data_ba41lasq _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H37 Fe2 N O4 P2 S2, C32 H12 B F24 ' _chemical_formula_sum 'C79 H49 B F24 Fe2 N O4 P2 S2' _chemical_formula_structural ? _chemical_formula_weight 1780.76 _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' _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 13.7224(6) _cell_length_b 17.4566(8) _cell_length_c 20.4323(9) _cell_angle_alpha 112.125(2) _cell_angle_beta 103.554(2) _cell_angle_gamma 96.384(3) _cell_volume 4298.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9987 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.80 _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.747 _exptl_crystal_size_mid 0.394 _exptl_crystal_size_min 0.368 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1794 _exptl_crystal_id ba41lasq _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (-2 1 2) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.7255 _exptl_absorpt_correction_T_max 0.8498 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; One distinct cell was identified using APEX2 (Bruker, 200 4) Six 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 ba41lasq _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type ? _diffrn_measurement_device 'Bruker Kappa/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 68738 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.52 _reflns_number_total 15916 _reflns_number_gt 11474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.0-1 (Bruker, 2004)' _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 disordered flourine atoms and the iron centers; 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 resolution. The acicular parent crystals were extremely difficult to see through to make a clean cut without damaging the crystal. Therefore, the data crystal was much longer than ideal. ; _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^)+(0.0548P)^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 15916 _refine_ls_number_parameters 1291 _refine_ls_number_restraints 2377 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.298 _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 0.69887(3) 0.94102(3) 0.45168(2) 0.02609(12) Uani 1 1 d . . . Fe2 Fe 0.58512(3) 0.81949(3) 0.32987(2) 0.02064(11) Uani 1 1 d . . . P1 P 0.48152(6) 0.80917(5) 0.22352(4) 0.02261(18) Uani 1 1 d . . . P2 P 0.49138(6) 0.69512(5) 0.30928(4) 0.02254(18) Uani 1 1 d . . . S1 S 0.70139(6) 0.92927(5) 0.33812(4) 0.02586(18) Uani 1 1 d . B . S2 S 0.71636(6) 0.80535(5) 0.41360(4) 0.02682(18) Uani 1 1 d . . . N1 N 0.80948(19) 0.80512(17) 0.30837(15) 0.0305(6) Uani 1 1 d . B . O1 O 0.63238(19) 0.93053(17) 0.57589(14) 0.0441(6) Uani 1 1 d . . . O2 O 0.91713(19) 1.01313(18) 0.53531(15) 0.0551(8) Uani 1 1 d . . . O3 O 0.6338(2) 1.10070(16) 0.46829(14) 0.0482(7) Uani 1 1 d . . . O4 O 0.44838(16) 0.90268(15) 0.40799(12) 0.0344(5) Uani 1 1 d . . . C1 C 0.6584(2) 0.9340(2) 0.52803(19) 0.0321(8) Uani 1 1 d . . . C2 C 0.8322(3) 0.9874(2) 0.5035(2) 0.0372(8) Uani 1 1 d . . . C3 C 0.6578(2) 1.0391(2) 0.46311(18) 0.0314(8) Uani 1 1 d . . . C4 C 0.8257(2) 0.7947(2) 0.37609(19) 0.0323(8) Uani 1 1 d . . . H4A H 0.8871 0.8375 0.4135 0.039 Uiso 1 1 calc R . . H4B H 0.8401 0.7380 0.3674 0.039 Uiso 1 1 calc R . . C5 C 0.8714(2) 0.7621(2) 0.26135(19) 0.0375(9) Uani 1 1 d D . . H5A H 0.8443 0.7628 0.2123 0.045 Uiso 1 1 calc R A 1 H5B H 0.8588 0.7020 0.2538 0.045 Uiso 1 1 calc R A 1 C6 C 0.9871(6) 0.7957(11) 0.2873(11) 0.035(3) Uani 0.41(4) 1 d PGDU B 1 C7 C 1.0601(11) 0.7822(12) 0.3393(11) 0.037(2) Uani 0.41(4) 1 d PGU B 1 H7 H 1.0396 0.7467 0.3615 0.045 Uiso 0.41(4) 1 calc PR B 1 C8 C 1.1632(9) 0.8205(14) 0.3587(9) 0.039(3) Uani 0.41(4) 1 d PGU B 1 H8 H 1.2131 0.8113 0.3942 0.047 Uiso 0.41(4) 1 calc PR B 1 C9 C 1.1932(7) 0.8724(11) 0.3261(11) 0.042(3) Uani 0.41(4) 1 d PGU B 1 H9 H 1.2636 0.8986 0.3394 0.050 Uiso 0.41(4) 1 calc PR B 1 C10 C 1.1201(13) 0.8860(10) 0.2741(13) 0.043(3) Uani 0.41(4) 1 d PGU B 1 H10 H 1.1407 0.9214 0.2519 0.052 Uiso 0.41(4) 1 calc PR B 1 C11 C 1.0171(11) 0.8476(13) 0.2547(12) 0.040(3) Uani 0.41(4) 1 d PGU B 1 H11 H 0.9671 0.8569 0.2191 0.048 Uiso 0.41(4) 1 calc PR B 1 C6B C 0.9855(4) 0.8023(8) 0.2902(7) 0.033(2) Uani 0.59(4) 1 d PGDU B 2 C7B C 1.0451(9) 0.7708(8) 0.3349(8) 0.042(2) Uani 0.59(4) 1 d PGU B 2 H7B H 1.0132 0.7293 0.3474 0.050 Uiso 0.59(4) 1 calc PR B 2 C8B C 1.1512(9) 0.8000(10) 0.3612(6) 0.045(2) Uani 0.59(4) 1 d PGU B 2 H8B H 1.1919 0.7784 0.3917 0.054 Uiso 0.59(4) 1 calc PR B 2 C9B C 1.1978(4) 0.8607(8) 0.3428(8) 0.045(3) Uani 0.59(4) 1 d PGU B 2 H9B H 1.2703 0.8806 0.3608 0.054 Uiso 0.59(4) 1 calc PR B 2 C10B C 1.1382(9) 0.8922(6) 0.2982(10) 0.042(2) Uani 0.59(4) 1 d PGU B 2 H10B H 1.1700 0.9336 0.2856 0.050 Uiso 0.59(4) 1 calc PR B 2 C11B C 1.0320(8) 0.8630(8) 0.2719(8) 0.0358(19) Uani 0.59(4) 1 d PGU B 2 H11B H 0.9913 0.8845 0.2413 0.043 Uiso 0.59(4) 1 calc PR B 2 C12 C 0.8152(2) 0.8921(2) 0.31919(19) 0.0304(7) Uani 1 1 d . . . H12A H 0.8233 0.8979 0.2743 0.037 Uiso 1 1 calc R B . H12B H 0.8767 0.9284 0.3611 0.037 Uiso 1 1 calc R . . C13 C 0.5113(2) 0.87597(19) 0.38358(17) 0.0249(7) Uani 1 1 d . . . C14 C 0.5208(2) 0.7393(2) 0.14719(16) 0.0241(7) Uani 1 1 d . . . C15 C 0.4561(3) 0.6627(2) 0.09470(18) 0.0324(8) Uani 1 1 d . . . H15 H 0.3883 