# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2191 # Neil G. Connelly # data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H20 Fe4 N4 Ni S8' _chemical_formula_weight 951.07 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.6970(10) _cell_length_b 15.1764(10) _cell_length_c 20.0577(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.224(8) _cell_angle_gamma 90.00 _cell_volume 3251.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 278 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 24.99 _exptl_crystal_description cubes _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method ? _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 2.854 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.782 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10179 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3686 _reflns_number_observed 2930 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^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 SHELXL _refine_ls_extinction_coef 0.00039(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3686 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_obs 0.0270 _refine_ls_wR_factor_all 0.0577 _refine_ls_wR_factor_obs 0.0542 _refine_ls_goodness_of_fit_all 0.984 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 0.984 _refine_ls_restrained_S_obs 1.043 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.7500 0.2500 0.5000 0.01929(11) Uani 1 d S . Fe1 Fe 0.34709(3) 0.16117(2) 0.73576(2) 0.02090(10) Uani 1 d . . Fe2 Fe 0.54292(3) 0.05526(2) 0.67331(2) 0.01753(9) Uani 1 d . . S1 S 0.72218(6) 0.34692(4) 0.57734(3) 0.0297(2) Uani 1 d . . S2 S 0.93926(6) 0.23078(4) 0.54317(3) 0.02532(15) Uani 1 d . . S3 S 0.37265(5) 0.01968(4) 0.72667(3) 0.02027(14) Uani 1 d . . S4 S 0.51680(5) 0.19687(4) 0.68120(3) 0.02114(14) Uani 1 d . . N1 N 0.4772(2) 0.4799(2) 0.65174(14) 0.0549(8) Uani 1 d . . N2 N 1.2392(2) 0.1224(2) 0.50941(13) 0.0501(7) Uani 1 d . . C1 C 1.0046(2) 0.1582(2) 0.48767(12) 0.0244(5) Uani 1 d . . C2 C 0.5150(2) 0.4339(2) 0.61243(15) 0.0351(7) Uani 1 d . . C3 C 0.5657(2) 0.3753(2) 0.56457(13) 0.0259(6) Uani 1 d . . C4 C 1.1350(3) 0.1374(2) 0.49906(13) 0.0324(6) Uani 1 d . . C5 C 0.1504(2) 0.1437(2) 0.7441(2) 0.0397(7) Uani 1 d . . H5A H 0.1091(2) 0.0908(2) 0.7629(2) 0.048 Uiso 1 calc R . C6 C 0.1895(3) 0.2183(2) 0.77974(15) 0.0435(8) Uani 1 d . . H6A H 0.1810(3) 0.2283(2) 0.82855(15) 0.052 Uiso 1 calc R . C7 C 0.2422(3) 0.2785(2) 0.7348(2) 0.0427(8) Uani 1 d . . H7A H 0.2751(3) 0.3386(2) 0.7460(2) 0.051 Uiso 1 calc R . C8 C 0.2321(2) 0.2399(2) 0.67009(14) 0.0353(7) Uani 1 d . . H8A H 0.2571(2) 0.2676(2) 0.62763(14) 0.042 Uiso 1 calc R . C9 C 0.1753(2) 0.1569(2) 0.67655(14) 0.0344(7) Uani 1 d . . H9A H 0.1548(2) 0.1147(2) 0.63925(14) 0.041 Uiso 1 calc R . C10 C 0.5468(2) -0.0622(2) 0.61913(12) 0.0273(6) Uani 1 d . . H10A H 0.5189(2) -0.1213(2) 0.63467(12) 0.033 Uiso 1 calc R . C10 C 0.6705(2) -0.0288(2) 0.62555(13) 0.0284(6) Uani 1 d . . H10B H 0.7446(2) -0.0593(2) 0.64773(13) 0.034 Uiso 1 calc R . C12 C 0.5485(3) 0.0726(2) 0.56783(12) 0.0295(6) Uani 1 d . . H12A H 0.5218(3) 0.1265(2) 0.54218(12) 0.035 Uiso 1 calc R . C13 C 0.6714(2) 0.0541(2) 0.59435(12) 0.0290(6) Uani 1 d . . H13A H 0.7460(2) 0.0933(2) 0.59124(12) 0.035 Uiso 1 calc R . C14 C 0.4709(2) 0.0008(2) 0.58293(12) 0.0280(6) Uani 1 d . . H14A H 0.3803(2) -0.0061(2) 0.56868(12) 0.034 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0174(2) 0.0190(2) 0.0217(2) 0.0009(2) 0.0029(2) -0.0007(2) Fe1 0.0222(2) 0.0227(2) 0.0175(2) 0.00167(14) -0.00041(13) 0.00015(14) Fe2 0.0188(2) 0.0192(2) 0.0147(2) 0.00037(13) 0.00184(13) -0.00263(13) S1 0.0197(3) 0.0330(4) 0.0361(4) -0.0119(3) 0.0005(3) -0.0003(3) S2 0.0227(3) 0.0303(4) 0.0228(3) -0.0035(3) -0.0002(2) 0.0046(3) S3 0.0193(3) 0.0234(3) 0.0183(3) -0.0033(2) 0.0031(2) -0.0034(2) S4 0.0250(3) 0.0207(3) 0.0179(3) 0.0029(2) 0.0027(2) 0.0024(2) N1 0.0323(15) 0.069(2) 0.063(2) -0.035(2) -0.0018(13) 0.0098(13) N2 0.0344(15) 0.073(2) 0.042(2) -0.0146(14) -0.0034(11) 0.0214(13) C1 0.0225(13) 0.0256(13) 0.0253(14) 0.0013(11) 0.0044(10) 0.0032(10) C2 0.0210(14) 0.041(2) 0.044(2) -0.0116(14) 0.0000(12) -0.0009(12) C3 0.0225(13) 0.0253(13) 0.030(2) -0.0032(11) 0.0064(10) 0.0002(10) C4 0.032(2) 0.042(2) 0.0232(15) -0.0065(12) -0.0004(11) 0.0084(12) C5 0.0181(14) 0.057(2) 0.044(2) 0.014(2) 0.0000(12) 0.0044(13) C6 0.035(2) 0.069(2) 0.026(2) 0.002(2) 