data_bm53nas _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H54 Fe Ni O3 P2 S2, 2(C H2 Cl2), B F4 ' _chemical_formula_sum 'C34 H58 B Cl4 F4 Fe Ni O3 P2 S2' _chemical_formula_structural ? _chemical_formula_weight 984.03 _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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.680(2) _cell_length_b 15.715(2) _cell_length_c 17.193(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.840(2) _cell_angle_gamma 90.00 _cell_volume 4501.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3591 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 24.01 _exptl_crystal_description 'plate' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.544 _exptl_crystal_size_mid 0.295 _exptl_crystal_size_min 0.062 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_crystal_id bm53nas _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 1.190 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.7292 _exptl_absorpt_correction_T_max 0.9402 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; One distinct cell was identified using APEX2 (Bruker, 2004). Three 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. No decay correction was applied. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id bm53nas _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 \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36785 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.39 _reflns_number_total 8246 _reflns_number_gt 4865 _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 unambiguous 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 atom Ni1; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed little dependence on amplitude or 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^)+(0.0495P)^2^+1.9360P] 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 8246 _refine_ls_number_parameters 600 _refine_ls_number_restraints 476 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _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 0.97980(3) 0.24073(4) 0.37104(3) 0.02883(16) Uani 1 1 d . . . Fe1 Fe 1.14559(4) 0.24265(4) 0.41156(4) 0.03547(19) Uani 1 1 d . . . P1 P 0.91586(7) 0.13435(8) 0.31416(7) 0.0323(3) Uani 1 1 d . . . P2 P 0.91283(7) 0.32675(8) 0.29135(7) 0.0322(3) Uani 1 1 d . . . S1 S 1.04740(7) 0.15384(7) 0.45365(7) 0.0340(3) Uani 1 1 d . . . S2 S 1.05149(7) 0.34690(7) 0.42484(7) 0.0352(3) Uani 1 1 d . . . O1 O 1.2541(2) 0.2750(2) 0.5510(2) 0.0578(10) Uani 1 1 d . . . O2 O 1.2349(2) 0.3550(3) 0.3106(2) 0.0751(13) Uani 1 1 d . . . O3 O 1.2304(2) 0.0947(2) 0.3520(2) 0.0598(10) Uani 1 1 d . . . C1 C 0.8661(3) 0.0666(3) 0.3838(3) 0.0380(12) Uani 1 1 d . . . H1A H 0.9096 0.0372 0.4156 0.046 Uiso 1 1 calc R . . C2 C 0.8124(3) -0.0030(3) 0.3477(3) 0.0421(12) Uani 1 1 d . . . H2A H 0.7688 0.0233 0.3146 0.051 Uiso 1 1 calc R . . H2B H 0.8443 -0.0399 0.3142 0.051 Uiso 1 1 calc R . . C3 C 0.7762(3) -0.0565(3) 0.4108(3) 0.0484(14) Uani 1 1 d . . . H3A H 0.7396 -0.0993 0.3862 0.058 Uiso 1 1 calc R . . H3B H 0.8197 -0.0873 0.4403 0.058 Uiso 1 1 calc R . . C4 C 0.7305(3) -0.0030(3) 0.4662(3) 0.0491(14) Uani 1 1 d . . . H4A H 0.7094 -0.0398 0.5072 0.059 Uiso 1 1 calc R . . H4B H 0.6844 0.0243 0.4377 0.059 Uiso 1 1 calc R . . C5 C 0.7844(3) 0.0649(3) 0.5035(3) 0.0480(13) Uani 1 1 d . . . H5A H 0.8285 0.0376 0.5351 0.058 Uiso 1 1 calc R . . H5B H 0.7530 0.1005 0.5386 0.058 Uiso 1 1 calc R . . C6 C 0.8194(3) 0.1209(3) 0.4407(3) 0.0397(12) Uani 1 1 d . . . H6A H 0.8558 0.1638 0.4655 0.048 Uiso 1 1 calc R . . H6B H 0.7755 0.1514 0.4117 0.048 Uiso 1 1 calc R . . C7 C 0.9721(3) 0.0604(3) 0.2530(3) 0.0429(13) Uani 1 1 d . . . H7A H 0.9313 0.0217 0.2272 0.052 Uiso 1 1 calc R . . C8 C 1.0313(3) 0.0036(3) 0.2978(3) 0.0562(15) Uani 1 1 d . . . H8A H 1.0032 -0.0273 0.3386 0.067 Uiso 1 1 calc R . . H8B H 1.0735 0.0392 0.3240 0.067 Uiso 1 1 calc R . . C9 C 1.0701(4) -0.0602(4) 0.2449(4) 0.0744(19) Uani 1 1 d . . . H9A H 1.0288 -0.1003 0.2237 0.089 Uiso 1 1 calc R . . H9B H 1.1110 -0.0934 0.2755 0.089 Uiso 1 1 calc R . . C10 C 1.1096(4) -0.0161(4) 0.1779(4) 0.084(2) Uani 1 1 d . . . H10A H 1.1559 0.0178 0.1986 0.101 Uiso 1 1 calc R . . H10B H 1.1299 -0.0594 0.1420 0.101 Uiso 1 1 calc R . . C11 C 1.0515(4) 0.0413(4) 0.1338(3) 0.089(2) Uani 1 1 d . . . H11A H 1.0088 0.0065 0.1075 0.107 Uiso 1 1 calc R . . H11B H 1.0800 0.0722 0.0933 0.107 Uiso 1 1 calc R . . C12 C 1.0132(4) 0.1059(4) 0.1877(3) 0.0726(19) Uani 1 1 d . . . H12A H 1.0551 0.1445 0.2103 0.087 Uiso 1 1 calc R . . H12B H 0.9734 0.1407 0.1573 0.087 Uiso 1 1 calc R . . C13 C 0.8357(3) 0.1766(3) 0.2481(3) 0.0378(12) Uani 1 1 d . . . H13A H 0.8259 0.1366 0.2041 0.045 Uiso 1 1 calc R . . H13B H 0.7856 0.1813 0.2762 0.045 Uiso 1 1 calc R . . C14 C 0.8578(3) 0.2642(3) 0.2163(3) 0.0372(12) Uani 1 1 d . . . H14A H 0.8083 0.2949 0.1987 0.045 Uiso 1 1 calc R . . H14B H 0.8914 0.2570 0.1708 0.045 Uiso 1 1 calc R . . C15 C 0.8359(2) 0.3944(3) 0.3347(2) 0.0315(11) Uani 1 1 d . . . H15A H 0.8166 0.4344 0.2926 0.038 Uiso 1 1 calc R . . C16 C 0.7622(3) 0.3446(3) 0.3577(3) 0.0552(15) Uani 1 1 d . . . H16A H 0.7411 0.3107 0.3126 0.066 Uiso 1 1 calc R . . H16B H 0.7778 0.3046 0.4003 0.066 Uiso 1 1 calc R . . C17 C 0.6971(3) 0.4036(4) 0.3842(3) 0.0618(16) Uani 1 1 d . . . H17A H 0.6777 0.4395 0.3398 0.074 Uiso 1 1 calc R . . H17B H 0.6513 0.3693 0.4010 0.074 Uiso 1 1 calc R . . C18 C 0.7266(3) 0.4603(3) 0.4507(3) 0.0541(15) Uani 1 1 d . . . H18A H 0.7387 0.4253 0.4977 0.065 Uiso 1 1 calc R . . H18B H 0.6841 0.5015 0.4628 0.065 Uiso 1 1 calc R . . C19 C 0.8015(3) 0.5082(3) 0.4297(3) 0.0555(15) Uani 1 1 d . . . H19A H 0.8226 0.5401 0.4759 0.067 Uiso 1 1 calc R . . H19B H 0.7870 0.5500 0.3883 0.067 Uiso 1 1 calc R . . C20 C 0.8670(3) 0.4497(3) 0.4017(3) 0.0467(13) Uani 1 1 d . . . H20A H 0.9125 0.4845 0.3848 0.056 Uiso 1 1 calc R . . H20B H 0.8871 0.4131 0.4453 0.056 Uiso 1 1 calc R . . C21 C 0.9783(3) 0.3986(3) 0.2386(2) 0.0366(12) Uani 1 1 d . . . H21A H 1.0039 0.4381 0.2782 0.044 Uiso 1 1 calc R . . C22 C 1.0458(3) 0.3498(3) 0.2028(3) 0.0477(14) Uani 1 1 d . . . H22A H 1.0228 0.3087 0.1641 0.057 Uiso 1 1 calc R . . H22B H 1.0759 0.3172 0.2440 0.057 Uiso 1 1 calc R . . C23 C 1.1034(3) 0.4095(4) 0.1630(3) 0.0610(16) Uani 1 1 d . . . H23A H 1.1307 0.4467 0.2025 0.073 Uiso 1 1 calc R . . H23B H 1.1449 0.3756 0.1379 0.073 Uiso 1 1 calc R . . C24 C 1.0585(4) 0.4642(4) 0.1019(3) 0.0694(18) Uani 1 1 d . . . H24A H 1.0964 0.5047 0.0792 0.083 Uiso 1 1 calc R . . H24B H 1.0362 0.4274 0.0594 0.083 Uiso 1 1 calc R . . C25 C 0.9910(3) 0.5133(4) 0.1371(3) 0.0568(16) Uani 