data_bm08sasq-sr _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H30 B2 F30 Fe N2 Ni O2 P2 S2, C4H8O, C5H12' _chemical_formula_sum 'C78 H50 B2 F30 Fe N2 Ni O3 P2 S2' _chemical_formula_structural ? _chemical_formula_weight 1895.44 _chemical_absolute_configuration ? _chemical_formula_iupac ? _chemical_formula_analytical ? _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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7927(16) _cell_length_b 17.481(2) _cell_length_c 18.899(2) _cell_angle_alpha 102.1330(10) _cell_angle_beta 107.4610(10) _cell_angle_gamma 100.6930(10) _cell_volume 4095.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9921 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.08 _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.348 _exptl_crystal_size_min 0.241 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_crystal_id bm08sasq-sr _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (0 1 0) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.8307 _exptl_absorpt_correction_T_max 0.9089 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; One distinct cell was identified using APEX2 (Bruker, 2010). Four frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2005) then corrected for absorption by integration using SHELXTL/XPREP V2005/2 (Bruker, 2005) before using SADABS (Bruker, 2005) to sort, merge, and scale the combined data. Combined data with complete or no overlap were used for refinement. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id bm08sasq-sr _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type ? _diffrn_measurement_device 'Siemens Platform/ApexII CCD' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16168 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.10 _reflns_number_total 16164 _reflns_number_gt 12345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2010.11-3 (Bruker, 2010)' _computing_cell_refinement 'SAINT V7.68A (Bruker, 2005)' _computing_data_reduction ; SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 (Bruker, 2005 & 2007) ; _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2005)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2005)' _computing_molecular_graphics ; SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) ; _computing_publication_material 'XCIF V6.12 (Bruker, 2005)' _refine_special_details ; Structure was phased by direct methods (Sheldrick, 2008). Systematic conditions suggested the ambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. The final difference Fourier map had no significant features. A final analysis of variance between observed and calculated structure factors showed some dependence on amplitude and little dependence on resolution. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^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 'noref' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16164 _refine_ls_number_parameters 1559 _refine_ls_number_restraints 2681 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.000 _refine_ls_abs_structure_details ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.24715(2) 0.107208(17) 0.332802(15) 0.03364(7) Uani 1 1 d . A . Ni1 Ni 0.376767(18) 0.148335(15) 0.228921(13) 0.03259(7) Uani 1 1 d . C . P1 P 0.33800(4) 0.13338(3) 0.10506(3) 0.03797(12) Uani 1 1 d D . . P2 P 0.53767(4) 0.14845(3) 0.23684(3) 0.03392(12) Uani 1 1 d . . . S1 S 0.21643(4) 0.15885(3) 0.22640(3) 0.03571(11) Uani 1 1 d . . . S2 S 0.41781(4) 0.18127(3) 0.35675(3) 0.03455(11) Uani 1 1 d . . . N1 N 0.18413(12) 0.23550(10) 0.43219(9) 0.0381(4) Uani 1 1 d . A . N2 N 0.26665(13) -0.05539(11) 0.24824(9) 0.0388(4) Uani 1 1 d . A . B1 B 0.13143(18) 0.28946(15) 0.47781(13) 0.0392(5) Uani 1 1 d D . . B2 B 0.2482(2) -0.14946(15) 0.21789(14) 0.0418(5) Uani 1 1 d D . . O1 O 0.02276(12) 0.02067(11) 0.28520(10) 0.0624(5) Uani 1 1 d . C . O2 O 0.32008(14) 0.05983(10) 0.47639(9) 0.0615(4) Uani 1 1 d . C . C1 C 0.10907(17) 0.05270(13) 0.30296(12) 0.0429(5) Uani 1 1 d . . . C2 C 0.29118(17) 0.07549(13) 0.42023(13) 0.0431(5) Uani 1 1 d . . . C3 C 0.21393(15) 0.19245(13) 0.39390(11) 0.0366(4) Uani 1 1 d . . . C4 C 0.2360(8) 0.3560(7) 0.5470(5) 0.038(3) Uani 0.215(7) 1 d PGDU A 1 C5 C 0.3009(9) 0.4094(9) 0.5247(4) 0.039(3) Uani 0.215(7) 1 d PGDU A 1 C6 C 0.3907(11) 0.4657(10) 0.5800(5) 0.041(3) Uani 0.215(7) 1 d PGDU A 1 C7 C 0.4157(10) 0.4684(10) 0.6576(5) 0.045(3) Uani 0.215(7) 1 d PGDU A 1 C8 C 0.3509(10) 0.4150(9) 0.6799(4) 0.042(3) Uani 0.215(7) 1 d PGDU A 1 C9 C 0.2610(9) 0.3587(8) 0.6246(5) 0.041(3) Uani 0.215(7) 1 d PGDU A 1 F1 F 0.2900(11) 0.3982(10) 0.4500(5) 0.038(3) Uani 0.215(7) 1 d PDU A 1 F2 F 0.4669(10) 0.5028(10) 0.5582(8) 0.048(3) Uani 0.215(7) 1 d PDU A 1 F3 F 0.5069(9) 0.5158(9) 0.7119(7) 0.049(3) Uani 0.215(7) 1 d PDU A 1 F4 F 0.3713(12) 0.4237(10) 0.7562(5) 0.048(3) Uani 0.215(7) 1 d PDU A 1 F5 F 0.1993(10) 0.3120(8) 0.6511(7) 0.044(3) Uani 0.215(7) 1 d PDU A 1 C4B C 0.2296(3) 0.3570(2) 0.54967(18) 0.0359(9) Uani 0.785(7) 1 d PDU A 2 C5B C 0.3089(3) 0.4067(3) 0.53499(19) 0.0370(8) Uani 0.785(7) 1 d PDU A 2 C6B C 0.3968(3) 0.4612(3) 0.5906(2) 0.0439(9) Uani 0.785(7) 1 d PDU A 2 C7B C 0.4121(3) 0.4689(3) 0.6670(2) 0.0486(10) Uani 0.785(7) 1 d PDU A 2 C8B C 0.3378(3) 0.4221(3) 0.68569(19) 0.0445(10) Uani 0.785(7) 1 d PDU A 2 C9B C 0.2502(3) 0.3680(3) 0.62764(19) 0.0397(9) Uani 0.785(7) 1 d PDU A 2 F1B F 0.2957(4) 0.4054(3) 0.46088(19) 0.0499(10) Uani 0.785(7) 1 d PDU A 2 F2B F 0.4632(3) 0.5125(3) 0.5711(3) 0.0651(12) Uani 0.785(7) 1 d PDU A 2 F3B F 0.4944(3) 0.5253(3) 0.7229(2) 0.0704(13) Uani 0.785(7) 1 d PDU A 2 F4B F 0.3514(4) 0.4285(3) 0.76080(17) 0.0685(13) Uani 0.785(7) 1 d PDU A 2 F5B F 0.1812(3) 0.3255(3) 0.6527(2) 0.0592(12) Uani 0.785(7) 1 d PDU A 2 C10 C 0.0562(4) 0.2258(3) 0.5072(4) 0.038(2) Uani 0.396(4) 1 d PGDU A 1 C11 C 0.0787(4) 0.1559(4) 0.5240(4) 0.0433(19) Uani 0.396(4) 1 d PGDU A 1 C12 C 0.0151(5) 0.1095(4) 0.5528(5) 0.050(2) Uani 0.396(4) 1 d PGDU A 1 C13 C -0.0709(5) 0.1330(4) 0.5649(5) 0.052(2) Uani 0.396(4) 1 d PGDU A 1 C14 C -0.0934(5) 0.2028(4) 0.5481(5) 0.053(2) Uani 0.396(4) 1 d PGDU A 1 C15 C -0.0299(5) 0.2492(3) 0.5193(5) 0.045(2) Uani 0.396(4) 1 d PGDU A 1 F6 F 0.1623(4) 0.1322(4) 0.5180(4) 0.0579(14) Uani 0.396(4) 1 d PDU A 1 F7 F 0.0360(6) 0.0417(3) 0.5694(4) 0.0651(17) Uani 0.396(4) 1 d PDU A 1 F8 F -0.1212(6) 0.0930(5) 0.6037(4) 0.0582(17) Uani 0.396(4) 1 d PDU A 1 F9 F -0.1767(4) 0.2232(4) 0.5606(4) 0.0671(16) Uani 0.396(4) 1 d PDU A 1 F10 F -0.0548(5) 0.3164(3) 0.5069(4) 0.0583(15) Uani 0.396(4) 1 d PDU A 1 C10B C 0.0546(3) 0.2310(3) 0.5069(3) 0.0384(16) Uani 0.604(4) 1 d PDU A 2 C11B C 0.0860(3) 0.1707(3) 0.5379(3) 0.0418(12) Uani 0.604(4) 1 d PDU A 2 C12B C 0.0271(4) 0.1200(3) 0.5656(4) 0.0494(14) Uani 0.604(4) 1 d PDU A 2 C13B C -0.0697(4) 0.1282(3) 0.5643(4) 0.0542(17) Uani 0.604(4) 1 d PDU A 2 C14B C -0.1054(3) 0.1869(3) 0.5356(4) 0.0482(13) Uani 0.604(4) 1 d PDU A 2 C15B C -0.0434(4) 0.2362(3) 0.5087(3) 0.0407(13) Uani 0.604(4) 1 d PDU A 2 F6B F 0.1836(3) 0.1608(3) 0.5451(2) 0.0587(10) Uani 0.604(4) 1 d PDU A 2 F7B F 0.0646(4) 0.0628(3) 0.5951(3) 0.0664(11) Uani 0.604(4) 1 d PDU A 2 F8B F -0.1332(4) 0.0747(3) 0.5848(3) 0.0715(15) Uani 0.604(4) 1 d PDU A 2 F9B F -0.2006(3) 0.1973(3) 0.5316(3) 0.0730(12) Uani 0.604(4) 1 d PDU A 2 F10B F -0.0839(3) 0.2943(2) 0.4829(3) 0.0603(11) Uani 0.604(4) 1 d PDU A 2 C16 C 0.0634(5) 0.3244(3) 0.4092(2) 0.0415(17) Uani 0.493(5) 1 d PGDU A 1 C17 C 0.0041(5) 0.2673(2) 0.3384(3) 0.0521(17) Uani 0.493(5) 1 d PGDU A 1 C18 C -0.0525(5) 0.2917(3) 0.2769(2) 0.0574(16) Uani 0.493(5) 1 d PGDU A 1 C19 C -0.0499(5) 0.3732(3) 0.2861(2) 0.0534(16) Uani 0.493(5) 1 d PGDU A 1 C20 C 0.0094(6) 0.4303(3) 0.3568(3) 0.0506(15) Uani 0.493(5) 1 d PGDU A 1 C21 C 0.0660(5) 0.4059(3) 0.4184(2) 0.0482(18) Uani 0.493(5) 1 d PGDU A 1 F11 F -0.0103(6) 0.1872(3) 0.3270(4) 0.0592(15) Uani 0.493(5) 1 d PDU A 1 F12 F -0.1129(5) 0.2378(3) 0.2098(3) 0.0844(17) Uani 0.493(5) 1 d PDU A 1 F13 F -0.1005(5) 0.3984(3) 0.2264(3) 0.0770(14) Uani 0.493(5) 1 d PDU A 1 F14 F 0.0065(6) 0.5077(3) 0.3677(3) 0.0718(15) Uani 0.493(5) 1 d PDU A 1 F15 F 0.1158(7) 0.4618(4) 0.4869(4) 0.0568(16) Uani 0.493(5) 1 d PDU A 1 C16B C 0.0616(6) 0.3309(3) 0.4169(3) 0.0413(16) Uani 0.507(5) 1 d PDU A 2 C17B C 0.0003(6) 0.2876(4) 0.3392(3) 0.0468(13) Uani 0.507(5) 1 d PDU A 2 C18B C -0.0454(6) 0.3216(4) 0.2818(3) 0.0601(16) Uani 0.507(5) 1 d PDU A 2 C19B C -0.0373(7) 0.4029(4) 0.3006(4) 0.0597(16) Uani 0.507(5) 1 d PDU A 2 C20B C 0.0110(7) 0.4477(4) 0.3756(4) 0.0580(16) Uani 0.507(5) 1 d PDU A 2 C21B C 0.0587(6) 0.4110(4) 0.4301(4) 0.0469(14) Uani 0.507(5) 1 d PDU A 2 F11B F -0.0086(7) 0.2071(3) 0.3164(4) 0.0681(17) Uani 0.507(5) 1 d PDU A 2 F12B F -0.0944(6) 0.2741(4) 0.2094(3) 0.102(2) Uani 0.507(5) 1 d PDU A 2 F13B F -0.0823(5) 0.4366(4) 0.2456(3) 0.0899(17) Uani 0.507(5) 1 d PDU A 2 F14B F 0.0211(6) 0.5279(3) 0.3955(4) 0.0831(18) Uani 0.507(5) 1 d PDU A 2 F15B F 0.1102(8) 0.4625(5) 0.5020(4) 0.069(2) Uani 0.507(5) 1 d PDU A 2 C22 C 0.26747(15) 0.01020(13) 0.27592(11) 0.0365(4) Uani 1 1 d . . . C23 C 0.3488(5) -0.1745(5) 0.2780(3) 0.049(2) Uani 0.377(4) 1 d PGDU B 1 C24 C 0.3567(6) -0.1512(6) 0.3549(3) 0.047(2) Uani 0.377(4) 1 d PGDU B 1 C25 C 0.4320(7) -0.1707(6) 0.4108(3) 0.055(2) Uani 0.377(4) 1 d PGDU B 1 C26 C 0.4993(6) -0.2134(5) 0.3897(3) 0.061(2) Uani 0.377(4) 1 d PGDU B 1 C27 C 0.4913(5) -0.2367(5) 0.3128(3) 0.060(2) Uani 0.377(4) 1 d PGDU B 1 C28 C 0.4160(5) -0.2172(4) 0.2569(3) 0.0501(19) Uani 0.377(4) 1 d PGDU B 1 F16 F 0.2995(5) -0.1063(5) 0.3799(5) 0.0516(17) Uani 0.377(4) 1 d PDU B 1 F17 F 0.4408(8) -0.1516(6) 0.4853(4) 0.068(2) Uani 0.377(4) 1 d PDU B 1 F18 F 0.5725(7) -0.2311(5) 0.4448(5) 0.064(2) Uani 0.377(4) 1 d PDU B 1 F19 F 0.5527(5) -0.2826(4) 0.2919(4) 0.087(2) Uani 0.377(4) 1 d PDU B 1 F20 F 0.4103(5) -0.2456(4) 0.1849(3) 0.0742(18) Uani 0.377(4) 1 d PDU B 1 C23B C 0.3393(4) -0.1733(3) 0.2803(2) 0.0409(13) Uani 0.623(4) 1 d PDU B 2 C24B C 0.3708(4) -0.1428(4) 0.3598(2) 0.0436(14) Uani 0.623(4) 1 d PDU B 2 C25B C 0.4407(5) -0.1664(4) 0.4142(2) 0.0530(15) Uani 0.623(4) 1 d PDU B 2 C26B C 0.4867(5) -0.2246(4) 0.3899(3) 0.0584(14) Uani 0.623(4) 1 d PDU B 2 C27B C 0.4587(4) -0.2585(3) 0.3123(3) 0.0603(13) Uani 0.623(4) 1 d PDU B 2 C28B C 0.3863(4) -0.2337(3) 0.2600(2) 0.0531(12) Uani 0.623(4) 1 d PDU B 2 F16B F 0.3249(4) -0.0880(3) 0.3886(3) 0.0615(13) Uani 0.623(4) 1 d PDU B 2 F17B F 0.4624(5) -0.1321(4) 0.4899(2) 0.0691(14) Uani 0.623(4) 1 d PDU B 2 F18B F 0.5539(5) -0.2523(4) 0.4398(3) 0.0829(16) Uani 0.623(4) 1 d PDU B 2 F19B F 0.5015(4) -0.3164(3) 0.2862(3) 0.0967(14) Uani 0.623(4) 1 d PDU B 2 F20B F 0.3609(4) -0.2726(2) 0.18430(19) 0.0791(12) Uani 0.623(4) 1 d PDU B 2 C29 C 0.2618(10) -0.1707(7) 0.1325(4) 0.042(3) Uani 0.195(7) 1 d PGDU B 1 C30 C 0.3318(11) -0.1158(7) 0.1154(5) 0.042(3) Uani 0.195(7) 1 d PGDU B 1 C31 C 0.3402(12) -0.1331(8) 0.0426(6) 0.048(3) Uani 0.195(7) 1 d PGDU B 1 C32 C 0.2788(12) -0.2055(8) -0.0131(5) 0.049(3) Uani 0.195(7) 1 d PGDU B 1 C33 C 0.2088(11) -0.2604(7) 0.0040(5) 0.051(3) Uani 0.195(7) 1 d PGDU B 1 C34 C 0.2003(10) -0.2431(7) 0.0768(5) 0.048(3) Uani 0.195(7) 1 d PGDU B 1 F21 F 0.3931(13) -0.0454(8) 0.1668(8) 0.039(3) Uani 0.195(7) 1 d PDU B 1 F22 F 0.4100(10) -0.0818(8) 0.0263(8) 0.039(4) Uani 0.195(7) 1 d PDU B 1 F23 F 0.2897(12) -0.2238(9) -0.0824(6) 0.049(3) Uani 0.195(7) 1 d PDU B 1 F24 F 0.1500(12) -0.3294(7) -0.0513(8) 0.065(4) Uani 0.195(7) 1 d PDU B 1 F25 F 0.1363(10) -0.2995(8) 0.0915(8) 0.062(3) Uani 0.195(7) 1 d PDU B 1 C29B C 0.2512(3) -0.1687(2) 0.12999(16) 0.0380(8) Uani 0.805(7) 1 d PDU B 2 C30B C 0.3259(3) -0.1213(2) 0.11124(18) 0.0427(9) Uani 0.805(7) 1 d PDU B 2 C31B C 0.3352(3) -0.1353(2) 0.03927(19) 0.0458(9) Uani 0.805(7) 1 d PDU B 2 C32B C 0.2685(3) -0.2018(3) -0.01856(18) 0.0520(10) Uani 0.805(7) 1 d PDU B 2 C33B C 0.1916(3) -0.2508(2) -0.00399(19) 0.0544(11) Uani 0.805(7) 1 d PDU B 2 C34B C 0.1852(3) -0.2346(2) 0.06874(19) 0.0458(9) Uani 0.805(7) 1 d PDU B 2 F21B F 0.3979(4) -0.0555(2) 0.1659(2) 0.0621(13) Uani 0.805(7) 1 d PDU B 2 F22B F 0.4079(4) -0.0838(3) 0.0254(3) 0.0719(15) Uani 