0.0026(12) 0.026(2) C7 0.041(2) 0.031(2) 0.055(2) -0.0055(14) -0.0146(14) 0.0160(13) C8 0.033(2) 0.043(2) 0.029(2) 0.0126(13) -0.0028(11) 0.0119(13) C9 0.0239(14) 0.044(2) 0.034(2) -0.0003(13) -0.0108(11) 0.0069(12) C10 0.040(2) 0.0234(13) 0.0197(14) -0.0067(10) 0.0090(11) -0.0043(11) C10 0.0278(14) 0.0328(14) 0.0252(15) -0.0054(11) 0.0083(11) 0.0052(11) C12 0.048(2) 0.0290(14) 0.0123(13) -0.0017(10) 0.0066(11) -0.0022(12) C13 0.0314(14) 0.036(2) 0.0210(14) -0.0055(11) 0.0120(11) -0.0090(12) C14 0.0315(15) 0.038(2) 0.0148(13) -0.0092(11) 0.0022(10) -0.0058(12) _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 S1 2.1703(6) 7_656 ? Ni1 S1 2.1703(6) . ? Ni1 S2 2.1763(6) . ? Ni1 S2 2.1764(6) 7_656 ? Fe1 C7 2.103(3) . ? Fe1 C8 2.120(3) . ? Fe1 C6 2.130(3) . ? Fe1 C9 2.132(3) . ? Fe1 C5 2.136(3) . ? Fe1 S3 2.1735(7) . ? Fe1 S4 2.2170(7) 2_656 ? Fe1 S4 2.2383(6) . ? Fe1 Fe2 2.6558(5) 2_656 ? Fe1 Fe2 2.9725(5) . ? Fe2 C10 2.090(2) . ? Fe2 C14 2.099(2) . ? Fe2 C10 2.134(2) . ? Fe2 C12 2.136(2) . ? Fe2 C13 2.154(2) . ? Fe2 S4 2.1741(7) . ? Fe2 S3 2.2199(7) 2_656 ? Fe2 S3 2.2301(6) . ? Fe2 Fe1 2.6557(5) 2_656 ? S1 C3 1.733(3) . ? S2 C1 1.740(2) . ? S3 Fe2 2.2199(7) 2_656 ? S4 Fe1 2.2169(7) 2_656 ? N1 C2 1.145(3) . ? N2 C4 1.146(3) . ? C1 C3 1.354(4) 7_656 ? C1 C4 1.436(3) . ? C2 C3 1.436(3) . ? C3 C1 1.354(4) 7_656 ? C5 C6 1.391(4) . ? C5 C9 1.411(4) . ? C6 C7 1.422(4) . ? C7 C8 1.422(4) . ? C8 C9 1.407(4) . ? C10 C10 1.416(4) . ? C10 C14 1.426(4) . ? C10 C13 1.406(4) . ? C12 C14 1.413(3) . ? C12 C13 1.418(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni1 S1 180.0 7_656 . ? S1 Ni1 S2 91.82(2) 7_656 . ? S1 Ni1 S2 88.18(2) . . ? S1 Ni1 S2 88.18(2) 7_656 7_656 ? S1 Ni1 S2 91.82(2) . 7_656 ? S2 Ni1 S2 180.0 . 7_656 ? C7 Fe1 C8 39.35(11) . . ? C7 Fe1 C6 39.25(12) . . ? C8 Fe1 C6 65.35(11) . . ? C7 Fe1 C9 65.05(11) . . ? C8 Fe1 C9 38.65(10) . . ? C6 Fe1 C9 64.27(11) . . ? C7 Fe1 C5 65.11(12) . . ? C8 Fe1 C5 65.12(11) . . ? C6 Fe1 C5 38.05(12) . . ? C9 Fe1 C5 38.59(11) . . ? C7 Fe1 S3 154.79(9) . . ? C8 Fe1 S3 125.16(8) . . ? C6 Fe1 S3 122.89(10) . . ? C9 Fe1 S3 91.82(8) . . ? C5 Fe1 S3 90.74(9) . . ? C7 Fe1 S4 97.34(9) . 2_656 ? C8 Fe1 S4 131.53(8) . 2_656 ? C6 Fe1 S4 95.22(9) . 2_656 ? C9 Fe1 S4 159.23(8) . 2_656 ? C5 Fe1 S4 125.40(9) . 2_656 ? S3 Fe1 S4 102.94(3) . 2_656 ? C7 Fe1 S4 103.72(9) . . ? C8 Fe1 S4 91.04(8) . . ? C6 Fe1 S4 141.84(10) . . ? C9 Fe1 S4 115.61(8) . . ? C5 Fe1 S4 153.87(8) . . ? S3 Fe1 S4 95.09(2) . . ? S4 Fe1 S4 77.98(3) 2_656 . ? C7 Fe1 Fe2 137.23(9) . 2_656 ? C8 Fe1 Fe2 170.77(8) . 2_656 ? C6 Fe1 Fe2 106.99(8) . 2_656 ? C9 Fe1 Fe2 134.33(8) . 2_656 ? C5 Fe1 Fe2 105.72(8) . 2_656 ? S3 Fe1 Fe2 53.61(2) . 2_656 ? S4 Fe1 Fe2 52.05(2) 2_656 2_656 ? S4 Fe1 Fe2 98.17(2) . 2_656 ? C7 Fe1 Fe2 147.31(9) . . ? C8 Fe1 Fe2 116.16(8) . . ? C6 Fe1 Fe2 170.87(10) . . ? C9 Fe1 Fe2 110.76(8) . . ? C5 Fe1 Fe2 133.34(9) . . ? S3 Fe1 Fe2 48.36(2) . . ? S4 Fe1 Fe2 90.01(2) 2_656 . ? S4 Fe1 Fe2 46.74(2) . . ? Fe2 Fe1 Fe2 70.527(14) 2_656 . ? C10 Fe2 C14 39.81(10) . . ? C10 Fe2 C10 39.15(10) . . ? C14 Fe2 C10 65.78(10) . . ? C10 Fe2 C12 65.64(10) . . ? C14 Fe2 C12 38.97(9) . . ? C10 Fe2 C12 64.84(10) . . ? C10 Fe2 C13 65.07(9) . . ? C14 Fe2 C13 65.18(10) . . ? C10 Fe2 C13 38.26(10) . . ? C12 Fe2 C13 38.59(10) . . ? C10 Fe2 S4 152.58(8) . . ? C14 Fe2 S4 114.20(8) . . ? C10 Fe2 S4 135.37(7) . . ? C12 Fe2 S4 87.78(7) . . ? C13 Fe2 S4 98.71(7) . . ? C10 Fe2 S3 104.09(8) . 2_656 ? C14 Fe2 S3 142.70(8) . 2_656 ? C10 Fe2 S3 91.28(8) . 2_656 ? C12 Fe2 S3 153.18(8) . 2_656 ? C13 Fe2 S3 114.74(8) . 2_656 ? S4 Fe2 S3 102.83(3) . 2_656 ? C10 Fe2 S3 94.81(7) . . ? C14 Fe2 S3 92.82(7) . . ? C10 Fe2 S3 129.11(7) . . ? C12 Fe2 S3 125.04(8) . . ? C13 Fe2 S3 157.32(7) . . ? S4 Fe2 S3 95.31(2) . . ? S3 Fe2 S3 79.00(3) 2_656 . ? C10 Fe2 Fe1 148.48(8) . 2_656 ? C14 Fe2 Fe1 163.42(7) . 2_656 ? C10 Fe2 Fe1 113.59(8) . 2_656 ? C12 Fe2 Fe1 124.73(7) . 2_656 ? C13 Fe2 Fe1 103.51(7) . 2_656 ? S4 Fe2 Fe1 53.53(2) . 2_656 ? S3 Fe2 Fe1 52.01(2) 2_656 2_656 ? S3 Fe2 Fe1 99.16(2) . 2_656 ? C10 Fe2 Fe1 135.70(7) . . ? C14 Fe2 Fe1 110.11(7) . . ? C10 Fe2 Fe1 174.85(7) . . ? C12 Fe2 Fe1 114.23(7) . . ? C13 Fe2 Fe1 143.89(7) . . ? S4 Fe2 Fe1 48.57(2) . . ? S3 Fe2 Fe1 90.64(2) 2_656 . ? S3 Fe2 Fe1 46.75(2) . . ? Fe1 Fe2 Fe1 71.268(15) 2_656 . ? C3 S1 Ni1 103.47(9) . . ? C1 S2 Ni1 103.19(9) . . ? Fe1 S3 Fe2 74.38(2) . 