1 1 d . . . H25A H 0.9610 0.5454 0.0955 0.068 Uiso 1 1 calc R . . H25B H 1.0139 0.5548 0.1753 0.068 Uiso 1 1 calc R . . C26 C 0.9336(3) 0.4544(3) 0.1772(3) 0.0452(13) Uani 1 1 d . . . H26A H 0.9056 0.4175 0.1379 0.054 Uiso 1 1 calc R . . H26B H 0.8926 0.4888 0.2026 0.054 Uiso 1 1 calc R . . C27 C 1.0195(3) 0.1887(3) 0.5510(2) 0.0404(12) Uani 1 1 d . . . H27A H 0.9826 0.1458 0.5718 0.048 Uiso 1 1 calc R . . H27B H 1.0685 0.1894 0.5859 0.048 Uiso 1 1 calc R . . C28 C 0.9796(3) 0.2755(3) 0.5548(3) 0.0412(12) Uani 1 1 d . . . H28A H 0.9288 0.2738 0.5225 0.049 Uiso 1 1 calc R . . H28B H 0.9658 0.2863 0.6092 0.049 Uiso 1 1 calc R . . C29 C 1.0289(3) 0.3484(3) 0.5281(2) 0.0394(12) Uani 1 1 d . . . H29A H 1.0803 0.3492 0.5596 0.047 Uiso 1 1 calc R . . H29B H 1.0002 0.4020 0.5388 0.047 Uiso 1 1 calc R . . C30 C 1.2113(3) 0.2610(3) 0.4986(3) 0.0419(12) Uani 1 1 d . . . C31 C 1.1993(3) 0.3118(4) 0.3490(3) 0.0497(14) Uani 1 1 d . . . C32 C 1.1973(3) 0.1524(4) 0.3750(3) 0.0476(14) Uani 1 1 d . . . C35 C 0.5179(5) 0.2527(16) 0.4354(11) 0.092(4) Uani 0.435(6) 1 d PDU A 1 H35A H 0.5195 0.3093 0.4102 0.110 Uiso 0.435(6) 1 calc PR A 1 H35B H 0.5254 0.2087 0.3952 0.110 Uiso 0.435(6) 1 calc PR A 1 Cl3 Cl 0.4268(4) 0.2384(6) 0.4768(5) 0.151(3) Uani 0.435(6) 1 d PDU A 1 Cl4 Cl 0.5938(4) 0.2452(3) 0.5076(2) 0.097(2) Uani 0.435(6) 1 d PDU A 1 C35B C 0.4904(16) 0.251(3) 0.419(2) 0.094(4) Uani 0.325(9) 1 d PDU B 2 H35C H 0.5277 0.2043 0.4352 0.112 Uiso 0.325(9) 1 calc PR B 2 H35D H 0.5088 0.2770 0.3710 0.112 Uiso 0.325(9) 1 calc PR B 2 Cl3B Cl 0.3936(5) 0.2123(7) 0.4048(7) 0.104(3) Uani 0.325(9) 1 d PDU B 2 Cl4B Cl 0.4873(7) 0.3262(7) 0.4924(5) 0.119(3) Uani 0.325(9) 1 d PDU B 2 C35C C 0.481(2) 0.255(4) 0.4196(12) 0.097(4) Uani 0.240(9) 1 d PDU C 3 H35E H 0.5171 0.2252 0.3845 0.116 Uiso 0.240(9) 1 calc PR C 3 H35F H 0.4593 0.3061 0.3928 0.116 Uiso 0.240(9) 1 calc PR C 3 Cl3C Cl 0.4028(7) 0.1876(7) 0.4424(10) 0.086(4) Uani 0.240(9) 1 d PDU C 3 Cl4C Cl 0.5319(12) 0.2819(11) 0.5058(6) 0.114(4) Uani 0.240(9) 1 d PDU C 3 F1 F 0.6405(7) 0.2669(9) 0.2135(8) 0.095(3) Uani 0.57(2) 1 d PDU D 1 F2 F 0.6156(10) 0.1277(7) 0.2026(6) 0.105(3) Uani 0.57(2) 1 d PDU D 1 F3 F 0.5234(5) 0.2132(9) 0.2496(7) 0.075(3) Uani 0.57(2) 1 d PDU D 1 F4 F 0.6372(10) 0.1860(11) 0.3212(7) 0.063(3) Uani 0.57(2) 1 d PDU D 1 B1 B 0.6046(6) 0.1989(6) 0.2471(6) 0.060(2) Uani 0.57(2) 1 d PDU D 1 F1B F 0.5405(11) 0.2500(12) 0.2544(11) 0.097(4) Uani 0.43(2) 1 d PDU D 2 F2B F 0.6520(8) 0.2282(12) 0.1908(9) 0.080(4) Uani 0.43(2) 1 d PDU D 2 F3B F 0.5675(12) 0.1212(7) 0.2086(8) 0.087(4) Uani 0.43(2) 1 d PDU D 2 F4B F 0.6419(13) 0.1732(15) 0.3107(9) 0.066(4) Uani 0.43(2) 1 d PDU D 2 B1B B 0.6011(7) 0.1933(8) 0.2420(7) 0.062(3) Uani 0.43(2) 1 d PDU D 2 C34 C 0.3418(10) 0.1355(8) 0.1999(8) 0.081(3) Uani 0.75(3) 1 d PDU E 1 H34A H 0.3911 0.1678 0.2152 0.097 Uiso 0.75(3) 1 calc PR E 1 H34B H 0.3195 0.1123 0.2477 0.097 Uiso 0.75(3) 1 calc PR E 1 Cl1 Cl 0.2720(6) 0.2040(5) 0.1542(8) 0.137(2) Uani 0.75(3) 1 d PDU E 1 Cl2 Cl 0.3662(4) 0.0524(3) 0.1393(4) 0.0650(15) Uani 0.75(3) 1 d PDU E 1 C34B C 0.360(3) 0.142(2) 0.213(2) 0.078(5) Uani 0.25(3) 1 d PDU E 2 H34C H 0.4146 0.1664 0.2133 0.094 Uiso 0.25(3) 1 calc PR E 2 H34D H 0.3492 0.1246 0.2668 0.094 Uiso 0.25(3) 1 calc PR E 2 Cl1B Cl 0.2905(15) 0.2180(14) 0.1812(16) 0.104(5) Uani 0.25(3) 1 d PDU E 2 Cl2B Cl 0.3554(18) 0.0530(13) 0.1531(19) 0.108(6) Uani 0.25(3) 1 d PDU E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0218(3) 0.0385(4) 0.0260(3) -0.0002(3) -0.0007(2) -0.0009(3) Fe1 0.0245(4) 0.0481(4) 0.0337(4) 0.0016(3) 0.0000(3) -0.0024(3) P1 0.0237(7) 0.0412(7) 0.0319(7) -0.0040(6) -0.0003(5) -0.0003(6) P2 0.0243(7) 0.0435(8) 0.0286(7) 0.0024(6) -0.0018(5) -0.0015(6) S1 0.0258(7) 0.0423(7) 0.0336(6) 0.0028(6) -0.0016(5) 0.0002(5) S2 0.0310(7) 0.0403(7) 0.0339(6) -0.0006(6) -0.0038(5) -0.0024(5) O1 0.048(2) 0.072(3) 0.052(2) -0.004(2) -0.0164(19) 0.003(2) O2 0.054(3) 0.093(3) 0.080(3) 0.025(3) 0.018(2) -0.019(2) O3 0.049(3) 0.066(3) 0.065(3) -0.003(2) 0.019(2) 0.008(2) C1 0.026(3) 0.044(3) 0.043(3) -0.001(2) -0.004(2) 0.000(2) C2 0.034(3) 0.044(3) 0.047(3) -0.003(2) -0.006(2) -0.005(2) C3 0.034(3) 0.048(3) 0.062(3) 0.008(3) -0.006(3) -0.011(3) C4 0.037(3) 0.058(3) 0.052(3) 0.010(3) 0.000(3) -0.009(3) C5 0.041(3) 0.064(4) 0.039(3) 0.002(3) 0.006(2) -0.007(3) C6 0.031(3) 0.049(3) 0.039(3) -0.004(2) 0.004(2) -0.009(2) C7 0.040(3) 0.048(3) 0.041(3) -0.006(2) 0.007(2) -0.003(2) C8 0.056(4) 0.057(4) 0.056(4) -0.010(3) 0.007(3) 0.017(3) C9 0.069(5) 0.073(4) 0.082(5) -0.014(4) 0.013(4) 0.024(4) C10 0.069(5) 0.093(5) 0.091(5) -0.019(4) 0.018(4) 0.032(4) C11 0.108(6) 0.102(6) 0.062(4) 0.006(4) 0.044(4) 0.041(5) C12 0.085(5) 0.077(4) 0.058(4) 0.010(3) 0.036(4) 0.024(4) C13 0.025(3) 0.054(3) 0.034(3) -0.002(2) -0.006(2) 0.000(2) C14 0.032(3) 0.050(3) 0.028(2) 0.002(2) -0.008(2) -0.002(2) C15 0.023(3) 0.038(3) 0.033(3) 0.005(2) -0.001(2) 0.004(2) C16 0.030(3) 0.062(4) 0.075(4) -0.021(3) 0.018(3) -0.014(3) C17 0.035(3) 0.078(4) 0.074(4) -0.014(3) 0.016(3) -0.001(3) C18 0.040(3) 0.068(4) 0.057(4) -0.006(3) 0.018(3) 0.005(3) C19 0.047(3) 0.051(3) 0.069(4) -0.012(3) 0.010(3) 0.000(3) C20 0.032(3) 0.053(3) 0.055(3) -0.010(3) 0.004(2) 0.003(3) C21 0.029(3) 0.055(3) 0.025(3) 0.008(2) 0.000(2) -0.004(2) C22 0.041(3) 0.068(4) 0.035(3) 0.006(3) 0.009(2) -0.002(3) C23 0.041(3) 0.091(5) 0.052(4) 0.014(3) 0.014(3) 0.003(3) C24 0.060(4) 0.101(5) 0.048(4) 0.018(3) 0.015(3) -0.011(4) C25 0.046(3) 0.072(4) 0.052(3) 0.029(3) -0.003(3) -0.011(3) C26 0.039(3) 0.056(3) 0.040(3) 0.014(3) -0.004(2) -0.003(3) C27 0.037(3) 0.056(3) 0.029(3) 0.008(2) 0.005(2) 0.002(2) C28 0.041(3) 0.058(3) 0.025(3) 0.000(2) 0.003(2) 0.006(3) C29 0.036(3) 0.048(3) 0.034(3) -0.006(2) -0.002(2) 0.000(2) C30 0.032(3) 0.048(3) 0.046(3) 0.001(3) 0.002(2) 0.003(2) C31 0.033(3) 0.069(4) 0.047(3) 0.005(3) 0.003(3) -0.008(3) C32 0.033(3) 0.063(4) 0.047(3) 0.003(3) 0.007(2) -0.001(3) C35 0.094(6) 0.102(6) 0.082(6) -0.010(5) 0.030(6) -0.009(6) Cl3 0.105(4) 0.203(6) 0.149(5) 0.001(5) 0.045(4) -0.006(4) Cl4 0.119(4) 0.112(4) 0.060(2) 0.021(2) 0.012(3) 0.008(3) C35B 0.093(7) 0.106(6) 0.084(6) -0.007(5) 0.028(6) -0.012(6) Cl3B 0.059(4) 0.145(6) 0.110(6) -0.020(5) 0.020(4) -0.001(4) Cl4B 0.142(6) 0.115(6) 0.101(5) -0.045(4) 0.031(4) -0.030(5) C35C 0.094(7) 0.110(6) 0.089(6) -0.009(6) 0.028(6) -0.012(6) Cl3C 0.061(5) 0.089(6) 0.111(7) -0.010(5) 0.030(5) 0.003(4) Cl4C 0.135(7) 0.133(7) 0.074(5) -0.013(5) 0.010(5) -0.015(6) F1 0.079(6) 0.135(7) 0.069(7) 0.039(5) -0.016(4) -0.039(6) F2 0.113(8) 0.128(6) 0.073(4) -0.037(4) 