0.6477 0.0963 0.039 Uiso 1 1 calc R . . C16 C 0.4905(3) 0.6087(2) 0.04053(19) 0.0399(9) Uani 1 1 d . . . H16 H 0.4463 0.5565 0.0046 0.048 Uiso 1 1 calc R . . C17 C 0.5894(3) 0.6307(2) 0.03852(19) 0.0395(9) Uani 1 1 d . . . H17 H 0.6132 0.5931 0.0013 0.047 Uiso 1 1 calc R . . C18 C 0.6536(3) 0.7064(2) 0.08993(18) 0.0348(8) Uani 1 1 d . . . H18 H 0.7211 0.7215 0.0878 0.042 Uiso 1 1 calc R . . C19 C 0.6198(2) 0.7603(2) 0.14458(18) 0.0303(7) Uani 1 1 d . . . H19 H 0.6646 0.8122 0.1807 0.036 Uiso 1 1 calc R . . C20 C 0.4857(2) 0.9101(2) 0.21642(17) 0.0274(7) Uani 1 1 d . . . C21 C 0.5137(3) 0.9250(2) 0.1607(2) 0.0472(10) Uani 1 1 d . . . H21 H 0.5309 0.8812 0.1236 0.057 Uiso 1 1 calc R . . C22 C 0.5167(4) 1.0041(3) 0.1592(3) 0.0704(14) Uani 1 1 d . . . H22 H 0.5363 1.0142 0.1211 0.084 Uiso 1 1 calc R . . C23 C 0.4920(4) 1.0669(3) 0.2117(3) 0.0677(13) Uani 1 1 d . . . H23 H 0.4949 1.1209 0.2103 0.081 Uiso 1 1 calc R . . C24 C 0.4627(4) 1.0529(3) 0.2669(2) 0.0565(11) Uani 1 1 d . . . H24 H 0.4447 1.0970 0.3033 0.068 Uiso 1 1 calc R . . C25 C 0.4595(3) 0.9749(2) 0.2691(2) 0.0408(9) Uani 1 1 d . . . H25 H 0.4391 0.9653 0.3072 0.049 Uiso 1 1 calc R . . C26 C 0.3441(2) 0.7646(2) 0.19775(17) 0.0264(7) Uani 1 1 d . . . C27 C 0.2826(3) 0.7891(2) 0.14821(19) 0.0371(8) Uani 1 1 d . . . H27 H 0.3136 0.8288 0.1336 0.044 Uiso 1 1 calc R . . C28 C 0.1767(3) 0.7571(3) 0.1193(2) 0.0449(10) Uani 1 1 d . . . H28 H 0.1367 0.7737 0.0843 0.054 Uiso 1 1 calc R . . C29 C 0.1311(3) 0.7023(2) 0.1412(2) 0.0400(9) Uani 1 1 d . . . H29 H 0.0587 0.6816 0.1221 0.048 Uiso 1 1 calc R . . C30 C 0.1888(2) 0.6753(2) 0.19169(18) 0.0307(8) Uani 1 1 d . . . C31 C 0.1378(3) 0.6185(2) 0.2132(2) 0.0385(9) Uani 1 1 d . . . H31 H 0.0653 0.5989 0.1929 0.046 Uiso 1 1 calc R . . C32 C 0.1892(3) 0.5912(2) 0.2617(2) 0.0421(9) Uani 1 1 d . . . H32 H 0.1535 0.5529 0.2755 0.051 Uiso 1 1 calc R . . C33 C 0.2961(3) 0.6201(2) 0.2915(2) 0.0355(8) Uani 1 1 d . . . H33 H 0.3319 0.6013 0.3264 0.043 Uiso 1 1 calc R . . C34 C 0.3514(2) 0.6745(2) 0.27228(17) 0.0262(7) Uani 1 1 d . . . C35 C 0.2986(2) 0.7060(2) 0.22154(17) 0.0255(7) Uani 1 1 d . . . C36 C 0.5088(2) 0.6764(2) 0.39285(18) 0.0287(7) Uani 1 1 d . . . C37 C 0.4757(3) 0.7276(2) 0.4500(2) 0.0435(9) Uani 1 1 d . . . H37 H 0.4450 0.7722 0.4453 0.052 Uiso 1 1 calc R . . C38 C 0.4868(4) 0.7146(3) 0.5133(2) 0.0575(12) Uani 1 1 d . . . H38 H 0.4638 0.7503 0.5521 0.069 Uiso 1 1 calc R . . C39 C 0.5309(4) 0.6501(3) 0.5210(2) 0.0602(12) Uani 1 1 d . . . H39 H 0.5374 0.6407 0.5645 0.072 Uiso 1 1 calc R . . C40 C 0.5654(3) 0.5997(3) 0.4653(2) 0.0554(11) Uani 1 1 d . . . H40 H 0.5969 0.5558 0.4708 0.066 Uiso 1 1 calc R . . C41 C 0.5548(3) 0.6122(2) 0.4013(2) 0.0387(9) Uani 1 1 d . . . H41 H 0.5789 0.5769 0.3631 0.046 Uiso 1 1 calc R . . C42 C 0.5254(2) 0.60561(19) 0.24496(17) 0.0253(7) Uani 1 1 d . . . C43 C 0.4608(3) 0.5250(2) 0.20960(19) 0.0363(8) Uani 1 1 d . . . H43 H 0.3944 0.5170 0.2156 0.044 Uiso 1 1 calc R . . C44 C 0.4924(3) 0.4568(2) 0.1661(2) 0.0448(9) Uani 1 1 d . . . H44 H 0.4483 0.4019 0.1429 0.054 Uiso 1 1 calc R . . C45 C 0.5878(3) 0.4682(2) 0.1563(2) 0.0428(9) Uani 1 1 d . . . H45 H 0.6100 0.4210 0.1267 0.051 Uiso 1 1 calc R . . C46 C 0.6511(3) 0.5473(2) 0.1890(2) 0.0413(9) Uani 1 1 d . . . H46 H 0.7165 0.5550 0.1813 0.050 Uiso 1 1 calc R . . C47 C 0.6202(2) 0.6161(2) 0.23308(18) 0.0314(8) Uani 1 1 d . . . H47 H 0.6643 0.6709 0.2553 0.038 Uiso 1 1 calc R . . B1 B 0.9032(3) 0.2393(2) 0.1643(2) 0.0289(8) Uani 1 1 d . . . F1 F 0.7765(5) 0.0071(7) -0.1386(4) 0.097(2) Uani 0.755(15) 1 d PDU C 1 F2 F 0.8866(8) -0.0670(4) -0.1243(3) 0.090(2) Uani 0.755(15) 1 d PDU C 1 F3 F 0.9357(5) 0.0617(5) -0.0981(3) 0.0838(18) Uani 0.755(15) 1 d PDU C 1 F1B F 0.8025(15) 0.0453(12) -0.1270(11) 0.073(5) Uani 0.245(15) 1 d PDU C 2 F2B F 0.820(2) -0.0749(6) -0.1365(7) 0.082(5) Uani 0.245(15) 1 d PDU C 2 F3B F 0.9514(8) 0.0248(16) -0.1018(11) 0.085(5) Uani 0.245(15) 1 d PDU C 2 F4 F 0.8578(4) -0.1226(5) 0.1092(5) 0.092(2) Uani 0.606(8) 1 d PDU D 1 F5 F 0.7038(5) -0.1314(5) 0.0586(4) 0.090(2) Uani 0.606(8) 1 d PDU D 1 F6 F 0.7732(8) -0.0464(3) 0.1682(3) 0.098(2) Uani 0.606(8) 1 d PDU D 1 F4B F 0.7915(11) -0.1509(4) 0.0500(6) 0.102(3) Uani 0.394(8) 1 d PDU D 2 F5B F 0.6961(6) -0.0780(8) 0.0990(8) 0.091(3) Uani 0.394(8) 1 d PDU D 2 F6B F 0.8504(8) -0.0621(6) 0.1624(5) 0.085(3) Uani 0.394(8) 1 d PDU D 2 F7 F 0.4325(3) 0.2250(4) 0.0894(2) 0.100(2) Uani 0.820(8) 1 d PDU E 1 F8 F 0.5225(3) 0.2292(3) 0.0214(2) 0.0882(16) Uani 0.820(8) 1 d PDU E 1 F9 F 0.4936(4) 0.1191(2) 0.0378(3) 0.0868(18) Uani 0.820(8) 1 d PDU E 1 F7B F 0.4394(10) 0.1585(13) 0.0861(8) 0.061(5) Uani 0.180(8) 1 d PDU E 2 F8B F 0.4746(16) 0.2558(8) 0.0538(12) 0.080(6) Uani 0.180(8) 1 d PDU E 2 F9B F 0.5235(15) 0.1440(13) 0.0113(8) 0.087(6) Uani 0.180(8) 1 d PDU E 2 F10 F 0.7699(11) 0.3616(17) 0.3949(11) 0.072(4) Uani 0.46(5) 1 d PDU F 1 F11 F 0.665(2) 0.4255(9) 0.3530(11) 0.098(5) Uani 0.46(5) 1 d PDU F 1 F12 F 0.6085(13) 0.3097(15) 0.3570(11) 0.099(5) Uani 0.46(5) 1 d PDU F 1 F10B F 0.7750(8) 0.3857(15) 0.3934(10) 0.074(4) Uani 0.54(5) 1 d PDU F 2 F11B F 0.6307(18) 0.4089(13) 0.3516(9) 0.099(4) Uani 0.54(5) 1 d PDU F 2 F12B F 0.637(2) 0.2902(10) 0.3594(8) 0.100(5) Uani 0.54(5) 1 d PDU F 2 F13 F 1.192(2) 0.2778(11) 0.0534(14) 