2_656 ? Fe1 S3 Fe2 84.90(2) . . ? Fe2 S3 Fe2 94.19(2) 2_656 . ? Fe2 S4 Fe1 74.42(2) . 2_656 ? Fe2 S4 Fe1 84.69(2) . . ? Fe1 S4 Fe1 95.16(3) 2_656 . ? C3 C1 C4 122.2(2) 7_656 . ? C3 C1 S2 120.5(2) 7_656 . ? C4 C1 S2 117.3(2) . . ? N1 C2 C3 178.2(3) . . ? C1 C3 C2 122.4(2) 7_656 . ? C1 C3 S1 120.7(2) 7_656 . ? C2 C3 S1 116.9(2) . . ? N2 C4 C1 178.2(3) . . ? C6 C5 C9 108.1(3) . . ? C6 C5 Fe1 70.7(2) . . ? C9 C5 Fe1 70.54(15) . . ? C5 C6 C7 108.4(3) . . ? C5 C6 Fe1 71.2(2) . . ? C7 C6 Fe1 69.4(2) . . ? C6 C7 C8 107.5(3) . . ? C6 C7 Fe1 71.4(2) . . ? C8 C7 Fe1 70.9(2) . . ? C9 C8 C7 107.2(3) . . ? C9 C8 Fe1 71.16(15) . . ? C7 C8 Fe1 69.7(2) . . ? C8 C9 C5 108.8(3) . . ? C8 C9 Fe1 70.2(2) . . ? C5 C9 Fe1 70.9(2) . . ? C10 C10 C14 108.0(2) . . ? C10 C10 Fe2 72.12(14) . . ? C14 C10 Fe2 70.46(14) . . ? C13 C10 C10 108.0(2) . . ? C13 C10 Fe2 71.64(14) . . ? C10 C10 Fe2 68.73(13) . . ? C14 C12 C13 108.1(2) . . ? C14 C12 Fe2 69.11(14) . . ? C13 C12 Fe2 71.39(14) . . ? C10 C13 C12 108.4(2) . . ? C10 C13 Fe2 70.09(13) . . ? C12 C13 Fe2 70.01(13) . . ? C12 C14 C10 107.5(2) . . ? C12 C14 Fe2 71.92(14) . . ? C10 C14 Fe2 69.73(14) . . ? _refine_diff_density_max 0.348 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.078 #=END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H40 Fe8 N4 Ni S12' _chemical_formula_weight 1563.07 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6645(11) _cell_length_b 16.224(2) _cell_length_c 15.863(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.836(10) _cell_angle_gamma 90.00 _cell_volume 2695.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 369 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 24.97 _exptl_crystal_description diamonds _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method ? _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 2.933 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.643 _exptl_absorpt_correction_T_max 0.887 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7640 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6171 _reflns_number_observed 5166 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+1.3834P] 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 6162 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_obs 0.0448 _refine_ls_wR_factor_all 0.1449 _refine_ls_wR_factor_obs 0.1311 _refine_ls_goodness_of_fit_all 1.256 _refine_ls_goodness_of_fit_obs 1.255 _refine_ls_restrained_S_all 1.263 _refine_ls_restrained_S_obs 1.255 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.5000 0.0000 -0.5000 0.0437(2) Uani 1 d S . Fe1 Fe 0.13570(5) 0.20897(3) -0.43828(3) 0.03046(15) Uani 1 d . . Fe2 Fe 0.31530(5) 0.37333(3) -0.37811(3) 0.02833(14) Uani 1 d . . Fe3 Fe 0.08657(5) 0.38436(3) -0.33522(3) 0.02835(14) Uani 1 d . . Fe4 Fe 0.26911(5) 0.22041(3) -0.28064(3) 0.02789(14) Uani 1 d . . S1 S 0.61328(13) 0.04133(8) -0.37948(8) 0.0534(3) Uani 1 d . . S2 S 0.55276(15) 0.10764(9) -0.56709(9) 0.0598(3) Uani 1 d . . S3 S 0.12664(9) 0.34667(6) -0.46064(6) 0.0332(2) Uani 1 d . . S4 S 0.06298(8) 0.24696(6) -0.32383(6) 0.0314(2) Uani 1 d . . S5 S 0.26729(9) 0.35491(5) -0.25157(5) 0.0285(2) Uani 1 d . . S6 S 0.33827(9) 0.23862(5) -0.40062(6) 0.0295(2) Uani 1 d . . N1 N 0.7549(6) 0.2303(4) -0.2737(4) 0.086(2) Uani 1 d . . N2 N 0.7117(5) 0.3116(3) -0.5228(4) 0.0730(14) Uani 1 d . . C1 C 0.6577(4) 0.1406(3) -0.4024(3) 0.0481(10) Uani 1 d . . C2 C 0.6345(4) 0.1685(3) -0.4845(3) 0.0496(11) Uani 1 d . . C3 C 0.7136(5) 0.1911(4) -0.3320(4) 0.0614(13) Uani 1 d . . C4 C 0.6777(5) 0.2479(3) -0.5056(4) 0.0535(11) Uani 1 d . . C5 C 0.1719(6) 0.1169(5) -0.5236(6) 0.089(3) Uani 1 d . . H5A H 0.2557(6) 0.1036(5) -0.5368(6) 0.106 Uiso 1 calc R . C6 C 0.1182(11) 0.0804(4) -0.4610(6) 0.110(4) Uani 1 d . . H6A H 0.1551(11) 0.0362(4) -0.4220(6) 0.132 Uiso 1 calc R . C7 C -0.0025(9) 0.1158(5) -0.4670(5) 0.100(3) Uani 1 d . . H7A H -0.0669(9) 0.1010(5) -0.4330(5) 0.120 Uiso 1 calc R . C8 C -0.0166(6) 0.1716(4) -0.5321(5) 0.077(2) Uani 1 d . . H8A H -0.0937(6) 0.2040(4) -0.5529(5) 0.092 Uiso 1 calc R . C9 C 0.0894(7) 0.1723(4) -0.5657(4) 0.076(2) Uani 1 d . . H9A H 0.1024(7) 0.2050(4) -0.6153(4) 0.091 Uiso 1 calc R . C10 C 0.4641(7) 0.4537(4) -0.3216(4) 0.079(2) Uani 1 d . . H10A H 0.4931(7) 0.4617(4) -0.2598(4) 0.095 Uiso 1 calc R . C11 C 0.5113(5) 0.3964(3) -0.3702(4) 0.0598(14) Uani 1 d . . H11A H 0.5811(5) 0.3577(3) -0.3500(4) 0.072 Uiso 1 calc R . C12 C 0.4494(5) 0.4062(4) -0.4529(3) 0.0598(15) Uani 