0.004(6) 0.022(6) F3 0.036(3) 0.123(7) 0.066(5) 0.011(5) -0.007(3) -0.002(4) F4 0.046(5) 0.102(7) 0.039(4) 0.004(4) -0.006(4) -0.006(5) B1 0.045(4) 0.096(5) 0.038(4) 0.000(4) -0.004(4) -0.003(5) F1B 0.086(8) 0.129(9) 0.078(6) -0.003(7) 0.007(6) 0.050(7) F2B 0.047(5) 0.143(9) 0.049(6) 0.015(6) 0.003(4) -0.014(6) F3B 0.093(9) 0.101(6) 0.066(6) -0.005(5) -0.020(6) -0.027(6) F4B 0.048(7) 0.099(8) 0.051(6) 0.009(6) -0.014(5) -0.007(6) B1B 0.047(5) 0.097(6) 0.040(5) -0.002(5) -0.004(4) 0.000(5) C34 0.074(6) 0.105(5) 0.065(5) -0.002(5) 0.016(4) -0.006(5) Cl1 0.131(4) 0.129(3) 0.149(5) -0.031(4) -0.006(4) 0.056(3) Cl2 0.070(2) 0.072(2) 0.054(2) 0.0007(14) 0.0157(16) -0.0046(15) C34B 0.073(9) 0.097(8) 0.065(8) 0.002(7) 0.011(7) -0.006(7) Cl1B 0.104(7) 0.111(7) 0.099(8) -0.002(6) 0.030(6) 0.020(6) Cl2B 0.107(9) 0.116(8) 0.103(9) 0.013(6) 0.014(7) -0.008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 P1 2.1876(13) . ? Ni1 P2 2.1910(13) . ? Ni1 S2 2.2270(13) . ? Ni1 S1 2.2348(13) . ? Ni1 Fe1 2.8182(9) . ? Fe1 C32 1.790(6) . ? Fe1 C31 1.799(6) . ? Fe1 C30 1.833(5) . ? Fe1 S2 2.2880(14) . ? Fe1 S1 2.2960(13) . ? P1 C1 1.832(5) . ? P1 C13 1.836(4) . ? P1 C7 1.854(5) . ? P2 C14 1.833(4) . ? P2 C21 1.841(4) . ? P2 C15 1.851(4) . ? S1 C27 1.843(4) . ? S2 C29 1.833(4) . ? O1 C30 1.144(5) . ? O2 C31 1.135(5) . ? O3 C32 1.142(6) . ? C1 C2 1.527(6) . ? C1 C6 1.537(6) . ? C1 H1A 1.0000 . ? C2 C3 1.521(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.506(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.516(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.532(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.513(6) . ? C7 C12 1.522(7) . ? C7 H7A 1.0000 . ? C8 C9 1.521(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.522(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.500(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.534(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.533(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.515(6) . ? C15 C16 1.527(6) . ? C15 H15A 1.0000 . ? C16 C17 1.515(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.513(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.516(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.525(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.518(6) . ? C21 C26 1.537(6) . ? C21 H21A 1.0000 . ? C22 C23 1.529(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.525(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.515(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.522(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.520(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.496(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C35 Cl3 1.725(12) . ? C35 Cl4 1.732(13) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35B Cl4B 1.728(13) . ? C35B Cl3B 1.731(12) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C35C Cl4C 1.729(14) . ? C35C Cl3C 1.732(13) . ? C35C H35E 0.9900 . ? C35C H35F 0.9900 . ? F1 B1 1.367(6) . ? F2 B1 1.374(6) . ? F3 B1 1.375(6) . ? F4 B1 1.375(6) . ? F1B B1B 1.370(7) . ? F2B B1B 1.367(7) . ? F3B B1B 1.377(7) . ? F4B B1B 1.371(7) . ? C34 Cl2 1.732(7) . ? C34 Cl1 1.744(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34B Cl2B 1.732(9) . ? C34B Cl1B 1.735(9) . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? 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 P1 Ni1 P2 88.27(5) . . ? P1 Ni1 S2 176.45(5) . . ? P2 Ni1 S2 92.53(5) . . ? P1 Ni1 S1 92.10(5) . . ? P2 Ni1 S1 179.25(5) . . ? S2 Ni1 S1 87.15(5) . . ? P1 Ni1 Fe1 124.70(4) . . ? P2 Ni1 Fe1 127.70(4) . . ? S2 Ni1 Fe1 52.35(3) . . ? S1 Ni1 Fe1 52.52(3) . . ? C32 Fe1 C31 90.3(2) . . ? C32 Fe1 C30 97.6(2) . . ? C31 Fe1 C30 95.6(2) . . ? C32 Fe1 S2 161.28(17) . . ? C31 Fe1 S2 89.51(18) . . ? C30 Fe1 S2 101.04(15) . . ? C32 Fe1 S1 89.57(16) . . ? C31 Fe1 S1 160.05(16) . . ? C30 Fe1 S1 104.18(16) . . ? S2 Fe1 S1 84.28(5) . . ? C32 Fe1 Ni1 112.85(16) . . ? C31 Fe1 Ni1 111.75(16) . . ? C30 Fe1 Ni1 137.99(15) . . ? S2 Fe1 Ni1 50.42(3) . . ? S1 Fe1 Ni1 50.57(3) . . ? C1 P1 C13 106.0(2) . . ? C1 P1 C7 105.4(2) . . ? C13 P1 C7 104.4(2) . . ? C1 P1 Ni1 112.23(15) . . ? C13 P1 Ni1 108.93(16) . . ? C7 P1 Ni1 118.92(17) . . ? C14 P2 C21 105.7(2) . . ? C14 P2 C15 105.0(2) . . ? C21 P2 C15 106.6(2) . . ? C14 P2 Ni1 109.36(15) . . ? C21 P2 Ni1 112.96(15) . . ? C15 P2 Ni1 116.41(15) . . ? C27 S1 Ni1 104.69(15) . . ? C27 S1 Fe1 108.79(16) . . ? Ni1 S1 Fe1 76.91(4) . . ? C29 S2 Ni1 106.27(16) . . ? C29 S2 Fe1 106.30(16) . . ? Ni1 S2 Fe1 77.23(4) . . ? C2 C1 C6 110.6(4) . . ? C2 C1 P1 115.2(3) . . ? C6 C1 P1 110.7(3) . . ? C2 C1 H1A 106.6 . . ? C6 C1 H1A 106.6 . . ? P1 C1 H1A 106.6 . . ? C3 C2 C1 110.5(4) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 112.0(4) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 110.7(4) . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 110.2(4) . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C1 110.7(4) . . ? C5 C6 H6A 109.5 . . ? C1 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C12 110.3(4) . . ? C8 C7 P1 114.6(3) . . ? C12 C7 P1 112.5(4) . . ? C8 C7 H7A 106.3 . . ? C12 C7 H7A 106.3 . . ? P1 C7 H7A 106.3 . . ? C7 C8 C9 111.7(4) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C10 111.4(5) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 111.3(5) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 111.7(5) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C7 C12 C11 110.5(5) . . ? C7 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 P1 111.4(3) . . ? C14 C13 H13A 109.3 . . ? P1 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? P1 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C13 C14 P2 110.6(3) . . ? C13 C14 H14A 109.5 . . ? P2 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? P2 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C20 C15 C16 110.3(4) . . ? C20 C15 P2 114.7(3) . . ? C16 C15 P2 113.2(3) . . ? C20 C15 H15A 106.0 . . ? C16 C15 H15A 106.0 . . ? P2 C15 H15A 106.0 . . ? C17 C16 C15 111.2(4) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C16 112.1(5) . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C19 110.7(4) . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C18 C19 C20 112.8(4) . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C15 C20 C19 111.2(4) . . ? C15 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C15 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C26 110.7(4) . . ? C22 C21 P2 111.1(3) . . ? C26 C21 P2 114.1(3) . . ? C22 C21 H21A 106.8 . . ? C26 C21 H21A 106.8 . . ? P2 C21 H21A 106.8 . . ? C21 C22 C23 111.5(4) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 110.9(4) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 111.2(4) . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 111.6(5) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C21 111.3(4) . . ? C25 C26 H26A 109.4 . . ? C21 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C21 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 S1 115.8(3) . . ? C28 C27 H27A 108.3 . . ? S1 C27 H27A 108.3 . . ? C28 C27 H27B 108.3 . . ? S1 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? C29 C28 C27 115.2(4) . . ? C29 C28 H28A 108.5 . . ? C27 C28 H28A 108.5 . . ? C29 C28 H28B 108.5 . . ? C27 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C28 C29 S2 115.4(3) . . ? C28 C29 H29A 108.4 . . ? S2 C29 H29A 108.4 . . ? C28 C29 H29B 108.4 . . ? S2 C29 H29B 108.4 . . ? H29A C29 H29B 107.5 . . ? O1 C30 Fe1 176.9(5) . . ? O2 C31 Fe1 178.3(5) . . ? O3 C32 Fe1 179.7(5) . . ? Cl3 C35 Cl4 108.8(11) . . ? Cl3 C35 H35A 109.9 . . ? Cl4 C35 H35A 109.9 . . ? Cl3 C35 H35B 109.9 . . ? Cl4 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? Cl4B C35B Cl3B 106.6(11) . . ? Cl4B C35B H35C 110.4 . . ? Cl3B C35B H35C 110.4 . . ? Cl4B C35B H35D 110.4 . . ? Cl3B C35B H35D 110.4 . . ? H35C C35B H35D 108.6 . . ? Cl4C C35C Cl3C 107.5(12) . . ? Cl4C C35C H35E 110.2 . . ? Cl3C C35C H35E 110.2 . . ? Cl4C C35C H35F 110.2 . . ? Cl3C C35C H35F 110.2 . . ? H35E C35C H35F 108.5 . . ? F1 B1 F2 109.1(7) . . ? F1 B1 F3 109.8(7) . . ? F2 B1 F3 108.1(7) . . ? F1 B1 F4 110.2(8) . . ? F2 B1 F4 109.7(8) . . ? F3 B1 F4 109.9(8) . . ? F2B B1B F1B 109.1(8) . . ? F2B B1B F4B 110.5(9) . . ? F1B B1B F4B 110.7(9) . . ? F2B B1B F3B 108.3(8) . . ? F1B B1B F3B 108.2(8) . . ? F4B B1B F3B 110.0(9) . . ? Cl2 C34 Cl1 111.5(5) . . ? Cl2 C34 H34A 109.3 . . ? Cl1 C34 H34A 109.3 . . ? Cl2 C34 H34B 109.3 . . ? Cl1 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? Cl2B C34B Cl1B 111.1(9) . . ? Cl2B C34B H34C 109.4 . . ? Cl1B C34B H34C 109.4 . . ? Cl2B C34B H34D 109.4 . . ? Cl1B C34B H34D 109.4 . . ? H34C C34B H34D 108.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.996 _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_time ? _refine_diff_density_max 0.414 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.075 _publ_requested_category fm _publ_section_references ; 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). 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 a dichloromethane/pentane solution. ; _publ_section_exptl_refinement ; A structural model consisting of the host ion pair plus two disordered dichloromethane solvate molecules was developed. One of the dichloromethane molecules was disordered over two sites and the other was disordered over 3 sites. Like C-Cl bond distances and Cl-C-Cl bond angles were restrained to be similar (esd 0.01 and 0.02 respectively). The sump of the occupancy for the dichloromethane disordered over three sites was restrained to be 1. The counter ion was also disordered over two sites. Like B-F bond distances and F-B-F bond angles were restrained to be similar (esd 0.01 and 0.02 respectively). Similar displacement amplitudes (esd 0.01) were imposed on disordered sites overlapping by less than the sum of v an der Waals radii. Rigid-bond restraints (esd 0.01) were imposed on displacement parameters for atoms in the disordered counter ion. Atoms in both disordered dichloromethane solvate molecules were also restrained to be relatively isotropic (esd 0.01). H atoms were included as riding idealized contributors and their 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 'Acta Crystallographica E' _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. ; loop_ _publ_author_name _publ_author_address 'Gray, Danielle L.' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Fuller, Amy L.' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Gao, Yi-Gui' ; University of Illinois School of Chemical Sciences, Box 59-1 505 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 0.2240 0.00 1.00 0.00 0.2720 0.00 0.00 1.00 0.0430 0.00 0.00 -1.00 0.0840 -1.00 0.00 -1.00 0.0310 1.00 0.00 1.00 0.0270 1.00 1.00 -1.00 0.1780 data_bm63nasq _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H54 Fe Ni O2 P4 S2, 2(B F4), 4(CH2Cl2)' _chemical_formula_sum 'C61 H62 B2 Cl8 F8 Fe Ni O2 P4 S2' _chemical_formula_structural ? _chemical_formula_weight 1586.89 _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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 13.4045(3) _cell_length_b 14.1949(4) _cell_length_c 21.2882(5) _cell_angle_alpha 78.9850(10) _cell_angle_beta 75.0720(10) _cell_angle_gamma 64.2600(10) _cell_volume 3510.93(15) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9944 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.07 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.261 _exptl_crystal_size_mid 0.237 _exptl_crystal_size_min 0.108 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_crystal_id bm63nasq _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 0 -1) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.992 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.8252 _exptl_absorpt_correction_T_max 0.9247 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; One distinct cell was identified using SMART (Bruker, 2010). Seven 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 SAINT/SADABS (Bruker, 2005) to sort, merge, and scale the combined data. No decay correction was applied. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id bm63nasq _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52991 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.42 _reflns_number_total 12834 _reflns_number_gt 8867 _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 highest peaks in the final difference Fourier map were in the vicinity of atoms Nickel center; 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 some 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^)+(0.0558P)^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 12834 _refine_ls_number_parameters 786 _refine_ls_number_restraints 548 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _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 0.68635(4) 0.40998(3) 0.32216(2) 0.02362(12) Uani 1 1 d . . . Ni1 Ni 0.52162(3) 0.60100(3) 0.240033(18) 0.02395(11) Uani 1 1 d . . . P1 P 0.86002(7) 0.37977(7) 0.33456(4) 0.0280(2) Uani 1 1 d . . . P2 P 0.73378(7) 0.23516(6) 0.34343(4) 0.0272(2) Uani 1 1 d . . . P3 P 0.53728(8) 0.74180(7) 0.18429(4) 0.0300(2) Uani 1 1 d . . . P4 P 0.39994(7) 