' C39 C37 117.6(31) . . ? F4 C39 C37 112.2(13) . . ? F5' C39 C37 97.5(30) . . ? F6 C39 C37 110.0(14) . . ? F6' C39 C37 106.5(24) . . ? F5 C39 C37 109.1(12) . . ? F15 Sb F12 90.8(4) . . ? F15 Sb F13 179.1(4) . . ? F12 Sb F13 89.5(4) . . ? F15 Sb F14 89.1(4) . . ? F12 Sb F14 179.6(4) . . ? F13 Sb F14 90.7(4) . . ? F15 Sb F16 89.7(3) . . ? F12 Sb F16 90.2(4) . . ? F13 Sb F16 91.2(3) . . ? F14 Sb F16 90.2(4) . . ? F15 Sb F11 91.4(3) . . ? F12 Sb F11 89.2(3) . . ? F13 Sb F11 87.8(3) . . ? F14 Sb F11 90.5(3) . . ? F16 Sb F11 178.8(3) . . ? _refine_diff_density_max 1.030 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.107 data_VG0005 _database_code_CSD 168895 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H54 N3 O2 Fe Sb F6' _chemical_formula_weight 996.54 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4639(12) _cell_length_b 17.1447(5) _cell_length_c 21.5722(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.439(7) _cell_angle_gamma 90.00 _cell_volume 4609.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 21.63 _cell_measurement_theta_max 30.68 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Red _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method ? _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 7.720 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.3561 _exptl_absorpt_correction_T_max 0.5676 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7141 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 60.01 _reflns_number_total 6786 _reflns_number_observed 5456 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 385 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+3.6099P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00026(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6401 _refine_ls_number_parameters 527 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_obs 0.0483 _refine_ls_wR_factor_all 0.1270 _refine_ls_wR_factor_obs 0.1157 _refine_ls_goodness_of_fit_all 1.033 _refine_ls_goodness_of_fit_obs 1.075 _refine_ls_restrained_S_all 1.049 _refine_ls_restrained_S_obs 1.075 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.24859(5) 0.74614(4) 0.58680(3) 0.0239(2) Uani 1 d . . O1 O 0.2649(3) 0.8062(2) 0.51019(14) 0.0302(7) Uani 1 d . . O2 O 0.2829(3) 0.8385(2) 0.63675(14) 0.0301(7) Uani 1 d . . N1 N 0.2052(3) 0.6272(2) 0.5865(2) 0.0243(7) Uani 1 d . . C2 C 0.2813(4) 0.5730(3) 0.5825(2) 0.0286(9) Uani 