1 d . . H12A H 0.4672(5) 0.3746(4) -0.5020(3) 0.072 Uiso 1 calc R . C13 C 0.3631(6) 0.4690(5) -0.4580(6) 0.094(3) Uani 1 d . . H13A H 0.3096(6) 0.4911(5) -0.5101(6) 0.112 Uiso 1 calc R . C14 C 0.3729(8) 0.4993(3) -0.3722(7) 0.099(3) Uani 1 d . . H14A H 0.3261(8) 0.5460(3) -0.3540(7) 0.119 Uiso 1 calc R . C15 C -0.0421(7) 0.4777(4) -0.3874(4) 0.080(2) Uani 1 d . . H15A H -0.0627(7) 0.4949(4) -0.4477(4) 0.097 Uiso 1 calc R . C16 C 0.0528(7) 0.5129(4) -0.3215(9) 0.113(4) Uani 1 d . . H16A H 0.1110(7) 0.5582(4) -0.3277(9) 0.135 Uiso 1 calc R . C17 C 0.0426(7) 0.4730(5) -0.2485(6) 0.095(3) Uani 1 d . . H17A H 0.0948(7) 0.4845(5) -0.1920(6) 0.115 Uiso 1 calc R . C18 C -0.0498(7) 0.4180(4) -0.2636(4) 0.071(2) Uani 1 d . . H18A H -0.0775(7) 0.3836(4) -0.2197(4) 0.085 Uiso 1 calc R . C19 C -0.1045(5) 0.4184(3) -0.3483(4) 0.0579(13) Uani 1 d . . H19A H -0.1786(5) 0.3859(3) -0.3756(4) 0.070 Uiso 1 calc R . C20 C 0.4361(5) 0.1771(5) -0.2022(5) 0.086(2) Uani 1 d . . H20A H 0.5224(5) 0.1990(5) -0.1993(5) 0.103 Uiso 1 calc R . C21 C 0.3513(7) 0.1992(3) -0.1501(3) 0.066(2) Uani 1 d . . H21A H 0.3662(7) 0.2411(3) -0.1048(3) 0.080 Uiso 1 calc R . C22 C 0.2445(6) 0.1510(4) -0.1708(4) 0.0623(15) Uani 1 d . . H22A H 0.1698(6) 0.1532(4) -0.1432(4) 0.075 Uiso 1 calc R . C23 C 0.2604(7) 0.0979(3) -0.2353(4) 0.068(2) Uani 1 d . . H23A H 0.1999(7) 0.0553(3) -0.2609(4) 0.081 Uiso 1 calc R . C24 C 0.3791(8) 0.1130(4) -0.2558(4) 0.085(3) Uani 1 d . . H24A H 0.4183(8) 0.0823(4) -0.2973(4) 0.102 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0441(4) 0.0435(4) 0.0467(4) 0.0091(3) 0.0164(4) 0.0107(3) Fe1 0.0296(3) 0.0282(3) 0.0344(3) -0.0073(2) 0.0080(2) -0.0024(2) Fe2 0.0324(3) 0.0240(3) 0.0301(3) -0.0008(2) 0.0097(2) -0.0047(2) Fe3 0.0297(3) 0.0262(3) 0.0289(3) -0.0004(2) 0.0050(2) 0.0059(2) Fe4 0.0293(3) 0.0243(3) 0.0313(3) 0.0051(2) 0.0087(2) 0.0034(2) S1 0.0618(7) 0.0541(7) 0.0468(6) 0.0103(5) 0.0163(6) 0.0054(6) S2 0.0689(9) 0.0572(7) 0.0520(7) 0.0163(6) 0.0081(6) -0.0040(6) S3 0.0389(5) 0.0329(4) 0.0266(4) 0.0001(3) 0.0034(4) 0.0030(4) S4 0.0272(4) 0.0300(4) 0.0392(5) -0.0017(3) 0.0121(4) 0.0004(3) S5 0.0316(4) 0.0274(4) 0.0258(4) 0.0002(3) 0.0039(3) 0.0013(3) S6 0.0286(4) 0.0266(4) 0.0358(4) -0.0006(3) 0.0122(4) -0.0003(3) N1 0.087(4) 0.097(4) 0.076(4) -0.020(3) 0.022(3) -0.023(3) N2 0.070(3) 0.054(3) 0.095(4) 0.015(3) 0.016(3) -0.002(2) C1 0.044(2) 0.049(2) 0.056(3) 0.007(2) 0.019(2) 0.011(2) C2 0.040(2) 0.051(3) 0.059(3) 0.010(2) 0.012(2) 0.012(2) C3 0.053(3) 0.067(3) 0.069(3) 0.003(3) 0.024(3) -0.002(2) C4 0.046(3) 0.052(3) 0.061(3) 0.009(2) 0.008(2) 0.008(2) C5 0.052(3) 0.084(5) 0.128(7) -0.079(5) 0.009(4) 0.001(3) C6 0.183(10) 0.028(3) 0.090(5) -0.013(3) -0.044(6) -0.001(4) C7 0.134(7) 0.089(5) 0.093(5) -0.055(4) 0.062(5) -0.084(5) C8 0.047(3) 0.080(4) 0.094(5) -0.051(4) -0.012(3) -0.001(3) C9 0.105(5) 0.075(4) 0.048(3) -0.032(3) 0.016(3) -0.029(4) C10 0.098(5) 0.079(4) 0.066(4) -0.027(3) 0.033(3) -0.063(4) C11 0.041(3) 0.054(3) 0.084(4) 0.010(3) 0.009(3) -0.019(2) C12 0.064(3) 0.069(3) 0.055(3) -0.016(3) 0.035(3) -0.036(3) C13 0.055(3) 0.092(5) 0.128(6) 0.079(5) 0.003(4) -0.024(3) C14 0.090(5) 0.026(2) 0.208(10) -0.010(4) 0.096(6) -0.014(3) C15 0.106(5) 0.082(4) 0.062(3) 0.036(3) 0.040(4) 0.073(4) C16 0.062(4) 0.029(3) 0.263(13) -0.017(5) 0.071(6) 0.004(2) C17 0.071(4) 0.093(5) 0.107(6) -0.066(5) -0.022(4) 0.046(4) C18 0.086(4) 0.079(4) 0.058(3) 0.018(3) 0.040(3) 0.052(4) C19 0.033(2) 0.055(3) 0.083(4) -0.017(3) 0.004(2) 0.014(2) C20 0.041(3) 0.106(5) 0.102(5) 0.074(5) -0.008(3) 0.005(3) C21 0.100(5) 0.047(3) 0.043(3) 0.015(2) -0.009(3) 0.009(3) C22 0.071(4) 0.063(3) 0.059(3) 0.033(3) 0.027(3) 0.013(3) C23 0.101(5) 0.031(2) 0.067(3) 0.021(2) 0.005(3) -0.009(3) C24 0.125(6) 0.071(4) 0.069(4) 0.036(3) 0.043(4) 0.070(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.1669(14) 3_654 ? Ni1 S1 2.1669(14) . ? Ni1 S2 2.1735(13) . ? Ni1 S2 2.1736(13) 3_654 ? Fe1 C9 2.076(5) . ? Fe1 C8 2.076(5) . ? Fe1 C5 2.099(5) . ? Fe1 C7 2.100(5) . ? Fe1 C6 2.120(6) . ? Fe1 S6 2.1840(11) . ? Fe1 S4 2.1925(10) . ? Fe1 S3 2.2614(11) . ? Fe1 Fe4 2.6409(9) . ? Fe2 C12 2.092(4) . ? Fe2 C11 2.104(5) . ? Fe2 C10 2.118(5) . ? Fe2 C13 2.126(5) . ? Fe2 C14 2.131(5) . ? Fe2 S5 2.1834(10) . ? Fe2 S3 2.2268(11) . ? Fe2 S6 2.2354(10) . ? Fe2 Fe3 2.6589(8) . ? Fe3 C18 2.080(5) . ? Fe3 C19 2.083(4) . ? Fe3 C17 2.103(6) . ? Fe3 C15 2.106(5) . ? Fe3 C16 2.134(6) . ? Fe3 