0.805(7) 1 d PDU B 2 F23B F 0.2767(4) -0.2159(3) -0.08880(17) 0.0794(14) Uani 0.805(7) 1 d PDU B 2 F24B F 0.1237(3) -0.3157(2) -0.0606(2) 0.0861(14) Uani 0.805(7) 1 d PDU B 2 F25B F 0.1094(2) -0.2881(2) 0.07816(18) 0.0588(9) Uani 0.805(7) 1 d PDU B 2 C35 C 0.1277(4) -0.1874(5) 0.2164(5) 0.047(2) Uani 0.381(6) 1 d PGDU B 1 C36 C 0.0481(5) -0.1523(5) 0.1860(6) 0.050(2) Uani 0.381(6) 1 d PGDU B 1 C37 C -0.0510(4) -0.1781(5) 0.1903(6) 0.058(2) Uani 0.381(6) 1 d PGDU B 1 C38 C -0.0704(4) -0.2390(5) 0.2251(6) 0.066(2) Uani 0.381(6) 1 d PGDU B 1 C39 C 0.0092(5) -0.2741(5) 0.2555(6) 0.062(2) Uani 0.381(6) 1 d PGDU B 1 C40 C 0.1083(4) -0.2483(5) 0.2512(6) 0.058(2) Uani 0.381(6) 1 d PGDU B 1 F26 F 0.0645(8) -0.0873(5) 0.1593(5) 0.0482(19) Uani 0.381(6) 1 d PDU B 1 F27 F -0.1268(6) -0.1411(5) 0.1650(6) 0.068(2) Uani 0.381(6) 1 d PDU B 1 F28 F -0.1671(5) -0.2638(5) 0.2275(5) 0.087(2) Uani 0.381(6) 1 d PDU B 1 F29 F -0.0079(7) -0.3326(5) 0.2897(5) 0.078(2) Uani 0.381(6) 1 d PDU B 1 F30 F 0.1827(6) -0.2807(5) 0.2884(6) 0.0596(19) Uani 0.381(6) 1 d PDU B 1 C35B C 0.1319(3) -0.1897(3) 0.2200(4) 0.0455(15) Uani 0.619(6) 1 d PDU B 2 C36B C 0.0445(4) -0.1627(4) 0.1880(4) 0.0471(13) Uani 0.619(6) 1 d PDU B 2 C37B C -0.0566(4) -0.1944(4) 0.1838(4) 0.0602(15) Uani 0.619(6) 1 d PDU B 2 C38B C -0.0780(4) -0.2605(4) 0.2108(4) 0.0706(16) Uani 0.619(6) 1 d PDU B 2 C39B C 0.0035(4) -0.2911(4) 0.2420(4) 0.0690(17) Uani 0.619(6) 1 d PDU B 2 C40B C 0.1026(4) -0.2557(4) 0.2468(4) 0.0618(17) Uani 0.619(6) 1 d PDU B 2 F26B F 0.0558(5) -0.1046(3) 0.1511(4) 0.0533(13) Uani 0.619(6) 1 d PDU B 2 F27B F -0.1359(4) -0.1650(4) 0.1488(4) 0.0751(15) Uani 0.619(6) 1 d PDU B 2 F28B F -0.1763(3) -0.2941(4) 0.2054(3) 0.0945(16) Uani 0.619(6) 1 d PDU B 2 F29B F -0.0165(5) -0.3559(3) 0.2677(4) 0.103(2) Uani 0.619(6) 1 d PDU B 2 F30B F 0.1751(5) -0.2964(4) 0.2712(4) 0.0835(19) Uani 0.619(6) 1 d PDU B 2 C41 C 0.24293(16) 0.26944(13) 0.26476(12) 0.0427(5) Uani 1 1 d . C . H41A H 0.2161 0.2919 0.2210 0.051 Uiso 1 1 calc R . . H41B H 0.2026 0.2802 0.2994 0.051 Uiso 1 1 calc R . . C42 C 0.35781(17) 0.31438(13) 0.30887(13) 0.0444(5) Uani 1 1 d . . . H42A H 0.3622 0.3727 0.3275 0.053 Uiso 1 1 calc R C . H42B H 0.3960 0.3092 0.2720 0.053 Uiso 1 1 calc R . . C43 C 0.41602(16) 0.28777(12) 0.37787(12) 0.0417(5) Uani 1 1 d . C . H43A H 0.3831 0.2986 0.4175 0.050 Uiso 1 1 calc R . . H43B H 0.4898 0.3219 0.4006 0.050 Uiso 1 1 calc R . . C44 C 0.2912(6) 0.2181(3) 0.0772(5) 0.040(2) Uani 0.499(13) 1 d PGDU C 1 C45 C 0.3537(5) 0.2976(4) 0.1024(6) 0.055(2) Uani 0.499(13) 1 d PGU C 1 H45A H 0.4278 0.3089 0.1274 0.066 Uiso 0.499(13) 1 calc PR C 1 C46 C 0.3078(7) 0.3605(3) 0.0911(6) 0.075(3) Uani 0.499(13) 1 d PGU C 1 H46A H 0.3505 0.4148 0.1084 0.090 Uiso 0.499(13) 1 calc PR C 1 C47 C 0.1994(8) 0.3439(5) 0.0546(7) 0.082(3) Uani 0.499(13) 1 d PGU C 1 H47A H 0.1680 0.3869 0.0469 0.098 Uiso 0.499(13) 1 calc PR C 1 C48 C 0.1369(5) 0.2644(6) 0.0294(7) 0.087(3) Uani 0.499(13) 1 d PGU C 1 H48A H 0.0628 0.2530 0.0044 0.104 Uiso 0.499(13) 1 calc PR C 1 C49 C 0.1828(5) 0.2015(4) 0.0407(6) 0.067(3) Uani 0.499(13) 1 d PGU C 1 H49A H 0.1401 0.1472 0.0235 0.080 Uiso 0.499(13) 1 calc PR C 1 C44B C 0.2890(6) 0.2198(3) 0.0859(5) 0.048(3) Uani 0.501(13) 1 d PGDU C 2 C45B C 0.3631(5) 0.2949(4) 0.1175(5) 0.048(2) Uani 0.501(13) 1 d PGU C 2 H45B H 0.4329 0.2992 0.1496 0.058 Uiso 0.501(13) 1 calc PR C 2 C46B C 0.3351(7) 0.3637(3) 0.1022(6) 0.069(2) Uani 0.501(13) 1 d PGU C 2 H46B H 0.3857 0.4151 0.1238 0.082 Uiso 0.501(13) 1 calc PR C 2 C47B C 0.2331(8) 0.3574(4) 0.0552(6) 0.075(3) Uani 0.501(13) 1 d PGU C 2 H47B H 0.2139 0.4044 0.0448 0.090 Uiso 0.501(13) 1 calc PR C 2 C48B C 0.1590(6) 0.2822(5) 0.0236(6) 0.073(3) Uani 0.501(13) 1 d PGU C 2 H48B H 0.0892 0.2779 -0.0084 0.087 Uiso 0.501(13) 1 calc PR C 2 C49B C 0.1870(5) 0.2134(4) 0.0390(6) 0.056(3) Uani 0.501(13) 1 d PGU C 2 H49B H 0.1364 0.1621 0.0174 0.067 Uiso 0.501(13) 1 calc PR C 2 C50 C 0.23908(16) 0.04446(14) 0.03480(12) 0.0441(5) Uani 1 1 d . C . C51 C 0.2275(2) 0.02914(17) -0.04327(13) 0.0606(7) Uani 1 1 d . . . H51A H 0.2732 0.0638 -0.0591 0.073 Uiso 1 1 calc R C . C52 C 0.1499(2) -0.03615(19) -0.09733(15) 0.0706(8) Uani 1 1 d . C . H52A H 0.1428 -0.0466 -0.1503 0.085 Uiso 1 1 calc R . . C53 C 0.0825(2) -0.08633(18) -0.07540(15) 0.0658(7) Uani 1 1 d . . . H53A H 0.0288 -0.1311 -0.1131 0.079 Uiso 1 1 calc R C . C54 C 0.09295(19) -0.07167(16) 0.00121(14) 0.0571(6) Uani 1 1 d . C . H54A H 0.0463 -0.1063 0.0164 0.068 Uiso 1 1 calc R . . C55 C 0.17115(17) -0.00664(14) 0.05635(12) 0.0460(5) Uani 1 1 d . . . H55A H 0.1782 0.0030 0.1093 0.055 Uiso 1 1 calc R C . C56 C 0.45798(16) 0.13796(15) 0.08063(12) 0.0447(5) Uani 1 1 d . C . H56A H 0.4400 0.1018 0.0280 0.054 Uiso 1 1 calc R . . H56B H 0.4883 0.1941 0.0810 0.054 Uiso 1 1 calc R . . C57 C 0.53936(16) 0.11172(13) 0.13899(11) 0.0400(5) Uani 1 1 d . C . H57A H 0.6105 0.1337 0.1384 0.048 Uiso 1 1 calc R . . H57B H 0.5235 0.0517 0.1240 0.048 Uiso 1 1 calc R . . C58 C 0.62227(15) 0.25168(12) 0.27855(12) 0.0385(5) Uani 1 1 d . C . C59 C 0.66844(16) 0.28212(14) 0.35865(13) 0.0460(5) Uani 1 1 d . . . H59A H 0.6569 0.2485 0.3905 0.055 Uiso 1 1 calc R C . C60 C 0.73136(18) 0.36151(15) 0.39227(15) 0.0549(6) Uani 1 1 d . C . H60A H 0.7631 0.3818 0.4470 0.066 Uiso 1 1 calc R . . C61 C 0.74788(19) 0.41087(15) 0.34664(16) 0.0571(6) Uani 1 1 d . . . H61A H 0.7904 0.4652 0.3697 0.069 Uiso 1 1 calc R C . C62 C 0.70206(19) 0.38080(15) 0.26695(16) 0.0596(6) Uani 1 1 d . C . H62A H 0.7131 0.4148 0.2354 0.072 Uiso 1 1 calc R . . C63 C 0.64079(17) 0.30214(14) 0.23323(14) 0.0491(5) Uani 1 1 d . . . H63A H 0.6107 0.2820 0.1785 0.059 Uiso 1 1 calc R C . C64 C 0.61062(15) 0.09167(13) 0.29300(11) 0.0388(5) Uani 1 1 d . C . C65 C 0.56276(16) 0.03891(13) 0.32560(12) 0.0428(5) Uani 1 1 d . . . H65A H 0.4905 0.0324 0.3193 0.051 Uiso 1 1 calc R C . C66 C 0.61991(18) -0.00422(16) 0.36719(14) 0.0561(6) Uani 1 1 d . C . H66A H 0.5869 -0.0399 0.3898 0.067 Uiso 1 1 calc R . . C67 C 0.7242(2) 0.00427(16) 0.37602(15) 0.0609(7) Uani 1 1 d . . . H67A H 0.7630 -0.0258 0.4044 0.073 Uiso 1 1 calc R C . C68 C 0.77312(18) 0.05664(17) 0.34359(15) 0.0609(7) Uani 1 1 d . C . H68A H 0.8452 0.0623 0.3496 0.073 Uiso 1 1 calc R . . C69 C 0.71675(17) 0.10052(15) 0.30262(14) 0.0510(6) Uani 1 1 d . . . H69A H 0.7503 0.1369 0.2809 0.061 Uiso 1 1 calc R C . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03171(15) 0.04151(16) 0.02890(14) 0.01180(12) 0.01258(11) 0.00735(12) Ni1 0.02830(13) 0.04558(15) 0.02792(13) 0.01551(11) 0.01141(10) 0.01095(11) P1 0.0345(3) 0.0536(3) 0.0304(3) 0.0180(2) 0.0128(2) 0.0131(2) P2 0.0295(2) 0.0434(3) 0.0334(3) 0.0166(2) 0.0132(2) 0.0104(2) S1 0.0296(2) 0.0491(3) 0.0313(2) 0.0154(2) 0.0112(2) 0.0118(2) S2 0.0296(2) 0.0454(3) 0.0288(2) 0.0128(2) 0.00995(19) 0.0086(2) N1 0.0331(9) 0.0468(10) 0.0360(9) 0.0125(8) 0.0157(7) 0.0073(8) N2 0.0383(9) 0.0464(11) 0.0326(9) 0.0142(8) 0.0114(7) 0.0117(8) B1 0.0358(12) 0.0493(14) 0.0367(12) 0.0125(10) 0.0178(10) 0.0122(11) B2 0.0483(14) 0.0421(13) 0.0354(12) 0.0145(10) 0.0136(11) 0.0109(11) O1 0.0383(9) 0.0716(12) 0.0689(11) 0.0147(9) 0.0196(8) -0.0001(8) O2 0.0765(12) 0.0678(11) 0.0382(9) 0.0272(8) 0.0145(8) 0.0103(9) C1 0.0435(12) 0.0481(13) 0.0395(11) 0.0119(10) 0.0194(10) 0.0108(10) C2 0.0440(12) 0.0432(12) 0.0423(12) 0.0130(10) 0.0187(10) 0.0055(10) C3 0.0296(10) 0.0461(12) 0.0312(10) 0.0129(9) 0.0098(8) 0.0029(9) C4 0.040(4) 0.043(4) 0.036(4) 0.012(4) 0.015(4) 0.017(4) C5 0.035(4) 0.043(4) 0.041(4) 0.015(4) 0.014(4) 0.008(4) C6 0.041(4) 0.044(4) 0.042(4) 0.016(3) 0.018(3) 0.011(4) C7 0.036(4) 0.047(4) 0.047(4) 0.010(4) 0.014(4) 0.007(4) C8 0.045(4) 0.050(4) 0.033(4) 0.010(3) 0.013(3) 0.023(4) C9 0.043(4) 0.044(4) 0.041(4) 0.017(3) 0.014(3) 0.018(3) F1 0.040(4) 0.049(5) 0.031(4) 0.015(3) 0.021(3) 0.012(4) F2 0.045(4) 0.050(5) 0.046(4) 0.008(4) 0.030(3) -0.006(4) F3 0.040(4) 0.059(5) 0.040(4) 0.002(4) 0.015(3) 0.006(3) F4 0.054(4) 0.061(5) 0.033(4) 0.015(3) 0.021(3) 0.015(4) F5 0.044(4) 0.058(5) 0.032(4) 0.014(3) 0.019(3) 0.009(4) C4B 0.0320(14) 0.0436(16) 0.0377(16) 0.0140(14) 0.0167(13) 0.0130(13) C5B 0.0384(16) 0.0433(16) 0.0340(14) 0.0146(13) 0.0144(13) 0.0149(13) C6B 0.0377(16) 0.0439(17) 0.0519(18) 0.0163(15) 0.0182(14) 0.0077(14) C7B 0.0383(16) 0.0475(18) 0.0462(17) 0.0046(15) 0.0034(15) 0.0080(15) C8B 0.0451(17) 0.0547(18) 0.0339(15) 0.0107(13) 0.0109(13) 0.0209(15) C9B 0.0397(15) 0.0449(17) 0.0398(15) 0.0141(13) 0.0186(12) 0.0133(14) F1B 0.0569(17) 0.0541(18) 0.0377(14) 0.0120(13) 0.0233(13) 0.0024(14) F2B 0.0567(16) 0.0577(18) 0.070(2) 0.0046(15) 0.0291(14) -0.0069(13) F3B 0.0510(16) 0.0707(19) 0.0600(18) -0.0088(13) 0.0058(14) 0.0011(14) F4B 0.075(2) 0.085(2) 0.0333(13) 0.0107(12) 0.0101(12) 0.0134(17) F5B 0.0624(18) 0.074(2) 0.0400(13) 0.0173(12) 0.0251(12) 0.0030(15) C10 0.032(3) 0.050(3) 0.039(3) 0.007(3) 0.025(3) 0.009(3) C11 0.049(3) 0.049(3) 0.042(3) 0.018(3) 0.024(2) 0.017(3) C12 0.055(3) 0.047(3) 0.056(3) 0.018(3) 0.028(3) 0.013(3) C13 0.045(3) 0.056(3) 0.065(3) 0.021(3) 0.037(3) 0.005(3) C14 0.044(3) 0.054(3) 0.064(3) 0.012(3) 0.026(3) 0.013(3) C15 0.041(3) 0.045(3) 0.052(3) 0.015(3) 0.023(3) 0.008(3) F6 0.070(3) 0.065(3) 0.073(3) 0.036(2) 0.049(2) 0.039(2) F7 0.076(4) 0.057(3) 0.078(4) 0.031(2) 0.037(3) 0.025(2) F8 0.056(3) 0.052(3) 0.073(3) 0.021(2) 0.039(2) -0.001(2) F9 0.053(3) 0.075(3) 0.090(4) 0.023(3) 0.050(2) 0.018(2) F10 0.062(3) 0.048(3) 0.083(3) 0.018(2) 0.049(2) 0.022(2) C10B 0.037(2) 0.042(2) 0.034(2) 0.012(2) 0.011(2) 0.009(2) C11B 0.041(2) 0.051(2) 0.046(2) 0.016(2) 0.0268(18) 0.0183(18) C12B 0.049(2) 0.051(2) 0.058(3) 0.022(2) 0.026(2) 0.019(2) C13B 0.051(3) 0.051(2) 0.067(3) 0.026(2) 0.027(3) 0.007(2) C14B 0.031(2) 0.055(2) 0.066(3) 0.017(2) 0.0277(19) 0.0096(18) C15B 0.035(2) 0.041(2) 0.052(2) 0.0163(19) 0.0201(19) 0.0127(18) F6B 0.0520(16) 0.084(3) 0.074(2) 0.0446(18) 0.0418(15) 0.0399(16) F7B 0.065(2) 0.077(2) 0.088(3) 0.054(2) 0.0429(19) 0.0327(18) F8B 0.059(2) 0.065(3) 0.101(3) 0.034(2) 0.044(2) 0.0039(18) F9B 0.0409(16) 0.087(3) 0.111(3) 0.042(2) 0.0426(18) 0.0212(17) F10B 0.0505(19) 0.060(2) 0.095(3) 0.041(2) 0.0399(17) 0.0268(16) C16 0.034(3) 0.058(3) 0.041(3) 0.017(2) 0.021(2) 0.016(2) C17 0.045(3) 0.064(3) 0.046(3) 0.016(2) 0.007(2) 0.026(3) C18 0.054(3) 0.071(3) 0.042(3) 0.011(3) 0.011(2) 0.019(3) C19 0.051(3) 0.074(4) 0.042(3) 0.027(3) 0.013(2) 0.028(3) C20 0.055(3) 0.065(3) 0.051(3) 0.027(2) 0.028(2) 0.034(2) C21 0.046(3) 0.069(3) 0.041(3) 0.018(2) 0.024(2) 0.023(2) F11 0.055(2) 0.053(2) 0.053(2) 0.007(2) 0.0036(18) 0.012(2) F12 0.079(3) 0.095(4) 0.046(2) 0.003(2) -0.0108(18) 0.021(3) F13 0.081(3) 0.107(3) 0.049(2) 0.040(2) 0.0111(18) 0.037(3) F14 0.075(3) 0.076(3) 0.067(3) 0.036(2) 0.014(2) 0.029(2) F15 0.068(3) 0.050(2) 0.050(2) 0.0132(19) 0.012(2) 0.026(2) C16B 0.035(3) 0.063(3) 0.031(2) 0.015(2) 0.016(2) 0.014(2) C17B 0.038(2) 0.061(3) 0.044(3) 0.014(2) 0.011(2) 0.025(2) C18B 0.052(3) 0.079(4) 0.040(3) 0.019(3) 0.000(2) 0.021(3) C19B 0.053(3) 0.079(3) 0.052(3) 0.033(3) 0.012(2) 0.024(3) C20B 0.054(3) 0.074(3) 0.063(3) 0.032(3) 0.027(3) 0.033(3) C21B 0.043(2) 0.066(3) 0.049(3) 0.030(2) 0.027(2) 0.023(2) F11B 0.062(2) 0.059(3) 0.057(3) 0.008(2) -0.009(2) 0.014(2) F12B 0.102(3) 0.120(4) 0.045(2) 0.019(3) -0.014(2) 0.012(3) F13B 0.076(3) 0.115(4) 0.085(3) 0.068(3) 0.008(2) 0.031(3) F14B 0.084(3) 0.075(3) 0.097(4) 0.045(3) 0.018(3) 0.037(2) F15B 0.075(3) 0.065(3) 0.066(3) 0.015(2) 0.019(3) 0.030(2) C22 0.0317(10) 0.0497(13) 0.0273(10) 0.0155(9) 0.0080(8) 0.0079(9) C23 0.057(4) 0.049(4) 0.040(3) 0.020(3) 0.013(3) 0.013(3) C24 0.043(3) 0.056(3) 0.044(3) 0.023(3) 0.014(3) 0.012(3) C25 0.054(3) 0.066(4) 0.045(3) 0.025(3) 0.013(3) 0.012(3) C26 0.066(4) 0.056(3) 0.057(3) 0.029(3) 0.004(3) 0.022(3) C27 0.073(4) 0.057(3) 0.061(3) 0.027(3) 0.023(3) 0.030(3) C28 0.065(3) 0.051(3) 0.046(3) 0.024(2) 0.025(3) 0.022(3) F16 0.049(3) 0.075(3) 0.037(3) 0.017(2) 0.020(2) 0.020(3) F17 0.067(4) 0.091(4) 0.038(3) 0.029(2) 0.009(2) 0.007(3) F18 0.073(3) 0.046(3) 0.060(3) 0.022(2) -0.003(2) 0.019(3) F19 0.104(4) 0.087(4) 0.077(3) 0.019(3) 0.017(3) 0.070(3) F20 0.100(4) 