1 d . . C3 C 0.2549(5) 0.4950(3) 0.5746(2) 0.0388(12) Uani 1 d . . H3A H 0.3093(5) 0.4563(3) 0.5723(2) 0.047 Uiso 1 calc R . C4 C 0.1476(5) 0.4748(3) 0.5700(3) 0.0430(12) Uani 1 d . . H4A H 0.1278(5) 0.4220(3) 0.5631(3) 0.052 Uiso 1 calc R . C5 C 0.0695(4) 0.5312(3) 0.5754(2) 0.0354(11) Uani 1 d . . H5A H -0.0044(4) 0.5180(3) 0.5735(2) 0.042 Uiso 1 calc R . C6 C 0.1019(4) 0.6075(3) 0.5837(2) 0.0273(9) Uani 1 d . . C7 C 0.3922(4) 0.6042(3) 0.5913(2) 0.0307(10) Uani 1 d . . N7 N 0.3982(3) 0.6784(2) 0.5966(2) 0.0278(8) Uani 1 d . . C8 C 0.4828(5) 0.5474(3) 0.5971(3) 0.0476(14) Uani 1 d . . H8A H 0.4844(5) 0.5139(3) 0.5603(3) 0.071 Uiso 1 d R . H8B H 0.4727(5) 0.5152(3) 0.6341(3) 0.071 Uiso 1 d R . H8C H 0.5508(5) 0.5759(3) 0.6006(3) 0.071 Uiso 1 d R . C9 C 0.0277(4) 0.6749(3) 0.5940(2) 0.0295(10) Uani 1 d . . N9 N 0.0733(3) 0.7413(2) 0.5977(2) 0.0274(8) Uani 1 d . . C10 C -0.0894(4) 0.6581(3) 0.6011(3) 0.0453(13) Uani 1 d . . H10A H -0.0997(4) 0.6227(3) 0.6362(3) 0.068 Uiso 1 d R . H10B H -0.1171(4) 0.6338(3) 0.5632(3) 0.068 Uiso 1 d R . H10C H -0.1279(4) 0.7070(3) 0.6087(3) 0.068 Uiso 1 d R . C11 C 0.4972(4) 0.7156(3) 0.6142(2) 0.0304(10) Uani 1 d . . C12 C 0.5250(4) 0.7180(3) 0.6773(2) 0.0373(11) Uani 1 d . . C13 C 0.6174(5) 0.7594(3) 0.6944(3) 0.0467(13) Uani 1 d . . H13A H 0.6375(5) 0.7628(3) 0.7369(3) 0.056 Uiso 1 calc R . C14 C 0.6793(5) 0.7953(3) 0.6501(3) 0.0492(14) Uani 1 d . . H14A H 0.7428(5) 0.8221(3) 0.6623(3) 0.059 Uiso 1 calc R . C15 C 0.6506(4) 0.7928(3) 0.5889(3) 0.0414(12) Uani 1 d . . H15A H 0.6939(4) 0.8188(3) 0.5593(3) 0.050 Uiso 1 calc R . C16 C 0.5587(4) 0.7527(3) 0.5687(2) 0.0330(10) Uani 1 d . . C17 C 0.4579(5) 0.6790(4) 0.7273(3) 0.0481(14) Uani 1 d . . H17A H 0.3937(5) 0.6554(4) 0.7065(3) 0.058 Uiso 1 calc R . C18 C 0.4175(7) 0.7366(5) 0.7755(4) 0.073(2) Uani 1 d . . H18A H 0.3750(7) 0.7089(5) 0.8065(4) 0.110 Uiso 1 calc R . H18B H 0.3728(7) 0.7762(5) 0.7551(4) 0.110 Uiso 1 calc R . H18C H 0.4788(7) 0.7620(5) 0.7958(4) 0.110 Uiso 1 calc R . C19 C 0.5202(8) 0.6128(5) 0.7590(4) 0.079(2) Uani 1 d . . H19A H 0.5458(8) 0.5761(5) 0.7276(4) 0.118 Uiso 1 calc R . H19B H 0.4729(8) 0.5855(5) 0.7880(4) 0.118 Uiso 1 calc R . H19C H 0.5816(8) 0.6345(5) 0.7818(4) 0.118 Uiso 1 calc R . C20 C 0.5289(4) 0.7486(3) 0.5003(2) 0.0361(11) Uani 1 d . . H20A H 0.4494(4) 0.7417(3) 0.4973(2) 0.043 Uiso 1 calc R . C21 C 0.5812(6) 0.6771(4) 0.4704(3) 