0.060(4) Uani 0.37(4) 1 d PDU G 1 F14 F 1.152(2) 0.3444(17) -0.0125(8) 0.064(4) Uani 0.37(4) 1 d PDU G 1 F15 F 1.2348(14) 0.4135(13) 0.1016(14) 0.097(6) Uani 0.37(4) 1 d PDU G 1 F13B F 1.2146(11) 0.3002(12) 0.0765(11) 0.082(3) Uani 0.63(4) 1 d PDU G 2 F14B F 1.1363(12) 0.3182(12) -0.0190(3) 0.072(3) Uani 0.63(4) 1 d PDU G 2 F15B F 1.2219(9) 0.4243(5) 0.0814(8) 0.078(3) Uani 0.63(4) 1 d PDU G 2 F16 F 0.7529(8) 0.4397(15) 0.0356(11) 0.064(5) Uani 0.318(17) 1 d PDU H 1 F17 F 0.8918(12) 0.5129(10) 0.0343(12) 0.064(4) Uani 0.318(17) 1 d PDU H 1 F18 F 0.8661(12) 0.5320(8) 0.1322(6) 0.056(4) Uani 0.318(17) 1 d PDU H 1 F16B F 0.7534(3) 0.4431(7) 0.0566(5) 0.0489(17) Uani 0.682(17) 1 d PDU H 2 F17B F 0.8475(7) 0.4699(7) -0.0029(4) 0.071(2) Uani 0.682(17) 1 d PDU H 2 F18B F 0.8783(6) 0.5480(4) 0.1133(5) 0.081(3) Uani 0.682(17) 1 d PDU H 2 F19 F 1.1760(8) 0.1617(5) 0.4079(3) 0.088(2) Uani 0.544(8) 1 d PDU I 1 F20 F 1.2457(7) 0.1469(8) 0.3238(7) 0.136(3) Uani 0.544(8) 1 d PDU I 1 F21 F 1.0951(8) 0.0766(4) 0.3006(6) 0.142(4) Uani 0.544(8) 1 d PDU I 1 F19B F 1.2502(8) 0.1856(5) 0.3934(7) 0.126(4) Uani 0.456(8) 1 d PDU I 2 F20B F 1.1771(8) 0.0950(5) 0.2860(4) 0.072(2) Uani 0.456(8) 1 d PDU I 2 F21B F 1.1011(9) 0.1141(8) 0.3660(9) 0.129(4) Uani 0.456(8) 1 d PDU I 2 F22 F 1.0710(13) 0.4857(18) 0.4445(15) 0.087(5) Uani 0.42(6) 1 d PDU J 1 F23 F 1.2221(18) 0.4674(19) 0.4728(10) 0.078(5) Uani 0.42(6) 1 d PDU J 1 F24 F 1.171(3) 0.5048(14) 0.3835(10) 0.085(5) Uani 0.42(6) 1 d PDU J 1 F22B F 1.0821(13) 0.4741(10) 0.4589(10) 0.070(3) Uani 0.58(6) 1 d PDU J 2 F23B F 1.2387(9) 0.4764(11) 0.4608(11) 0.077(4) Uani 0.58(6) 1 d PDU J 2 F24B F 1.1390(17) 0.5127(8) 0.3862(7) 0.067(3) Uani 0.58(6) 1 d PDU J 2 C48 C 0.8796(2) 0.1405(2) 0.10493(18) 0.0319(8) Uani 1 1 d . . . C49 C 0.8848(3) 0.1142(2) 0.03249(18) 0.0345(8) Uani 1 1 d . . . H49 H 0.9068 0.1558 0.0165 0.041 Uiso 1 1 calc R . . C50 C 0.8588(3) 0.0289(2) -0.0171(2) 0.0419(9) Uani 1 1 d . C . C51 C 0.8286(3) -0.0334(2) 0.0041(2) 0.0442(9) Uani 1 1 d . . . H51 H 0.8125 -0.0916 -0.0293 0.053 Uiso 1 1 calc R . . C52 C 0.8223(3) -0.0091(2) 0.0758(2) 0.0400(9) Uani 1 1 d . D . C53 C 0.8457(3) 0.0753(2) 0.1240(2) 0.0349(8) Uani 1 1 d . . . H53 H 0.8387 0.0899 0.1722 0.042 Uiso 1 1 calc R . . C54 C 0.8619(3) 0.0068(3) -0.0945(2) 0.0581(12) Uani 1 1 d D . . C55 C 0.7906(3) -0.0758(2) 0.1005(2) 0.0558(11) Uani 1 1 d D . . C56 C 0.7954(2) 0.2543(2) 0.18343(17) 0.0275(7) Uani 1 1 d . . . C57 C 0.7031(3) 0.2251(2) 0.12560(19) 0.0337(8) Uani 1 1 d . . . H57 H 0.7052 0.1966 0.0763 0.040 Uiso 1 1 calc R . . C58 C 0.6094(3) 0.2357(2) 0.13700(19) 0.0335(8) Uani 1 1 d . E . C59 C 0.6031(3) 0.2772(2) 0.2076(2) 0.0372(8) Uani 1 1 d . . . H59 H 0.5390 0.2853 0.2159 0.045 Uiso 1 1 calc R . . C60 C 0.6919(3) 0.3064(2) 0.26567(19) 0.0361(8) Uani 1 1 d . F . C61 C 0.7859(3) 0.2952(2) 0.25400(19) 0.0338(8) Uani 1 1 d . . . H61 H 0.8458 0.3160 0.2955 0.041 Uiso 1 1 calc R . . C62 C 0.5144(3) 0.2010(2) 0.0723(2) 0.0481(10) Uani 1 1 d D . . C63 C 0.6833(3) 0.3487(3) 0.3425(2) 0.0617(13) Uani 1 1 d D . . C64 C 0.9388(2) 0.3032(2) 0.12833(17) 0.0283(7) Uani 1 1 d . . . C65 C 1.0304(2) 0.3019(2) 0.10900(19) 0.0347(8) Uani 1 1 d . . . H65 H 1.0717 0.2649 0.1187 0.042 Uiso 1 1 calc R . . C66 C 1.0631(2) 0.3522(2) 0.07658(19) 0.0340(8) Uani 1 1 d . G . C67 C 1.0055(2) 0.4074(2) 0.06186(19) 0.0335(8) Uani 1 1 d . . . H67 H 1.0279 0.4426 0.0399 0.040 Uiso 1 1 calc R . . C68 C 0.9150(2) 0.4100(2) 0.07992(18) 0.0306(7) Uani 1 1 d . H . C69 C 0.8828(2) 0.3592(2) 0.11255(17) 0.0282(7) Uani 1 1 d . . . H69 H 0.8202 0.3627 0.1246 0.034 Uiso 1 1 calc R . . C70 C 1.1589(3) 0.3477(3) 0.0542(2) 0.0521(11) Uani 1 1 d D . . C71 C 0.8519(3) 0.4682(2) 0.0641(2) 0.0417(9) Uani 1 1 d D . . C72 C 0.9961(2) 0.2601(2) 0.24041(18) 0.0307(7) Uani 1 1 d . J . C73 C 1.0406(3) 0.1998(2) 0.25829(19) 0.0370(8) Uani 1 1 d . . . H73 H 1.0185 0.1420 0.2238 0.044 Uiso 1 1 calc R . . C74 C 1.1163(3) 0.2214(3) 0.3249(2) 0.0465(10) Uani 1 1 d . I . C75 C 1.1509(3) 0.3039(3) 0.3764(2) 0.0465(10) Uani 1 1 d . . . H75 H 1.2020 0.3182 0.4220 0.056 Uiso 1 1 calc R . . C76 C 1.1096(3) 0.3655(2) 0.3602(2) 0.0402(9) Uani 1 1 d . J . C78 C 1.1598(4) 0.1533(3) 0.3406(2) 0.0715(15) Uani 1 1 d D . . C79 C 1.1433(3) 0.4561(3) 0.4156(2) 0.0551(11) Uani 1 1 d D . . C77 C 1.0349(3) 0.3439(2) 0.29360(19) 0.0340(8) Uani 1 1 d . . . H77 H 1.0089 0.3878 0.2836 0.041 Uiso 1 1 calc R J . 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 0.0230(2) 0.0273(3) 0.0231(3) 0.0049(2) 0.00718(19) 0.00650(19) Fe2 0.0184(2) 0.0225(2) 0.0205(2) 0.00749(19) 0.00689(18) 0.00577(18) P1 0.0230(4) 0.0239(4) 0.0203(4) 0.0080(4) 0.0072(3) 0.0053(3) P2 0.0211(4) 0.0239(4) 0.0238(4) 0.0098(4) 0.0087(3) 0.0063(3) S1 0.0220(4) 0.0271(4) 0.0280(4) 0.0103(4) 0.0087(3) 0.0046(3) S2 0.0223(4) 0.0305(4) 0.0274(4) 0.0115(4) 0.0064(3) 0.0090(3) N1 0.0220(13) 0.0338(16) 0.0313(16) 0.0069(13) 0.0107(12) 0.0079(12) O1 0.0522(16) 0.0554(17) 0.0340(14) 0.0215(13) 0.0212(13) 0.0199(13) O2 0.0257(14) 0.0642(19) 0.0466(17) -0.0024(15) 0.0044(12) 0.0053(13) O3 0.0606(17) 0.0373(15) 0.0495(17) 0.0134(13) 0.0243(14) 0.0222(14) O4 0.0274(12) 0.0420(14) 0.0354(14) 0.0122(12) 0.0148(11) 0.0158(11) C1 0.0321(18) 0.0315(19) 0.0297(19) 0.0091(16) 0.0070(16) 0.0137(15) C2 0.031(2) 