0.090(4) 0.050(2) 0.017(2) 0.030(2) 0.064(3) C23B 0.044(2) 0.043(2) 0.041(2) 0.019(2) 0.0161(18) 0.0126(19) C24B 0.039(2) 0.056(2) 0.041(2) 0.022(2) 0.0156(18) 0.013(2) C25B 0.050(2) 0.067(3) 0.042(2) 0.029(2) 0.008(2) 0.012(2) C26B 0.068(3) 0.064(3) 0.051(2) 0.034(2) 0.014(2) 0.026(2) C27B 0.077(3) 0.056(2) 0.067(2) 0.0342(19) 0.029(2) 0.037(2) C28B 0.070(3) 0.059(2) 0.0443(19) 0.0235(18) 0.0282(18) 0.027(2) F16B 0.061(2) 0.092(3) 0.0423(19) 0.0248(17) 0.0201(17) 0.036(2) F17B 0.073(3) 0.091(3) 0.0414(19) 0.0280(16) 0.0101(16) 0.023(2) F18B 0.090(3) 0.085(3) 0.082(3) 0.053(2) 0.011(2) 0.039(3) F19B 0.130(3) 0.100(3) 0.093(2) 0.046(2) 0.042(2) 0.081(2) F20B 0.117(3) 0.080(2) 0.0522(16) 0.0194(15) 0.0262(18) 0.060(2) C29 0.043(4) 0.044(4) 0.036(4) 0.015(4) 0.006(4) 0.012(4) C30 0.038(4) 0.048(4) 0.039(4) 0.015(4) 0.015(4) 0.008(4) C31 0.043(4) 0.058(4) 0.041(4) 0.013(4) 0.015(4) 0.009(4) C32 0.048(4) 0.064(4) 0.036(4) 0.015(4) 0.014(4) 0.014(4) C33 0.050(4) 0.057(4) 0.038(4) 0.007(4) 0.012(4) 0.009(4) C34 0.049(4) 0.051(4) 0.039(4) 0.014(4) 0.012(4) 0.006(4) F21 0.040(5) 0.038(5) 0.038(5) 0.011(4) 0.016(4) 0.005(4) F22 0.040(6) 0.047(6) 0.036(5) 0.022(5) 0.020(5) -0.001(5) F23 0.056(5) 0.059(5) 0.039(5) 0.007(4) 0.025(4) 0.024(4) F24 0.070(6) 0.061(5) 0.039(5) -0.011(4) 0.013(4) -0.003(4) F25 0.070(6) 0.050(5) 0.054(5) 0.019(4) 0.014(4) -0.003(4) C29B 0.0371(15) 0.0439(16) 0.0355(15) 0.0137(13) 0.0132(12) 0.0133(13) C30B 0.0382(16) 0.0467(17) 0.0382(16) 0.0089(14) 0.0109(14) 0.0079(14) C31B 0.0413(16) 0.0573(18) 0.0411(16) 0.0195(15) 0.0161(14) 0.0094(15) C32B 0.0522(18) 0.072(2) 0.0300(15) 0.0145(14) 0.0146(14) 0.0131(16) C33B 0.0528(19) 0.0592(19) 0.0351(15) 0.0051(14) 0.0071(14) 0.0003(16) C34B 0.0456(17) 0.0514(17) 0.0384(15) 0.0163(13) 0.0127(13) 0.0074(14) F21B 0.0582(18) 0.0613(19) 0.0506(17) -0.0032(14) 0.0239(14) -0.0079(16) F22B 0.068(2) 0.083(2) 0.065(2) 0.0159(19) 0.0380(19) 0.003(2) F23B 0.074(2) 0.115(3) 0.0353(14) 0.0142(14) 0.0204(13) -0.0015(19) F24B 0.077(2) 0.099(2) 0.0474(15) -0.0036(15) 0.0171(14) -0.0219(18) F25B 0.0611(15) 0.0581(15) 0.0446(14) 0.0087(10) 0.0191(12) -0.0077(12) C35 0.054(4) 0.050(4) 0.040(3) 0.019(3) 0.022(3) 0.005(3) C36 0.047(3) 0.059(4) 0.042(3) 0.013(3) 0.018(3) 0.005(3) C37 0.051(3) 0.070(4) 0.052(3) 0.021(3) 0.022(3) 0.004(3) C38 0.058(3) 0.077(4) 0.060(3) 0.023(3) 0.031(3) -0.007(3) C39 0.071(3) 0.066(4) 0.055(3) 0.026(3) 0.034(3) 0.001(3) C40 0.061(3) 0.062(4) 0.055(3) 0.022(3) 0.026(3) 0.009(3) F26 0.046(3) 0.047(3) 0.043(3) 0.018(2) 0.007(2) 0.003(2) F27 0.051(3) 0.078(4) 0.064(4) 0.013(3) 0.016(2) 0.009(3) F28 0.067(3) 0.103(5) 0.095(4) 0.034(3) 0.046(3) -0.005(3) F29 0.089(4) 0.073(4) 0.080(4) 0.036(3) 0.045(3) 0.000(3) F30 0.066(3) 0.049(3) 0.069(3) 0.029(3) 0.025(2) 0.013(2) C35B 0.052(2) 0.048(2) 0.037(2) 0.014(2) 0.015(2) 0.012(2) C36B 0.052(2) 0.052(2) 0.037(2) 0.0206(18) 0.017(2) 0.004(2) C37B 0.047(2) 0.078(3) 0.050(3) 0.020(2) 0.013(2) 0.010(2) C38B 0.060(2) 0.085(3) 0.061(3) 0.021(3) 0.029(2) -0.010(2) C39B 0.071(3) 0.067(3) 0.067(3) 0.031(3) 0.027(2) -0.001(2) C40B 0.066(3) 0.065(3) 0.056(3) 0.027(2) 0.021(2) 0.010(2) F26B 0.044(2) 0.058(2) 0.056(2) 0.028(2) 0.0115(17) 0.0061(17) F27B 0.0474(19) 0.104(3) 0.073(3) 0.032(3) 0.0194(17) 0.012(2) F28B 0.068(2) 0.115(4) 0.094(3) 0.034(3) 0.0380(19) -0.013(2) F29B 0.111(3) 0.083(3) 0.117(4) 0.053(3) 0.046(3) -0.005(2) F30B 0.089(3) 0.063(3) 0.105(4) 0.047(3) 0.030(2) 0.014(2) C41 0.0438(11) 0.0485(12) 0.0459(12) 0.0205(10) 0.0208(10) 0.0194(10) C42 0.0486(12) 0.0395(12) 0.0505(13) 0.0159(10) 0.0229(10) 0.0119(10) C43 0.0396(11) 0.0407(12) 0.0420(12) 0.0087(9) 0.0159(9) 0.0049(9) C44 0.055(4) 0.058(5) 0.032(3) 0.024(3) 0.027(3) 0.036(4) C45 0.061(4) 0.062(4) 0.051(4) 0.037(3) 0.016(3) 0.020(3) C46 0.089(6) 0.047(4) 0.094(6) 0.037(4) 0.022(5) 0.031(3) C47 0.072(6) 0.082(6) 0.098(6) 0.042(5) 0.017(5) 0.038(5) C48 0.076(5) 0.087(5) 0.096(6) 0.044(5) 0.012(5) 0.027(4) C49 0.074(6) 0.071(4) 0.061(5) 0.029(4) 0.014(5) 0.036(4) C44B 0.048(4) 0.068(6) 0.030(3) 0.024(3) 0.011(3) 0.011(4) C45B 0.063(4) 0.065(4) 0.033(3) 0.030(3) 0.019(3) 0.032(3) C46B 0.072(4) 0.080(6) 0.054(4) 0.028(4) 0.009(4) 0.034(4) C47B 0.074(6) 0.076(5) 0.090(6) 0.041(4) 0.023(5) 0.043(4) C48B 0.063(4) 0.084(6) 0.077(5) 0.038(4) 0.008(4) 0.043(4) C49B 0.048(5) 0.060(4) 0.063(5) 0.027(4) 0.010(4) 0.025(4) C50 0.0386(11) 0.0604(14) 0.0354(11) 0.0185(10) 0.0103(9) 0.0172(10) C51 0.0619(15) 0.0785(18) 0.0350(12) 0.0190(12) 0.0114(11) 0.0100(14) C52 0.0694(18) 0.093(2) 0.0348(13) 0.0155(14) 0.0070(12) 0.0090(16) C53 0.0547(15) 0.0728(18) 0.0470(15) 0.0073(13) -0.0027(12) 0.0093(13) C54 0.0445(13) 0.0641(16) 0.0544(15) 0.0182(12) 0.0078(11) 0.0098(12) C55 0.0398(11) 0.0607(14) 0.0379(11) 0.0177(10) 0.0109(9) 0.0143(11) C56 0.0428(12) 0.0622(14) 0.0336(11) 0.0162(10) 0.0184(9) 0.0129(10) C57 0.0362(10) 0.0508(12) 0.0379(11) 0.0151(9) 0.0178(9) 0.0121(9) C58 0.0304(10) 0.0431(11) 0.0460(12) 0.0148(9) 0.0162(9) 0.0120(9) C59 0.0384(11) 0.0514(13) 0.0476(13) 0.0148(10) 0.0158(10) 0.0088(10) C60 0.0461(13) 0.0537(15) 0.0569(14) 0.0044(12) 0.0149(11) 0.0126(11) C61 0.0458(13) 0.0435(13) 0.0792(18) 0.0161(13) 0.0200(13) 0.0101(11) C62 0.0561(15) 0.0487(14) 0.0755(18) 0.0293(13) 0.0205(13) 0.0090(12) C63 0.0458(12) 0.0534(14) 0.0502(13) 0.0202(11) 0.0168(10) 0.0122(11) C64 0.0344(10) 0.0461(12) 0.0373(11) 0.0159(9) 0.0115(9) 0.0115(9) C65 0.0333(10) 0.0555(13) 0.0433(12) 0.0236(10) 0.0120(9) 0.0119(10) C66 0.0482(13) 0.0679(16) 0.0601(15) 0.0371(13) 0.0162(11) 0.0169(12) C67 0.0539(14) 0.0718(17) 0.0665(16) 0.0391(14) 0.0145(12) 0.0281(13) C68 0.0374(12) 0.0798(18) 0.0749(17) 0.0376(14) 0.0176(12) 0.0232(12) C69 0.0384(12) 0.0614(15) 0.0637(15) 0.0319(12) 0.0211(11) 0.0165(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.819(2) . ? Fe1 C2 1.821(2) . ? Fe1 C3 1.900(2) . ? Fe1 C22 1.924(2) . ? Fe1 S2 2.3250(6) . ? Fe1 S1 2.3307(6) . ? Ni1 P2 2.1787(6) . ? Ni1 P1 2.1849(6) . ? Ni1 S2 2.2274(6) . ? Ni1 S1 2.2401(6) . ? P1 C50 1.816(2) . ? P1 C44B 1.824(5) . ? P1 C44 1.834(4) . ? P1 C56 1.839(2) . ? P2 C64 1.816(2) . ? P2 C58 1.819(2) . ? P2 C57 1.834(2) . ? S1 C41 1.840(2) . ? S2 C43 1.827(2) . ? N1 C3 1.150(2) . ? N1 B1 1.565(3) . ? N2 C22 1.152(3) . ? N2 B2 1.568(3) . ? B1 C10B 1.630(4) . ? B1 C4B 1.644(4) . ? B1 C16B 1.650(5) . ? B1 C16 1.659(4) . ? B1 C4 1.659(6) . ? B1 C10 1.674(5) . ? B2 C23B 1.630(4) . ? B2 C29B 1.639(3) . ? B2 C35B 1.644(5) . ? B2 C29 1.654(7) . ? B2 C35 1.661(5) . ? B2 C23 1.701(5) . ? O1 C1 1.130(2) . ? O2 C2 1.127(3) . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 F1 1.342(7) . ? C5 C6 1.3900 . ? C6 F2 1.348(7) . ? C6 C7 1.3900 . ? C7 F3 1.343(7) . ? C7 C8 1.3900 . ? C8 F4 1.352(7) . ? C8 C9 1.3900 . ? C9 F5 1.346(7) . ? C4B C9B 1.378(4) . ? C4B C5B 1.399(4) . ? C5B F1B 1.352(3) . ? C5B C6B 1.367(4) . ? C6B F2B 1.348(4) . ? C6B C7B 1.368(4) . ? C7B F3B 1.343(3) . ? C7B C8B 1.367(4) . ? C8B F4B 1.352(4) . ? C8B C9B 1.380(4) . ? C9B F5B 1.357(3) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 F6 1.324(5) . ? C11 C12 1.3900 . ? C12 F7 1.348(5) . ? C12 C13 1.3900 . ? C13 F8 1.359(5) . ? C13 C14 1.3900 . ? C14 F9 1.335(5) . ? C14 C15 1.3900 . ? C15 F10 1.331(5) . ? C10B C15B 1.382(4) . ? C10B C11B 1.384(5) . ? C11B F6B 1.359(4) . ? C11B C12B 1.379(5) . ? C12B F7B 1.354(4) . ? C12B C13B 1.361(5) . ? C13B F8B 1.357(5) . ? C13B C14B 1.361(5) . ? C14B F9B 1.341(4) . ? C14B C15B 1.380(5) . ? C15B F10B 1.356(4) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 F11 1.340(5) . ? C17 C18 1.3900 . ? C18 F12 1.328(5) . ? C18 C19 1.3900 . ? C19 F13 1.343(4) . ? C19 C20 1.3900 . ? C20 F14 1.336(5) . ? C20 C21 1.3900 . ? C21 F15 1.337(5) . ? C16B C21B 1.379(6) . ? C16B C17B 1.412(6) . ? C17B F11B 1.352(6) . ? C17B C18B 1.389(6) . ? C18B F12B 1.334(6) . ? C18B C19B 1.365(6) . ? C19B F13B 1.348(6) . ? C19B C20B 1.357(6) . ? C20B F14B 1.341(6) . ? C20B C21B 1.390(6) . ? C21B F15B 1.354(6) . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 F16 1.327(6) . ? C24 C25 1.3900 . ? C25 F17 1.339(6) . ? C25 C26 1.3900 . ? C26 F18 1.349(5) . ? C26 C27 1.3900 . ? C27 F19 1.355(5) . ? C27 C28 1.3900 . ? C28 F20 1.318(5) . ? C23B C28B 1.383(5) . ? C23B C24B 1.384(4) . ? C24B F16B 1.352(4) . ? C24B C25B 1.374(4) . ? C25B F17B 1.346(4) . ? C25B C26B 1.366(5) . ? C26B F18B 1.348(5) . ? C26B C27B 1.364(5) . ? C27B F19B 1.343(5) . ? C27B C28B 1.382(5) . ? C28B F20B 1.355(4) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 F21 1.339(7) . ? C30 C31 1.3900 . ? C31 F22 1.341(7) . ? C31 C32 1.3900 . ? C32 F23 1.342(7) . ? C32 C33 1.3900 . ? C33 F24 1.343(7) . ? C33 C34 1.3900 . ? C34 F25 1.331(7) . ? C29B C30B 1.378(3) . ? C29B C34B 1.384(3) . ? C30B F21B 1.355(3) . ? C30B C31B 1.380(3) . ? C31B F22B 1.344(3) . ? C31B C32B 1.364(4) . ? C32B F23B 1.341(3) . ? C32B C33B 1.368(4) . ? C33B F24B 1.343(3) . ? C33B C34B 1.377(4) . ? C34B F25B 1.347(3) . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 F26 1.346(6) . ? C36 C37 1.3900 . ? C37 F27 1.350(6) . ? C37 C38 1.3900 . ? C38 F28 1.341(6) . ? C38 C39 1.3900 . ? C39 F29 1.341(6) . ? C39 C40 1.3900 . ? C40 F30 1.348(6) . ? C35B C36B 1.391(5) . ? C35B C40B 1.395(5) . ? C36B F26B 1.359(5) . ? C36B C37B 1.375(5) . ? C37B F27B 1.348(5) . ? C37B C38B 1.376(5) . ? C38B F28B 1.338(5) . ? C38B C39B 1.364(6) . ? C39B F29B 1.338(5) . ? C39B C40B 1.359(5) . ? C40B F30B 1.359(5) . ? C41 C42 1.514(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.525(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C45 H45A 0.9500 . ? C46 C47 1.3900 . ? C46 H46A 0.9500 . ? C47 C48 1.3900 . ? C47 H47A 0.9500 . ? C48 C49 1.3900 . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C44B C45B 1.3900 . ? C44B C49B 1.3900 . ? C45B C46B 1.3900 . ? C45B H45B 0.9500 . ? C46B C47B 1.3900 . ? C46B H46B 0.9500 . ? C47B C48B 1.3900 . ? C47B H47B 0.9500 . ? C48B C49B 1.3900 . ? C48B H48B 0.9500 . ? C49B H49B 0.9500 . ? C50 C55 1.383(3) . ? C50 C51 1.397(3) . ? C51 C52 1.376(4) . ? C51 H51A 0.9500 . ? C52 C53 1.373(4) . ? C52 H52A 0.9500 . ? C53 C54 1.374(4) . ? C53 H53A 0.9500 . ? C54 C55 1.383(3) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? C56 C57 1.532(3) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.392(3) . ? C58 C63 1.394(3) . ? C59 C60 1.391(3) . ? C59 H59A 0.9500 . ? C60 C61 1.378(4) . ? C60 H60A 0.9500 . ? C61 C62 1.384(4) . ? C61 H61A 0.9500 . ? C62 C63 1.374(3) . ? C62 H62A 0.9500 . ? C63 H63A 0.9500 . ? C64 C65 1.387(3) . ? C64 C69 1.394(3) . ? C65 C66 1.380(3) . ? C65 H65A 0.9500 . ? C66 C67 1.374(3) . ? C66 H66A 0.9500 . ? C67 C68 1.387(3) . ? C67 H67A 0.9500 . ? C68 C69 1.379(3) . ? C68 H68A 0.9500 . ? C69 H69A 0.9500 . ? 