0.0528(15) Uani 1 d . . H21A H 0.5623(6) 0.6302(4) 0.4940(3) 0.079 Uiso 1 calc R . H21B H 0.6593(6) 0.6836(4) 0.4706(3) 0.079 Uiso 1 calc R . H21C H 0.5554(6) 0.6717(4) 0.4276(3) 0.079 Uiso 1 calc R . C22 C 0.5579(5) 0.8210(4) 0.4640(3) 0.0497(14) Uani 1 d . . H22A H 0.5365(5) 0.8143(4) 0.4206(3) 0.075 Uiso 1 calc R . H22B H 0.6355(5) 0.8296(4) 0.4666(3) 0.075 Uiso 1 calc R . H22C H 0.5204(5) 0.8661(4) 0.4815(3) 0.075 Uiso 1 calc R . C23 C 0.0113(4) 0.8114(3) 0.6066(2) 0.0280(9) Uani 1 d . . C24 C -0.0338(4) 0.8480(3) 0.5547(2) 0.0327(10) Uani 1 d . . C25 C -0.0921(4) 0.9155(3) 0.5647(3) 0.0435(12) Uani 1 d . . H25A H -0.1243(4) 0.9413(3) 0.5302(3) 0.052 Uiso 1 calc R . C26 C -0.1047(5) 0.9465(3) 0.6233(3) 0.0452(13) Uani 1 d . . H26A H -0.1463(5) 0.9924(3) 0.6291(3) 0.054 Uiso 1 calc R . C27 C -0.0568(4) 0.9105(3) 0.6732(3) 0.0381(11) Uani 1 d . . H27A H -0.0642(4) 0.9328(3) 0.7132(3) 0.046 Uiso 1 calc R . C28 C 0.0023(4) 0.8424(3) 0.6666(2) 0.0319(10) Uani 1 d . . C29 C -0.0173(4) 0.8161(3) 0.4891(2) 0.0391(11) Uani 1 d . . H29A H 0.0417(4) 0.7766(3) 0.4909(2) 0.047 Uiso 1 calc R . C30 C 0.0166(5) 0.8807(4) 0.4448(3) 0.056(2) Uani 1 d . . H30A H 0.0265(5) 0.8588(4) 0.4032(3) 0.084 Uiso 1 calc R . H30B H 0.0842(5) 0.9037(4) 0.4594(3) 0.084 Uiso 1 calc R . H30C H -0.0391(5) 0.9210(4) 0.4432(3) 0.084 Uiso 1 calc R . C31 C -0.1181(6) 0.7757(5) 0.4628(3) 0.063(2) Uani 1 d . . H31A H -0.1404(6) 0.7341(5) 0.4910(3) 0.095 Uiso 1 calc R . H31B H -0.1019(6) 0.7533(5) 0.4221(3) 0.095 Uiso 1 calc R . H31C H -0.1761(6) 0.8139(5) 0.4585(3) 0.095 Uiso 1 calc R . C32 C 0.0522(4) 0.8032(3) 0.7228(2) 0.0368(11) Uani 1 d . . H32A H 0.1077(4) 0.7657(3) 0.7078(2) 0.044 Uiso 1 calc R . C33 C 0.1073(6) 0.8604(4) 0.7666(3) 0.056(2) Uani 1 d . . H33A H 0.1380(6) 0.8320(4) 0.8019(3) 0.085 Uiso 1 calc R . H33B H 0.0548(6) 0.8985(4) 0.7815(3) 0.085 Uiso 1 calc R . H33C H 0.1647(6) 0.8877(4) 0.7445(3) 0.085 Uiso 1 calc R . C34 C -0.0333(6) 0.7564(4) 0.7574(3) 0.055(2) Uani 1 d . . H34A H -0.0006(6) 0.7312(4) 0.7937(3) 0.082 Uiso 1 calc R . H34B H -0.0634(6) 0.7165(4) 0.7298(3) 0.082 Uiso 1 calc R . H34C H -0.0905(6) 0.7915(4) 0.7709(3) 0.082 Uiso 1 calc R . C35 C 0.2925(4) 0.8768(3) 0.5040(2) 0.0282(9) Uani 1 d . . C36 C 0.3065(4) 0.9282(3) 0.5544(2) 0.0346(10) Uani 1 d . . H36A H 0.3208(4) 0.9814(3) 0.5454(2) 0.042 Uiso 1 calc R . C37 C 0.3007(4) 0.9065(3) 0.6168(2) 0.0305(10) Uani 1 d . . C38 