0.037(2) 0.034(2) 0.0025(17) 0.0127(17) 0.0100(16) C3 0.0300(18) 0.0317(19) 0.0267(18) 0.0042(16) 0.0113(15) 0.0073(15) C4 0.0220(16) 0.0340(19) 0.039(2) 0.0127(17) 0.0082(15) 0.0121(14) C5 0.0254(17) 0.041(2) 0.033(2) 0.0000(17) 0.0112(15) 0.0079(16) C6 0.026(4) 0.034(4) 0.032(5) -0.001(4) 0.008(4) 0.008(4) C7 0.025(4) 0.033(4) 0.041(4) 0.004(4) 0.007(4) 0.010(4) C8 0.024(4) 0.034(6) 0.043(4) 0.004(4) 0.001(4) 0.005(4) C9 0.028(4) 0.038(5) 0.041(6) 0.001(4) 0.006(4) 0.006(4) C10 0.033(5) 0.046(5) 0.034(6) 0.002(5) 0.006(4) 0.009(4) C11 0.030(4) 0.037(5) 0.037(5) 0.002(4) 0.008(4) 0.003(4) C6B 0.025(3) 0.034(3) 0.030(3) -0.002(3) 0.014(3) 0.014(3) C7B 0.026(4) 0.038(4) 0.044(4) 0.001(3) 0.007(3) 0.007(3) C8B 0.031(4) 0.034(5) 0.049(4) -0.003(3) 0.004(3) 0.011(3) C9B 0.023(3) 0.043(4) 0.049(5) -0.002(4) 0.009(3) 0.007(3) C10B 0.028(4) 0.045(3) 0.032(5) -0.004(4) 0.010(4) 0.001(3) C11B 0.024(3) 0.039(4) 0.030(4) 0.000(3) 0.009(3) 0.004(3) C12 0.0231(16) 0.0367(19) 0.0308(19) 0.0107(16) 0.0121(14) 0.0076(14) C13 0.0271(16) 0.0257(17) 0.0208(16) 0.0101(14) 0.0045(14) 0.0061(14) C14 0.0267(16) 0.0292(17) 0.0203(16) 0.0120(14) 0.0092(13) 0.0108(14) C15 0.0286(17) 0.0347(19) 0.0315(19) 0.0103(16) 0.0112(15) 0.0063(15) C16 0.042(2) 0.0327(19) 0.031(2) -0.0004(16) 0.0094(17) 0.0050(16) C17 0.044(2) 0.042(2) 0.029(2) 0.0074(17) 0.0165(17) 0.0169(18) C18 0.0343(19) 0.044(2) 0.0301(19) 0.0150(17) 0.0166(16) 0.0108(17) C19 0.0281(17) 0.0333(18) 0.0277(18) 0.0111(16) 0.0097(15) 0.0031(15) C20 0.0269(16) 0.0276(17) 0.0259(18) 0.0114(15) 0.0045(14) 0.0054(14) C21 0.068(3) 0.041(2) 0.049(2) 0.028(2) 0.030(2) 0.021(2) C22 0.106(4) 0.065(3) 0.085(4) 0.056(3) 0.057(3) 0.040(3) C23 0.100(4) 0.041(3) 0.084(4) 0.040(3) 0.038(3) 0.029(3) C24 0.084(3) 0.038(2) 0.054(3) 0.019(2) 0.025(2) 0.028(2) C25 0.057(2) 0.034(2) 0.037(2) 0.0167(18) 0.0166(18) 0.0189(18) C26 0.0220(15) 0.0304(17) 0.0236(17) 0.0071(15) 0.0073(13) 0.0072(14) C27 0.0319(19) 0.047(2) 0.033(2) 0.0193(18) 0.0067(16) 0.0112(17) C28 0.035(2) 0.057(3) 0.042(2) 0.024(2) 0.0016(17) 0.0115(19) C29 0.0205(17) 0.049(2) 0.037(2) 0.0086(19) -0.0006(16) 0.0062(16) C30 0.0234(16) 0.0301(18) 0.0287(18) 0.0020(15) 0.0080(14) 0.0051(14) C31 0.0230(17) 0.037(2) 0.044(2) 0.0069(18) 0.0094(16) -0.0002(15) C32 0.0319(19) 0.038(2) 0.057(3) 0.019(2) 0.0188(18) -0.0007(16) C33 0.0305(18) 0.0338(19) 0.046(2) 0.0194(18) 0.0135(16) 0.0072(15) C34 0.0221(15) 0.0252(17) 0.0275(18) 0.0064(15) 0.0084(14) 0.0047(13) C35 0.0212(15) 0.0261(17) 0.0228(17) 0.0028(14) 0.0073(13) 0.0053(13) C36 0.0240(16) 0.0347(18) 0.0288(18) 0.0155(16) 0.0083(14) 0.0032(14) C37 0.062(2) 0.042(2) 0.041(2) 0.0227(19) 0.028(2) 0.0172(19) C38 0.083(3) 0.060(3) 0.037(2) 0.022(2) 0.032(2) 0.013(2) C39 0.073(3) 0.079(3) 0.040(2) 0.041(3) 0.015(2) 0.013(3) C40 0.056(3) 0.072(3) 0.059(3) 0.048(3) 0.015(2) 0.023(2) C41 0.0357(19) 0.048(2) 0.040(2) 0.0245(19) 0.0112(17) 0.0176(17) C42 0.0271(16) 0.0255(17) 0.0230(17) 0.0087(14) 0.0080(14) 0.0090(14) C43 0.0333(18) 0.0329(19) 0.041(2) 0.0110(17) 0.0164(17) 0.0048(16) C44 0.053(2) 0.0247(19) 0.045(2) 0.0019(17) 0.0184(19) 0.0019(17) C45 0.050(2) 0.035(2) 0.039(2) 0.0057(18) 0.0186(19) 0.0163(18) C46 0.038(2) 0.043(2) 0.042(2) 0.0099(19) 0.0210(18) 0.0162(18) C47 0.0301(17) 0.0298(18) 0.0314(19) 0.0082(16) 0.0114(15) 0.0075(15) B1 0.032(2) 0.029(2) 0.026(2) 0.0118(17) 0.0088(17) 0.0082(17) F1 0.072(3) 0.157(6) 0.040(3) 0.022(4) 0.003(2) 0.040(4) F2 0.128(5) 0.085(3) 0.057(3) 0.009(2) 0.045(3) 0.061(3) F3 0.103(4) 0.100(4) 0.051(2) 0.018(3) 0.047(2) 0.029(3) F1B 0.103(10) 0.078(9) 0.042(8) 0.033(7) 0.009(6) 0.033(7) F2B 0.123(10) 0.064(7) 0.045(6) 0.005(5) 0.034(7) 0.009(7) F3B 0.062(6) 0.124(10) 0.060(7) 0.012(7) 0.041(5) 0.038(7) F4 0.074(3) 0.086(4) 0.149(6) 0.092(4) 0.023(4) 0.019(3) F5 0.073(4) 0.082(4) 0.088(4) 0.053(4) -0.023(3) -0.043(3) F6 0.171(6) 0.057(3) 0.077(4) 0.031(3) 0.062(4) -0.002(4) F4B 0.159(8) 0.038(4) 0.115(7) 0.024(4) 0.074(6) 0.009(5) F5B 0.057(5) 0.100(7) 0.141(8) 0.070(6) 0.047(5) 0.002(4) F6B 0.093(6) 0.079(6) 0.085(6) 0.066(5) -0.010(5) -0.013(5) F7 0.0417(19) 0.142(5) 0.073(3) 0.004(3) -0.0002(17) 0.035(2) F8 0.076(3) 0.117(4) 0.065(3) 0.058(3) -0.015(2) -0.002(2) F9 0.080(3) 0.046(2) 0.084(3) 0.015(2) -0.037(2) -0.0071(18) F7B 0.040(7) 0.080(9) 0.054(7) 0.034(7) 0.007(5) -0.023(6) F8B 0.080(9) 0.062(8) 0.089(9) 0.041(7) -0.014(7) 0.027(7) F9B 0.072(9) 0.098(10) 0.057(8) 0.005(7) -0.001(7) 0.024(8) F10 0.078(6) 0.099(9) 0.033(5) 0.017(6) 0.021(4) 0.027(5) F11 0.095(9) 0.096(6) 0.079(6) -0.004(5) 0.040(6) 0.049(6) F12 0.074(6) 0.147(8) 0.071(5) 0.021(5) 0.059(5) 0.014(6) F10B 0.065(5) 0.091(8) 0.037(5) -0.004(4) 0.019(3) 0.011(4) F11B 0.082(7) 0.126(7) 0.070(5) -0.001(5) 0.044(5) 0.056(6) F12B 0.109(8) 0.126(7) 0.062(4) 0.023(4) 0.064(5) -0.010(5) F13 0.052(8) 0.073(7) 0.087(8) 0.046(6) 0.044(6) 0.038(5) F14 0.061(7) 0.087(9) 0.084(7) 0.057(5) 0.050(5) 0.035(6) F15 0.048(6) 0.110(8) 0.106(9) 0.018(6) 0.026(6) 0.006(6) F13B 0.046(5) 0.133(6) 0.115(7) 0.084(6) 0.045(4) 0.049(5) F14B 0.071(5) 0.104(7) 0.072(4) 0.043(3) 0.053(3) 0.039(5) F15B 0.029(3) 0.102(4) 0.112(5) 0.057(4) 0.029(3) -0.002(3) F16 0.056(7) 0.061(7) 0.066(9) 0.040(6) -0.014(5) 0.002(5) F17 0.077(7) 0.071(7) 0.106(8) 0.075(6) 0.065(6) 0.042(5) F18 