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 C1 Fe1 C2 95.83(9) . . ? C1 Fe1 C3 86.07(9) . . ? C2 Fe1 C3 86.32(9) . . ? C1 Fe1 C22 87.45(9) . . ? C2 Fe1 C22 88.78(9) . . ? C3 Fe1 C22 171.43(8) . . ? C1 Fe1 S2 172.92(7) . . ? C2 Fe1 S2 91.23(7) . . ? C3 Fe1 S2 94.89(6) . . ? C22 Fe1 S2 92.23(6) . . ? C1 Fe1 S1 92.59(7) . . ? C2 Fe1 S1 171.57(7) . . ? C3 Fe1 S1 93.98(6) . . ? C22 Fe1 S1 91.90(6) . . ? S2 Fe1 S1 80.350(18) . . ? P2 Ni1 P1 88.05(2) . . ? P2 Ni1 S2 93.207(19) . . ? P1 Ni1 S2 172.26(2) . . ? P2 Ni1 S1 175.34(2) . . ? P1 Ni1 S1 93.70(2) . . ? S2 Ni1 S1 84.490(19) . . ? C50 P1 C44B 105.3(2) . . ? C50 P1 C44 103.3(2) . . ? C50 P1 C56 106.16(10) . . ? C44B P1 C56 108.1(3) . . ? C44 P1 C56 104.2(3) . . ? C50 P1 Ni1 120.50(7) . . ? C44B P1 Ni1 106.3(3) . . ? C44 P1 Ni1 111.5(3) . . ? C56 P1 Ni1 109.86(7) . . ? C64 P2 C58 103.13(9) . . ? C64 P2 C57 105.13(9) . . ? C58 P2 C57 107.59(10) . . ? C64 P2 Ni1 121.67(7) . . ? C58 P2 Ni1 109.66(6) . . ? C57 P2 Ni1 108.82(7) . . ? C41 S1 Ni1 100.78(7) . . ? C41 S1 Fe1 106.46(7) . . ? Ni1 S1 Fe1 86.377(18) . . ? C43 S2 Ni1 101.14(7) . . ? C43 S2 Fe1 105.87(7) . . ? Ni1 S2 Fe1 86.807(18) . . ? C3 N1 B1 173.86(19) . . ? C22 N2 B2 168.41(19) . . ? N1 B1 C10B 108.2(2) . . ? N1 B1 C4B 105.4(2) . . ? C10B B1 C4B 112.9(3) . . ? N1 B1 C16B 106.9(3) . . ? C10B B1 C16B 110.3(4) . . ? C4B B1 C16B 112.6(3) . . ? N1 B1 C16 101.0(3) . . ? C10B B1 C16 111.9(3) . . ? C4B B1 C16 116.2(3) . . ? N1 B1 C4 101.6(5) . . ? C10B B1 C4 115.7(4) . . ? C16B B1 C4 113.3(6) . . ? C16 B1 C4 116.4(5) . . ? N1 B1 C10 105.4(3) . . ? C4B B1 C10 113.1(3) . . ? C16B B1 C10 112.5(4) . . ? C16 B1 C10 113.9(4) . . ? C4 B1 C10 115.7(4) . . ? N2 B2 C23B 106.3(2) . . ? N2 B2 C29B 107.2(2) . . ? C23B B2 C29B 115.2(3) . . ? N2 B2 C35B 105.2(3) . . ? C23B B2 C35B 109.7(3) . . ? C29B B2 C35B 112.5(3) . . ? N2 B2 C29 108.8(5) . . ? C23B B2 C29 109.9(6) . . ? C35B B2 C29 116.3(5) . . ? N2 B2 C35 103.6(3) . . ? C23B B2 C35 113.0(4) . . ? C29B B2 C35 110.6(4) . . ? C29 B2 C35 114.5(5) . . ? N2 B2 C23 107.1(3) . . ? C29B B2 C23 110.7(3) . . ? C35B B2 C23 113.6(4) . . ? C29 B2 C23 105.5(6) . . ? C35 B2 C23 116.9(4) . . ? O1 C1 Fe1 178.2(2) . . ? O2 C2 Fe1 176.6(2) . . ? N1 C3 Fe1 170.42(18) . . ? C5 C4 C9 120.0 . . ? C5 C4 B1 117.4(5) . . ? C9 C4 B1 122.6(5) . . ? F1 C5 C6 118.0(7) . . ? F1 C5 C4 120.8(7) . . ? C6 C5 C4 120.0 . . ? F2 C6 C5 119.9(7) . . ? F2 C6 C7 117.9(7) . . ? C5 C6 C7 120.0 . . ? F3 C7 C8 117.7(7) . . ? F3 C7 C6 121.9(7) . . ? C8 C7 C6 120.0 . . ? F4 C8 C7 118.9(7) . . ? F4 C8 C9 120.8(7) . . ? C7 C8 C9 120.0 . . ? F5 C9 C8 116.5(6) . . ? F5 C9 C4 123.4(6) . . ? C8 C9 C4 120.0 . . ? C9B C4B C5B 112.4(2) . . ? C9B C4B B1 127.1(3) . . ? C5B C4B B1 120.3(2) . . ? F1B C5B C6B 116.5(3) . . ? F1B C5B C4B 118.5(3) . . ? C6B C5B C4B 124.8(3) . . ? F2B C6B C5B 120.5(3) . . ? F2B C6B C7B 119.6(3) . . ? C5B C6B C7B 119.6(3) . . ? F3B C7B C8B 120.2(3) . . ? F3B C7B C6B 120.9(3) . . ? C8B C7B C6B 118.8(3) . . ? F4B C8B C7B 119.8(3) . . ? F4B C8B C9B 120.5(3) . . ? C7B C8B C9B 119.7(3) . . ? F5B C9B C4B 120.6(3) . . ? F5B C9B C8B 114.7(3) . . ? C4B C9B C8B 124.7(3) . . ? C11 C10 C15 120.0 . . ? C11 C10 B1 124.2(3) . . ? C15 C10 B1 115.7(3) . . ? F6 C11 C10 123.4(4) . . ? F6 C11 C12 116.5(4) . . ? C10 C11 C12 120.0 . . ? F7 C12 C11 120.6(5) . . ? F7 C12 C13 119.4(5) . . ? C11 C12 C13 120.0 . . ? F8 C13 C14 121.5(5) . . ? F8 C13 C12 117.8(5) . . ? C14 C13 C12 120.0 . . ? F9 C14 C15 121.9(4) . . ? F9 C14 C13 118.1(4) . . ? C15 C14 C13 120.0 . . ? F10 C15 C14 116.3(4) . . ? F10 C15 C10 123.6(4) . . ? C14 C15 C10 120.0 . . ? C15B C10B C11B 111.6(3) . . ? C15B C10B B1 126.8(3) . . ? C11B C10B B1 121.5(3) . . ? F6B C11B C12B 115.5(4) . . ? F6B C11B C10B 119.3(4) . . ? C12B C11B C10B 125.2(3) . . ? F7B C12B C13B 119.3(4) . . ? F7B C12B C11B 121.0(4) . . ? C13B C12B C11B 119.7(3) . . ? F8B C13B C14B 120.2(4) . . ? F8B C13B C12B 121.0(4) . . ? C14B C13B C12B 118.6(3) . . ? F9B C14B C13B 121.5(4) . . ? F9B C14B C15B 118.9(4) . . ? C13B C14B C15B 119.6(3) . . ? F10B C15B C14B 115.7(4) . . ? F10B C15B C10B 118.9(4) . . ? C14B C15B C10B 125.4(3) . . ? C17 C16 C21 120.0 . . ? C17 C16 B1 116.2(3) . . ? C21 C16 B1 123.8(3) . . ? F11 C17 C18 116.2(4) . . ? F11 C17 C16 123.5(4) . . ? C18 C17 C16 120.0 . . ? F12 C18 C17 120.9(4) . . ? F12 C18 C19 119.0(4) . . ? C17 C18 C19 120.0 . . ? F13 C19 C18 120.8(4) . . ? F13 C19 C20 119.1(4) . . ? C18 C19 C20 120.0 . . ? F14 C20 C21 119.6(4) . . ? F14 C20 C19 120.3(4) . . ? C21 C20 C19 120.0 . . ? F15 C21 C20 118.0(4) . . ? F15 C21 C16 121.8(4) . . ? C20 C21 C16 120.0 . . ? C21B C16B C17B 109.8(4) . . ? C21B C16B B1 127.4(4) . . ? C17B C16B B1 122.7(4) . . ? F11B C17B C18B 116.3(5) . . ? F11B C17B C16B 118.1(5) . . ? C18B C17B C16B 125.4(5) . . ? F12B C18B C19B 121.7(5) . . ? F12B C18B C17B 119.0(6) . . ? C19B C18B C17B 119.3(5) . . ? F13B C19B C20B 120.9(6) . . ? F13B C19B C18B 119.9(5) . . ? C20B C19B C18B 119.1(5) . . ? F14B C20B C19B 120.3(5) . . ? F14B C20B C21B 120.5(5) . . ? C19B C20B C21B 118.9(5) . . ? F15B C21B C16B 119.2(5) . . ? F15B C21B C20B 113.9(6) . . ? C16B C21B C20B 126.9(5) . . ? N2 C22 Fe1 166.37(17) . . ? C24 C23 C28 120.0 . . ? C24 C23 B2 113.0(3) . . ? C28 C23 B2 126.9(3) . . ? F16 C24 C25 116.6(5) . . ? F16 C24 C23 123.3(5) . . ? C25 C24 C23 120.0 . . ? F17 C25 C26 117.7(5) . . ? F17 C25 C24 122.3(5) . . ? C26 C25 C24 120.0 . . ? F18 C26 C25 119.3(5) . . ? F18 C26 C27 120.7(5) . . ? C25 C26 C27 120.0 . . ? F19 C27 C28 120.2(4) . . ? F19 C27 C26 119.7(4) . . ? C28 C27 C26 120.0 . . ? F20 C28 C27 115.8(4) . . ? F20 C28 C23 124.1(4) . . ? C27 C28 C23 120.0 . . ? C28B C23B C24B 111.5(3) . . ? C28B C23B B2 123.4(3) . . ? C24B C23B B2 124.7(3) . . ? F16B C24B C25B 115.1(4) . . ? F16B C24B C23B 118.5(4) . . ? C25B C24B C23B 126.3(3) . . ? F17B C25B C26B 121.4(4) . . ? F17B C25B C24B 119.7(4) . . ? C26B C25B C24B 118.9(3) . . ? F18B C26B C27B 119.3(4) . . ? F18B C26B C25B 122.3(4) . . ? C27B C26B C25B 118.3(3) . . ? F19B C27B C26B 120.0(4) . . ? F19B C27B C28B 119.5(4) . . ? C26B C27B C28B 120.5(4) . . ? F20B C28B C27B 116.2(4) . . ? F20B C28B C23B 119.3(4) . . ? C27B C28B C23B 124.4(4) . . ? C30 C29 C34 120.0 . . ? C30 C29 B2 120.4(5) . . ? C34 C29 B2 119.5(5) . . ? F21 C30 C29 122.5(8) . . ? F21 C30 C31 117.5(8) . . ? C29 C30 C31 120.0 . . ? F22 C31 C32 119.4(7) . . ? F22 C31 C30 120.5(7) . . ? C32 C31 C30 120.0 . . ? F23 C32 C31 120.1(7) . . ? F23 C32 C33 119.8(7) . . ? C31 C32 C33 120.0 . . ? F24 C33 C34 121.5(8) . . ? F24 C33 C32 118.5(8) . . ? C34 C33 C32 120.0 . . ? F25 C34 C33 117.6(7) . . ? F25 C34 C29 122.3(7) . . ? C33 C34 C29 120.0 . . ? C30B C29B C34B 113.1(2) . . ? C30B C29B B2 121.8(2) . . ? C34B C29B B2 125.0(2) . . ? F21B C30B C29B 119.9(3) . . ? F21B C30B C31B 115.1(3) . . ? C29B C30B C31B 125.0(3) . . ? F22B C31B C32B 119.9(3) . . ? F22B C31B C30B 120.9(3) . . ? C32B C31B C30B 119.2(3) . . ? F23B C32B C31B 119.6(3) . . ? F23B C32B C33B 121.6(3) . . ? C31B C32B C33B 118.7(2) . . ? F24B C33B C32B 119.7(3) . . ? F24B C33B C34B 120.1(3) . . ? C32B C33B C34B 120.2(3) . . ? F25B C34B C33B 115.8(3) . . ? F25B C34B C29B 120.4(3) . . ? C33B C34B C29B 123.8(3) . . ? C36 C35 C40 120.0 . . ? C36 C35 B2 118.9(4) . . ? C40 C35 B2 120.8(4) . . ? F26 C36 C35 123.0(5) . . ? F26 C36 C37 116.6(5) . . ? C35 C36 C37 120.0 . . ? F27 C37 C36 120.3(5) . . ? F27 C37 C38 119.5(5) . . ? C36 C37 C38 120.0 . . ? F28 C38 C39 121.1(5) . . ? F28 C38 C37 118.9(5) . . ? C39 C38 C37 120.0 . . ? F29 C39 C38 120.8(5) . . ? F29 C39 C40 119.2(5) . . ? C38 C39 C40 120.0 . . ? F30 C40 C39 115.5(5) . . ? F30 C40 C35 124.2(5) . . ? C39 C40 C35 120.0 . . ? C36B C35B C40B 110.3(4) . . ? C36B C35B B2 121.4(4) . . ? C40B C35B B2 128.2(4) . . ? F26B C36B C37B 115.3(4) . . ? F26B C36B C35B 118.5(4) . . ? C37B C36B C35B 125.9(4) . . ? F27B C37B C36B 120.5(5) . . ? F27B C37B C38B 119.8(4) . . ? C36B C37B C38B 119.5(4) . . ? F28B C38B C39B 121.3(5) . . ? F28B C38B C37B 120.7(5) . . ? C39B C38B C37B 118.0(4) . . ? F29B C39B C40B 121.5(5) . . ? F29B C39B C38B 118.5(5) . . ? C40B C39B C38B 120.0(4) . . ? F30B C40B C39B 114.6(5) . . ? F30B C40B C35B 118.4(5) . . ? C39B C40B C35B 126.4(4) . . ? C42 C41 S1 115.19(14) . . ? C42 C41 H41A 108.5 . . ? S1 C41 H41A 108.5 . . ? C42 C41 H41B 108.5 . . ? S1 C41 H41B 108.5 . . ? H41A C41 H41B 107.5 . . ? C41 C42 C43 117.28(18) . . ? C41 C42 H42A 108.0 . . ? C43 C42 H42A 108.0 . . ? C41 C42 H42B 108.0 . . ? C43 C42 H42B 108.0 . . ? H42A C42 H42B 107.2 . . ? C42 C43 S2 115.57(15) . . ? C42 C43 H43A 108.4 . . ? S2 C43 H43A 108.4 . . ? C42 C43 H43B 108.4 . . ? S2 C43 H43B 108.4 . . ? H43A C43 H43B 107.4 . . ? C45 C44 C49 120.0 . . ? C45 C44 P1 123.7(4) . . ? C49 C44 P1 115.2(4) . . ? C46 C45 C44 120.0 . . ? C46 C45 H45A 120.0 . . ? C44 C45 H45A 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47A 120.0 . . ? C48 C47 H47A 120.0 . . ? C49 C48 C47 120.0 . . ? C49 C48 H48A 120.0 . . ? C47 C48 H48A 120.0 . . ? C48 C49 C44 120.0 . . ? C48 C49 H49A 120.0 . . ? C44 C49 H49A 120.0 . . ? C45B C44B C49B 120.0 . . ? C45B C44B P1 115.7(4) . . ? C49B C44B P1 124.2(4) . . ? C46B C45B C44B 120.0 . . ? C46B C45B H45B 120.0 . . ? C44B C45B H45B 120.0 . . ? C45B C46B C47B 120.0 . . ? C45B C46B H46B 120.0 . . ? C47B C46B H46B 120.0 . . ? C46B C47B C48B 120.0 . . ? C46B C47B H47B 120.0 . . ? C48B C47B H47B 120.0 . . ? C49B C48B C47B 120.0 . . ? C49B C48B H48B 120.0 . . ? C47B C48B H48B 120.0 . . ? C48B C49B C44B 120.0 . . ? C48B C49B H49B 120.0 . . ? C44B C49B H49B 120.0 . . ? C55 C50 C51 118.9(2) . . ? C55 C50 P1 121.35(16) . . ? C51 C50 P1 119.65(18) . . ? C52 C51 C50 120.1(2) . . ? C52 C51 H51A 120.0 . . ? C50 C51 H51A 120.0 . . ? C53 C52 C51 120.6(2) . . ? C53 C52 H52A 119.7 . . ? C51 C52 H52A 119.7 . . ? C52 C53 C54 119.9(2) . . ? C52 C53 H53A 120.1 . . ? C54 C53 H53A 120.1 . . ? C53 C54 C55 120.3(2) . . ? C53 C54 H54A 119.9 . . ? C55 C54 H54A 119.9 . . ? C50 C55 C54 120.3(2) . . ? C50 C55 H55A 119.8 . . ? C54 C55 H55A 119.8 . . ? C57 C56 P1 110.36(14) . . ? C57 C56 H56A 109.6 . . ? P1 C56 H56A 109.6 . . ? C57 C56 H56B 109.6 . . ? P1 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? C56 C57 P2 110.79(14) . . ? C56 C57 H57A 109.5 . . ? P2 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? P2 C57 H57B 109.5 . . ? H57A C57 H57B 108.1 . . ? C59 C58 C63 118.7(2) . . ? C59 C58 P2 118.94(16) . . ? C63 C58 P2 122.35(16) . . ? C60 C59 C58 120.2(2) . . ? C60 C59 H59A 119.9 . . ? C58 C59 H59A 119.9 . . ? C61 C60 C59 120.3(2) . . ? C61 C60 H60A 119.8 . . ? C59 C60 H60A 119.8 . . ? C60 C61 C62 119.6(2) . . ? C60 C61 H61A 120.2 . . ? C62 C61 H61A 120.2 . . ? C63 C62 C61 120.5(2) . . ? C63 C62 H62A 119.8 . . ? C61 C62 H62A 119.8 . . ? C62 C63 C58 120.7(2) . . ? C62 C63 H63A 119.7 . . ? C58 C63 H63A 119.7 . . ? C65 C64 C69 119.32(19) . . ? C65 C64 P2 121.46(15) . . ? C69 C64 P2 119.21(16) . . ? C66 C65 C64 120.2(2) . . ? C66 C65 H65A 119.9 . . ? C64 C65 H65A 119.9 . . ? C67 C66 C65 120.3(2) . . ? C67 C66 H66A 119.9 . . ? C65 C66 H66A 119.9 . . ? C66 C67 C68 120.2(2) . . ? C66 C67 H67A 119.9 . . ? C68 C67 H67A 119.9 . . ? C69 C68 C67 119.8(2) . . ? C69 C68 H68A 120.1 . . ? C67 C68 H68A 120.1 . . ? C68 C69 C64 120.2(2) . . ? C68 C69 H69A 119.9 . . ? C64 C69 H69A 119.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.10 _diffrn_measured_fraction_theta_full 0.994 _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_time ? _refine_diff_density_max 0.298 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.051 _publ_requested_category 'FM' _publ_section_references ; Allen, F.H., Kennard, O., and Taylor, R. (1983). Accounts Chem. Res. 16, 146-153. Bruker (2010). APEX2. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2005). SAINT, SHELXTL, XCIF, XPREP. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2007). SADABS, TWINABS. Bruker AXS, Inc., Madison, Wisconsin, USA. CrystalMaker (1994). CrystalMaker, a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd., Oxford, England (www.crystalmaker.com). Spek, A. L. and van der Sluis, P. (1990). Acta Cryst. A46, 194-201. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 ; _publ_section_figure_captions ; Figure 1. SHELXTL (Bruker, 2005) plot showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. ; _publ_section_exptl_prep ; Crystals were grown from THF and pentane at -30C. ; _publ_section_exptl_refinement ; A structural model consisting of the host plus one disordered THF and one disordered pentane solvate molecule was developed; however, positions for the idealized solvate molecules were poorly determined. This model converged with wR2 = 0.2164 and R1 = 0.0604 for 1599 parameters with 2681 restraints against 16165 data. Since positions for the solvate molecules were poorly determined a second structural model was refined with contributions from the solvate molecules removed from the diffraction data using the bypass procedure in PLATON (Spek, 1990). No positions for the host network differed by more than two su's between these two refined models. The electron count from the "squeeze" model converged in good agreement with the number of solvate molecules predicted by the complete refinement. The "squeezed" model converged with wR2 = 0.1035 and R1 = 0.0363 for 1559 parameters with 2681 restraints against 16164 data. Six tris-(pentafluorophenyl) rings on the host molecule were each modeled as disordered over two sites. The primary orientation of the phenyl ring was constrained to be a aperfect hexagon (C-C = 1.39/%A). The secondary orientaions phenyl ring and F position geometries were then restrained to be the same as primary orientaion rings (esd 0.01). Like phenyl ring C-B atom bonds were restrained to be similar (esd 0.01). One phenyl ring on the host molecule was modeled as disordered over two sites. The phenyl rings were constrained to be perfect hexagons (C-C = 1.39/%A). Like phenyl ring C-P atom bonds were restrained to be similar (esd 0.01). Similar displacement amplitudes (esd 0.01) were imposed on all disordered sites overlapping by less than the sum of van der Waals radii (Allen et al, 1983). The F atoms on the pentafluorophenyl ring (C35-C40) were also restrained to behave relatively isotropic. H atoms were included as riding idealized contributors. H atom U's were assigned as 1.2 times carrier U~eq~. ; _publ_contact_author ; Thomas B. Rauchfuss University of Illinois School of Chemical Sciences, Box 12-6 600 South Mathews Avenue Urbana, Illinois 61801 USA ; _publ_contact_author_phone '1 217 333 7355' _publ_contact_author_fax '1 217 244 3186' _publ_contact_author_email rauchfuz@illinois.edu _publ_contact_letter ; ; _publ_requested_journal 'Journal of the American Chemical Society' _publ_requested_coeditor_name ? _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; The Materials Chemistry Laboratory at the University of Illinois was supported in part by grants NSF CHE 95-03145 and NSF CHE 03-43032 from the National Science Foundation. ; _platon_squeeze_details ; One solvent molecule of THF and pentane were found in the unit cell but were poorly resolved. The found electron count matches the expected for one THF and pentane. ; loop_ _publ_author_name _publ_author_address 'Manor, Brian C.' ; University of Illinois School of Chemical Sciences 600 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Rauchfuss, Thomas B.' ; University of Illinois School of Chemical Sciences 600 South Mathews Avenue Urbana, Illinois 61801 USA ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 1.00 0.00 0.1140 0.00 -1.00 0.00 0.0850 0.00 0.00 1.00 0.1850 -1.00 1.00 0.00 0.0800 2.00 -1.00 -2.00 0.1080 2.00 1.00 -2.00 0.0890 -2.00 1.00 2.00 0.1710 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.118 0.500 1.000 854 170 ' ' #start Validation Reply Form _vrf_CHEMW03_bm08sasq-sr ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 1895.44 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 69.00 828.76 H 1.01 30.00 30.24 B 10.81 2.00 21.62 N 14.01 2.00 28.01 O 16.00 2.00 32.00 F 19.00 30.00 569.94 P 30.97 2.00 61.95 S 32.07 2.00 64.13 Fe 55.85 1.00 55.85 Ni 58.69 1.00 58.69 Calculated formula weight 1751.19 RESPONSE: The given and expected molecular weights were found to differ. This difference is a result from one poorly defined THF solvent molecule and one poorly defined pentane solvent molecule being squeezed from the crystal structure. The reported moiety and sum formulas include the squeezed solvent molecules to reflect the true contents of the crystal. ; #===End data_bm59uasq-sr-p _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C68 H31 B2 F30 Fe N2 Ni O P2 S2, C8 H20 N, C2 H4 Cl4 ; _chemical_formula_sum 'C77 H53 B2 Cl2 F30 Fe N3 Ni O P2 S2' _chemical_formula_structural ? _chemical_formula_weight 1939.36 _chemical_absolute_configuration ? _chemical_formula_iupac ? _chemical_formula_analytical ? _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' 'B' 'B' 0.0013 0.0007 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.598(2) _cell_length_b 15.368(2) _cell_length_c 19.946(3) _cell_angle_alpha 95.559(2) _cell_angle_beta 98.804(2) _cell_angle_gamma 113.598(2) _cell_volume 3990.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 9927 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.17 _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.462 _exptl_crystal_size_mid 0.357 _exptl_crystal_size_min 0.134 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_crystal_id bm59uasq-sr-p _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (-1 -4 0) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.8048 _exptl_absorpt_correction_T_max 0.9321 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; One distinct cell was identified using APEX II (Bruker, 2010). Four frame series were corrected for absorption by integration using SHELXTL/XPREP V2005/2 (Bruker, 2005) before using SADABS (Bruker, 2005) to sort, merge, and scale the combined data. No decay correction was applied. ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id bm59uasq-sr-p _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type ? _diffrn_measurement_device 'Siemens Platform/CCD' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43992 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.39 _reflns_number_total 14596 _reflns_number_gt 11524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction ; SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 (Bruker, 2005 & 2007) ; _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2005)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2005)' _computing_molecular_graphics ; SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) ; _computing_publication_material 'XCIF V6.12 (Bruker, 2005)' _refine_special_details ; Structure was phased by direct methods (Sheldrick,2008). Systematic conditions suggested the ambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. The highest peaks in the final difference Fourier map were in the vicinity of atoms Fe1 Ni1 P1 P2; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed some dependence on amplitude and little dependence on resolution. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.5820P] 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 'noref' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14596 _refine_ls_number_parameters 1279 _refine_ls_number_restraints 1071 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 _refine_ls_abs_structure_details ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.57734(2) 0.379878(18) 0.205037(14) 0.02733(7) Uani 1 1 d . A . Fe1 Fe 0.55977(2) 0.52595(2) 0.263276(15) 0.02731(8) Uani 1 1 d . A . H1 H 0.6320(18) 0.4773(17) 0.2704(12) 0.053(7) Uiso 1 1 d . . . S1 S 0.43665(4) 0.36834(4) 0.24905(3) 0.03091(13) Uani 1 1 d . . . S2 S 0.55969(4) 0.48996(4) 0.14872(3) 0.03081(13) Uani 1 1 d . . . P1 P 0.62440(4) 0.29452(4) 0.27022(3) 0.03334(14) Uani 1 1 d D . . P2 P 0.63608(4) 0.32726(4) 0.12639(3) 0.03127(13) Uani 1 1 d . . . B1 B 0.33318(18) 0.66481(17) 0.25041(13) 0.0274(5) Uani 1 1 d . . . B2 B 0.85493(19) 0.79861(17) 0.28956(14) 0.0345(6) Uani 1 1 d D . . N1 N 0.41258(13) 0.62097(12) 0.25160(9) 0.0286(4) Uani 1 1 d . . . N2 N 0.75381(14) 0.70715(13) 0.27894(10) 0.0350(4) Uani 1 1 d . A . O1 O 0.55988(16) 0.54018(15) 0.40973(9) 0.0651(6) Uani 1 1 d . . . C1 C 0.56346(18) 0.53570(16) 0.35227(13) 0.0403(6) Uani 1 1 d . . . C2 C 0.46813(16) 0.58470(14) 0.25276(10) 0.0268(5) Uani 1 1 d . . . C3 C 0.34788(16) 0.72727(14) 0.32598(11) 0.0286(5) Uani 1 1 d . . . C4 C 0.28437(16) 0.77335(15) 0.33342(11) 0.0315(5) Uani 1 1 d . . . C5 C 0.29441(18) 0.83487(16) 0.39195(12) 0.0373(5) Uani 1 1 d . . . C6 C 0.37109(19) 0.85333(16) 0.44762(12) 0.0405(6) Uani 1 1 d . . . C7 C 0.43593(19) 0.80965(17) 0.44395(12) 0.0401(6) Uani 1 1 d . . . C8 C 0.42346(17) 0.74796(16) 0.38463(12) 0.0346(5) Uani 1 1 d . . . F1 F 0.20657(9) 0.75777(9) 0.28002(7) 0.0389(3) Uani 1 1 d . . . F2 F 0.23074(11) 0.87864(10) 0.39397(8) 0.0527(4) Uani 1 1 d . . . F3 F 0.38253(12) 0.91344(11) 0.50518(7) 0.0595(4) Uani 1 1 d . . . F4 F 0.51089(12) 0.82612(11) 0.49877(7) 0.0579(4) Uani 1 1 d . . . F5 F 0.49047(11) 0.70759(11) 0.38684(7) 0.0500(4) Uani 1 1 d . . . C9 C 0.22191(16) 0.57028(14) 0.22533(11) 0.0302(5) Uani 1 1 d . . . C10 C 0.19531(17) 0.51483(15) 0.16028(12) 0.0340(5) Uani 1 1 d . . . C11 C 0.10739(19) 0.43121(17) 0.13683(13) 0.0454(6) Uani 1 1 d . . . C12 C 0.03971(19) 0.39856(17) 0.17954(15) 0.0511(7) Uani 1 1 d . . . C13 C 0.06199(19) 0.44899(18) 0.24421(14) 0.0473(6) Uani 1 1 d . . . C14 C 0.15149(17) 0.53212(16) 0.26597(13) 0.0376(5) Uani 1 1 d . . . F6 F 0.25856(10) 0.54253(9) 0.11598(7) 0.0416(3) Uani 1 1 d . . . F7 F 0.08661(12) 0.38192(11) 0.07296(8) 0.0661(5) Uani 1 1 d . . . F8 F -0.04752(13) 0.31807(12) 0.15759(10) 0.0810(6) Uani 1 1 d . . . F9 F -0.00214(12) 0.41725(12) 0.28749(9) 0.0734(5) Uani 1 1 d . . . F10 F 0.16830(11) 0.57468(10) 0.33212(7) 0.0510(4) Uani 1 1 d . . . C15 C 0.35942(15) 0.74447(14) 0.19803(11) 0.0278(5) Uani 1 1 d . . . C16 C 0.45801(16) 0.81729(15) 0.20970(12) 0.0333(5) Uani 1 1 d . . . C17 C 0.48824(18) 0.89024(16) 0.17231(13) 0.0398(6) Uani 1 1 d . . . C18 C 0.4195(2) 0.89286(16) 0.11845(13) 0.0421(6) Uani 1 1 d . . . C19 C 0.32065(18) 0.82369(16) 0.10410(12) 0.0382(6) Uani 1 1 d . . . C20 C 0.29248(16) 0.75260(14) 0.14405(11) 0.0310(5) Uani 1 1 d . . . F11 F 0.53034(9) 0.81906(9) 0.26187(7) 0.0430(3) Uani 1 1 d . . . F12 F 0.58511(11) 0.96009(10) 0.18824(8) 0.0571(4) Uani 1 1 d . . . F13 F 0.44742(12) 0.96390(10) 0.08089(8) 0.0590(4) Uani 1 1 d . . . F14 F 0.25165(11) 0.82634(10) 0.05198(7) 0.0511(4) Uani 1 1 d . . . F15 F 0.19270(9) 0.68994(9) 0.12813(7) 0.0406(3) Uani 1 1 d . . . C21 C 0.67830(17) 0.63907(15) 0.27264(11) 0.0313(5) Uani 1 1 d . . . C22 C 0.8290(3) 0.8946(2) 0.3070(3) 0.0356(15) Uani 0.560(5) 1 d PGDU A 1 C23 C 0.7517(4) 0.8857(3) 0.3424(3) 0.0370(15) Uani 0.560(5) 1 d PGDU A 1 C24 C 0.7269(4) 0.9631(3) 0.3561(4) 0.0427(15) Uani 0.560(5) 1 d PGDU A 1 C25 C 0.7794(4) 1.0494(3) 0.3344(3) 0.0448(14) Uani 0.560(5) 1 d PGDU A 1 C26 C 0.8568(4) 1.0583(2) 0.2990(3) 0.0462(14) Uani 0.560(5) 1 d PGDU A 1 C27 C 0.8816(3) 0.9809(3) 0.2853(3) 0.0451(15) Uani 0.560(5) 1 d PGDU A 1 F16 F 0.7045(4) 0.8089(3) 0.3705(3) 0.0423(12) Uani 0.560(5) 1 d PDU A 1 F17 F 0.6529(4) 0.9559(5) 0.3904(3) 0.0502(13) Uani 0.560(5) 1 d PDU A 1 F18 F 0.7608(4) 1.1265(4) 0.3510(4) 0.0561(14) Uani 0.560(5) 1 d PDU A 1 F19 F 0.9073(4) 1.1433(3) 0.2796(3) 0.0708(15) Uani 0.560(5) 1 d PDU A 1 F20 F 0.9565(3) 0.9964(4) 0.2514(3) 0.0621(15) Uani 0.560(5) 1 d PDU A 1 C22B C 0.8237(5) 0.8889(4) 0.3006(4) 0.0335(18) Uani 0.440(5) 1 d PDU A 2 C23B C 0.7635(6) 0.8970(5) 0.3465(5) 0.0338(17) Uani 0.440(5) 1 d PDU A 2 C24B C 0.7316(7) 0.9693(5) 0.3582(5) 0.0417(18) Uani 0.440(5) 1 d PDU A 2 C25B C 0.7676(7) 1.0478(5) 0.3272(5) 0.0477(16) Uani 0.440(5) 1 d PDU A 2 C26B C 0.8309(6) 1.0482(5) 0.2841(4) 0.0482(16) Uani 0.440(5) 1 d PDU A 2 C27B C 0.8572(6) 0.9726(5) 0.2720(4) 0.0411(15) Uani 0.440(5) 1 d PDU A 2 F16B F 0.7285(7) 0.8243(5) 0.3822(4) 0.0533(19) Uani 0.440(5) 1 d PDU A 2 F17B F 0.6722(6) 0.9665(7) 0.4039(5) 0.061(2) Uani 0.440(5) 1 d PDU A 2 F18B F 0.7377(6) 1.1190(5) 0.3368(5) 0.064(2) Uani 0.440(5) 1 d PDU A 2 F19B F 0.8724(7) 1.1260(5) 0.2546(4) 0.090(2) Uani 0.440(5) 1 d PDU A 2 F20B F 0.9230(6) 0.9814(5) 0.2294(4) 0.076(2) Uani 0.440(5) 1 d PDU A 2 C28 C 0.93157(16) 0.78980(15) 0.35608(12) 0.0328(5) Uani 1 1 d . A . C29 C 0.94943(17) 0.70715(16) 0.35558(12) 0.0349(5) Uani 1 1 d . . . C30 C 1.01161(19) 0.69257(17) 0.40840(13) 0.0424(6) Uani 1 1 d . A . C31 C 1.06060(19) 0.76267(18) 0.46584(13) 0.0450(6) Uani 1 1 d . . . C32 C 1.04619(18) 0.84560(17) 0.46926(13) 0.0420(6) Uani 1 1 d . A . C33 C 0.98377(17) 0.85774(16) 0.41501(12) 0.0371(5) Uani 1 1 d . . . F21 F 0.90411(11) 0.63519(9) 0.30081(7) 0.0480(4) Uani 1 1 d . A . F22 F 1.02440(12) 0.61022(11) 0.40420(8) 0.0611(4) Uani 1 1 d . . . F23 F 1.12165(13) 0.75073(12) 0.51826(8) 0.0701(5) Uani 1 1 d . A . F24 F 1.09295(12) 0.91469(11) 0.52574(8) 0.0633(4) Uani 1 1 d . . . F25 F 0.97650(11) 0.94333(9) 0.42283(8) 0.0552(4) Uani 1 1 d . A . C34 C 0.8988(5) 0.7922(8) 0.2176(3) 0.033(3) Uani 0.304(7) 1 d PGDU A 1 C35 C 0.8396(4) 0.7380(8) 0.1540(3) 0.035(2) Uani 0.304(7) 1 d PGDU A 1 C36 C 0.8857(5) 0.7329(8) 0.0987(3) 0.038(2) Uani 0.304(7) 1 d PGDU A 1 C37 C 0.9911(5) 0.7820(10) 0.1069(4) 0.039(2) Uani 0.304(7) 1 d PGDU A 1 C38 C 1.0503(4) 0.8362(12) 0.1705(4) 0.038(2) Uani 0.304(7) 1 d PGDU A 1 C39 C 1.0041(5) 0.8413(10) 0.2259(3) 0.033(2) Uani 0.304(7) 1 d PGDU A 1 F26 F 0.7378(5) 0.6950(9) 0.1410(6) 0.048(2) Uani 