C 0.2820(3) 0.8552(2) 0.39082(14) 0.0385(11) Uani 1 d G . H38A H 0.2476(3) 0.8070(2) 0.39939(14) 0.046 Uiso 1 calc R . C39 C 0.3010(3) 0.8772(2) 0.32986(12) 0.0489(14) Uani 1 d G . H39A H 0.2797(4) 0.8439(3) 0.29676(15) 0.059 Uiso 1 calc R . C40 C 0.3513(3) 0.9477(2) 0.31732(11) 0.052(2) Uani 1 d G . H40A H 0.3643(5) 0.9627(3) 0.27565(12) 0.063 Uiso 1 calc R . C41 C 0.3825(3) 0.9964(2) 0.3657(2) 0.0500(14) Uani 1 d G . H41A H 0.4168(4) 1.0446(2) 0.3572(2) 0.060 Uiso 1 calc R . C42 C 0.3634(3) 0.9745(2) 0.42671(13) 0.0391(11) Uani 1 d G . H42A H 0.3847(4) 1.0077(2) 0.4598(2) 0.047 Uiso 1 calc R . C43 C 0.3132(3) 0.9039(2) 0.43925(10) 0.0314(10) Uani 1 d G . C44 C 0.2910(3) 1.0450(2) 0.65596(15) 0.0502(14) Uani 1 d G . H44A H 0.2526(3) 1.0595(2) 0.61954(15) 0.060 Uiso 1 calc R . C45 C 0.3154(4) 1.10066(15) 0.7007(2) 0.065(2) Uani 1 d G . H45A H 0.2938(6) 1.1533(2) 0.6949(3) 0.078 Uiso 1 calc R . C46 C 0.3716(4) 1.0794(2) 0.7540(2) 0.062(2) Uani 1 d G . H46A H 0.3883(5) 1.1174(3) 0.7846(2) 0.074 Uiso 1 calc R . C47 C 0.4033(3) 1.0023(2) 0.76252(13) 0.056(2) Uani 1 d G . H47A H 0.4416(5) 0.9878(3) 0.7989(2) 0.067 Uiso 1 calc R . C48 C 0.3788(3) 0.9466(2) 0.7178(2) 0.0445(13) Uani 1 d G . H48A H 0.4005(5) 0.8940(2) 0.7236(2) 0.053 Uiso 1 calc R . C49 C 0.3226(3) 0.9679(2) 0.66450(13) 0.0325(10) Uani 1 d G . Sb Sb 0.22922(3) 0.58805(2) 0.38541(2) 0.04160(14) Uani 1 d . . F1 F 0.2110(4) 0.6808(2) 0.3431(2) 0.0790(13) Uani 1 d . . F2 F 0.3208(5) 0.6336(3) 0.4425(2) 0.101(2) Uani 1 d . . F3 F 0.3429(4) 0.5625(3) 0.3346(2) 0.0886(15) Uani 1 d . . F4 F 0.1341(4) 0.5379(3) 0.3321(2) 0.0875(15) Uani 1 d . . F5 F 0.1142(4) 0.6105(3) 0.4369(2) 0.092(2) Uani 1 d . . F6 F 0.2447(5) 0.4939(3) 0.4280(2) 0.089(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0236(4) 0.0177(3) 0.0305(4) 0.0008(2) 0.0040(3) -0.0015(2) O1 0.034(2) 0.025(2) 0.031(2) -0.0020(12) 0.0030(13) -0.0030(13) O2 0.031(2) 0.029(2) 0.030(2) 0.0008(13) 0.0020(13) -0.0031(13) N1 0.027(2) 0.020(2) 0.026(2) -0.0012(14) 0.0052(14) 0.0013(15) C2 0.038(3) 0.023(2) 0.025(2) 0.000(2) 0.004(2) 0.001(2) C3 0.051(3) 0.024(2) 0.042(3) -0.003(2) 0.012(2) 0.004(2) C4 0.059(3) 0.021(2) 0.049(3) -0.006(2) 0.009(3) -0.010(2) C5 0.040(3) 0.030(2) 0.036(3) -0.001(2) 0.007(2) -0.011(2) C6 0.029(2) 0.028(2) 0.026(2) 0.001(2) 0.007(2) -0.004(2) C7 0.033(3) 0.029(2) 0.030(2) 0.000(2) 0.004(2) 0.005(2) N7 0.028(2) 0.026(2) 