0.055(5) 0.033(5) 0.090(6) 0.025(5) 0.032(5) 0.026(5) F16B 0.028(2) 0.070(3) 0.071(4) 0.052(3) 0.014(2) 0.018(2) F17B 0.092(4) 0.102(5) 0.076(4) 0.070(4) 0.053(4) 0.064(4) F18B 0.059(3) 0.028(2) 0.125(5) 0.025(3) -0.014(3) 0.006(2) F19 0.143(7) 0.088(5) 0.051(3) 0.046(3) 0.017(4) 0.055(5) F20 0.163(7) 0.156(7) 0.141(7) 0.083(6) 0.062(6) 0.124(6) F21 0.202(8) 0.066(4) 0.116(6) 0.042(4) -0.041(6) 0.050(5) F19B 0.130(7) 0.077(5) 0.120(7) 0.032(5) -0.051(5) 0.050(5) F20B 0.120(6) 0.058(4) 0.056(4) 0.029(3) 0.030(4) 0.060(4) F21B 0.180(8) 0.122(7) 0.163(8) 0.116(6) 0.077(6) 0.068(6) F22 0.085(6) 0.069(7) 0.084(9) 0.007(6) 0.015(6) 0.044(5) F23 0.088(7) 0.071(8) 0.042(6) 0.007(4) -0.014(5) 0.021(6) F24 0.098(10) 0.046(6) 0.083(7) 0.017(5) 0.002(6) -0.001(6) F22B 0.095(5) 0.054(4) 0.055(5) 0.008(3) 0.027(4) 0.032(4) F23B 0.059(4) 0.054(4) 0.077(6) 0.011(4) -0.024(4) 0.004(3) F24B 0.087(7) 0.044(4) 0.052(4) 0.016(3) -0.005(4) 0.012(4) C48 0.0302(18) 0.0341(19) 0.0309(19) 0.0116(16) 0.0101(15) 0.0102(15) C49 0.0356(19) 0.039(2) 0.0294(19) 0.0137(17) 0.0101(16) 0.0115(16) C50 0.042(2) 0.046(2) 0.029(2) 0.0075(18) 0.0069(17) 0.0155(18) C51 0.041(2) 0.032(2) 0.042(2) 0.0035(18) 0.0023(18) 0.0072(17) C52 0.036(2) 0.032(2) 0.044(2) 0.0111(18) 0.0074(17) 0.0042(16) C53 0.0358(19) 0.0338(19) 0.034(2) 0.0124(17) 0.0126(16) 0.0061(16) C54 0.068(3) 0.055(3) 0.037(2) 0.004(2) 0.012(2) 0.020(3) C55 0.063(3) 0.036(2) 0.064(3) 0.014(2) 0.024(3) 0.006(2) C56 0.0337(18) 0.0251(17) 0.0273(18) 0.0138(15) 0.0112(15) 0.0055(14) C57 0.041(2) 0.0347(19) 0.0275(19) 0.0133(16) 0.0129(16) 0.0085(16) C58 0.0338(18) 0.0339(19) 0.035(2) 0.0173(17) 0.0086(16) 0.0072(16) C59 0.0316(19) 0.039(2) 0.045(2) 0.0178(18) 0.0183(17) 0.0090(16) C60 0.038(2) 0.037(2) 0.033(2) 0.0102(17) 0.0162(17) 0.0068(16) C61 0.0326(18) 0.037(2) 0.0272(18) 0.0115(16) 0.0075(15) 0.0015(15) C62 0.039(2) 0.056(3) 0.045(2) 0.018(2) 0.0103(19) 0.009(2) C63 0.048(3) 0.083(4) 0.039(3) 0.007(3) 0.019(2) 0.009(3) C64 0.0292(17) 0.0302(18) 0.0218(17) 0.0084(15) 0.0065(14) 0.0030(14) C65 0.0289(18) 0.042(2) 0.036(2) 0.0188(17) 0.0096(16) 0.0117(16) C66 0.0273(17) 0.045(2) 0.0328(19) 0.0182(17) 0.0120(15) 0.0069(16) C67 0.0327(18) 0.039(2) 0.034(2) 0.0197(17) 0.0139(16) 0.0059(16) C68 0.0312(17) 0.0327(18) 0.0263(18) 0.0112(16) 0.0082(15) 0.0059(15) C69 0.0256(16) 0.0322(18) 0.0267(18) 0.0112(15) 0.0106(14) 0.0038(14) C70 0.036(2) 0.075(3) 0.067(3) 0.046(3) 0.025(2) 0.020(2) C71 0.039(2) 0.046(2) 0.054(3) 0.030(2) 0.022(2) 0.0123(18) C72 0.0321(18) 0.0341(19) 0.0328(19) 0.0179(16) 0.0136(15) 0.0112(15) C73 0.049(2) 0.035(2) 0.0276(19) 0.0113(16) 0.0126(17) 0.0144(17) C74 0.062(3) 0.050(2) 0.035(2) 0.023(2) 0.013(2) 0.030(2) C75 0.051(2) 0.053(3) 0.032(2) 0.016(2) 0.0034(18) 0.021(2) C76 0.039(2) 0.042(2) 0.034(2) 0.0126(18) 0.0057(17) 0.0116(17) C78 0.097(4) 0.062(3) 0.054(3) 0.029(3) 0.002(3) 0.035(3) C79 0.057(3) 0.049(3) 0.044(3) 0.014(2) -0.003(2) 0.012(2) C77 0.0329(18) 0.036(2) 0.036(2) 0.0174(17) 0.0111(16) 0.0123(16) _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 C2 1.800(4) . ? Fe1 C3 1.811(4) . ? Fe1 C1 1.815(4) . ? Fe1 S2 2.2578(9) . ? Fe1 S1 2.2600(9) . ? Fe1 Fe2 2.5685(6) . ? Fe2 C13 1.769(3) . ? Fe2 P1 2.2305(9) . ? Fe2 P2 2.2321(9) . ? Fe2 S1 2.2798(9) . ? Fe2 S2 2.2812(9) . ? P1 C20 1.818(3) . ? P1 C14 1.822(3) . ? P1 C26 1.827(3) . ? P2 C42 1.814(3) . ? P2 C36 1.824(3) . ? P2 C34 1.831(3) . ? S1 C12 1.824(3) . ? S2 C4 1.835(3) . ? N1 C4 1.432(4) . ? N1 C12 1.440(4) . ? N1 C5 1.480(4) . ? O1 C1 1.136(4) . ? O2 C2 1.137(4) . ? O3 C3 1.134(4) . ? O4 C13 1.152(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6B 1.517(6) . ? C5 C6 1.519(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.3900 . ? C6 C11 1.3900 . ? C7 C8 1.3900 . ? C7 H7 0.9500 . ? C8 C9 1.3900 . ? C8 H8 0.9500 . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C6B C7B 1.3900 . ? C6B C11B 1.3900 . ? C7B C8B 1.3900 . ? C7B H7B 0.9500 . ? C8B C9B 1.3900 . ? C8B H8B 0.9500 . ? C9B C10B 1.3900 . ? C9B H9B 0.9500 . ? C10B C11B 1.3900 . ? C10B H10B 0.9500 . ? C11B H11B 0.9500 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C19 1.386(4) . ? C14 C15 1.391(5) . ? C15 C16 1.376(5) . ? C15 H15 0.9500 . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.374(5) . ? C17 H17 0.9500 . ? C18 C19 1.377(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.384(5) . ? C20 C25 1.387(5) . ? C21 C22 1.388(6) . ? C21 H21 0.9500 . ? C22 C23 1.354(6) . ? C22 H22 0.9500 . ? C23 C24 1.376(6) . ? C23 H23 0.9500 . ? C24 C25 1.376(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.387(5) . ? C26 C35 1.431(4) . ? C27 C28 1.394(5) . ? C27 H27 0.9500 . ? C28 C29 1.351(5) . ? C28 H28 0.9500 . ? C29 C30 1.407(5) . ? C29 H29 0.9500 . ? C30 C31 1.408(5) . ? C30 C35 1.440(4) . ? C31 C32 1.345(5) . ? C31 H31 0.9500 . ? C32 C33 1.401(5) . ? C32 H32 0.9500 . ? C33 C34 1.375(5) . ? C33 H33 0.9500 . ? C34 C35 1.438(4) . ? C36 C37 1.386(5) . ? C36 C41 1.392(5) . ? C37 C38 1.372(5) . ? C37 H37 0.9500 . ? C38 C39 1.378(6) . ? C38 H38 0.9500 . ? C39 C40 1.373(6) . ? C39 H39 0.9500 . ? C40 C41 1.382(5) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.383(4) . ? C42 C43 1.395(5) . ? C43 C44 1.376(5) . ? C43 H43 0.9500 . ? C44 C45 1.375(5) . ? C44 H44 0.9500 . ? C45 C46 