0.304(7) 1 d PDU A 1 F27 F 0.8268(7) 0.6860(9) 0.0367(4) 0.057(2) Uani 0.304(7) 1 d PDU A 1 F28 F 1.0341(7) 0.7780(11) 0.0523(5) 0.050(2) Uani 0.304(7) 1 d PDU A 1 F29 F 1.1517(6) 0.8864(11) 0.1764(7) 0.051(3) Uani 0.304(7) 1 d PDU A 1 F30 F 1.0655(8) 0.8969(10) 0.2851(5) 0.045(3) Uani 0.304(7) 1 d PDU A 1 C34B C 0.9042(3) 0.7987(4) 0.22122(19) 0.0327(12) Uani 0.696(7) 1 d PDU A 2 C35B C 0.8435(3) 0.7594(4) 0.1551(2) 0.0441(13) Uani 0.696(7) 1 d PDU A 2 C36B C 0.8795(4) 0.7541(4) 0.0961(2) 0.0543(15) Uani 0.696(7) 1 d PDU A 2 C37B C 0.9822(4) 0.7899(5) 0.0991(2) 0.0502(14) Uani 0.696(7) 1 d PDU A 2 C38B C 1.0466(3) 0.8311(5) 0.1616(2) 0.0381(11) Uani 0.696(7) 1 d PDU A 2 C39B C 1.0075(3) 0.8352(5) 0.2195(2) 0.0319(11) Uani 0.696(7) 1 d PDU A 2 F26B F 0.7412(3) 0.7231(5) 0.1471(3) 0.0737(18) Uani 0.696(7) 1 d PDU A 2 F27B F 0.8145(4) 0.7101(5) 0.0354(2) 0.102(2) Uani 0.696(7) 1 d PDU A 2 F28B F 1.0196(4) 0.7840(6) 0.0421(2) 0.082(2) Uani 0.696(7) 1 d PDU A 2 F29B F 1.1489(3) 0.8675(5) 0.1666(3) 0.0504(12) Uani 0.696(7) 1 d PDU A 2 F30B F 1.0767(4) 0.8823(4) 0.2793(2) 0.0392(11) Uani 0.696(7) 1 d PDU A 2 C40 C 0.33012(17) 0.35164(17) 0.18009(13) 0.0416(6) Uani 1 1 d . . . H40A H 0.2718 0.2900 0.1806 0.050 Uiso 1 1 calc R . . H40B H 0.3086 0.4041 0.1900 0.050 Uiso 1 1 calc R . . C41 C 0.35269(18) 0.35050(17) 0.10877(12) 0.0428(6) Uani 1 1 d . . . H41A H 0.2880 0.3313 0.0748 0.051 Uiso 1 1 calc R . . H41B H 0.3785 0.3009 0.0999 0.051 Uiso 1 1 calc R . . C42 C 0.42965(18) 0.44573(17) 0.09733(12) 0.0393(6) Uani 1 1 d . . . H42A H 0.4037 0.4951 0.1069 0.047 Uiso 1 1 calc R . . H42B H 0.4332 0.4397 0.0480 0.047 Uiso 1 1 calc R . . C43 C 0.52378(17) 0.17723(15) 0.27138(12) 0.0336(5) Uani 1 1 d . B . C44 C 0.53204(19) 0.12381(16) 0.32322(13) 0.0417(6) Uani 1 1 d . . . H44A H 0.5899 0.1500 0.3603 0.050 Uiso 1 1 calc R B . C45 C 0.4557(2) 0.03286(17) 0.32022(14) 0.0500(7) Uani 1 1 d . B . H45A H 0.4616 -0.0035 0.3552 0.060 Uiso 1 1 calc R . . C46 C 0.3720(2) -0.00483(16) 0.26717(14) 0.0484(7) Uani 1 1 d . . . H46A H 0.3196 -0.0670 0.2659 0.058 Uiso 1 1 calc R B . C47 C 0.3627(2) 0.04685(16) 0.21506(13) 0.0442(6) Uani 1 1 d . B . H47A H 0.3050 0.0199 0.1778 0.053 Uiso 1 1 calc R . . C48 C 0.43836(18) 0.13789(15) 0.21807(12) 0.0373(5) Uani 1 1 d . . . H48A H 0.4317 0.1740 0.1831 0.045 Uiso 1 1 calc R B . C49 C 0.6855(4) 0.3496(4) 0.35923(15) 0.0419(13) Uani 0.642(10) 1 d PGDU B 1 C50 C 0.7915(4) 0.3907(4) 0.3796(2) 0.0535(13) Uani 0.642(10) 1 d PGU B 1 H50A H 0.8321 0.3912 0.3466 0.064 Uiso 0.642(10) 1 calc PR B 1 C51 C 0.8380(3) 0.4311(4) 0.4482(2) 0.0654(15) Uani 0.642(10) 1 d PGU B 1 H51A H 0.9104 0.4592 0.4620 0.078 Uiso 0.642(10) 1 calc PR B 1 C52 C 0.7785(4) 0.4305(4) 0.49643(16) 0.0544(15) Uani 0.642(10) 1 d PGU B 1 H52A H 0.8102 0.4581 0.5433 0.065 Uiso 0.642(10) 1 calc PR B 1 C53 C 0.6725(4) 0.3894(4) 0.47610(19) 0.0549(14) Uani 0.642(10) 1 d PGU B 1 H53A H 0.6318 0.3889 0.5091 0.066 Uiso 0.642(10) 1 calc PR B 1 C54 C 0.6260(3) 0.3489(5) 0.4075(2) 0.0488(12) Uani 0.642(10) 1 d PGU B 1 H54A H 0.5536 0.3208 0.3936 0.059 Uiso 0.642(10) 1 calc PR B 1 C49B C 0.6747(8) 0.3418(8) 0.3625(3) 0.044(2) Uani 0.358(10) 1 d PGDU B 2 C50B C 0.7770(7) 0.3773(8) 0.3952(4) 0.058(2) Uani 0.358(10) 1 d PGU B 2 H50B H 0.8263 0.3756 0.3697 0.069 Uiso 0.358(10) 1 calc PR B 2 C51B C 0.8071(7) 0.4152(7) 0.4652(4) 0.060(2) Uani 0.358(10) 1 d PGU B 2 H51B H 0.8770 0.4395 0.4875 0.072 Uiso 0.358(10) 1 calc PR B 2 C52B C 0.7350(8) 0.4177(6) 0.5026(3) 0.055(2) Uani 0.358(10) 1 d PGU B 2 H52B H 0.7556 0.4436 0.5504 0.065 Uiso 0.358(10) 1 calc PR B 2 C53B C 0.6327(7) 0.3822(8) 0.4699(4) 0.056(2) Uani 0.358(10) 1 d PGU B 2 H53B H 0.5834 0.3839 0.4954 0.067 Uiso 0.358(10) 1 calc PR B 2 C54B C 0.6026(6) 0.3442(9) 0.3999(4) 0.054(2) Uani 0.358(10) 1 d PGU B 2 H54B H 0.5327 0.3200 0.3776 0.065 Uiso 0.358(10) 1 calc PR B 2 C55 C 0.71758(19) 0.26461(18) 0.23211(14) 0.0465(6) Uani 1 1 d . B . H55A H 0.7843 0.3216 0.2412 0.056 Uiso 1 1 calc R . . H55B H 0.7277 0.2117 0.2520 0.056 Uiso 1 1 calc R . . C56 C 0.6736(2) 0.23357(17) 0.15535(14) 0.0447(6) Uani 1 1 d . B . H56A H 0.6134 0.1704 0.1459 0.054 Uiso 1 1 calc R . . H56B H 0.7254 0.2275 0.1308 0.054 Uiso 1 1 calc R . . C57 C 0.54844(17) 0.27387(15) 0.04329(12) 0.0348(5) Uani 1 1 d . B . C58 C 0.4782(2) 0.17703(17) 0.03074(15) 0.0499(7) Uani 1 1 d . . . H58A H 0.4811 0.1369 0.0636 0.060 Uiso 1 1 calc R B . C59 C 0.4046(2) 0.1400(2) -0.02974(17) 0.0633(8) Uani 1 1 d . B . H59A H 0.3575 0.0740 -0.0383 0.076 Uiso 1 1 calc R . . C60 C 0.3984(2) 0.1970(2) -0.07742(16) 0.0579(8) Uani 1 1 d . . . H60A H 0.3469 0.1708 -0.1184 0.070 Uiso 1 1 calc R B . C61 C 0.4671(2) 0.29222(19) -0.06568(14) 0.0504(7) Uani 1 1 d . B . H61A H 0.4632 0.3318 -0.0987 0.060 Uiso 1 1 calc R . . C62 C 0.54181(18) 0.33056(16) -0.00587(12) 0.0394(6) Uani 1 1 d . . . H62A H 0.5892 0.3964 0.0017 0.047 Uiso 1 1 calc R B . C63 C 0.75403(16) 0.41373(15) 0.10917(11) 0.0306(5) Uani 1 1 d . B . C64 C 0.81486(17) 0.49561(15) 0.15814(12) 0.0346(5) Uani 1 1 d . . . H64A H 0.7912 0.5089 0.1980 0.042 Uiso 1 1 calc R B . C65 C 0.90970(17) 0.55791(17) 0.14925(13) 0.0402(6) Uani 1 1 d . B . H65A H 0.9521 0.6127 0.1836 0.048 Uiso 1 1 calc R . . C66 C 0.94247(18) 0.54006(18) 0.09021(13) 0.0447(6) Uani 1 1 d . . . H66A H 1.0068 0.5838 0.0834 0.054 Uiso 1 1 calc R B . C67 C 0.88283(19) 0.45966(19) 0.04139(13) 0.0480(7) Uani 1 1 d . B . H67A H 0.9061 0.4478 0.0010 0.058 Uiso 1 1 calc R . . C68 C 0.78931(18) 0.39594(17) 0.05063(12) 0.0405(6) Uani 1 1 d . . . H68A H 0.7488 0.3398 0.0170 0.049 Uiso 1 1 calc R B . N3 N 0.22561(15) 0.23469(15) 0.40150(11) 0.0437(5) Uani 1 1 d U . . C69 C 0.1580(2) 0.1670(2) 0.33633(15) 0.0622(8) Uani 1 1 d U . . H69A H 0.1202 0.1992 0.3113 0.075 Uiso 1 1 calc R . . H69B H 0.1070 0.1092 0.3490 0.075 Uiso 1 1 calc R . . C70 C 0.2132(3) 0.1349(2) 0.28817(18) 0.0821(10) Uani 1 1 d U . . H70A H 0.1648 0.0975 0.2451 0.123 Uiso 1 1 calc R . . H70B H 0.2426 0.0946 0.3098 0.123 Uiso 1 1 calc R . . H70C H 0.2680 0.1915 0.2783 0.123 Uiso 1 1 calc R . . C71 C 0.3002(2) 0.32936(19) 0.38732(16) 0.0571(7) Uani 1 1 d U . . H71A H 0.3442 0.3693 0.4318 0.068 Uiso 1 1 calc R . . H71B H 0.3449 0.3158 0.3592 0.068 Uiso 1 1 calc R . . C72 C 0.2531(3) 0.3875(3) 0.35080(18) 0.0826(10) Uani 1 1 d U . . H72A H 0.3073 0.4474 0.3445 0.124 Uiso 1 1 calc R . . H72B H 0.2097 0.4027 0.3784 0.124 Uiso 1 1 calc R . . H72C H 0.2116 0.3501 0.3057 0.124 Uiso 1 1 calc R . . C73 C 0.2904(2) 0.1909(2) 0.44007(17) 0.0634(8) Uani 1 1 d U . . H73A H 0.3395 0.1865 0.4122 0.076 Uiso 1 1 calc R . . H73B H 0.3307 0.2353 0.4839 0.076 Uiso 1 1 calc R . . C74 C 0.2312(3) 0.0921(2) 0.45635(19) 0.0798(10) Uani 1 1 d U . . H74A H 0.2783 0.0724 0.4845 0.120 Uiso 1 1 calc R . . H74B H 0.1974 0.0456 0.4133 0.120 Uiso 1 1 calc R . . H74C H 0.1797 0.0944 0.4818 0.120 Uiso 1 1 calc R . . C75 C 0.1549(2) 0.2507(2) 0.44427(15) 0.0609(8) Uani 1 1 d U . . H75A H 0.1090 0.1876 0.4538 0.073 Uiso 1 1 calc R . . H75B H 0.1116 0.2757 0.4166 0.073 Uiso 1 1 calc R . . C76 C 0.2077(3) 0.3198(2) 0.51251(16) 0.0730(9) Uani 1 1 d U . . H76A H 0.1562 0.3245 0.5370 0.110 Uiso 1 1 calc R . . H76B H 0.2507 0.3837 0.5038 0.110 Uiso 1 1 calc R . . H76C H 0.2505 0.2957 0.5407 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03024(15) 0.02758(13) 0.03078(16) 0.01034(11) 0.01231(12) 0.01562(11) Fe1 0.02691(16) 0.02729(15) 0.03042(17) 0.00543(12) 0.00833(13) 0.01325(13) S1 0.0302(3) 0.0307(3) 0.0349(3) 0.0102(2) 0.0131(2) 0.0127(2) S2 0.0374(3) 0.0312(3) 0.0331(3) 0.0120(2) 0.0152(2) 0.0197(2) P1 0.0330(3) 0.0340(3) 0.0387(3) 0.0155(3) 0.0108(3) 0.0166(3) P2 0.0357(3) 0.0260(3) 0.0388(3) 0.0092(2) 0.0173(3) 0.0156(2) B1 0.0244(12) 0.0313(12) 0.0294(13) 0.0052(10) 0.0077(10) 0.0138(10) B2 0.0281(13) 0.0295(12) 0.0437(16) 0.0075(11) 0.0069(12) 0.0100(11) N1 0.0287(10) 0.0300(9) 0.0278(10) 0.0025(7) 0.0071(8) 0.0131(8) N2 0.0297(10) 0.0317(10) 0.0420(12) 0.0045(8) 0.0066(9) 0.0120(9) O1 0.0937(15) 0.0815(14) 0.0300(11) 0.0093(9) 0.0137(10) 0.0468(12) C1 0.0437(14) 0.0396(13) 0.0409(15) 0.0058(11) 0.0067(12) 0.0218(11) C2 0.0278(11) 0.0272(10) 0.0236(11) 0.0031(8) 0.0084(9) 0.0091(9) C3 0.0287(11) 0.0269(10) 0.0328(12) 0.0065(9) 0.0118(9) 0.0121(9) C4 0.0310(12) 0.0309(11) 0.0341(13) 0.0086(9) 0.0108(10) 0.0126(9) C5 0.0421(13) 0.0346(12) 0.0453(15) 0.0091(10) 0.0211(12) 0.0216(11) C6 0.0512(15) 0.0363(12) 0.0323(13) -0.0011(10) 0.0170(12) 0.0153(11) C7 0.0440(14) 0.0453(13) 0.0293(13) 0.0045(10) 0.0072(11) 0.0180(11) C8 0.0346(12) 0.0421(12) 0.0337(13) 0.0070(10) 0.0122(10) 0.0208(10) F1 0.0351(7) 0.0427(7) 0.0445(8) 0.0034(6) 0.0070(6) 0.0234(6) F2 0.0567(9) 0.0522(8) 0.0632(10) 0.0021(7) 0.0224(8) 0.0353(7) F3 0.0788(11) 0.0596(9) 0.0419(9) -0.0096(7) 0.0178(8) 0.0332(8) F4 0.0625(10) 0.0742(10) 0.0327(8) -0.0059(7) -0.0041(7) 0.0329(8) F5 0.0531(9) 0.0711(9) 0.0360(8) -0.0026(7) -0.0011(7) 0.0429(8) C9 0.0283(11) 0.0287(10) 0.0376(13) 0.0066(9) 0.0062(10) 0.0162(9) C10 0.0323(12) 0.0331(11) 0.0384(13) 0.0059(10) 0.0066(10) 0.0161(10) C11 0.0446(15) 0.0355(12) 0.0479(16) -0.0011(11) -0.0032(12) 0.0152(11) C12 0.0354(14) 0.0355(13) 0.0669(19) 0.0103(13) 0.0008(13) 0.0027(11) C13 0.0356(14) 0.0437(14) 0.0594(18) 0.0184(13) 0.0141(13) 0.0098(11) C14 0.0352(13) 0.0356(12) 0.0436(14) 0.0100(11) 0.0101(11) 0.0152(10) F6 0.0431(8) 0.0431(7) 0.0369(8) -0.0010(6) 0.0091(6) 0.0180(6) F7 0.0687(11) 0.0483(9) 0.0552(10) -0.0122(8) -0.0048(8) 0.0095(8) F8 0.0521(10) 0.0525(9) 0.0964(14) 0.0062(9) 0.0001(9) -0.0135(8) F9 0.0530(10) 0.0654(10) 0.0883(13) 0.0253(9) 0.0343(9) 0.0018(8) F10 0.0530(9) 0.0496(8) 0.0460(9) 0.0096(7) 0.0260(7) 0.0114(7) C15 0.0285(11) 0.0274(10) 0.0296(12) 0.0026(9) 0.0090(9) 0.0135(9) C16 0.0304(12) 0.0346(11) 0.0349(13) 0.0019(10) 0.0066(10) 0.0148(10) C17 0.0376(13) 0.0312(12) 0.0463(15) 0.0039(11) 0.0153(12) 0.0085(10) C18 0.0579(16) 0.0345(12) 0.0431(15) 0.0136(11) 0.0247(13) 0.0222(12) C19 0.0465(14) 0.0402(12) 0.0343(13) 0.0066(10) 0.0090(11) 0.0246(11) C20 0.0310(12) 0.0277(10) 0.0330(12) 0.0021(9) 0.0073(10) 0.0117(9) F11 0.0295(7) 0.0428(7) 0.0454(8) 0.0029(6) -0.0001(6) 0.0078(6) F12 0.0459(9) 0.0404(8) 0.0685(11) 0.0084(7) 0.0175(8) 0.0000(7) F13 0.0795(11) 0.0426(8) 0.0637(10) 0.0284(7) 0.0319(9) 0.0244(8) F14 0.0629(9) 0.0546(8) 0.0437(8) 0.0175(7) 0.0061(7) 0.0326(7) F15 0.0316(7) 0.0400(7) 0.0472(8) 0.0097(6) 0.0013(6) 0.0141(6) C21 0.0316(12) 0.0337(11) 0.0339(13) 0.0047(9) 0.0073(10) 0.0192(10) C22 0.026(2) 0.036(2) 0.041(3) 0.005(2) -0.004(2) 0.013(2) C23 0.033(2) 0.035(2) 0.034(3) -0.005(2) -0.004(2) 0.011(2) C24 0.036(3) 0.052(2) 0.038(3) -0.004(2) -0.001(2) 0.021(2) C25 0.051(3) 0.051(2) 0.042(3) 0.004(2) -0.004(2) 0.037(2) C26 0.042(3) 0.044(2) 0.053(3) 0.014(2) -0.003(2) 0.0214(19) C27 0.032(3) 0.042(2) 0.060(3) 0.011(2) -0.002(2) 0.0174(19) F16 0.047(2) 0.0295(19) 0.042(2) -0.0024(16) 0.0166(18) 0.0070(17) F17 0.049(2) 0.059(2) 0.043(3) -0.0083(19) 0.0078(19) 0.0280(19) F18 0.069(3) 0.062(2) 0.053(3) 0.0019(17) -0.011(2) 0.0525(18) F19 0.074(3) 0.0405(18) 0.104(4) 0.024(2) 0.021(2) 0.0273(17) F20 0.041(2) 0.0378(18) 0.113(4) 0.019(2) 0.036(2) 0.0140(16) C22B 0.027(3) 0.033(3) 0.037(3) 0.001(3) 0.004(3) 0.011(3) C23B 0.030(3) 0.028(2) 0.031(3) 0.000(2) 0.000(3) 0.004(2) C24B 0.037(3) 0.048(3) 0.038(3) -0.008(3) 0.000(3) 0.022(3) C25B 0.053(3) 0.053(3) 0.048(3) 0.010(3) -0.003(3) 0.037(2) C26B 0.050(3) 0.049(3) 0.060(3) 0.025(2) 0.006(3) 0.034(2) C27B 0.025(3) 0.046(3) 0.061(3) 0.019(2) 0.013(3) 0.020(2) F16B 0.063(4) 0.030(2) 0.046(3) -0.005(2) 0.021(3) -0.002(2) F17B 0.059(4) 0.071(4) 0.049(4) -0.014(3) 0.011(3) 0.028(3) F18B 0.077(4) 0.080(3) 0.064(4) 0.019(3) 0.002(3) 0.066(3) F19B 0.138(6) 0.065(3) 0.108(5) 0.055(3) 0.053(4) 0.067(3) F20B 0.087(4) 0.060(4) 0.120(5) 0.054(3) 0.071(4) 0.044(3) C28 0.0266(11) 0.0349(11) 0.0371(13) 0.0062(10) 0.0108(10) 0.0117(9) C29 0.0340(12) 0.0371(12) 0.0323(13) 0.0013(10) 0.0082(10) 0.0144(10) C30 0.0461(14) 0.0434(13) 0.0479(15) 0.0095(11) 0.0111(12) 0.0283(12) C31 0.0436(14) 0.0527(15) 0.0412(15) 0.0108(12) 0.0015(12) 0.0250(12) C32 0.0365(13) 