0.62274(6) 0.18178(4) 0.0275(2) Uani 1 1 d . . . S1 S 0.62261(7) 0.59189(6) 0.31056(4) 0.02734(19) Uani 1 1 d . . . S2 S 0.50741(7) 0.45732(6) 0.30098(4) 0.02633(19) Uani 1 1 d . . . O1 O 0.6115(2) 0.41142(18) 0.46462(11) 0.0421(6) Uani 1 1 d . . . O2 O 0.78856(19) 0.38289(17) 0.18267(11) 0.0370(6) Uani 1 1 d . . . C1 C 0.8597(3) 0.4379(3) 0.40363(15) 0.0317(8) Uani 1 1 d . . . C2 C 0.8738(3) 0.3800(3) 0.46361(16) 0.0392(9) Uani 1 1 d . . . H2A H 0.8889 0.3074 0.4681 0.047 Uiso 1 1 calc R . . C3 C 0.8659(3) 0.4277(3) 0.51706(18) 0.0511(11) Uani 1 1 d . . . H3A H 0.8773 0.3870 0.5576 0.061 Uiso 1 1 calc R . . C4 C 0.8421(4) 0.5321(4) 0.51176(19) 0.0546(11) Uani 1 1 d . . . H4A H 0.8358 0.5644 0.5486 0.065 Uiso 1 1 calc R . . C5 C 0.8270(4) 0.5909(3) 0.4526(2) 0.0555(11) Uani 1 1 d . . . H5A H 0.8111 0.6636 0.4488 0.067 Uiso 1 1 calc R . . C6 C 0.8349(3) 0.5449(3) 0.39882(18) 0.0427(9) Uani 1 1 d . . . H6A H 0.8234 0.5862 0.3585 0.051 Uiso 1 1 calc R . . C7 C 0.9497(3) 0.4211(3) 0.26531(15) 0.0329(8) Uani 1 1 d . . . C8 C 0.9045(3) 0.5164(3) 0.22848(18) 0.0484(10) Uani 1 1 d . . . H8A H 0.8271 0.5613 0.2410 0.058 Uiso 1 1 calc R . . C9 C 0.9697(4) 0.5470(4) 0.1743(2) 0.0589(12) Uani 1 1 d . . . H9A H 0.9373 0.6125 0.1500 0.071 Uiso 1 1 calc R . . C10 C 1.0810(4) 0.4830(4) 0.1555(2) 0.0604(12) Uani 1 1 d . . . H10A H 1.1258 0.5036 0.1179 0.073 Uiso 1 1 calc R . . C11 C 1.1281(3) 0.3891(4) 0.1909(2) 0.0590(12) Uani 1 1 d . . . H11A H 1.2056 0.3450 0.1777 0.071 Uiso 1 1 calc R . . C12 C 1.0632(3) 0.3575(3) 0.24610(19) 0.0477(10) Uani 1 1 d . . . H12A H 1.0968 0.2924 0.2705 0.057 Uiso 1 1 calc R . . C13 C 0.9354(3) 0.2368(3) 0.34867(16) 0.0344(8) Uani 1 1 d . . . H13A H 0.9733 0.2063 0.3063 0.041 Uiso 1 1 calc R . . H13B H 0.9939 0.2204 0.3742 0.041 Uiso 1 1 calc R . . C14 C 0.8518(3) 0.1883(3) 0.38595(16) 0.0326(8) Uani 1 1 d . . . H14A H 0.8235 0.2091 0.4312 0.039 Uiso 1 1 calc R . . H14B H 0.8901 0.1107 0.3879 0.039 Uiso 1 1 calc R . . C15 C 0.6245(3) 0.1985(2) 0.39778(16) 0.0325(8) Uani 1 1 d . . . C16 C 0.6241(4) 0.1719(3) 0.46419(18) 0.0512(10) Uani 1 1 d . . . H16A H 0.6826 0.1707 0.4822 0.061 Uiso 1 1 calc R . . C17 C 0.5370(5) 0.1470(4) 0.5039(2) 0.0695(13) Uani 1 1 d . . . H17A H 0.5360 0.1291 0.5494 0.083 Uiso 1 1 calc R . . C18 C 0.4537(4) 0.1481(4) 0.4785(3) 0.0734(14) Uani 1 1 d . . . H18A H 0.3956 0.1298 0.5061 0.088 Uiso 1 1 calc R . . C19 C 0.4526(4) 0.1759(3) 0.4124(2) 0.0635(12) Uani 1 1 d . . . H19A H 0.3929 0.1784 0.3949 0.076 Uiso 1 1 calc R . . C20 C 0.5383(3) 0.1997(3) 0.37267(19) 0.0473(10) Uani 1 1 d . . . H20A H 0.5386 0.2172 0.3273 0.057 Uiso 1 1 calc R . . C21 C 0.7819(3) 0.1568(2) 0.27487(15) 0.0284(7) Uani 1 1 d . . . C22 C 0.7220(3) 0.1910(3) 0.22410(16) 0.0374(8) Uani 1 1 d . . . H22A H 0.6565 0.2551 0.2256 0.045 Uiso 1 1 calc R . . C23 C 0.7579(3) 0.1315(3) 0.17142(18) 0.0468(10) Uani 1 1 d . . . H23A H 0.7176 0.1558 0.1368 0.056 Uiso 1 1 calc R . . C24 C 0.8517(4) 0.0374(3) 0.16913(19) 0.0511(10) Uani 1 1 d . . . H24A H 0.8757 -0.0035 0.1333 0.061 Uiso 1 1 calc R . . C25 C 0.9100(3) 0.0035(3) 0.21893(19) 0.0516(11) Uani 1 1 d . . . H25A H 0.9746 -0.0613 0.2174 0.062 Uiso 1 1 calc R . . C26 C 0.8768(3) 0.0618(3) 0.27151(17) 0.0397(9) Uani 1 1 d . . . H26A H 0.9189 0.0370 0.3054 0.048 Uiso 1 1 calc R . . C27 C 0.6385(3) 0.4121(2) 0.40924(16) 0.0295(7) Uani 1 1 d . . . C28 C 0.7460(3) 0.3957(2) 0.23585(16) 0.0278(7) Uani 1 1 d . . . C29 C 0.5032(3) 0.6428(3) 0.37884(15) 0.0336(8) Uani 1 1 d . . . H29A H 0.5282 0.6064 0.4201 0.040 Uiso 1 1 calc R . . H29B H 0.4841 0.7183 0.3794 0.040 Uiso 1 1 calc R . . C30 C 0.3964(3) 0.6306(3) 0.37738(16) 0.0364(8) Uani 1 1 d . . . H30A H 0.3407 0.6569 0.4176 0.044 Uiso 1 1 calc R . . H30B H 0.3646 0.6773 0.3401 0.044 Uiso 1 1 calc R . . C31 C 0.4056(3) 0.5220(3) 0.37210(15) 0.0351(8) Uani 1 1 d . . . H31A H 0.3302 0.5274 0.3703 0.042 Uiso 1 1 calc R . . H31B H 0.4275 0.4769 0.4122 0.042 Uiso 1 1 calc R . . C32 C 0.5613(3) 0.8252(3) 0.22859(16) 0.0349(8) Uani 1 1 d . . . C33 C 0.6690(4) 0.8212(3) 0.2224(2) 0.0512(10) Uani 1 1 d . . . H33A H 0.7306 0.7785 0.1923 0.061 Uiso 1 1 calc R . . C34 C 0.6858(4) 0.8799(4) 0.2607(2) 0.0671(13) Uani 1 1 d . . . H34A H 0.7590 0.8780 0.2562 0.080 Uiso 1 1 calc R . . C35 C 0.5982(5) 0.9401(4) 0.3047(2) 0.0699(15) Uani 1 1 d . . . H35A H 0.6114 0.9786 0.3313 0.084 Uiso 1 1 calc R . . C36 C 0.4922(4) 0.9460(3) 0.31118(19) 0.0561(12) Uani 1 1 d . . . H36A H 0.4316 0.9899 0.3412 0.067 Uiso 1 1 calc R . . C37 C 0.4723(4) 0.8874(3) 0.27366(17) 0.0464(10) Uani 1 1 d . . . H37A H 0.3986 0.8901 0.2789 0.056 Uiso 1 1 calc R . . C38 C 0.6479(3) 0.7145(3) 0.11163(15) 0.0333(8) Uani 1 1 d . . . C39 C 0.6674(4) 0.7947(3) 0.0693(2) 0.0669(14) Uani 1 1 d . . . H39A H 0.6205 0.8657 0.0775 0.080 Uiso 1 1 calc R . . C40 C 0.7546(5) 0.7721(4) 0.0154(2) 0.0792(16) Uani 1 1 d . . . H40A H 0.7677 0.8276 -0.0131 0.095 Uiso 1 1 calc R . . C41 C 0.8223(4) 0.6697(3) 0.00282(19) 0.0559(11) Uani 1 1 d . . . H41A H 0.8816 0.6542 -0.0346 0.067 Uiso 1 1 calc R . . C42 C 0.8042(3) 0.5912(3) 0.04384(19) 0.0500(10) Uani 1 1 d . . . H42A H 0.8513 0.5203 0.0355 0.060 Uiso 1 1 calc R . . C43 C 0.7169(3) 0.6134(3) 0.09832(17) 0.0412(9) Uani 1 1 d . . . H43A H 0.7052 0.5572 0.1268 0.049 Uiso 1 1 calc R . . C44 C 0.4046(3) 0.8200(3) 0.15617(17) 0.0364(8) Uani 1 1 d . . . H44A H 0.3445 0.8547 0.1929 0.044 Uiso 1 1 calc R . . H44B H 0.4136 0.8750 0.1217 0.044 Uiso 1 1 calc R . . C45 C 0.3728(3) 0.7470(2) 0.12932(15) 0.0345(8) Uani 1 1 d . . . H45A H 0.4174 0.7323 0.0846 0.041 Uiso 1 1 calc R . . H45B H 0.2918 0.7817 0.1268 0.041 Uiso 1 1 calc R . . C46 C 0.2652(3) 0.6352(3) 0.23489(15) 0.0307(8) Uani 1 1 d . . . C47 C 0.2380(3) 0.5485(3) 0.25349(17) 0.0421(9) Uani 1 1 d . . . H47A H 0.2891 0.4824 0.2379 0.051 Uiso 1 1 calc R . . C48 C 0.1357(4) 0.5591(4) 0.29500(19) 0.0557(11) Uani 1 1 d . . . H48A H 0.1162 0.5003 0.3073 0.067 Uiso 1 1 calc R . . C49 C 0.0625(3) 0.6545(4) 0.31845(19) 0.0545(11) Uani 1 1 d . . . H49A H -0.0077 0.6616 0.3464 0.065 Uiso 1 1 calc R . . C50 C 0.0905(3) 0.7390(4) 0.30163(19) 0.0551(11) Uani 1 1 d . . . H50A H 0.0406 0.8040 0.3190 0.066 Uiso 1 1 calc R . . C51 C 0.1913(3) 0.7308(3) 0.25938(17) 0.0426(9) Uani 1 1 d . . . H51A H 0.2097 0.7902 0.2473 0.051 Uiso 1 1 calc R . . C52 C 0.4328(3) 0.5238(2) 0.12854(14) 0.0282(7) Uani 1 1 d . . . C53 C 0.3515(3) 0.5288(3) 0.09682(16) 0.0393(9) Uani 1 1 d . . . H53A H 0.2781 0.5838 0.1033 0.047 Uiso 1 1 calc R . . C54 C 0.3788(3) 0.4528(3) 0.05580(17) 0.0467(10) Uani 1 1 d . . . H54A H 0.3240 0.4571 