1.369(5) . ? C45 H45 0.9500 . ? C46 C47 1.383(5) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? B1 C48 1.632(5) . ? B1 C64 1.639(5) . ? B1 C56 1.640(5) . ? B1 C72 1.649(5) . ? F1 C54 1.301(5) . ? F2 C54 1.322(5) . ? F3 C54 1.350(6) . ? F1B C54 1.327(8) . ? F2B C54 1.331(8) . ? F3B C54 1.291(8) . ? F4 C55 1.322(5) . ? F5 C55 1.315(5) . ? F6 C55 1.372(5) . ? F4B C55 1.331(6) . ? F5B C55 1.285(6) . ? F6B C55 1.255(6) . ? F7 C62 1.319(4) . ? F8 C62 1.328(5) . ? F9 C62 1.295(5) . ? F7B C62 1.347(7) . ? F8B C62 1.285(8) . ? F9B C62 1.314(8) . ? F10 C63 1.331(8) . ? F11 C63 1.339(8) . ? F12 C63 1.321(8) . ? F10B C63 1.335(7) . ? F11B C63 1.321(7) . ? F12B C63 1.335(7) . ? F13 C70 1.342(8) . ? F14 C70 1.324(8) . ? F15 C70 1.328(8) . ? F13B C70 1.320(7) . ? F14B C70 1.330(6) . ? F15B C70 1.343(6) . ? F16 C71 1.301(8) . ? F17 C71 1.303(7) . ? F18 C71 1.368(8) . ? F16B C71 1.328(5) . ? F17B C71 1.367(5) . ? F18B C71 1.322(6) . ? F19 C78 1.288(6) . ? F20 C78 1.308(7) . ? F21 C78 1.350(7) . ? F19B C78 1.333(6) . ? F20B C78 1.288(6) . ? F21B C78 1.314(7) . ? F22 C79 1.326(8) . ? F23 C79 1.325(8) . ? F24 C79 1.329(8) . ? F22B C79 1.337(7) . ? F23B C79 1.332(7) . ? F24B C79 1.337(7) . ? C48 C49 1.397(5) . ? C48 C53 1.403(5) . ? C49 C50 1.395(5) . ? C49 H49 0.9500 . ? C50 C51 1.372(5) . ? C50 C54 1.493(5) . ? C51 C52 1.391(5) . ? C51 H51 0.9500 . ? C52 C53 1.378(5) . ? C52 C55 1.494(6) . ? C53 H53 0.9500 . ? C56 C61 1.392(4) . ? C56 C57 1.400(5) . ? C57 C58 1.380(5) . ? C57 H57 0.9500 . ? C58 C59 1.378(5) . ? C58 C62 1.491(5) . ? C59 C60 1.370(5) . ? C59 H59 0.9500 . ? C60 C61 1.388(5) . ? C60 C63 1.501(5) . ? C61 H61 0.9500 . ? C64 C69 1.392(4) . ? C64 C65 1.404(4) . ? C65 C66 1.379(5) . ? C65 H65 0.9500 . ? C66 C67 1.385(5) . ? C66 C70 1.490(5) . ? C67 C68 1.377(4) . ? C67 H67 0.9500 . ? C68 C69 1.386(4) . ? C68 C71 1.483(5) . ? C69 H69 0.9500 . ? C72 C73 1.394(5) . ? C72 C77 1.400(5) . ? C73 C74 1.392(5) . ? C73 H73 0.9500 . ? C74 C75 1.370(5) . ? C74 C78 1.492(6) . ? C75 C76 1.379(5) . ? C75 H75 0.9500 . ? C76 C77 1.385(5) . ? C76 C79 1.496(5) . ? C77 H77 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 C2 Fe1 C3 97.21(16) . . ? C2 Fe1 C1 96.06(15) . . ? C3 Fe1 C1 93.37(14) . . ? C2 Fe1 S2 95.45(12) . . ? C3 Fe1 S2 166.30(11) . . ? C1 Fe1 S2 90.47(11) . . ? C2 Fe1 S1 100.59(12) . . ? C3 Fe1 S1 86.16(11) . . ? C1 Fe1 S1 163.27(11) . . ? S2 Fe1 S1 86.39(3) . . ? C2 Fe1 Fe2 140.70(11) . . ? C3 Fe1 Fe2 110.41(11) . . ? C1 Fe1 Fe2 109.16(11) . . ? S2 Fe1 Fe2 55.97(2) . . ? S1 Fe1 Fe2 55.91(2) . . ? C13 Fe2 P1 93.71(10) . . ? C13 Fe2 P2 91.72(10) . . ? P1 Fe2 P2 88.11(3) . . ? C13 Fe2 S1 100.36(10) . . ? P1 Fe2 S1 92.21(3) . . ? P2 Fe2 S1 167.87(3) . . ? C13 Fe2 S2 104.43(10) . . ? P1 Fe2 S2 161.84(3) . . ? P2 Fe2 S2 90.54(3) . . ? S1 Fe2 S2 85.38(3) . . ? C13 Fe2 Fe1 68.06(10) . . ? P1 Fe2 Fe1 135.89(3) . . ? P2 Fe2 Fe1 130.26(3) . . ? S1 Fe2 Fe1 55.18(2) . . ? S2 Fe2 Fe1 55.11(2) . . ? C20 P1 C14 107.28(14) . . ? C20 P1 C26 103.55(15) . . ? C14 P1 C26 103.50(14) . . ? C20 P1 Fe2 113.39(11) . . ? C14 P1 Fe2 108.81(10) . . ? C26 P1 Fe2 119.33(11) . . ? C42 P2 C36 104.60(15) . . ? C42 P2 C34 103.72(14) . . ? C36 P2 C34 102.84(14) . . ? C42 P2 Fe2 112.69(10) . . ? C36 P2 Fe2 112.80(11) . . ? C34 P2 Fe2 118.73(11) . . ? C12 S1 Fe1 109.53(11) . . ? C12 S1 Fe2 109.24(11) . . ? Fe1 S1 Fe2 68.91(3) . . ? C4 S2 Fe1 109.38(12) . . ? C4 S2 Fe2 107.89(11) . . ? Fe1 S2 Fe2 68.92(3) . . ? C4 N1 C12 112.9(3) . . ? C4 N1 C5 114.2(3) . . ? C12 N1 C5 113.1(3) . . ? O1 C1 Fe1 179.0(3) . . ? O2 C2 Fe1 177.0(3) . . ? O3 C3 Fe1 177.4(3) . . ? N1 C4 S2 113.8(2) . . ? N1 C4 H4A 108.8 . . ? S2 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 . . ? S2 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N1 C5 C6B 115.2(6) . . ? N1 C5 C6 119.0(8) . . ? N1 C5 H5A 107.6 . . ? C6B C5 H5A 107.7 . . ? C6 C5 H5A 107.6 . . ? N1 C5 H5B 107.6 . . ? C6B C5 H5B 111.4 . . ? C6 C5 H5B 107.6 . . ? H5A C5 H5B 107.0 . . ? C7 C6 C11 120.0 . . ? C7 C6 C5 127.4(12) . . ? C11 C6 C5 112.5(12) . . ? C6 C7 C8 120.0 . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C6 120.0 . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? C7B C6B C11B 120.0 . . ? C7B C6B C5 115.2(9) . . ? C11B C6B C5 124.7(9) . . ? C8B C7B C6B 120.0 . . ? C8B C7B H7B 120.0 . . ? C6B C7B H7B 120.0 . . ? C7B C8B C9B 120.0 . . ? C7B C8B H8B 120.0 . . ? C9B C8B H8B 120.0 . . ? C10B C9B C8B 120.0 . . ? C10B C9B H9B 120.0 . . ? C8B C9B H9B 120.0 . . ? C11B C10B C9B 120.0 . . ? C11B C10B H10B 120.0 . . ? C9B C10B H10B 120.0 . . ? C10B C11B C6B 120.0 . . ? C10B C11B H11B 120.0 . . ? C6B C11B H11B 120.0 . . ? N1 C12 S1 112.5(2) . . ? N1 C12 H12A 109.1 . . ? S1 C12 H12A 109.1 . . ? N1 C12 H12B 109.1 . . ? S1 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? O4 C13 Fe2 167.6(3) . . ? C19 C14 C15 119.5(3) . . ? C19 C14 P1 119.0(2) . . ? C15 C14 P1 121.3(2) . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 119.9(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.8(3) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C14 120.3(3) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? C21 C20 C25 118.7(3) . . ? C21 C20 P1 122.9(3) . . ? C25 C20 P1 118.4(3) . . ? C20 C21 C22 119.9(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.4(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 119.7(4) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C20 120.7(4) . . ? C24 C25 H25 119.6 . . ? C20 C25 H25 119.6 . . ? C27 C26 C35 119.9(3) . . ? C27 C26 P1 114.3(2) . . ? C35 C26 P1 125.7(2) . . ? C26 C27 C28 121.9(3) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? C29 C28 C27 119.7(3) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 121.3(3) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C29 C30 C31 119.3(3) . . ? C29 C30 C35 120.4(3) . . ? C31 C30 C35 120.4(3) . . ? C32 C31 C30 121.6(3) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C33 119.1(3) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 122.6(3) . . ? C34 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C33 C34 C35 119.7(3) . . ? C33 C34 P2 115.8(2) . . ? C35 C34 P2 124.4(2) . . ? C26 C35 C34 126.6(3) . . ? C26 C35 C30 116.8(3) . . ? C34 C35 C30 116.6(3) . . ? C37 C36 C41 118.7(3) . . ? C37 C36 P2 119.4(3) . . ? C41 C36 P2 122.0(3) . . ? C38 C37 C36 120.8(4) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 120.4(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 119.5(4) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 120.7(4) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C40 C41 C36 120.0(4) . . ? C40 C41 H41 120.0 . . ? C36 C41 H41 120.0 . . ? C47 C42 C43 118.6(3) . . ? C47 C42 P2 119.4(2) . . ? C43 C42 P2 121.9(2) . . ? C44 C43 C42 120.6(3) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 119.9(3) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.2(3) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 120.3(3) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C42 C47 C46 120.4(3) . . ? C42 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C48 B1 C64 110.6(3) . . ? C48 B1 C56 106.0(3) . . ? C64 B1 C56 110.5(3) . . ? C48 B1 C72 112.1(3) . . ? C64 B1 C72 107.3(3) . . ? C56 B1 C72 110.4(3) . . ? C49 C48 C53 115.3(3) . . ? C49 C48 B1 124.7(3) . . ? C53 C48 B1 119.9(3) . . ? C50 C49 C48 122.2(3) . . ? C50 C49 H49 118.9 . . ? C48 C49 H49 118.9 . . ? C51 C50 C49 120.9(3) . . ? C51 C50 C54 120.4(4) . . ? C49 C50 C54 118.6(4) . . ? C50 C51 C52 118.1(3) . . ? C50 C51 H51 120.9 . . ? C52 C51 H51 120.9 . . ? C53 C52 C51 120.8(4) . . ? C53 C52 C55 120.1(3) . . ? C51 C52 C55 119.2(3) . . ? C52 C53 C48 122.6(3) . . ? C52 C53 H53 118.7 . . ? C48 C53 H53 118.7 . . ? F3B C54 F1 123.9(11) . . ? F3B C54 F2 74.6(9) . . ? F1 C54 F2 108.8(5) . . ? F3B C54 F1B 106.1(11) . . ? F2 C54 F1B 129.3(10) . . ? F3B C54 F2B 109.4(9) . . ? F1 C54 F2B 76.0(9) . . ? F1B C54 F2B 103.0(9) . . ? F1 C54 F3 105.6(5) . . ? F2 C54 F3 103.0(4) . . ? F1B C54 F3 81.0(10) . . ? F2B C54 F3 132.2(8) . . ? F3B C54 C50 115.9(9) . . ? F1 C54 C50 113.4(5) . . ? F2 C54 C50 112.9(4) . . ? F1B C54 C50 111.6(10) . . ? F2B C54 C50 110.1(7) . . ? F3 C54 C50 112.3(4) . . ? F6B C55 F5B 114.2(7) . . ? F6B C55 F5 132.5(6) . . ? F5B C55 F5 46.3(5) . . ? F6B C55 F4 57.0(5) . . ? F5B C55 F4 136.3(6) . . ? F5 C55 F4 104.4(5) . . ? F6B C55 F4B 110.2(7) . . ? F5B C55 F4B 105.9(7) . . ? F5 C55 F4B 59.8(5) . . ? F4 C55 F4B 54.3(5) . . ? F6B C55 F6 51.4(5) . . ? F5B C55 F6 64.3(6) . . ? F5 C55 F6 101.0(5) . . ? F4 C55 F6 101.6(5) . . ? F4B C55 F6 136.1(5) . . ? F6B C55 C52 110.7(5) . . ? F5B C55 C52 107.2(5) . . ? F5 C55 C52 116.5(4) . . ? F4 C55 C52 115.9(4) . . ? F4B C55 C52 108.5(5) . . ? F6 C55 C52 115.3(4) . . ? C61 C56 C57 115.0(3) . . ? C61 C56 B1 125.6(3) . . ? C57 C56 B1 119.4(3) . . ? C58 C57 C56 123.0(3) . . ? C58 C57 H57 118.5 . . ? C56 C57 H57 118.5 . . ? C57 C58 C59 120.4(3) . . ? C57 C58 C62 119.5(3) . . ? C59 C58 C62 120.1(3) . . ? C60 C59 C58 118.3(3) . . ? C60 C59 H59 120.9 . . ? C58 C59 H59 120.9 . . ? C59 C60 C61 121.2(3) . . ? C59 C60 C63 117.7(3) . . ? C61 C60 C63 121.1(3) . . ? C60 C61 C56 122.2(3) . . ? C60 C61 H61 118.9 . . ? C56 C61 H61 118.9 . . ? F8B C62 F9 129.8(8) . . ? F8B C62 F9B 105.9(10) . . ? F8B C62 F7 57.6(11) . . ? F9 C62 F7 108.9(4) . . ? F9B C62 F7 130.9(9) . . ? F8B C62 F8 47.9(11) . . ? F9 C62 F8 105.0(4) . . ? F9B C62 F8 65.2(11) . . ? F7 C62 F8 103.5(4) . . ? F8B C62 F7B 105.2(10) . . ? F9 C62 F7B 63.7(9) . . ? F9B C62 F7B 103.0(10) . . ? F7 C62 F7B 51.3(8) . . ? F8 C62 F7B 137.0(7) . . ? F8B C62 C58 116.0(8) . . ? F9 C62 C58 113.5(3) . . ? F9B C62 C58 115.1(9) . . ? F7 C62 C58 113.4(3) . . ? F8 C62 C58 111.8(3) . . ? F7B C62 C58 110.5(6) . . ? F11B C63 F12 84.3(9) . . ? F11B C63 F10 119.0(13) . . ? F12 C63 F10 107.1(10) . . ? F11B C63 F10B 105.4(8) . . ? F12 C63 F10B 120.5(14) . . ? F11B C63 F12B 107.9(8) . . ? F10 C63 F12B 90.4(12) . . ? F10B C63 F12B 107.4(9) . . ? F12 C63 F11 105.6(8) . . ? F10 C63 F11 106.2(9) . . ? F10B C63 F11 89.4(11) . . ? F12B C63 F11 128.3(9) . . ? F11B C63 C60 114.5(8) . . ? F12 C63 C60 115.9(9) . . ? F10 C63 C60 112.8(11) . . ? F10B C63 C60 112.4(10) . . ? F12B C63 C60 108.9(8) . . ? F11 C63 C60 108.6(10) . . ? C69 C64 C65 115.2(3) . . ? C69 C64 B1 124.9(3) . . ? C65 C64 B1 119.9(3) . . ? C66 C65 C64 122.7(3) . . ? C66 C65 H65 118.6 . . ? C64 C65 H65 118.6 . . ? C65 C66 C67 120.5(3) . . ? C65 C66 C70 121.8(3) . . ? C67 C66 C70 117.7(3) . . ? C68 C67 C66 118.2(3) . . ? C68 C67 H67 120.9 . . ? C66 C67 H67 120.9 . . ? C67 C68 C69 120.9(3) . . ? C67 C68 C71 119.0(3) . . ? C69 C68 C71 120.1(3) . . ? C68 