0.0422(13) 0.0386(14) -0.0020(11) 0.0012(11) 0.0123(11) C33 0.0329(12) 0.0341(12) 0.0449(14) 0.0041(10) 0.0075(11) 0.0157(10) F21 0.0612(9) 0.0450(8) 0.0410(8) -0.0035(6) 0.0029(7) 0.0308(7) F22 0.0779(11) 0.0564(9) 0.0630(10) 0.0073(8) 0.0042(8) 0.0470(8) F23 0.0791(11) 0.0743(11) 0.0563(10) 0.0055(8) -0.0174(9) 0.0442(9) F24 0.0692(10) 0.0570(9) 0.0486(9) -0.0130(7) -0.0171(8) 0.0267(8) F25 0.0551(9) 0.0368(7) 0.0641(10) -0.0085(7) -0.0116(8) 0.0223(7) C34 0.028(3) 0.032(4) 0.037(4) 0.009(3) 0.007(3) 0.010(3) C35 0.029(3) 0.040(4) 0.035(3) 0.016(3) 0.004(3) 0.012(3) C36 0.039(3) 0.050(4) 0.027(3) 0.015(3) 0.000(3) 0.021(3) C37 0.040(3) 0.053(4) 0.030(3) 0.014(3) 0.011(3) 0.023(3) C38 0.035(3) 0.042(4) 0.034(3) 0.008(3) 0.006(3) 0.012(3) C39 0.032(3) 0.033(4) 0.033(3) 0.003(3) 0.009(3) 0.011(3) F26 0.024(3) 0.068(5) 0.034(4) 0.013(3) 0.001(3) 0.002(3) F27 0.039(3) 0.095(5) 0.028(3) 0.003(3) 0.003(3) 0.021(3) F28 0.043(3) 0.085(5) 0.026(4) 0.015(3) 0.015(3) 0.029(3) F29 0.033(3) 0.065(6) 0.045(4) -0.002(4) 0.021(3) 0.009(3) F30 0.027(4) 0.043(4) 0.045(4) -0.013(3) 0.010(3) -0.002(3) C34B 0.0308(19) 0.030(2) 0.035(2) 0.0063(18) 0.0015(17) 0.0122(18) C35B 0.0326(19) 0.044(2) 0.043(2) 0.0151(17) -0.0020(17) 0.0050(16) C36B 0.058(2) 0.055(3) 0.032(2) 0.0112(18) -0.0068(17) 0.012(2) C37B 0.058(2) 0.056(2) 0.0285(19) 0.0132(18) 0.0092(18) 0.015(2) C38B 0.0360(19) 0.037(2) 0.038(2) 0.0060(18) 0.0110(17) 0.0109(18) C39B 0.0314(18) 0.0286(19) 0.0291(19) -0.0001(16) 0.0027(16) 0.0087(16) F26B 0.0346(18) 0.092(4) 0.063(3) 0.025(2) -0.0155(15) 0.0006(16) F27B 0.086(3) 0.133(4) 0.0333(19) 0.009(2) -0.0213(19) 0.007(3) F28B 0.095(3) 0.099(3) 0.0315(19) 0.007(2) 0.017(2) 0.020(3) F29B 0.0439(18) 0.051(2) 0.051(2) 0.0025(17) 0.0189(15) 0.0135(13) F30B 0.0279(15) 0.049(2) 0.0315(16) -0.0058(13) 0.0057(12) 0.0097(13) C40 0.0273(12) 0.0397(13) 0.0534(16) 0.0074(11) 0.0069(11) 0.0106(10) C41 0.0369(13) 0.0474(14) 0.0418(15) 0.0017(11) -0.0023(11) 0.0205(11) C42 0.0479(14) 0.0496(13) 0.0294(13) 0.0110(10) 0.0065(11) 0.0295(12) C43 0.0355(12) 0.0330(11) 0.0389(13) 0.0117(10) 0.0141(10) 0.0175(10) C44 0.0455(14) 0.0407(13) 0.0446(15) 0.0193(11) 0.0111(12) 0.0208(11) C45 0.0581(17) 0.0396(13) 0.0586(17) 0.0260(12) 0.0179(14) 0.0211(12) C46 0.0556(16) 0.0258(11) 0.0612(18) 0.0107(12) 0.0182(14) 0.0117(11) C47 0.0482(15) 0.0303(12) 0.0502(16) 0.0040(11) 0.0078(12) 0.0141(11) C48 0.0463(14) 0.0300(11) 0.0404(14) 0.0114(10) 0.0150(11) 0.0178(10) C49 0.049(2) 0.036(2) 0.043(2) 0.018(2) 0.0081(19) 0.018(2) C50 0.048(2) 0.062(3) 0.047(2) 0.022(2) 0.005(2) 0.019(2) C51 0.056(3) 0.068(3) 0.057(3) 0.015(2) -0.001(2) 0.014(2) C52 0.064(3) 0.051(3) 0.044(2) 0.005(2) -0.002(2) 0.025(2) C53 0.062(3) 0.054(2) 0.038(2) 0.011(2) -0.002(2) 0.017(3) C54 0.053(2) 0.048(2) 0.035(2) 0.004(2) 0.0038(19) 0.013(2) C49B 0.052(4) 0.034(3) 0.041(3) 0.025(3) -0.002(3) 0.013(3) C50B 0.055(3) 0.058(4) 0.053(4) 0.015(3) -0.001(3) 0.020(3) C51B 0.058(4) 0.058(4) 0.055(4) 0.009(3) -0.010(3) 0.022(3) C52B 0.059(5) 0.047(4) 0.043(4) 0.013(3) -0.012(3) 0.015(4) C53B 0.064(4) 0.054(4) 0.042(3) 0.014(3) -0.008(3) 0.022(4) C54B 0.064(4) 0.052(3) 0.035(3) 0.014(3) -0.003(3) 0.016(3) C55 0.0411(14) 0.0496(14) 0.0688(18) 0.0313(13) 0.0248(13) 0.0300(12) C56 0.0510(15) 0.0382(12) 0.0646(18) 0.0221(12) 0.0296(13) 0.0296(12) C57 0.0351(12) 0.0284(11) 0.0423(14) 0.0006(10) 0.0180(11) 0.0125(10) C58 0.0537(16) 0.0323(12) 0.0584(17) 0.0029(12) 0.0234(14) 0.0098(12) C59 0.0533(18) 0.0389(14) 0.075(2) -0.0137(15) 0.0152(16) 0.0013(13) C60 0.0470(16) 0.0531(16) 0.0597(19) -0.0155(14) -0.0008(14) 0.0169(13) C61 0.0477(15) 0.0488(15) 0.0524(17) 0.0009(13) 0.0068(13) 0.0211(13) C62 0.0370(13) 0.0301(11) 0.0470(15) 0.0007(10) 0.0081(11) 0.0116(10) C63 0.0300(11) 0.0321(11) 0.0347(13) 0.0085(9) 0.0127(10) 0.0156(9) C64 0.0373(13) 0.0381(12) 0.0330(13) 0.0052(10) 0.0137(10) 0.0185(10) C65 0.0326(13) 0.0408(13) 0.0403(14) -0.0002(11) 0.0074(11) 0.0103(10) C66 0.0288(13) 0.0541(15) 0.0481(16) 0.0073(12) 0.0160(11) 0.0120(11) C67 0.0390(14) 0.0600(16) 0.0411(15) -0.0001(12) 0.0208(12) 0.0144(12) C68 0.0369(13) 0.0417(13) 0.0394(14) -0.0001(11) 0.0146(11) 0.0125(11) N3 0.0376(11) 0.0537(12) 0.0459(12) 0.0153(10) 0.0190(10) 0.0203(10) C69 0.0678(19) 0.0722(19) 0.0495(17) 0.0089(14) 0.0124(15) 0.0329(16) C70 0.113(3) 0.071(2) 0.077(2) 0.0149(17) 0.052(2) 0.041(2) C71 0.0630(18) 0.0555(16) 0.0702(19) 0.0272(14) 0.0420(15) 0.0291(14) C72 0.123(3) 0.091(2) 0.085(2) 0.0470(19) 0.059(2) 0.077(2) C73 0.0536(17) 0.0573(16) 0.079(2) 0.0255(15) 0.0070(15) 0.0229(14) C74 0.090(2) 0.0589(18) 0.085(2) 0.0310(17) 0.0128(19) 0.0239(17) C75 0.0533(17) 0.0729(19) 0.0586(18) 0.0106(15) 0.0311(14) 0.0220(15) C76 0.088(2) 0.0657(19) 0.060(2) 0.0083(16) 0.0325(18) 0.0212(17) _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 Ni1 P2 2.1381(7) . ? Ni1 P1 2.1592(7) . ? Ni1 S2 2.1952(6) . ? Ni1 S1 2.3045(7) . ? Ni1 Fe1 2.5497(5) . ? Ni1 H1 1.71(2) . ? Fe1 C1 1.758(3) . ? Fe1 C21 1.866(2) . ? Fe1 C2 1.889(2) . ? Fe1 S2 2.2980(7) . ? Fe1 S1 2.3244(6) . ? Fe1 H1 1.52(2) . ? S1 C40 1.826(2) . ? S2 C42 1.831(2) . ? P1 C49 1.812(3) . ? P1 C43 1.818(2) . ? P1 C49B 1.832(5) . ? P1 C55 1.841(2) . ? P2 C63 1.813(2) . ? P2 C57 1.818(2) . ? P2 C56 1.845(2) . ? B1 N1 1.555(3) . ? B1 C3 1.642(3) . ? B1 C9 1.649(3) . ? B1 C15 1.653(3) . ? B2 N2 1.544(3) . ? B2 C22B 1.630(6) . ? B2 C34B 1.636(4) . ? B2 C28 1.653(3) . ? B2 C34 1.668(6) . ? B2 C22 1.682(4) . ? N1 C2 1.152(3) . ? N2 C21 1.155(3) . ? O1 C1 1.152(3) . ? C3 C4 1.389(3) . ? C3 C8 1.392(3) . ? C4 F1 1.358(2) . ? C4 C5 1.379(3) . ? C5 F2 1.351(3) . ? C5 C6 1.368(3) . ? C6 F3 1.346(3) . ? C6 C7 1.368(3) . ? C7 F4 1.347(3) . ? C7 C8 1.382(3) . ? C8 F5 1.350(2) . ? C9 C14 1.386(3) . ? C9 C10 1.388(3) . ? C10 F6 1.350(3) . ? C10 C11 1.377(3) . ? C11 F7 1.341(3) . ? C11 C12 1.377(4) . ? C12 F8 1.344(3) . ? C12 C13 1.359(4) . ? C13 F9 1.350(3) . ? C13 C14 1.382(3) . ? C14 F10 1.354(3) . ? C15 C20 1.390(3) . ? C15 C16 1.391(3) . ? C16 F11 1.354(3) . ? C16 C17 1.369(3) . ? C17 F12 1.354(3) . ? C17 C18 1.369(3) . ? C18 F13 1.347(3) . ? C18 C19 1.371(3) . ? C19 F14 1.348(3) . ? C19 C20 1.381(3) . ? C20 F15 1.351(2) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 F16 1.333(4) . ? C23 C24 1.3900 . ? C24 F17 1.339(4) . ? C24 C25 1.3900 . ? C25 F18 1.341(4) . ? C25 C26 1.3900 . ? C26 F19 1.348(4) . ? C26 C27 1.3900 . ? C27 F20 1.326(4) . ? C22B C23B 1.393(6) . ? C22B C27B 1.394(6) . ? C23B F16B 1.352(6) . ? C23B C24B 1.379(6) . ? C24B F17B 1.343(6) . ? C24B C25B 1.361(6) . ? C25B F18B 1.340(6) . ? C25B C26B 1.352(6) . ? C26B F19B 1.346(6) . ? C26B C27B 1.374(6) . ? C27B F20B 1.353(6) . ? C28 C33 1.380(3) . ? C28 C29 1.395(3) . ? C29 F21 1.347(2) . ? C29 C30 1.378(3) . ? C30 F22 1.348(3) . ? C30 C31 1.370(3) . ? C31 F23 1.343(3) . ? C31 C32 1.369(3) . ? C32 F24 1.347(3) . ? C32 C33 1.382(3) . ? C33 F25 1.358(3) . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 F26 1.332(6) . ? C35 C36 1.3900 . ? C36 F27 1.340(6) . ? C36 C37 1.3900 . ? C37 F28 1.346(6) . ? C37 C38 1.3900 . ? C38 F29 1.347(6) . ? C38 C39 1.3900 . ? C39 F30 1.341(6) . ? C34B C39B 1.390(4) . ? C34B C35B 1.396(4) . ? C35B F26B 1.346(4) . ? C35B C36B 1.367(5) . ? C36B F27B 1.343(4) . ? C36B C37B 1.363(5) . ? C37B F28B 1.345(4) . ? C37B C38B 1.361(5) . ? C38B F29B 1.351(4) . ? C38B C39B 1.372(4) . ? C39B F30B 1.358(4) . ? C40 C41 1.509(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.511(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.385(3) . ? C43 C44 1.401(3) . ? C44 C45 1.384(3) . ? C44 H44A 0.9500 . ? C45 C46 1.367(4) . ? C45 H45A 0.9500 . ? C46 C47 1.390(3) . ? C46 H46A 0.9500 . ? C47 C48 1.381(3) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C50 H50A 0.9500 . ? C51 C52 1.3900 . ? C51 H51A 0.9500 . ? C52 C53 1.3900 . ? C52 H52A 0.9500 . ? C53 C54 1.3900 . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C49B C50B 1.3900 . ? C49B C54B 1.3900 . ? C50B C51B 1.3900 . ? C50B H50B 0.9500 . ? C51B C52B 1.3900 . ? C51B H51B 0.9500 . ? C52B C53B 1.3900 . ? C52B H52B 0.9500 . ? C53B C54B 1.3900 . ? C53B H53B 0.9500 . ? C54B H54B 0.9500 . ? C55 C56 1.515(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C62 1.391(3) . ? C57 C58 1.399(3) . ? C58 C59 1.384(4) . ? C58 H58A 0.9500 . ? C59 C60 1.370(4) . ? C59 H59A 0.9500 . ? C60 C61 1.374(4) . ? C60 H60A 0.9500 . ? C61 C62 1.382(3) . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? C63 C64 1.388(3) . ? C63 C68 1.392(3) . ? C64 C65 1.383(3) . ? C64 H64A 0.9500 . ? C65 C66 1.381(3) . ? C65 H65A 0.9500 . ? C66 C67 1.371(3) . ? C66 H66A 0.9500 . ? C67 C68 1.378(3) . ? C67 H67A 0.9500 . ? C68 H68A 0.9500 . ? N3 C69 1.506(3) . ? N3 C75 1.512(3) . ? N3 C71 1.513(3) . ? N3 C73 1.526(3) . ? C69 C70 1.510(4) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.505(4) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.512(4) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.522(4) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? 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 P2 Ni1 P1 87.77(3) . . ? P2 Ni1 S2 92.89(2) . . ? P1 Ni1 S2 168.45(3) . . ? P2 Ni1 S1 147.71(2) . . ? P1 Ni1 S1 97.12(2) . . ? S2 Ni1 S1 88.48(2) . . ? P2 Ni1 Fe1 145.50(2) . . ? P1 Ni1 Fe1 117.81(2) . . ? S2 Ni1 Fe1 57.350(19) . . ? S1 Ni1 Fe1 56.952(16) . . ? P2 Ni1 H1 132.7(8) . . ? P1 Ni1 H1 90.5(8) . . ? S2 Ni1 H1 80.6(8) . . ? S1 Ni1 H1 79.4(8) . . ? Fe1 Ni1 H1 35.2(8) . . ? C1 Fe1 C21 94.01(10) . . ? C1 Fe1 C2 90.61(10) . . ? C21 Fe1 C2 95.96(9) . . ? C1 Fe1 S2 170.17(8) . . ? C21 Fe1 S2 90.08(7) . . ? C2 Fe1 S2 97.86(6) . . ? C1 Fe1 S1 88.49(8) . . ? C21 Fe1 S1 167.09(7) . . ? C2 Fe1 S1 96.68(6) . . ? S2 Fe1 S1 85.59(2) . . ? C1 Fe1 Ni1 116.64(8) . . ? C21 Fe1 Ni1 111.75(7) . . ? C2 Fe1 Ni1 138.29(6) . . ? S2 Fe1 Ni1 53.547(15) . . ? S1 Fe1 Ni1 56.202(18) . . ? C1 Fe1 H1 90.3(9) . . ? C21 Fe1 H1 84.8(9) . . ? C2 Fe1 H1 178.8(9) . . ? S2 Fe1 H1 81.2(9) . . ? S1 Fe1 H1 82.5(9) . . ? Ni1 Fe1 H1 40.5(9) . . ? C40 S1 Ni1 110.67(8) . . ? C40 S1 Fe1 108.39(8) . . ? Ni1 S1 Fe1 66.846(18) . . ? C42 S2 Ni1 110.89(8) . . ? C42 S2 Fe1 109.88(8) . . ? Ni1 S2 Fe1 69.10(2) . . ? C49 P1 C43 106.76(19) . . ? C43 P1 C49B 101.4(3) . . ? C49 P1 C55 106.5(2) . . ? C43 P1 C55 103.53(11) . . ? C49B P1 C55 110.1(4) . . ? C49 P1 Ni1 117.4(2) . . ? C43 P1 Ni1 114.52(8) . . ? C49B P1 Ni1 119.3(4) . . ? C55 P1 Ni1 106.97(8) . . ? C63 P2 C57 106.25(10) . . ? C63 P2 C56 102.31(11) . . ? C57 P2 C56 106.78(11) . . ? C63 P2 Ni1 115.61(7) . . ? C57 P2 Ni1 115.77(7) . . ? C56 P2 Ni1 108.97(8) . . ? N1 B1 C3 111.17(17) . . ? N1 B1 C9 103.86(16) . . ? C3 B1 C9 113.93(18) . . ? N1 B1 C15 107.14(17) . . ? C3 B1 C15 105.07(16) . . ? C9 B1 C15 115.59(18) . . ? N2 B2 C22B 105.4(3) . . ? N2 B2 C34B 109.4(2) . . ? C22B B2 C34B 111.1(4) . . ? N2 B2 C28 105.42(18) . . ? C22B B2 C28 115.8(3) . . ? C34B B2 C28 109.4(2) . . ? N2 B2 C34 105.8(3) . . ? C22B B2 C34 112.6(6) . . ? C28 B2 C34 110.9(4) . . ? N2 B2 C22 107.6(2) . . ? C34B B2 C22 113.3(3) . . ? C28 B2 C22 111.3(3) . . ? C34 B2 C22 115.1(5) . . ? C2 N1 B1 177.0(2) . . ? C21 N2 B2 178.4(2) . . ? O1 C1 Fe1 176.1(2) . . ? N1 C2 Fe1 174.85(18) . . ? C4 C3 C8 113.22(19) . . ? C4 C3 B1 118.60(19) . . ? C8 C3 B1 127.95(19) . . ? F1 C4 C5 116.69(19) . . ? F1 C4 C3 118.81(19) . . ? C5 C4 C3 124.5(2) . . ? F2 C5 C6 120.0(2) . . ? F2 C5 C4 120.5(2) . . ? C6 C5 C4 119.5(2) . . ? F3 C6 C5 120.5(2) . . ? F3 C6 C7 120.5(2) . . ? C5 C6 C7 119.0(2) . . ? F4 C7 C6 119.6(2) . . ? F4 C7 C8 120.4(2) . . ? C6 C7 C8 120.0(2) . . ? F5 C8 C7 115.2(2) . . ? F5 C8 C3 121.05(19) . . ? C7 C8 C3 123.7(2) . . ? C14 C9 C10 113.2(2) . . ? C14 C9 B1 126.0(2) . . ? C10 C9 B1 120.49(19) . . ? F6 C10 C11 116.3(2) . . ? F6 C10 C9 119.32(19) . . ? C11 C10 C9 124.4(2) . . ? F7 C11 C10 120.9(2) . . ? F7 C11 C12 119.8(2) . . ? C10 C11 C12 119.3(2) . . ? F8 C12 C13 120.3(3) . . ? F8 C12 C11 120.6(3) . . ? C13 C12 C11 119.2(2) . . ? F9 C13 C12 120.2(2) . . ? F9 C13 C14 120.0(2) . . ? C12 C13 C14 119.7(2) . . ? F10 C14 C13 115.0(2) . . ? F10 C14 C9 120.80(19) . . ? C13 C14 C9 124.2(2) . . ? C20 C15 C16 113.33(19) . . ? C20 