S5 2.1777(10) . ? Fe3 S3 2.1988(10) . ? Fe3 S4 2.2543(10) . ? Fe4 C20 2.093(5) . ? Fe4 C24 2.096(5) . ? Fe4 C21 2.119(5) . ? Fe4 C23 2.122(4) . ? Fe4 C22 2.132(5) . ? Fe4 S6 2.1867(10) . ? Fe4 S4 2.2183(10) . ? Fe4 S5 2.2311(10) . ? S1 C1 1.736(5) . ? S2 C2 1.739(5) . ? N1 C3 1.140(8) . ? N2 C4 1.146(7) . ? C1 C2 1.357(7) . ? C1 C3 1.424(8) . ? C2 C4 1.428(7) . ? C5 C9 1.343(11) . ? C5 C6 1.371(12) . ? C6 C7 1.396(13) . ? C7 C8 1.359(11) . ? C8 C9 1.337(9) . ? C10 C14 1.358(11) . ? C10 C11 1.364(9) . ? C11 C12 1.363(8) . ? C12 C13 1.365(10) . ? C13 C14 1.433(12) . ? C15 C19 1.381(9) . ? C15 C16 1.430(12) . ? C16 C17 1.348(12) . ? C17 C18 1.317(11) . ? C18 C19 1.361(8) . ? C20 C21 1.383(10) . ? C20 C24 1.406(11) . ? C21 C22 1.369(9) . ? C22 C23 1.372(9) . ? C23 C24 1.387(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni1 S1 180.0 3_654 . ? S1 Ni1 S2 88.24(5) 3_654 . ? S1 Ni1 S2 91.76(5) . . ? S1 Ni1 S2 91.76(5) 3_654 3_654 ? S1 Ni1 S2 88.24(5) . 3_654 ? S2 Ni1 S2 180.0 . 3_654 ? C9 Fe1 C8 37.6(3) . . ? C9 Fe1 C5 37.5(3) . . ? C8 Fe1 C5 62.9(2) . . ? C9 Fe1 C7 63.5(3) . . ? C8 Fe1 C7 38.0(3) . . ? C5 Fe1 C7 63.6(3) . . ? C9 Fe1 C6 63.6(3) . . ? C8 Fe1 C6 63.8(3) . . ? C5 Fe1 C6 37.9(3) . . ? C7 Fe1 C6 38.6(4) . . ? C9 Fe1 S6 111.8(2) . . ? C8 Fe1 S6 149.4(2) . . ? C5 Fe1 S6 92.3(2) . . ? C7 Fe1 S6 146.7(3) . . ? C6 Fe1 S6 108.3(3) . . ? C9 Fe1 S4 146.2(2) . . ? C8 Fe1 S4 109.0(2) . . ? C5 Fe1 S4 150.5(3) . . ? C7 Fe1 S4 92.2(2) . . ? C6 Fe1 S4 112.6(3) . . ? S6 Fe1 S4 101.37(4) . . ? C9 Fe1 S3 97.8(2) . . ? C8 Fe1 S3 99.9(2) . . ? C5 Fe1 S3 127.5(3) . . ? C7 Fe1 S3 132.0(3) . . ? C6 Fe1 S3 161.1(2) . . ? S6 Fe1 S3 80.57(4) . . ? S4 Fe1 S3 80.84(4) . . ? C9 Fe1 Fe4 158.3(2) . . ? C8 Fe1 Fe4 155.3(2) . . ? C5 Fe1 Fe4 121.9(2) . . ? C7 Fe1 Fe4 119.2(3) . . ? C6 Fe1 Fe4 104.2(2) . . ? S6 Fe1 Fe4 52.87(3) . . ? S4 Fe1 Fe4 53.67(3) . . ? S3 Fe1 Fe4 94.51(3) . . ? C12 Fe2 C11 37.9(2) . . ? C12 Fe2 C10 63.0(2) . . ? C11 Fe2 C10 37.7(2) . . ? C12 Fe2 C13 37.8(3) . . ? C11 Fe2 C13 63.8(2) . . ? C10 Fe2 C13 63.8(3) . . ? C12 Fe2 C14 63.8(2) . . ? C11 Fe2 C14 63.4(2) . . ? C10 Fe2 C14 37.3(3) . . ? C13 Fe2 C14 39.3(3) . . ? C12 Fe2 S5 149.3(2) . . ? C11 Fe2 S5 111.8(2) . . ? C10 Fe2 S5 88.9(2) . . ? C13 Fe2 S5 140.5(3) . . ? C14 Fe2 S5 101.9(3) . . ? C12 Fe2 S3 110.8(2) . . ? C11 Fe2 S3 147.9(2) . . ? C10 Fe2 S3 152.9(2) . . ? C13 Fe2 S3 94.8(2) . . ? C14 Fe2 S3 115.7(3) . . ? S5 Fe2 S3 99.89(4) . . ? C12 Fe2 S6 93.0(2) . . ? C11 Fe2 S6 92.6(2) . . ? C10 Fe2 S6 125.0(2) . . ? C13 Fe2 S6 124.9(3) . . ? C14 Fe2 S6 154.9(2) . . ? S5 Fe2 S6 93.71(4) . . ? S3 Fe2 S6 80.22(4) . . ? C12 Fe2 Fe3 152.4(2) . . ? C11 Fe2 Fe3 157.2(2) . . ? C10 Fe2 Fe3 120.0(2) . . ? C13 Fe2 Fe3 116.0(2) . . ? C14 Fe2 Fe3 101.2(2) . . ? S5 Fe2 Fe3 52.34(3) . . ? S3 Fe2 Fe3 52.59(3) . . ? S6 Fe2 Fe3 103.89(3) . . ? C18 Fe3 C19 38.2(2) . . ? C18 Fe3 C17 36.7(3) . . ? C19 Fe3 C17 63.3(2) . . ? C18 Fe3 C15 63.6(2) . . ? C19 Fe3 C15 38.5(3) . . ? C17 Fe3 C15 63.7(3) . . ? C18 Fe3 C16 62.6(3) . . ? C19 Fe3 C16 64.6(2) . . ? C17 Fe3 C16 37.1(3) . . ? C15 Fe3 C16 39.4(3) . . ? C18 Fe3 S5 110.7(2) . . ? C19 Fe3 S5 148.9(2) . . ? C17 Fe3 S5 91.8(2) . . ? C15 Fe3 S5 146.5(3) . . ? C16 Fe3 S5 107.4(3) . . ? C18 Fe3 S3 147.4(2) . . ? C19 Fe3 S3 109.6(2) . . ? C17 Fe3 S3 152.5(3) . . ? C15 Fe3 S3 93.9(2) . . ? C16 Fe3 S3 115.4(4) . . ? S5 Fe3 S3 100.95(4) . . ? C18 Fe3 S4 96.7(2) . . ? C19 Fe3 S4 98.5(2) . . ? C17 Fe3 S4 125.6(3) . . ? C15 Fe3 S4 131.9(3) . . ? C16 Fe3 S4 159.2(2) . . ? S5 Fe3 S4 80.42(4) . . ? S3 Fe3 S4 80.86(4) . . ? C18 Fe3 Fe2 157.9(2) . . ? C19 Fe3 Fe2 156.8(2) . . ? C17 Fe3 Fe2 122.8(3) . . ? C15 Fe3 Fe2 120.6(2) . . ? C16 Fe3 Fe2 105.8(2) . . ? S5 Fe3 Fe2 52.53(3) . . ? S3 Fe3 Fe2 53.56(3) . . ? S4 Fe3 Fe2 94.33(3) . . ? C20 Fe4 C24 39.2(3) . . ? C20 Fe4 C21 38.3(3) . . ? C24 Fe4 C21 64.4(3) . . ? C20 Fe4 C23 64.6(3) . . ? C24 Fe4 C23 38.4(3) . . ? C21 Fe4 C23 63.4(2) . . ? C20 Fe4 C22 63.8(2) . . ? C24 Fe4 C22 63.7(2) . . ? C21 Fe4 C22 37.6(2) . . ? C23 Fe4 C22 37.6(2) . . ? C20 Fe4 S6 100.0(2) . . ? C24 Fe4 S6 90.4(2) . . ? C21 Fe4 S6 136.7(2) . . ? C23 Fe4 S6 117.7(2) . . ? C22 Fe4 S6 153.7(2) . . ? C20 Fe4 S4 158.7(2) . . ? C24 Fe4 S4 135.0(3) . . ? C21 Fe4 S4 122.5(2) . . ? C23 Fe4 S4 100.5(2) . . ? C22 Fe4 S4 95.1(2) . . ? S6 Fe4 S4 100.47(4) . . ? C20 Fe4 S5 104.2(3) . . ? C24 Fe4 S5 143.2(3) . . ? C21 Fe4 S5 88.6(2) . . ? C23 Fe4 