0.030(2) -0.0004(15) 0.0017(15) 0.002(2) C8 0.037(3) 0.031(3) 0.076(4) -0.001(2) 0.000(3) 0.010(2) C9 0.027(2) 0.030(2) 0.032(2) 0.004(2) 0.006(2) -0.004(2) N9 0.025(2) 0.022(2) 0.035(2) -0.0014(15) 0.007(2) 0.000(2) C10 0.027(3) 0.038(3) 0.071(4) -0.002(3) 0.010(2) -0.006(2) C11 0.023(2) 0.026(2) 0.042(3) -0.003(2) -0.002(2) 0.007(2) C12 0.035(3) 0.037(3) 0.040(3) 0.004(2) -0.005(2) 0.001(2) C13 0.048(3) 0.047(3) 0.044(3) -0.005(2) -0.015(3) 0.000(3) C14 0.038(3) 0.046(3) 0.064(4) -0.005(3) -0.011(3) -0.010(2) C15 0.026(3) 0.041(3) 0.057(3) -0.001(2) 0.004(2) -0.004(2) C16 0.025(2) 0.027(2) 0.046(3) -0.001(2) 0.005(2) 0.002(2) C17 0.051(3) 0.059(4) 0.033(3) 0.008(2) -0.006(2) -0.008(3) C18 0.094(6) 0.068(5) 0.057(4) 0.010(3) 0.017(4) 0.007(4) C19 0.107(7) 0.066(5) 0.064(4) 0.017(4) 0.011(4) 0.014(4) C20 0.024(2) 0.042(3) 0.042(3) -0.004(2) 0.010(2) -0.002(2) C21 0.065(4) 0.046(3) 0.048(3) -0.012(3) 0.014(3) 0.003(3) C22 0.039(3) 0.054(3) 0.056(3) 0.011(3) 0.006(3) 0.003(3) C23 0.024(2) 0.025(2) 0.035(2) 0.002(2) 0.007(2) 0.000(2) C24 0.023(2) 0.038(2) 0.038(3) 0.005(2) 0.001(2) -0.003(2) C25 0.037(3) 0.038(3) 0.056(3) 0.013(2) 0.004(2) 0.007(2) C26 0.040(3) 0.030(2) 0.066(4) 0.000(2) 0.014(3) 0.008(2) C27 0.037(3) 0.031(2) 0.046(3) -0.007(2) 0.012(2) 0.000(2) C28 0.026(2) 0.031(2) 0.038(3) 0.001(2) 0.008(2) -0.005(2) C29 0.033(3) 0.051(3) 0.033(3) 0.006(2) 0.001(2) -0.001(2) C30 0.043(3) 0.077(4) 0.048(3) 0.019(3) 0.011(3) -0.003(3) C31 0.062(4) 0.085(5) 0.043(3) -0.003(3) 0.007(3) -0.028(4) C32 0.035(3) 0.042(3) 0.033(3) 0.000(2) 0.008(2) 0.007(2) C33 0.059(4) 0.073(4) 0.037(3) -0.009(3) 0.003(3) -0.005(3) C34 0.069(4) 0.053(3) 0.044(3) 0.016(3) 0.017(3) -0.003(3) C35 0.028(2) 0.024(2) 0.033(2) 0.001(2) 0.005(2) 0.001(2) C36 0.048(3) 0.022(2) 0.034(2) 0.001(2) 0.004(2) -0.003(2) C37 0.028(2) 0.030(2) 0.033(2) -0.005(2) 0.002(2) -0.003(2) C38 0.040(3) 0.042(3) 0.033(3) -0.002(2) 0.009(2) 0.006(2) C39 0.048(3) 0.066(4) 0.033(3) -0.003(3) 0.011(2) 0.010(3) C40 0.053(3) 0.069(4) 0.036(3) 0.013(3) 0.022(3) 0.016(3) C41 0.052(3) 0.044(3) 0.055(3) 0.017(3) 0.023(3) 0.005(3) C42 0.041(3) 0.036(3) 0.041(3) 0.007(2) 0.010(2) 0.002(2) C43 0.030(2) 0.033(2) 0.031(2) 0.002(2) 0.007(2) 0.004(2) C44 0.066(4) 0.035(3) 0.049(3) -0.016(2) -0.003(3) -0.001(3) C45 0.091(5) 0.039(3) 0.066(4) -0.023(3) 0.009(4) -0.002(3) C46 0.087(5) 0.059(4) 0.041(3) -0.027(3) 0.013(3) -0.025(4) C47 