0.0334 0.056 Uiso 1 1 calc R . . C55 C 0.4824(4) 0.3724(3) 0.04696(17) 0.0482(10) Uani 1 1 d . . . H55A H 0.4982 0.3193 0.0201 0.058 Uiso 1 1 calc R . . C56 C 0.5647(3) 0.3672(3) 0.07653(17) 0.0454(10) Uani 1 1 d . . . H56A H 0.6383 0.3128 0.0685 0.054 Uiso 1 1 calc R . . C57 C 0.5392(3) 0.4425(3) 0.11833(16) 0.0372(8) Uani 1 1 d . . . H57A H 0.5951 0.4381 0.1400 0.045 Uiso 1 1 calc R . . B1 B 0.7465(9) 0.0479(9) 0.0046(5) 0.056(3) Uani 0.51(2) 1 d PDU A 1 F1 F 0.7636(13) -0.0218(7) 0.0594(6) 0.069(3) Uani 0.51(2) 1 d PDU A 1 F2 F 0.8487(10) 0.0234(11) -0.0392(8) 0.093(3) Uani 0.51(2) 1 d PDU A 1 F3 F 0.6696(13) 0.0396(16) -0.0242(7) 0.070(4) Uani 0.51(2) 1 d PDU A 1 F4 F 0.7084(16) 0.1489(8) 0.0208(8) 0.069(3) Uani 0.51(2) 1 d PDU A 1 B1B B 0.7351(10) 0.0451(9) 0.0098(5) 0.057(3) Uani 0.49(2) 1 d PDU A 2 F1B F 0.7075(16) 0.0034(11) 0.0725(4) 0.081(3) Uani 0.49(2) 1 d PDU A 2 F2B F 0.8506(9) -0.0015(9) -0.0115(8) 0.086(3) Uani 0.49(2) 1 d PDU A 2 F3B F 0.6832(12) 0.0251(16) -0.0314(7) 0.064(3) Uani 0.49(2) 1 d PDU A 2 F4B F 0.6996(17) 0.1519(8) 0.0101(9) 0.071(4) Uani 0.49(2) 1 d PDU A 2 B2 B 0.1556(7) 0.9091(8) 0.4021(5) 0.064(4) Uani 0.419(7) 1 d PDU B 1 F5 F 0.0586(5) 0.9411(7) 0.3803(4) 0.076(2) Uani 0.419(7) 1 d PDU B 1 F6 F 0.1583(12) 0.9948(8) 0.4192(5) 0.151(4) Uani 0.419(7) 1 d PDU B 1 F7 F 0.2460(7) 0.8710(9) 0.3530(5) 0.082(3) Uani 0.419(7) 1 d PDU B 1 F8 F 0.1636(12) 0.8389(10) 0.4557(5) 0.098(4) Uani 0.419(7) 1 d PDU B 1 B2B B 0.1664(6) 0.9017(5) 0.4031(4) 0.057(3) Uani 0.581(7) 1 d PDU B 2 F5B F 0.0729(5) 0.9915(5) 0.4050(4) 0.103(2) Uani 0.581(7) 1 d PDU B 2 F6B F 0.2513(5) 0.9180(6) 0.4167(3) 0.118(2) Uani 0.581(7) 1 d PDU B 2 F7B F 0.2093(7) 0.8690(7) 0.3418(3) 0.093(3) Uani 0.581(7) 1 d PDU B 2 F8B F 0.1490(8) 0.8199(6) 0.4424(4) 0.098(3) Uani 0.581(7) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0236(3) 0.0251(2) 0.0203(2) -0.00228(18) -0.00378(19) -0.0084(2) Ni1 0.0255(2) 0.0245(2) 0.0209(2) -0.00196(16) -0.00438(17) -0.00939(18) P1 0.0245(5) 0.0329(5) 0.0260(4) -0.0050(4) -0.0055(4) -0.0099(4) P2 0.0297(5) 0.0248(4) 0.0247(4) -0.0014(3) -0.0060(4) -0.0088(4) P3 0.0367(5) 0.0268(5) 0.0268(4) -0.0008(4) -0.0062(4) -0.0139(4) P4 0.0283(5) 0.0289(5) 0.0243(4) -0.0034(3) -0.0063(4) -0.0097(4) S1 0.0298(5) 0.0255(4) 0.0273(4) -0.0029(3) -0.0074(4) -0.0106(4) S2 0.0254(4) 0.0274(4) 0.0258(4) -0.0011(3) -0.0051(3) -0.0110(4) O1 0.0460(16) 0.0473(15) 0.0238(13) -0.0021(11) -0.0020(11) -0.0138(12) O2 0.0404(15) 0.0393(14) 0.0230(13) -0.0046(10) -0.0008(11) -0.0108(11) C1 0.0255(19) 0.045(2) 0.0269(17) -0.0090(15) -0.0006(15) -0.0163(16) C2 0.042(2) 0.046(2) 0.0308(19) -0.0049(16) -0.0086(17) -0.0178(18) C3 0.059(3) 0.074(3) 0.031(2) -0.0062(19) -0.0130(19) -0.034(2) C4 0.063(3) 0.072(3) 0.044(2) -0.027(2) 0.001(2) -0.038(2) C5 0.065(3) 0.053(3) 0.059(3) -0.020(2) -0.008(2) -0.029(2) C6 0.053(2) 0.041(2) 0.039(2) -0.0036(17) -0.0095(18) -0.0236(19) C7 0.028(2) 0.048(2) 0.0290(18) -0.0129(16) 0.0008(15) -0.0211(17) C8 0.030(2) 0.068(3) 0.044(2) 0.004(2) -0.0021(18) -0.023(2) C9 0.048(3) 0.083(3) 0.046(2) 0.011(2) -0.004(2) -0.037(3) C10 0.065(3) 0.095(4) 0.040(2) -0.016(2) 0.007(2) -0.055(3) C11 0.034(2) 0.084(3) 0.061(3) -0.033(3) 0.020(2) -0.031(2) C12 0.035(2) 0.057(3) 0.051(2) -0.021(2) 0.0017(19) -0.017(2) C13 0.0276(19) 0.036(2) 0.0376(19) -0.0080(15) -0.0144(16) -0.0052(16) C14 0.033(2) 0.0276(18) 0.0316(18) -0.0028(14) -0.0097(15) -0.0048(15) C15 0.038(2) 0.0218(17) 0.0328(19) -0.0044(14) 0.0013(16) -0.0115(15) C16 0.066(3) 0.054(3) 0.033(2) -0.0035(18) 0.002(2) -0.030(2) C17 0.094(4) 0.072(3) 0.041(2) 0.000(2) 0.007(3) -0.044(3) C18 0.073(4) 0.077(3) 0.075(3) -0.012(3) 0.022(3) -0.052(3) C19 0.058(3) 0.068(3) 0.066(3) -0.006(2) 0.005(2) -0.037(3) C20 0.043(2) 0.055(3) 0.048(2) -0.0075(19) 0.0008(19) -0.028(2) C21 0.0319(19) 0.0243(17) 0.0294(17) -0.0015(14) -0.0054(15) -0.0124(15) C22 0.040(2) 0.033(2) 0.039(2) -0.0033(16) -0.0105(17) -0.0124(17) C23 0.065(3) 0.043(2) 0.040(2) -0.0036(18) -0.021(2) -0.023(2) C24 0.068(3) 0.042(2) 0.045(2) -0.0173(19) -0.010(2) -0.018(2) C25 0.057(3) 0.035(2) 0.053(2) -0.0119(19) -0.012(2) -0.0054(19) C26 0.048(2) 0.031(2) 0.035(2) -0.0033(16) -0.0103(17) -0.0097(18) C27 0.0272(19) 0.0246(17) 0.032(2) -0.0007(14) -0.0083(15) -0.0052(15) C28 0.0256(18) 0.0226(17) 0.032(2) -0.0020(14) -0.0074(16) -0.0064(14) C29 0.041(2) 0.0281(18) 0.0265(17) -0.0075(14) -0.0057(16) -0.0082(16) C30 0.034(2) 0.037(2) 0.0265(18) -0.0072(15) -0.0010(15) -0.0046(16) C31 0.0253(19) 0.049(2) 0.0245(17) -0.0022(15) 0.0006(15) -0.0126(17) C32 0.050(2) 0.0275(18) 0.0333(19) 0.0019(15) -0.0145(18) -0.0192(17) C33 0.053(3) 0.049(2) 0.061(3) -0.006(2) -0.014(2) -0.027(2) C34 0.074(3) 0.067(3) 0.084(3) -0.002(3) -0.030(3) -0.045(3) C35 0.121(5) 0.055(3) 0.058(3) -0.002(2) -0.039(3) -0.048(3) C36 0.089(4) 0.039(2) 0.041(2) -0.0061(18) -0.021(2) -0.021(2) C37 0.064(3) 0.038(2) 0.037(2) -0.0025(17) -0.013(2) -0.018(2) C38 0.039(2) 0.035(2) 0.0268(18) -0.0047(15) -0.0016(16) -0.0178(17) C39 0.094(4) 0.029(2) 0.052(3) -0.0017(19) 0.016(3) -0.020(2) C40 0.117(4) 0.060(3) 0.046(3) 0.000(2) 0.024(3) -0.047(3) C41 0.066(3) 0.065(3) 0.037(2) -0.012(2) 0.010(2) -0.035(2) C42 0.048(3) 0.044(2) 0.054(3) -0.0132(19) 0.002(2) -0.018(2) C43 0.042(2) 0.036(2) 0.039(2) 0.0008(16) -0.0026(18) -0.0143(18) C44 0.042(2) 0.0279(18) 0.0346(19) 0.0005(15) -0.0105(17) -0.0102(16) C45 0.041(2) 0.0337(19) 0.0264(17) -0.0013(14) -0.0109(16) -0.0111(17) C46 0.0263(19) 0.037(2) 0.0260(17) -0.0050(15) -0.0084(15) -0.0080(16) C47 0.044(2) 0.050(2) 0.038(2) -0.0107(17) -0.0027(18) -0.0245(19) C48 0.055(3) 0.091(3) 0.040(2) -0.016(2) 0.002(2) -0.051(3) C49 0.032(2) 0.090(3) 0.038(2) -0.018(2) 0.0054(18) -0.024(2) C50 0.038(2) 0.067(3) 0.044(2) -0.019(2) 0.000(2) -0.005(2) C51 0.039(2) 0.049(2) 0.033(2) -0.0089(17) -0.0037(18) -0.0118(19) C52 0.0325(19) 0.0285(18) 0.0233(16) -0.0045(13) -0.0028(15) -0.0126(16) C53 0.031(2) 0.051(2) 0.035(2) -0.0161(17) -0.0053(16) -0.0102(18) C54 0.051(3) 0.067(3) 0.035(2) -0.0107(19) -0.0102(19) -0.032(2) C55 0.071(3) 0.051(2) 0.0278(19) -0.0128(17) 0.004(2) -0.033(2) C56 0.049(2) 0.035(2) 0.038(2) -0.0107(17) 0.0016(19) -0.0072(18) C57 0.040(2) 0.036(2) 0.0319(19) -0.0049(16) -0.0085(17) -0.0116(18) B1 0.077(5) 0.045(4) 0.052(5) -0.008(4) -0.027(4) -0.020(4) F1 0.086(6) 0.055(4) 0.068(5) 0.008(3) -0.049(4) -0.016(4) F2 0.092(5) 0.091(6) 0.094(6) -0.041(5) 0.005(4) -0.036(4) F3 0.081(5) 0.069(6) 0.064(6) -0.005(5) -0.031(4) -0.025(5) F4 0.103(5) 0.043(4) 0.055(5) -0.018(3) -0.031(4) -0.010(4) B1B 