S5 147.5(2) . . ? C22 Fe4 S5 109.9(2) . . ? S6 Fe4 S5 93.74(4) . . ? S4 Fe4 S5 80.06(4) . . ? C20 Fe4 Fe1 141.8(3) . . ? C24 Fe4 Fe1 107.6(2) . . ? C21 Fe4 Fe1 164.6(2) . . ? C23 Fe4 Fe1 101.8(2) . . ? C22 Fe4 Fe1 127.6(2) . . ? S6 Fe4 Fe1 52.78(3) . . ? S4 Fe4 Fe1 52.77(3) . . ? S5 Fe4 Fe1 103.91(3) . . ? C1 S1 Ni1 103.4(2) . . ? C2 S2 Ni1 103.1(2) . . ? Fe3 S3 Fe2 73.85(4) . . ? Fe3 S3 Fe1 98.20(4) . . ? Fe2 S3 Fe1 95.31(4) . . ? Fe1 S4 Fe4 73.56(3) . . ? Fe1 S4 Fe3 98.60(4) . . ? Fe4 S4 Fe3 95.61(4) . . ? Fe3 S5 Fe2 75.13(3) . . ? Fe3 S5 Fe4 97.45(4) . . ? Fe2 S5 Fe4 86.06(4) . . ? Fe1 S6 Fe4 74.35(3) . . ? Fe1 S6 Fe2 97.28(4) . . ? Fe4 S6 Fe2 85.87(4) . . ? C2 C1 C3 122.3(5) . . ? C2 C1 S1 120.2(4) . . ? C3 C1 S1 117.4(4) . . ? C1 C2 C4 121.2(5) . . ? C1 C2 S2 120.5(4) . . ? C4 C2 S2 118.3(4) . . ? N1 C3 C1 177.1(6) . . ? N2 C4 C2 179.6(6) . . ? C9 C5 C6 109.0(7) . . ? C9 C5 Fe1 70.3(3) . . ? C6 C5 Fe1 71.9(4) . . ? C5 C6 C7 106.1(7) . . ? C5 C6 Fe1 70.2(3) . . ? C7 C6 Fe1 69.9(3) . . ? C8 C7 C6 107.2(7) . . ? C8 C7 Fe1 70.0(3) . . ? C6 C7 Fe1 71.4(4) . . ? C9 C8 C7 109.1(7) . . ? C9 C8 Fe1 71.2(3) . . ? C7 C8 Fe1 72.0(4) . . ? C8 C9 C5 108.6(7) . . ? C8 C9 Fe1 71.2(3) . . ? C5 C9 Fe1 72.2(4) . . ? C14 C10 C11 109.7(6) . . ? C14 C10 Fe2 71.9(4) . . ? C11 C10 Fe2 70.6(3) . . ? C12 C11 C10 107.5(6) . . ? C12 C11 Fe2 70.6(3) . . ? C10 C11 Fe2 71.7(3) . . ? C11 C12 C13 110.1(6) . . ? C11 C12 Fe2 71.5(3) . . ? C13 C12 Fe2 72.5(3) . . ? C12 C13 C14 105.8(6) . . ? C12 C13 Fe2 69.8(3) . . ? C14 C13 Fe2 70.5(3) . . ? C10 C14 C13 106.9(6) . . ? C10 C14 Fe2 70.8(3) . . ? C13 C14 Fe2 70.1(3) . . ? C19 C15 C16 106.5(6) . . ? C19 C15 Fe3 69.9(3) . . ? C16 C15 Fe3 71.3(3) . . ? C17 C16 C15 106.0(6) . . ? C17 C16 Fe3 70.2(3) . . ? C15 C16 Fe3 69.3(3) . . ? C18 C17 C16 110.3(7) . . ? C18 C17 Fe3 70.7(3) . . ? C16 C17 Fe3 72.7(4) . . ? C17 C18 C19 110.1(6) . . ? C17 C18 Fe3 72.6(4) . . ? C19 C18 Fe3 71.1(3) . . ? C18 C19 C15 107.1(6) . . ? C18 C19 Fe3 70.8(3) . . ? C15 C19 Fe3 71.6(3) . . ? C21 C20 C24 107.2(6) . . ? C21 C20 Fe4 71.9(3) . . ? C24 C20 Fe4 70.5(3) . . ? C22 C21 C20 108.5(6) . . ? C22 C21 Fe4 71.7(3) . . ? C20 C21 Fe4 69.8(3) . . ? C21 C22 C23 108.9(6) . . ? C21 C22 Fe4 70.7(3) . . ? C23 C22 Fe4 70.8(3) . . ? C22 C23 C24 108.0(6) . . ? C22 C23 Fe4 71.6(3) . . ? C24 C23 Fe4 69.8(3) . . ? C23 C24 C20 107.4(5) . . ? C23 C24 Fe4 71.8(3) . . ? C20 C24 Fe4 70.3(3) . . ? _refine_diff_density_max 1.888 _refine_diff_density_min -1.770 _refine_diff_density_rms 0.598 #=END data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H20 Fe4 N8 Pt2 S12' _chemical_formula_weight 1562.90 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.4336(10) _cell_length_b 15.681(2) _cell_length_c 20.781(3) _cell_angle_alpha 99.398(9) _cell_angle_beta 109.254(14) _cell_angle_gamma 103.937(13) _cell_volume 4443.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 167 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 24.89 _exptl_crystal_description plates _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.336 _exptl_crystal_density_method ? _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 8.149 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.911 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21349 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 15053 _reflns_number_observed 12507 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0117P)^2^+36.1636P] 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 15050 _refine_ls_number_parameters 1117 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_obs 0.0402 _refine_ls_wR_factor_all 0.0900 _refine_ls_wR_factor_obs 0.0778 _refine_ls_goodness_of_fit_all 1.184 _refine_ls_goodness_of_fit_obs 1.133 _refine_ls_restrained_S_all 1.185 _refine_ls_restrained_S_obs 1.133 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.77150(2) 0.03455(2) 0.50977(2) 0.02311(8) Uani 1 d . . Pt2 Pt 0.85348(2) 0.05493(2) 0.32800(2) 0.02255(8) Uani 1 d . . Pt3 Pt 0.76548(2) -0.03222(2) 0.14316(2) 0.02353(8) Uani 1 d . . Pt4 Pt 0.51686(3) -0.75156(2) 0.05125(2) 0.02648(9) Uani 1 d . . Fe1 Fe 0.32468(9) -0.42213(8) -0.32042(6) 0.0221(3) Uani 1 d . . Fe2 Fe 0.34267(9) -0.43262(8) -0.44483(6) 0.0224(3) Uani 1 d . . Fe3 Fe 0.49872(9) -0.25282(8) -0.31656(6) 0.0219(3) Uani 1 d . . Fe4 Fe 0.51178(9) -0.41080(8) -0.29172(6) 0.0230(3) Uani 1 d . . Fe5 Fe 0.97254(9) -0.74255(9) -0.09199(7) 