C15 B1 127.88(19) . . ? C16 C15 B1 118.68(19) . . ? F11 C16 C17 116.2(2) . . ? F11 C16 C15 119.35(19) . . ? C17 C16 C15 124.4(2) . . ? F12 C17 C16 120.8(2) . . ? F12 C17 C18 119.7(2) . . ? C16 C17 C18 119.5(2) . . ? F13 C18 C17 120.6(2) . . ? F13 C18 C19 120.1(2) . . ? C17 C18 C19 119.3(2) . . ? F14 C19 C18 119.9(2) . . ? F14 C19 C20 120.6(2) . . ? C18 C19 C20 119.4(2) . . ? F15 C20 C19 115.41(19) . . ? F15 C20 C15 120.64(19) . . ? C19 C20 C15 123.9(2) . . ? N2 C21 Fe1 177.43(19) . . ? C23 C22 C27 120.0 . . ? C23 C22 B2 118.7(3) . . ? C27 C22 B2 121.3(3) . . ? F16 C23 C24 116.2(4) . . ? F16 C23 C22 123.5(4) . . ? C24 C23 C22 120.0 . . ? F17 C24 C23 120.8(4) . . ? F17 C24 C25 119.2(4) . . ? C23 C24 C25 120.0 . . ? F18 C25 C26 119.2(4) . . ? F18 C25 C24 120.7(4) . . ? C26 C25 C24 120.0 . . ? F19 C26 C25 118.6(4) . . ? F19 C26 C27 121.4(4) . . ? C25 C26 C27 120.0 . . ? F20 C27 C26 115.6(3) . . ? F20 C27 C22 124.4(3) . . ? C26 C27 C22 120.0 . . ? C23B C22B C27B 108.4(4) . . ? C23B C22B B2 123.5(5) . . ? C27B C22B B2 127.8(5) . . ? F16B C23B C24B 115.4(6) . . ? F16B C23B C22B 117.0(6) . . ? C24B C23B C22B 127.6(5) . . ? F17B C24B C25B 119.8(6) . . ? F17B C24B C23B 120.8(7) . . ? C25B C24B C23B 119.3(5) . . ? F18B C25B C26B 122.0(6) . . ? F18B C25B C24B 121.0(6) . . ? C26B C25B C24B 117.0(5) . . ? F19B C26B C25B 119.4(6) . . ? F19B C26B C27B 119.1(6) . . ? C25B C26B C27B 121.5(5) . . ? F20B C27B C26B 116.8(6) . . ? F20B C27B C22B 117.3(6) . . ? C26B C27B C22B 125.9(5) . . ? C33 C28 C29 113.3(2) . . ? C33 C28 B2 126.9(2) . . ? C29 C28 B2 119.80(19) . . ? F21 C29 C30 116.0(2) . . ? F21 C29 C28 119.7(2) . . ? C30 C29 C28 124.3(2) . . ? F22 C30 C31 119.8(2) . . ? F22 C30 C29 120.8(2) . . ? C31 C30 C29 119.4(2) . . ? F23 C31 C32 120.1(2) . . ? F23 C31 C30 120.9(2) . . ? C32 C31 C30 118.9(2) . . ? F24 C32 C31 119.6(2) . . ? F24 C32 C33 120.5(2) . . ? C31 C32 C33 119.9(2) . . ? F25 C33 C28 120.6(2) . . ? F25 C33 C32 115.3(2) . . ? C28 C33 C32 124.1(2) . . ? C35 C34 C39 120.0 . . ? C35 C34 B2 125.1(4) . . ? C39 C34 B2 114.7(4) . . ? F26 C35 C36 116.6(5) . . ? F26 C35 C34 123.2(5) . . ? C36 C35 C34 120.0 . . ? F27 C36 C35 119.1(5) . . ? F27 C36 C37 120.7(5) . . ? C35 C36 C37 120.0 . . ? F28 C37 C38 120.9(6) . . ? F28 C37 C36 119.1(6) . . ? C38 C37 C36 120.0 . . ? F29 C38 C37 118.8(6) . . ? F29 C38 C39 121.1(6) . . ? C37 C38 C39 120.0 . . ? F30 C39 C38 116.8(6) . . ? F30 C39 C34 123.2(6) . . ? C38 C39 C34 120.0 . . ? C39B C34B C35B 111.0(3) . . ? C39B C34B B2 126.8(3) . . ? C35B C34B B2 122.2(3) . . ? F26B C35B C36B 115.9(4) . . ? F26B C35B C34B 118.9(4) . . ? C36B C35B C34B 125.2(3) . . ? F27B C36B C37B 119.3(4) . . ? F27B C36B C35B 120.5(4) . . ? C37B C36B C35B 120.1(3) . . ? F28B C37B C38B 120.4(4) . . ? F28B C37B C36B 121.3(4) . . ? C38B C37B C36B 118.3(4) . . ? F29B C38B C37B 120.1(4) . . ? F29B C38B C39B 120.1(4) . . ? C37B C38B C39B 119.8(3) . . ? F30B C39B C38B 116.2(4) . . ? F30B C39B C34B 118.2(4) . . ? C38B C39B C34B 125.5(3) . . ? C41 C40 S1 115.01(16) . . ? C41 C40 H40A 108.5 . . ? S1 C40 H40A 108.5 . . ? C41 C40 H40B 108.5 . . ? S1 C40 H40B 108.5 . . ? H40A C40 H40B 107.5 . . ? C40 C41 C42 114.4(2) . . ? C40 C41 H41A 108.7 . . ? C42 C41 H41A 108.7 . . ? C40 C41 H41B 108.7 . . ? C42 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C41 C42 S2 116.52(16) . . ? C41 C42 H42A 108.2 . . ? S2 C42 H42A 108.2 . . ? C41 C42 H42B 108.2 . . ? S2 C42 H42B 108.2 . . ? H42A C42 H42B 107.3 . . ? C48 C43 C44 119.0(2) . . ? C48 C43 P1 119.06(17) . . ? C44 C43 P1 121.87(17) . . ? C45 C44 C43 119.9(2) . . ? C45 C44 H44A 120.1 . . ? C43 C44 H44A 120.1 . . ? C46 C45 C44 120.3(2) . . ? C46 C45 H45A 119.8 . . ? C44 C45 H45A 119.8 . . ? C45 C46 C47 120.7(2) . . ? C45 C46 H46A 119.7 . . ? C47 C46 H46A 119.7 . . ? C48 C47 C46 119.2(2) . . ? C48 C47 H47A 120.4 . . ? C46 C47 H47A 120.4 . . ? C47 C48 C43 120.9(2) . . ? C47 C48 H48A 119.5 . . ? C43 C48 H48A 119.5 . . ? C50 C49 C54 120.0 . . ? C50 C49 P1 120.2(3) . . ? C54 C49 P1 119.8(3) . . ? C51 C50 C49 120.0 . . ? C51 C50 H50A 120.0 . . ? C49 C50 H50A 120.0 . . ? C52 C51 C50 120.0 . . ? C52 C51 H51A 120.0 . . ? C50 C51 H51A 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 H54A 120.0 . . ? C49 C54 H54A 120.0 . . ? C50B C49B C54B 120.0 . . ? C50B C49B P1 125.0(6) . . ? C54B C49B P1 115.0(6) . . ? C49B C50B C51B 120.0 . . ? C49B C50B H50B 120.0 . . ? C51B C50B H50B 120.0 . . ? C52B C51B C50B 120.0 . . ? C52B C51B H51B 120.0 . . ? C50B C51B H51B 120.0 . . ? C51B C52B C53B 120.0 . . ? C51B C52B H52B 120.0 . . ? C53B C52B H52B 120.0 . . ? C52B C53B C54B 120.0 . . ? C52B C53B H53B 120.0 . . ? C54B C53B H53B 120.0 . . ? C53B C54B C49B 120.0 . . ? C53B C54B H54B 120.0 . . ? C49B C54B H54B 120.0 . . ? C56 C55 P1 106.51(16) . . ? C56 C55 H55A 110.4 . . ? P1 C55 H55A 110.4 . . ? C56 C55 H55B 110.4 . . ? P1 C55 H55B 110.4 . . ? H55A C55 H55B 108.6 . . ? C55 C56 P2 106.98(16) . . ? C55 C56 H56A 110.3 . . ? P2 C56 H56A 110.3 . . ? C55 C56 H56B 110.3 . . ? P2 C56 H56B 110.3 . . ? H56A C56 H56B 108.6 . . ? C62 C57 C58 118.6(2) . . ? C62 C57 P2 120.80(16) . . ? C58 C57 P2 120.2(2) . . ? C59 C58 C57 119.7(3) . . ? C59 C58 H58A 120.2 . . ? C57 C58 H58A 120.2 . . ? C60 C59 C58 121.1(2) . . ? C60 C59 H59A 119.5 . . ? C58 C59 H59A 119.5 . . ? C59 C60 C61 119.8(3) . . ? C59 C60 H60A 120.1 . . ? C61 C60 H60A 120.1 . . ? C60 C61 C62 120.2(3) . . ? C60 C61 H61A 119.9 . . ? C62 C61 H61A 119.9 . . ? C61 C62 C57 120.8(2) . . ? C61 C62 H62A 119.6 . . ? C57 C62 H62A 119.6 . . ? C64 C63 C68 119.1(2) . . ? C64 C63 P2 119.30(17) . . ? C68 C63 P2 121.40(17) . . ? C65 C64 C63 120.4(2) . . ? C65 C64 H64A 119.8 . . ? C63 C64 H64A 119.8 . . ? C66 C65 C64 119.6(2) . . ? C66 C65 H65A 120.2 . . ? C64 C65 H65A 120.2 . . ? C67 C66 C65 120.4(2) . . ? C67 C66 H66A 119.8 . . ? C65 C66 H66A 119.8 . . ? C66 C67 C68 120.3(2) . . ? C66 C67 H67A 119.8 . . ? C68 C67 H67A 119.8 . . ? C67 C68 C63 120.1(2) . . ? C67 C68 H68A 119.9 . . ? C63 C68 H68A 119.9 . . ? C69 N3 C75 106.3(2) . . ? C69 N3 C71 112.2(2) . . ? C75 N3 C71 110.8(2) . . ? C69 N3 C73 110.6(2) . . ? C75 N3 C73 110.9(2) . . ? C71 N3 C73 106.06(19) . . ? N3 C69 C70 115.1(3) . . ? N3 C69 H69A 108.5 . . ? C70 C69 H69A 108.5 . . ? N3 C69 H69B 108.5 . . ? C70 C69 H69B 108.5 . . ? H69A C69 H69B 107.5 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 N3 115.7(2) . . ? C72 C71 H71A 108.4 . . ? N3 C71 H71A 108.4 . . ? C72 C71 H71B 108.4 . . ? N3 C71 H71B 108.4 . . ? H71A C71 H71B 107.4 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 N3 115.3(2) . . ? C74 C73 H73A 108.5 . . ? N3 C73 H73A 108.5 . . ? C74 C73 H73B 108.5 . . ? N3 C73 H73B 108.5 . . ? H73A C73 H73B 107.5 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N3 C75 C76 115.3(2) . . ? N3 C75 H75A 108.5 . . ? C76 C75 H75A 108.5 . . ? N3 C75 H75B 108.5 . . ? C76 C75 H75B 108.5 . . ? H75A C75 H75B 107.5 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.994 _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_time ? _refine_diff_density_max 0.378 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.048 _publ_requested_category FM _publ_section_references ; Allen, F.H., Kennard, O., and Taylor, R. (1983). Accounts Chem. Res. 16, 146-153. Bruker (2001). SMART. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2005). SAINT, SHELXTL, XCIF, XPREP. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2007). SADABS, TWINABS. Bruker AXS, Inc., Madison, Wisconsin, USA. Spek, A. L. and van der Sluis, P. (1990). Acta Cryst. A46, 194-201. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 ; _publ_section_figure_captions ; Figure 1. SHELXTL (Bruker, 2005) plot showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. ; _publ_section_exptl_prep ; Crystals were grown from diffusion of hexanes into dichloromethane at 0C. ; _publ_section_exptl_refinement ; A structural model consisting of the host and tetraethylammonium counter ion plus two disordered dichloromethane solvate molecules was developed; however, positions for the idealized solvate molecules were poorly determined. This model converged with wR2 = 0.1156 and R1 = 0.0567 for 1305 parameters with 1054 restraints against 14597 data. Since positions for the solvate molecules were poorly determined a second structural model was refined with contributions from the solvate molecules removed from the diffraction data using the bypass procedure in PLATON (Spek, 1990). No positions for the host network differed by more than two su's between these two refined models. The electron count from the "squeeze" model converged in good agreement with the number of solvate molecules predicted by the complete refinement. The "squeezed" model converged with wR2 = 0.0930 and R1 = 0.0478 for 1267 parameters with 1056 restraints against 14596 data. Two of the tris-(pentafluoropheyl) rings on the anion were modeled as disordered over two sites. The primary orientation of the phenyl ring was constrained to be a aperfect hexagon (C-C = 1.39/%A). The secondary orientaions phenyl ring and F position geometries were then restrained to be the same as primary orientaion rings (esd 0.01). Like phenyl ring C-B atom bonds were restrained to be similar (esd 0.01). One phenyl ring on the host molecule was modeled as disordered over two sites. The phenyl rings were constrained to be perfect hexagons (C-C = 1.39/%A). Like phenyl ring C-P atom bonds were restrained to be similar (esd 0.01). Similar displacement amplitudes (esd 0.01) were imposed on all disordered sites overlapping by less than the sum of van der Waals radii (Allen et al, 1983). The tetraethylammonium was restrained to behave relatively isotropic. Methyl H atom positions, R-CH~3~, were optimized by rotation about R-C bonds with idealized C-H, R--H and H--H distances. The bridging hydride was located by the difference map and allowed to refine. Remaining H atoms were included as riding idealized contributors. Hydride H atom U was allowed to refine. Methyl H atom U's were assigned as 1.5 times U~eq~ of the carrier atom; remaining non-hydride H atom U's were assigned as 1.2 times carrier U~eq~. ; _publ_contact_author ; Danielle L. Gray University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; _publ_contact_author_phone '1 217 244 1708' _publ_contact_author_fax '1 217 244 8068' _publ_contact_author_email dgray@illinois.edu _publ_contact_letter ; Please consider this CIF submission for publication as a structural paper in Acta Crystallographica E. ; _publ_requested_journal 'Journal of the American Chemical Society' _publ_requested_coeditor_name ? _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; The Materials Chemistry Laboratory at the University of Illinois was supported in part by grants NSF CHE 95-03145 and NSF CHE 03-43032 from the National Science Foundation. ; _platon_squeeze_details ; The unit cell was found to contain two solvent molecules of dichloromethane that were poorly resolved. The electron count was found to be slightly higher than expected. ; loop_ _publ_author_name _publ_author_address 'Manor, Brian C.' ; University of Illinois School of Chemical Sciences 600 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Rauchfuss, Thomas B.' ; University of Illinois School of Chemical Sciences 600 South Mathews Avenue Urbana, Illinois 61801 USA ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 -1.00 0.0670 0.00 0.00 1.00 0.0410 -3.00 0.00 2.00 0.0590 3.00 0.00 -2.00 0.1620 1.00 3.00 -2.00 0.1800 3.00 -3.00 -1.00 0.1430 0.00 4.00 -1.00 0.1870 -4.00 0.00 -1.00 0.0710 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 291 77 ' ' 2 0.028 0.384 0.432 10 0 ' ' 3 0.972 0.616 0.568 10 0 ' ' #start Validation Reply Form _vrf_PLAT051_bm59uasq-sr-p ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by 9.85 % RESPONSE: The calculated Mu was found to differ from the given Mu. This difference is a result from two poorly defined dichloromethane solvent molecules being squeezed from the crystal structure. The reported moiety and sum formulas include the squeezed dichloromethane solvent molecules to reflect the true contents of the crystal. ;