0.067(4) 0.070(4) 0.031(3) -0.011(3) 0.002(3) -0.025(3) C48 0.054(3) 0.047(3) 0.033(3) -0.004(2) 0.002(2) -0.011(3) C49 0.036(3) 0.030(2) 0.032(2) -0.007(2) 0.007(2) -0.010(2) Sb 0.0441(2) 0.0441(2) 0.0366(2) 0.00050(14) 0.00217(13) -0.0160(2) F1 0.108(4) 0.058(2) 0.070(3) 0.015(2) -0.011(2) -0.008(2) F2 0.115(4) 0.111(4) 0.077(3) 0.009(3) -0.042(3) -0.066(3) F3 0.068(3) 0.108(4) 0.090(3) 0.021(3) 0.027(2) 0.011(3) F4 0.091(3) 0.108(4) 0.063(3) -0.023(2) -0.006(2) -0.044(3) F5 0.088(3) 0.109(4) 0.078(3) -0.019(3) 0.039(3) -0.010(3) F6 0.136(5) 0.061(2) 0.070(3) 0.020(2) 0.002(3) -0.024(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 Fe O1 1.959(3) . ? Fe O2 1.960(3) . ? Fe N1 2.109(4) . ? Fe N9 2.201(4) . ? Fe N7 2.205(4) . ? O1 C35 1.266(6) . ? O2 C37 1.264(6) . ? N1 C2 1.332(6) . ? N1 C6 1.332(6) . ? C2 C3 1.388(7) . ? C2 C7 1.493(7) . ? C3 C4 1.384(8) . ? C4 C5 1.377(8) . ? C5 C6 1.380(7) . ? C6 C9 1.498(7) . ? C7 N7 1.279(6) . ? C7 C8 1.496(7) . ? N7 C11 1.438(6) . ? C9 N9 1.275(6) . ? C9 C10 1.496(7) . ? N9 C23 1.442(6) . ? C11 C12 1.403(7) . ? C11 C16 1.403(7) . ? C12 C13 1.400(8) . ? C12 C17 1.525(8) . ? C13 C14 1.377(9) . ? C14 C15 1.367(9) . ? C15 C16 1.403(7) . ? C16 C20 1.520(7) . ? C17 C18 1.522(10) . ? C17 C19 1.533(9) . ? C20 C22 1.513(8) . ? C20 C21 1.532(7) . ? C23 C24 1.398(7) . ? C23 C28 1.403(7) . ? C24 C25 1.385(7) . ? C24 C29 1.533(7) . ? C25 C26 1.383(9) . ? C26 C27 1.372(8) . ? C27 C28 1.389(7) . ? C28 C32 1.517(7) . ? C29 C30 1.525(8) . ? C29 C31 1.539(8) . ? C32 C33 1.522(8) . ? C32 C34 1.533(8) . ? C35 C36 1.410(7) . ? C35 C43 1.496(5) . ? C36 C37 1.399(7) . ? C37 C49 1.496(5) . ? C38 C39 1.39 . ? C38 C43 1.39 . ? C39 C40 1.39 . ? C40 C41 1.39 . ? C41 C42 1.39 . ? C42 C43 1.39 . ? C44 C45 1.39 . ? C44 C49 1.39 . ? C45 C46 1.39 . ? C46 C47 1.39 . ? C47 C48 1.39 . ? C48 C49 1.39 . ? Sb F2 1.846(4) . ? Sb F1 1.846(4) . ? Sb F3 1.851(4) . ? Sb F4 1.857(4) . ? Sb F5 1.860(4) . ? Sb F6 1.867(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 O1 Fe O2 90.91(13) . . ? O1 Fe N1 122.26(13) . . ? O2 Fe N1 146.81(14) . . ? O1 Fe N9 102.65(14) . . ? O2 Fe N9 100.64(14) . . ? N1 Fe N9 73.08(14) . . ? O1 Fe N7 105.35(14) . . ? O2 Fe N7 101.04(14) . . ? N1 Fe N7 73.03(14) . . ? N9 Fe N7 144.02(14) . . ? C35 O1 Fe 128.4(3) . . ? C37 O2 Fe 126.6(3) . . ? C2 N1 C6 120.5(4) . . ? C2 N1 Fe 119.5(3) . . ? C6 N1 Fe 119.6(3) . . ? N1 C2 C3 120.9(5) . . ? N1 