0.0276(3) Uani 1 d . . Fe6 Fe 0.84010(9) -0.65435(9) -0.20466(7) 0.0261(3) Uani 1 d . . Fe7 Fe 0.83715(9) -0.84178(8) -0.21729(6) 0.0220(3) Uani 1 d . . Fe8 Fe 1.00303(9) -0.66829(8) -0.21413(7) 0.0254(3) Uani 1 d . . S1 S 0.9316(2) 0.0684(2) 0.53206(13) 0.0321(5) Uani 1 d . . S2 S 0.7777(2) 0.1765(2) 0.49805(13) 0.0313(5) Uani 1 d . . S3 S 0.6102(2) -0.00076(15) 0.48513(13) 0.0309(5) Uani 1 d . . S4 S 0.7630(2) -0.1115(2) 0.51054(13) 0.0297(5) Uani 1 d . . S5 S 1.0103(2) 0.0760(2) 0.34243(12) 0.0286(5) Uani 1 d . . S6 S 0.8700(2) 0.20005(15) 0.32035(12) 0.0285(5) Uani 1 d . . S7 S 0.6971(2) 0.0355(2) 0.31242(12) 0.0279(5) Uani 1 d . . S8 S 0.8344(2) -0.0911(2) 0.33525(12) 0.0279(5) Uani 1 d . . S9 S 0.9221(2) 0.0049(2) 0.15380(12) 0.0295(5) Uani 1 d . . S10 S 0.7655(2) 0.1105(2) 0.13617(12) 0.0289(5) Uani 1 d . . S11 S 0.6094(2) -0.0698(2) 0.13426(12) 0.0278(5) Uani 1 d . . S12 S 0.7673(2) -0.1739(2) 0.15226(13) 0.0293(5) Uani 1 d . . S13 S 0.3613(2) -0.7763(2) 0.04120(12) 0.0306(5) Uani 1 d . . S14 S 0.5089(2) -0.8927(2) 0.06722(14) 0.0353(6) Uani 1 d . . S15 S 0.6678(2) -0.7328(2) 0.05283(13) 0.0342(5) Uani 1 d . . S16 S 0.5245(2) -0.6126(2) 0.03075(13) 0.0314(5) Uani 1 d . . S17 S 0.3795(2) -0.51408(14) -0.37262(12) 0.0249(5) Uani 1 d . . S18 S 0.3377(2) -0.31213(14) -0.37813(11) 0.0243(5) Uani 1 d . . S19 S 0.5030(2) -0.36552(15) -0.39079(11) 0.0239(5) Uani 1 d . . S20 S 0.4567(2) -0.31591(15) -0.24181(11) 0.0250(5) Uani 1 d . . S21 S 0.9861(2) -0.6091(2) -0.11879(12) 0.0327(5) Uani 1 d . . S22 S 0.8546(2) -0.75009(14) -0.28580(11) 0.0247(5) Uani 1 d . . S23 S 0.8207(2) -0.74707(15) -0.13671(12) 0.0271(5) Uani 1 d . . S24 S 0.9970(2) -0.79982(15) -0.18434(11) 0.0235(5) Uani 1 d . . N1 N 1.1352(7) 0.2640(7) 0.5389(6) 0.056(3) Uani 1 d . . N2 N 0.9496(7) 0.3849(6) 0.4917(5) 0.049(2) Uani 1 d . . N3 N 0.3955(7) -0.2054(6) 0.4382(5) 0.047(2) Uani 1 d . . N4 N 0.5732(6) -0.3367(6) 0.4673(5) 0.039(2) Uani 1 d . . N5 N 1.2272(6) 0.2526(6) 0.3565(5) 0.043(2) Uani 1 d . . N6 N 1.0484(7) 0.4070(6) 0.3245(5) 0.047(2) Uani 1 d . . N7 N 0.4769(6) -0.1385(6) 0.3002(5) 0.048(2) Uani 1 d . . N8 N 0.6431(7) -0.2969(6) 0.3203(5) 0.047(2) Uani 1 d . . N9 N 1.1258(6) 0.1973(7) 0.1689(5) 0.052(2) Uani 1 d . . N10 N 0.4187(7) -0.2675(7) 0.1353(5) 0.051(2) Uani 1 d . . N10 N 0.9278(7) 0.3338(6) 0.1497(5) 0.044(2) Uani 1 d . . N11 N 0.6152(7) -0.3920(6) 0.1553(5) 0.049(2) Uani 1 d . . N13 N 0.1533(7) -0.9582(7) 0.0388(5) 0.050(2) Uani 1 d . . N14 N 0.3315(8) -1.0962(7) 0.0747(6) 0.061(3) Uani 1 d . . N15 N 0.8467(7) -0.5824(6) 0.0024(5) 0.047(2) Uani 1 d . . N16 N 0.6857(7) -0.4296(7) -0.0115(6) 0.060(3) Uani 1 d . . C1 C 0.9614(6) 0.1763(6) 0.5220(5) 0.028(2) Uani 1 d . . C2 C 1.0590(7) 0.2214(7) 0.5311(6) 0.038(2) Uani 1 d . . C3 C 0.8940(7) 0.2227(6) 0.5062(5) 0.029(2) Uani 1 d . . C4 C 0.9231(7) 0.3118(7) 0.4971(5) 0.034(2) Uani 1 d . . C5 C 0.5766(7) -0.1165(6) 0.4755(5) 0.027(2) Uani 1 d . . C6 C 0.4751(8) -0.1638(6) 0.4542(5) 0.034(2) Uani 1 d . . C7 C 0.6410(6) -0.1631(6) 0.4858(4) 0.025(2) Uani 1 d . . C8 C 0.6053(7) -0.2606(6) 0.4759(5) 0.031(2) Uani 1 d . . C9 C 1.0487(6) 0.1872(6) 0.3405(4) 0.026(2) Uani 1 d . . C10 C 1.1485(7) 0.2242(6) 0.3499(5) 0.031(2) Uani 1 d . . C11 C 0.9886(6) 0.2411(6) 0.3306(5) 0.026(2) Uani 1 d . . C12 C 1.0222(7) 0.3331(7) 0.3278(5) 0.034(2) Uani 1 d . . C13 C 0.6571(6) -0.0754(6) 0.3151(4) 0.026(2) Uani 1 d . . C14 C 0.5570(7) -0.1099(7) 0.3067(5) 0.035(2) Uani 1 d . . C15 C 0.7154(6) -0.1294(6) 0.3242(5) 0.027(2) Uani 1 d . . C16 C 0.6766(7) -0.2222(6) 0.3238(5) 0.031(2) Uani 1 d . . C17 C 0.9505(7) 0.1179(6) 0.1520(5) 0.030(2) Uani 1 d . . C18 C 1.0470(7) 0.1617(7) 0.1604(5) 0.034(2) Uani 1 d . . C19 C 0.8816(7) 0.1633(6) 0.1447(5) 0.029(2) Uani 1 d . . C20 C 0.9077(6) 0.2585(7) 0.1468(5) 0.027(2) Uani 1 d . . C21 C 0.5850(6) -0.1810(6) 0.1398(4) 0.024(2) Uani 1 d . . C22 C 0.4915(7) -0.2277(7) 0.1364(5) 0.032(2) Uani 1 d . . C23 C 0.6523(6) -0.2256(6) 0.1470(5) 0.028(2) Uani 1 d . . C24 C 0.6310(6) -0.3195(6) 0.1508(5) 0.030(2) Uani 1 d . . C25 C 0.3273(7) -0.8867(7) 0.0473(4) 0.030(2) Uani 1 d . . C26 C 0.2303(8) -0.9259(7) 0.0420(5) 0.036(2) Uani 1 d . . C27 C 0.3922(7) -0.9368(6) 0.0593(5) 0.030(2) Uani 1 d . . C28 C 0.3593(8) -1.0265(7) 0.0664(5) 0.039(2) Uani 1 d . . C29 C 0.6951(7) -0.6323(6) 0.0305(5) 0.029(2) Uani 1 d . . C30 C 0.7812(7) -0.6034(7) 0.0164(5) 0.036(2) Uani 1 d . . C31 C 