C69 C64 122.5(3) . . ? C68 C69 H69 118.8 . . ? C64 C69 H69 118.8 . . ? F13B C70 F14 117.5(14) . . ? F13B C70 F15 86.6(11) . . ? F14 C70 F15 106.6(10) . . ? F13B C70 F14B 108.3(8) . . ? F15 C70 F14B 124.3(12) . . ? F13B C70 F15B 105.6(7) . . ? F14 C70 F15B 87.0(11) . . ? F14B C70 F15B 105.8(7) . . ? F14 C70 F13 104.3(10) . . ? F15 C70 F13 106.7(10) . . ? F14B C70 F13 91.1(11) . . ? F15B C70 F13 123.5(11) . . ? F13B C70 C66 114.1(7) . . ? F14 C70 C66 116.3(12) . . ? F15 C70 C66 111.3(10) . . ? F14B C70 C66 110.2(7) . . ? F15B C70 C66 112.3(6) . . ? F13 C70 C66 111.1(10) . . ? F16 C71 F17 114.0(10) . . ? F16 C71 F18B 113.2(12) . . ? F17 C71 F18B 73.0(7) . . ? F17 C71 F16B 128.3(8) . . ? F18B C71 F16B 104.8(6) . . ? F16 C71 F17B 84.4(8) . . ? F18B C71 F17B 106.4(4) . . ? F16B C71 F17B 102.1(5) . . ? F16 C71 F18 105.5(10) . . ? F17 C71 F18 98.4(7) . . ? F16B C71 F18 91.4(8) . . ? F17B C71 F18 131.3(6) . . ? F16 C71 C68 118.0(12) . . ? F17 C71 C68 113.7(5) . . ? F18B C71 C68 116.9(5) . . ? F16B C71 C68 112.6(5) . . ? F17B C71 C68 112.6(3) . . ? F18 C71 C68 104.3(7) . . ? C73 C72 C77 115.0(3) . . ? C73 C72 B1 125.2(3) . . ? C77 C72 B1 119.8(3) . . ? C74 C73 C72 122.2(3) . . ? C74 C73 H73 118.9 . . ? C72 C73 H73 118.9 . . ? C75 C74 C73 121.1(3) . . ? C75 C74 C78 119.5(4) . . ? C73 C74 C78 119.3(4) . . ? C74 C75 C76 118.3(3) . . ? C74 C75 H75 120.9 . . ? C76 C75 H75 120.9 . . ? C75 C76 C77 120.4(3) . . ? C75 C76 C79 120.0(3) . . ? C77 C76 C79 119.5(3) . . ? F19 C78 F20B 128.7(5) . . ? F19 C78 F20 108.3(6) . . ? F20B C78 F20 50.9(5) . . ? F19 C78 F21B 52.8(6) . . ? F20B C78 F21B 106.2(7) . . ? F20 C78 F21B 136.5(7) . . ? F19 C78 F19B 54.4(6) . . ? F20B C78 F19B 105.0(7) . . ? F20 C78 F19B 59.4(6) . . ? F21B C78 F19B 105.2(7) . . ? F19 C78 F21 103.3(6) . . ? F20B C78 F21 57.3(5) . . ? F20 C78 F21 106.6(7) . . ? F21B C78 F21 54.7(6) . . ? F19B C78 F21 137.1(6) . . ? F19 C78 C74 115.0(5) . . ? F20B C78 C74 116.4(4) . . ? F20 C78 C74 111.3(5) . . ? F21B C78 C74 112.2(6) . . ? F19B C78 C74 111.1(5) . . ? F21 C78 C74 111.7(4) . . ? F23 C79 F22 105.5(10) . . ? F23 C79 F24 108.6(10) . . ? F22 C79 F24 107.0(10) . . ? F22 C79 F23B 118.1(14) . . ? F24 C79 F23B 91.1(12) . . ? F23 C79 F24B 120.9(14) . . ? F22 C79 F24B 86.9(12) . . ? F23B C79 F24B 105.9(8) . . ? F23 C79 F22B 91.0(13) . . ? F24 C79 F22B 123.4(14) . . ? F23B C79 F22B 106.4(8) . . ? F24B C79 F22B 104.3(7) . . ? F23 C79 C76 112.0(12) . . ? F22 C79 C76 113.9(12) . . ? F24 C79 C76 109.6(11) . . ? F23B C79 C76 114.1(9) . . ? F24B C79 C76 114.6(7) . . ? F22B C79 C76 110.8(7) . . ? C76 C77 C72 122.9(3) . . ? C76 C77 H77 118.6 . . ? C72 C77 H77 118.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.52 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.503 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.056 _publ_requested_category FM _publ_section_references ; Bruker (2004). 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 of dichloromethane and pentane. ; _publ_section_exptl_refinement ; A structural model consisting of the host plus a disordered "BARF" anion plus three disordered dichloromethane molecules was developed; however, positions for the idealized solvate molecules were poorly determined. This model converged with wR2 = 0.1533 and R1 = 0.0754. 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. This model converged with wR2 = 0.1068 and R1 = 0.0427 for 1291 parameters with 2377 restraints against 15916 data. Disorder of the phenyl group in the disulfide ligand on the main molecule was resolved with distances between the atom pairs restrained to possess similar values (esd 0.01). Rigid-bond restraints (esd 0.01) were imposed on displacement parameters. Distances between atom pairs of the disordered and non-disordered portion of the molecule were restrained to possess the same value (esd 0.01). The flourine atoms in the "Barf" anion were restrained so the anisotropic U^ij^ values of the atoms behaved more isotropically (esd 0.01) and similar displacement amplitudes (esd 0.01) were imposed on disordered sites overlapping by less than the sum of van der Waals radii. H atoms were included as riding idealized contributors and the 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 '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 positions for the three dichloromethane solvate molecules were poorly determined. Therefore, 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). The electron count from the "squeeze" model was consistent with three molecules of dichloromethane. This model converged in good agreement with the number of solvate molecules predicted by the complete refinement. ; 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 2.00 1.00 0.1840 0.00 -2.00 -1.00 0.1740 -2.00 -1.00 0.00 0.2620 1.00 0.00 0.00 0.3100 0.00 1.00 -2.00 0.1990 0.00 -1.00 2.00 0.1010 1.00 -2.00 2.00 0.1490 -1.00 2.00 -2.00 0.2140 0.00 1.00 -1.00 0.1760 0.00 -1.00 1.00 0.1510 -1.00 -1.00 1.00 0.2560 -1.00 -1.00 0.00 0.2220 -2.00 1.00 1.00 0.3750 2.00 -1.00 -1.00 0.3730 1.00 2.00 -2.00 0.2080 -1.00 -2.00 2.00 0.1950 1.00 0.00 -2.00 0.3270 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 -0.041 0.286 0.505 240 79 ' ' 2 0.041 0.714 0.494 240 79 ' ' 3 0.331 0.340 0.270 97 38 ' ' 4 0.669 0.660 0.730 97 38 ' '