0.077(5) 0.047(5) 0.049(5) -0.010(4) -0.030(4) -0.017(4) F1B 0.113(7) 0.083(5) 0.056(4) -0.006(3) -0.026(4) -0.042(5) F2B 0.068(4) 0.071(5) 0.097(6) -0.016(4) -0.031(4) 0.003(3) F3B 0.083(6) 0.060(5) 0.050(4) -0.020(4) -0.030(4) -0.014(4) F4B 0.102(6) 0.041(4) 0.060(6) -0.018(3) -0.027(5) -0.009(4) B2 0.072(5) 0.058(5) 0.065(5) -0.005(5) -0.021(5) -0.024(5) F5 0.065(4) 0.080(5) 0.083(4) 0.008(3) -0.043(3) -0.020(3) F6 0.162(7) 0.118(6) 0.185(6) -0.059(5) -0.039(6) -0.047(5) F7 0.047(4) 0.086(5) 0.077(5) 0.022(4) 0.011(4) -0.019(4) F8 0.102(6) 0.105(6) 0.050(4) 0.023(4) -0.033(4) -0.011(5) B2B 0.070(5) 0.052(4) 0.055(4) -0.006(4) -0.024(4) -0.024(4) F5B 0.062(3) 0.067(4) 0.135(5) 0.010(3) -0.026(3) 0.012(3) F6B 0.098(4) 0.138(5) 0.135(4) -0.026(4) -0.047(3) -0.044(4) F7B 0.131(6) 0.083(4) 0.061(3) -0.016(3) -0.024(4) -0.033(4) F8B 0.089(4) 0.068(4) 0.089(5) 0.021(3) 0.018(4) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C27 1.800(3) . ? Fe1 C28 1.817(3) . ? Fe1 P1 2.2536(9) . ? Fe1 P2 2.2618(9) . ? Fe1 S1 2.3254(9) . ? Fe1 S2 2.3345(9) . ? Ni1 P4 2.1799(9) . ? Ni1 P3 2.1855(9) . ? Ni1 S1 2.2190(8) . ? Ni1 S2 2.2535(9) . ? P1 C1 1.817(3) . ? P1 C7 1.825(3) . ? P1 C13 1.836(3) . ? P2 C21 1.816(3) . ? P2 C15 1.821(3) . ? P2 C14 1.833(3) . ? P3 C38 1.814(3) . ? P3 C32 1.819(3) . ? P3 C44 1.825(3) . ? P4 C52 1.806(3) . ? P4 C46 1.821(3) . ? P4 C45 1.841(3) . ? S1 C29 1.842(3) . ? S2 C31 1.837(3) . ? O1 C27 1.140(4) . ? O2 C28 1.139(4) . ? C1 C2 1.390(4) . ? C1 C6 1.395(5) . ? C2 C3 1.391(5) . ? C2 H2A 0.9500 . ? C3 C4 1.363(5) . ? C3 H3A 0.9500 . ? C4 C5 1.381(5) . ? C4 H4A 0.9500 . ? C5 C6 1.383(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.387(5) . ? C7 C8 1.392(5) . ? C8 C9 1.380(5) . ? C8 H8A 0.9500 . ? C9 C10 1.365(6) . ? C9 H9A 0.9500 . ? C10 C11 1.368(6) . ? C10 H10A 0.9500 . ? C11 C12 1.397(5) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.536(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.385(5) . ? C15 C16 1.391(5) . ? C16 C17 1.392(6) . ? C16 H16A 0.9500 . ? C17 C18 1.355(7) . ? C17 H17A 0.9500 . ? C18 C19 1.389(6) . ? C18 H18A 0.9500 . ? C19 C20 1.369(5) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C26 1.394(4) . ? C21 C22 1.399(4) . ? C22 C23 1.390(5) . ? C22 H22A 0.9500 . ? C23 C24 1.379(5) . ? C23 H23A 0.9500 . ? C24 C25 1.368(5) . ? C24 H24A 0.9500 . ? C25 C26 1.383(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C29 C30 1.524(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.516(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.393(5) . ? C32 C37 1.394(5) . ? C33 C34 1.388(6) . ? C33 H33A 0.9500 . ? C34 C35 1.361(7) . ? C34 H34A 0.9500 . ? C35 C36 1.359(6) . ? C35 H35A 0.9500 . ? C36 C37 1.398(5) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 C43 1.365(5) . ? C38 C39 1.386(5) . ? C39 C40 1.382(6) . ? C39 H39A 0.9500 . ? C40 C41 1.374(6) . ? C40 H40A 0.9500 . ? C41 C42 1.347(5) . ? C41 H41A 0.9500 . ? C42 C43 1.390(5) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 C45 1.523(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C51 1.390(5) . ? C46 C47 1.391(5) . ? C47 C48 1.390(5) . ? C47 H47A 0.9500 . ? C48 C49 1.379(6) . ? C48 H48A 0.9500 . ? C49 C50 1.366(6) . ? C49 H49A 0.9500 . ? C50 C51 1.388(5) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 C57 1.386(4) . ? C52 C53 1.394(4) . ? C53 C54 1.382(5) . ? C53 H53A 0.9500 . ? C54 C55 1.355(5) . ? C54 H54A 0.9500 . ? C55 C56 1.374(5) . ? C55 H55A 0.9500 . ? C56 C57 1.393(5) . ? C56 H56A 0.9500 . ? C57 H57A 0.9500 . ? B1 F1 1.376(6) . ? B1 F4 1.377(6) . ? B1 F3 1.383(6) . ? B1 F2 1.385(7) . ? B1B F4B 1.378(6) . ? B1B F1B 1.378(6) . ? B1B F2B 1.380(7) . ? B1B F3B 1.384(6) . ? B2 F5 1.352(7) . ? B2 F6 1.353(7) . ? B2 F8 1.357(7) . ? B2 F7 1.359(7) . ? B2B F5B 1.343(6) . ? B2B F6B 1.363(6) . ? B2B F7B 1.364(6) . ? B2B F8B 1.365(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Fe1 C28 174.38(14) . . ? C27 Fe1 P1 89.26(10) . . ? C28 Fe1 P1 87.16(10) . . ? C27 Fe1 P2 84.23(10) . . ? C28 Fe1 P2 91.29(10) . . ? P1 Fe1 P2 87.88(3) . . ? C27 Fe1 S1 90.23(10) . . ? C28 Fe1 S1 94.39(10) . . ? P1 Fe1 S1 94.90(3) . . ? P2 Fe1 S1 173.78(4) . . ? C27 Fe1 S2 94.54(10) . . ? C28 Fe1 S2 89.43(10) . . ? P1 Fe1 S2 173.53(4) . . ? P2 Fe1 S2 97.70(3) . . ? S1 Fe1 S2 79.87(3) . . ? P4 Ni1 P3 87.03(3) . . ? P4 Ni1 S1 171.23(4) . . ? P3 Ni1 S1 93.82(3) . . ? P4 Ni1 S2 95.06(3) . . ? P3 Ni1 S2 177.64(4) . . ? S1 Ni1 S2 83.95(3) . . ? C1 P1 C7 105.21(15) . . ? C1 P1 C13 107.68(15) . . ? C7 P1 C13 105.68(16) . . ? C1 P1 Fe1 113.93(11) . . ? C7 P1 Fe1 117.13(11) . . ? C13 P1 Fe1 106.61(11) . . ? C21 P2 C15 104.88(15) . . ? C21 P2 C14 106.82(15) . . ? C15 P2 C14 106.85(15) . . ? C21 P2 Fe1 118.19(10) . . ? C15 P2 Fe1 115.07(11) . . ? C14 P2 Fe1 104.28(11) . . ? C38 P3 C32 106.20(16) . . ? C38 P3 C44 106.33(16) . . ? C32 P3 C44 107.46(16) . . ? C38 P3 Ni1 113.55(11) . . ? C32 P3 Ni1 116.06(11) . . ? C44 P3 Ni1 106.69(12) . . ? C52 P4 C46 105.47(15) . . ? C52 P4 C45 105.97(14) . . ? C46 P4 C45 106.42(15) . . ? C52 P4 Ni1 118.99(11) . . ? C46 P4 Ni1 109.98(10) . . ? C45 P4 Ni1 109.29(11) . . ? C29 S1 Ni1 96.98(11) . . ? C29 S1 Fe1 107.32(11) . . ? Ni1 S1 Fe1 89.61(3) . . ? C31 S2 Ni1 98.23(11) . . ? C31 S2 Fe1 106.13(11) . . ? Ni1 S2 Fe1 88.55(3) . . ? C2 C1 C6 118.6(3) . . ? C2 C1 P1 121.2(3) . . ? C6 C1 P1 120.0(3) . . ? C1 C2 C3 120.4(4) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C4 C3 C2 120.6(4) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? C12 C7 C8 117.9(3) . . ? C12 C7 P1 121.5(3) . . ? C8 C7 P1 120.5(3) . . ? C9 C8 C7 121.4(4) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C7 C12 C11 120.0(4) . . ? C7 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 P1 109.9(2) . . ? C14 C13 H13A 109.7 . . ? P1 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? P1 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C13 C14 P2 108.7(2) . . ? C13 C14 H14A 109.9 . . ? P2 C14 H14A 109.9 . . ? C13 C14 H14B 109.9 . . ? P2 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C20 C15 C16 119.3(3) . . ? C20 C15 P2 119.2(3) . . ? C16 C15 P2 121.4(3) . . ? C15 C16 C17 119.2(4) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C19 C18 119.4(4) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C19 C20 C15 120.9(4) . . ? C19 C20 H20A 119.5 . . ? C15 C20 H20A 119.5 . . ? C26 C21 C22 118.4(3) . . ? C26 C21 P2 121.8(2) . . ? C22 C21 P2 119.8(2) . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 119.4(4) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? C24 C25 C26 121.3(4) . . ? C24 C25 H25A 119.3 . . ? C26 C25 H25A 119.3 . . ? C25 C26 C21 120.1(3) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? O1 C27 Fe1 177.9(3) . . ? O2 C28 Fe1 176.4(3) . . ? C30 C29 S1 115.7(2) . . ? C30 C29 H29A 108.4 . . ? S1 C29 H29A 108.4 . . ? C30 C29 H29B 108.4 . . ? S1 C29 H29B 108.4 . . ? H29A C29 H29B 107.4 . . ? C31 C30 C29 118.3(3) . . ? C31 C30 H30A 107.7 . . ? C29 C30 H30A 107.7 . . ? C31 C30 H30B 107.7 . . ? C29 C30 H30B 107.7 . . ? H30A C30 H30B 107.1 . . ? C30 C31 S2 114.8(2) . . ? C30 C31 H31A 108.6 . . ? S2 C31 H31A 108.6 . . ? C30 C31 H31B 108.6 . . ? S2 C31 H31B 108.6 . . ? H31A C31 H31B 107.5 . . ? C33 C32 C37 119.3(3) . . ? C33 C32 P3 121.1(3) . . ? C37 C32 P3 119.4(3) . . ? C34 C33 C32 119.5(4) . . ? C34 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? C35 C34 C33 120.5(4) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C36 C35 C34 120.9(4) . . ? C36 C35 H35A 119.5 . . ? C34 C35 H35A 119.5 . . ? C35 C36 C37 120.1(4) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C32 C37 C36 119.6(4) . . ? C32 C37 H37A 120.2 . . ? C36 C37 H37A 120.2 . . ? C43 C38 C39 118.1(3) . . ? C43 C38 P3 120.5(3) . . ? C39 C38 P3 121.4(3) . . ? C40 C39 C38 120.5(4) . . ? C40 C39 H39A 119.7 . . ? C38 C39 H39A 119.7 . . ? C41 C40 C39 120.2(4) . . ? C41 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? C42 C41 C40 119.6(4) . . ? C42 C41 H41A 120.2 . . ? C40 C41 H41A 120.2 . . ? C41 C42 C43 120.4(4) . . ? C41 C42 H42A 119.8 . . ? C43 C42 H42A 119.8 . . ? C38 C43 C42 121.1(3) . . ? C38 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C45 C44 P3 108.2(2) . . ? C45 C44 H44A 110.1 . . ? P3 C44 H44A 110.1 . . ? C45 C44 H44B 110.1 . . ? P3 C44 H44B 110.1 . . ? H44A C44 H44B 108.4 . . ? C44 C45 P4 110.7(2) . . ? C44 C45 H45A 109.5 . . ? P4 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? P4 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C51 C46 C47 119.7(3) . . ? C51 C46 P4 119.8(3) . . ? C47 C46 P4 120.4(3) . . ? C48 C47 C46 119.6(4) . . ? C48 C47 H47A 120.2 . . ? C46 C47 H47A 120.2 . . ? C49 C48 C47 120.2(4) . . ? C49 C48 H48A 119.9 . . ? C47 C48 H48A 119.9 . . ? C50 C49 C48 120.2(4) . . ? C50 C49 H49A 119.9 . . ? C48 C49 H49A 119.9 . . ? C49 C50 C51 120.6(4) . . ? C49 C50 H50A 119.7 . . ? C51 C50 H50A 119.7 . . ? C50 C51 C46 119.6(4) . . ? C50 C51 H51A 120.2 . . ? C46 C51 H51A 120.2 . . ? C57 C52 C53 119.1(3) . . ? C57 C52 P4 120.5(2) . . ? C53 C52 P4 120.4(3) . . ? C54 C53 C52 119.4(3) . . ? C54 C53 H53A 120.3 . . ? C52 C53 H53A 120.3 . . ? C55 C54 C53 121.2(3) . . ? C55 C54 H54A 119.4 . . ? C53 C54 H54A 119.4 . . ? C54 C55 C56 120.4(4) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C55 C56 C57 119.4(4) . . ? C55 C56 H56A 120.3 . . ? C57 C56 H56A 120.3 . . ? C52 C57 C56 120.4(3) . . ? C52 C57 H57A 119.8 . . ? C56 C57 H57A 119.8 . . ? F1 B1 F4 110.1(8) . . ? F1 B1 F3 110.3(8) . . ? F4 B1 F3 110.1(8) . . ? F1 B1 F2 108.2(7) . . ? F4 B1 F2 109.1(8) . . ? F3 B1 F2 109.0(8) . . ? F4B B1B F1B 108.9(8) . . ? F4B B1B F2B 110.3(8) . . ? F1B B1B F2B 109.1(7) . . ? F4B B1B F3B 110.0(8) . . ? F1B B1B F3B 109.9(8) . . ? F2B B1B F3B 108.8(8) . . ? F5 B2 F6 107.3(8) . . ? F5 B2 F8 114.0(8) . . ? F6 B2 F8 106.9(8) . . ? F5 B2 F7 110.0(7) . . ? F6 B2 F7 107.1(8) . . ? F8 B2 F7 111.2(8) . . ? F5B B2B F6B 110.0(6) . . ? F5B B2B F7B 112.0(7) . . ? F6B B2B F7B 103.1(6) . . ? F5B B2B F8B 113.5(7) . . ? F6B B2B F8B 111.7(7) . . ? F7B B2B F8B 106.0(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.42 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.486 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.065 _publ_requested_category FM _publ_section_references ; 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 a mixture methylene chloride and pentane. ; _publ_section_exptl_refinement ; A structural model consisting of the host, including two BF~4~ counter-ions plus four disordered methylene chloride solvate molecules was developed; however, positions for the idealized solvate molecules were poorly determined. This model converged with wR2 = 0.1594 and R1 = 0.0787 for 894 parameters with 554 restraints against 12834 data. The disorder in the BF~4~ anoins were modeled so that the distances between atom pairs (esd 0.01) and angles (esd 0.02 were restrained to possess the same value (esd 0.01). Similar displacement amplitudes (esd 0.01) were imposed on disordered sites overlapping by less than the sum of van der Waals radii. The anisotropic U^ij^ values of the atoms were restrained to behave more isotropically (esd 0.01). 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 four methylene chloride solvent molecules predicted by the complete refinement. The "squeeze" model converged with wR2 = 0.1126 and R1 = 0.0697 for 786 parameters with 548 restraints against 12834 data. H atoms were included as riding idealized contributors. The 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 'Acta Crystallographica E' _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 electron count from the "squeeze" model converged in good agreement with the four methylene chloride solvent molecules predicted by the complete refinement. ; _vrf_CHEMW03_I ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: The ratio of given/expected moleuclar weight is different due to the use of "Squeeze" to remove the highly disordered solvent molecules. ; _vrf_PLAT043_I ; PROBLEM: Check Reported Molecular Weight ................ 1586.89 RESPONSE: The reported molecular weight differs from the calculated molecular weight due to the use of "squeeze" to remove the highly disordered solvent molecules. ; _vrf_PLAT044_I ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: The reported Dx differs from the calculated Dx due to the use of "squeeze" to remove the highly disordered solvent molecules. ; _vrf_PLAT051_I ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 31.42 Perc. RESPONSE: The Mu(calc) and Mu(CIF) ratios differ due to the use of "squeeze" to remove the highly disordered solvent molecules. ; loop_ _publ_author_name _publ_author_address 'Gray, Danielle L.' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Fuller, Amy L.' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Gao, Yi-Gui' ; University of Illinois School of Chemical Sciences, Box 59-1 505 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 0.0540 0.00 -1.00 0.00 0.0390 0.00 0.00 -1.00 0.0800 0.00 0.00 1.00 0.1250 -1.00 0.00 0.00 0.0890 1.00 0.00 0.00 0.0420 -1.00 0.00 -1.00 0.0830 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 0.169 0.181 0.203 436 182 ' ' 2 -0.169 0.819 -0.203 436 182 ' '