C2 C7 113.6(4) . . ? C3 C2 C7 125.4(4) . . ? C4 C3 C2 118.5(5) . . ? C5 C4 C3 120.2(4) . . ? C4 C5 C6 118.0(5) . . ? N1 C6 C5 121.9(4) . . ? N1 C6 C9 113.2(4) . . ? C5 C6 C9 124.8(4) . . ? N7 C7 C2 114.9(4) . . ? N7 C7 C8 126.7(5) . . ? C2 C7 C8 118.3(4) . . ? C7 N7 C11 120.9(4) . . ? C7 N7 Fe 117.8(3) . . ? C11 N7 Fe 121.0(3) . . ? N9 C9 C10 126.8(5) . . ? N9 C9 C6 115.0(4) . . ? C10 C9 C6 118.1(4) . . ? C9 N9 C23 120.9(4) . . ? C9 N9 Fe 118.0(3) . . ? C23 N9 Fe 121.0(3) . . ? C12 C11 C16 122.2(5) . . ? C12 C11 N7 118.3(4) . . ? C16 C11 N7 119.3(4) . . ? C13 C12 C11 117.9(5) . . ? C13 C12 C17 119.4(5) . . ? C11 C12 C17 122.7(5) . . ? C14 C13 C12 120.5(5) . . ? C15 C14 C13 120.8(5) . . ? C14 C15 C16 121.5(5) . . ? C15 C16 C11 117.0(5) . . ? C15 C16 C20 121.1(5) . . ? C11 C16 C20 121.9(4) . . ? C18 C17 C12 112.6(5) . . ? C18 C17 C19 110.2(6) . . ? C12 C17 C19 111.2(6) . . ? C22 C20 C16 113.9(5) . . ? C22 C20 C21 109.6(5) . . ? C16 C20 C21 110.1(5) . . ? C24 C23 C28 122.3(4) . . ? C24 C23 N9 118.6(4) . . ? C28 C23 N9 119.1(4) . . ? C25 C24 C23 117.4(5) . . ? C25 C24 C29 121.0(5) . . ? C23 C24 C29 121.6(4) . . ? C26 C25 C24 121.8(5) . . ? C27 C26 C25 119.5(5) . . ? C26 C27 C28 121.7(5) . . ? C27 C28 C23 117.3(5) . . ? C27 C28 C32 120.3(5) . . ? C23 C28 C32 122.3(4) . . ? C30 C29 C24 111.1(5) . . ? C30 C29 C31 109.0(5) . . ? C24 C29 C31 112.8(4) . . ? C28 C32 C33 113.0(5) . . ? C28 C32 C34 109.8(5) . . ? C33 C32 C34 110.4(5) . . ? O1 C35 C36 123.3(4) . . ? O1 C35 C43 116.4(4) . . ? C36 C35 C43 120.3(4) . . ? C37 C36 C35 124.7(4) . . ? O2 C37 C36 125.7(4) . . ? O2 C37 C49 116.6(4) . . ? C36 C37 C49 117.6(4) . . ? C39 C38 C43 120.0 . . ? C40 C39 C38 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C38 120.0 . . ? C42 C43 C35 122.2(3) . . ? C38 C43 C35 117.8(3) . . ? C45 C44 C49 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C49 120.0 . . ? C48 C49 C44 120.0 . . ? C48 C49 C37 118.1(3) . . ? C44 C49 C37 121.8(3) . . ? F2 Sb F1 92.2(2) . . ? F2 Sb F3 91.3(3) . . ? F1 Sb F3 90.2(2) . . ? F2 Sb F4 176.2(2) . . ? F1 Sb F4 91.0(2) . . ? F3 Sb F4 90.7(2) . . ? F2 Sb F5 89.4(3) . . ? F1 Sb F5 91.4(2) . . ? F3 Sb F5 178.3(2) . . ? F4 Sb F5 88.5(2) . . ? F2 Sb F6 88.6(2) . . ? F1 Sb F6 178.8(2) . . ? F3 Sb F6 90.6(2) . . ? F4 Sb F6 88.1(2) . . ? F5 Sb F6 87.9(3) . . ? _refine_diff_density_max 0.873 _refine_diff_density_min -1.344 _refine_diff_density_rms 0.081