0.6338(7) -0.5798(6) 0.0222(5) 0.031(2) Uani 1 d . . C32 C 0.6602(7) -0.4962(7) 0.0026(6) 0.038(2) Uani 1 d . . C33 C 0.1842(7) -0.5140(8) -0.3547(6) 0.050(3) Uani 1 d . . H33A H 0.1464(7) -0.5544(8) -0.4024(6) 0.060 Uiso 1 calc R . C34 C 0.1820(7) -0.4265(8) -0.3308(6) 0.044(3) Uani 1 d . . H34A H 0.1424(7) -0.3943(8) -0.3580(6) 0.053 Uiso 1 calc R . C35 C 0.2455(8) -0.3947(7) -0.2602(6) 0.044(3) Uani 1 d . . H35A H 0.2582(8) -0.3351(7) -0.2290(6) 0.053 Uiso 1 calc R . C36 C 0.2848(7) -0.4621(8) -0.2395(6) 0.046(3) Uani 1 d . . H36A H 0.3288(7) -0.4586(8) -0.1920(6) 0.056 Uiso 1 calc R . C37 C 0.2463(8) -0.5365(7) -0.2982(8) 0.051(3) Uani 1 d . . H37A H 0.2592(8) -0.5949(7) -0.2998(8) 0.061 Uiso 1 calc R . C38 C 0.3372(7) -0.4267(6) -0.5453(5) 0.032(2) Uani 1 d . . H38A H 0.3858(7) -0.3862(6) -0.5568(5) 0.038 Uiso 1 calc R . C39 C 0.3326(7) -0.5155(6) -0.5378(5) 0.035(2) Uani 1 d . . H39A H 0.3789(7) -0.5471(6) -0.5421(5) 0.042 Uiso 1 calc R . C40 C 0.2484(7) -0.5525(6) -0.5253(5) 0.038(2) Uani 1 d . . H40A H 0.2268(7) -0.6134(6) -0.5186(5) 0.046 Uiso 1 calc R . C41 C 0.1999(7) -0.4873(7) -0.5260(5) 0.040(2) Uani 1 d . . H41A H 0.1391(7) -0.4939(7) -0.5191(5) 0.048 Uiso 1 calc R . C42 C 0.2541(8) -0.4110(7) -0.5389(5) 0.040(3) Uani 1 d . . H42A H 0.2368(8) -0.3553(7) -0.5426(5) 0.048 Uiso 1 calc R . C43 C 0.6009(8) -0.1425(7) -0.2343(5) 0.042(3) Uani 1 d . . H43A H 0.6249(8) -0.1411(7) -0.1840(5) 0.050 Uiso 1 calc R . C44 C 0.6428(7) -0.1663(6) -0.2811(6) 0.035(2) Uani 1 d . . H44A H 0.7007(7) -0.1855(6) -0.2700(6) 0.042 Uiso 1 calc R . C45 C 0.5888(9) -0.1569(7) -0.3466(6) 0.053(3) Uani 1 d . . H45A H 0.6022(9) -0.1680(7) -0.3896(6) 0.063 Uiso 1 calc R . C46 C 0.5128(9) -0.1272(7) -0.3394(6) 0.053(3) Uani 1 d . . H46A H 0.4645(9) -0.1126(7) -0.3762(6) 0.064 Uiso 1 calc R . C47 C 0.5220(8) -0.1170(7) -0.2695(6) 0.045(3) Uani 1 d . . H47A H 0.4809(8) -0.0942(7) -0.2485(6) 0.054 Uiso 1 calc R . C48 C 0.5461(7) -0.5097(8) -0.2403(6) 0.048(3) Uani 1 d . . H48A H 0.5005(7) -0.5631(8) -0.2374(6) 0.057 Uiso 1 calc R . C49 C 0.5846(9) -0.5052(8) -0.2928(6) 0.056(4) Uani 1 d . . H49A H 0.5702(9) -0.5556(8) -0.3334(6) 0.068 Uiso 1 calc R . C50 C 0.6519(8) -0.4182(10) -0.2747(7) 0.061(4) Uani 1 d . . H50A H 0.6917(8) -0.3967(10) -0.3006(7) 0.073 Uiso 1 calc R . C51 C 0.6550(7) -0.3708(7) -0.2124(7) 0.050(3) Uani 1 d . . H51A H 0.6958(7) -0.3079(7) -0.1869(7) 0.059 Uiso 1 calc R . C52 C 0.5909(8) -0.4256(8) -0.1910(5) 0.043(3) Uani 1 d . . H52A H 0.5797(8) -0.4079(8) -0.1477(5) 0.051 Uiso 1 calc R . C53 C 1.0916(7) -0.7748(8) -0.0239(5) 0.041(3) Uani 1 d . . H53A H 1.1429(7) -0.7896(8) -0.0368(5) 0.050 Uiso 1 calc R . C54 C 1.0928(7) -0.6855(8) 0.0047(5) 0.046(3) Uani 1 d . . H54A H 1.1456(7) -0.6284(8) 0.0181(5) 0.055 Uiso 1 calc R . C55 C 1.0048(7) -0.6976(8) 0.0151(5) 0.042(3) Uani 1 d . . H55A H 0.9858(7) -0.6486(8) 0.0367(5) 0.051 Uiso 1 calc R . C56 C 0.9513(7) -0.7903(8) -0.0066(5) 0.045(3) Uani 1 d . . H56A H 0.8890(7) -0.8171(8) -0.0035(5) 0.054 Uiso 1 calc R . C57 C 1.0056(9) -0.8379(8) -0.0314(5) 0.049(3) Uani 1 d . . H57A H 0.9865(9) -0.9041(8) -0.0502(5) 0.059 Uiso 1 calc R . C58 C 0.8105(11) -0.5526(10) -0.2580(10) 0.075(5) Uani 1 d . . H58A H 0.8470(11) -0.5240(10) -0.2837(10) 0.090 Uiso 1 calc R . C59 C 0.8289(11) -0.5219(10) -0.1877(11) 0.101(7) Uani 1 d . . H59A H 0.8791(11) -0.4665(10) -0.1544(11) 0.122 Uiso 1 calc R . C60 C 0.7595(15) -0.5808(15) -0.1737(8) 0.089(6) Uani 1 d . . H60A H 0.7504(15) -0.5740(15) -0.1288(8) 0.107 Uiso 1 calc R . C61 C 0.7001(9) -0.6462(10) -0.2360(10) 0.071(5) Uani 1 d . . H61A H 0.6414(9) -0.6947(10) -0.2435(10) 0.086 Uiso 1 calc R . C62 C 0.7339(11) -0.6274(10) -0.2853(7) 0.068(4) Uani 1 d . . H62A H 0.7049(11) -0.6624(10) -0.3350(7) 0.081 Uiso 1 calc R . C63 C 0.8291(7) -0.9807(6) -0.2371(6) 0.039(2) Uani 1 d . . H63A H 0.8842(7) -1.0042(6) -0.2263(6) 0.047 Uiso 1 calc R . C64 C 0.7809(7) -0.9633(6) -0.1925(5) 0.040(3) Uani 1 d . . H64A H 0.7970(7) -0.9722(6) -0.1449(5) 0.048 Uiso 1 calc R . C65 C 0.7038(7) -0.9334(6) -0.2281(6) 0.037(2) Uani 1 d . . H65A H 0.6567(7) -0.9183(6) -0.2100(6) 0.044 Uiso 1 calc R . C66 C 0.7061(6) -0.9307(6) -0.2950(5) 0.032(2) Uani 1 d . . H66A H 0.6602(6) -0.9139(6) -0.3320(5) 0.039 Uiso 1 calc R . C67 C 0.7837(7) -0.9601(6) -0.3007(5) 0.034(2) Uani 1 d . . H67A H 0.8007(7) -0.9676(6) -0.3422(5) 0.041 Uiso 1 calc R . C68 C 1.0408(9) -0.5708(11) -0.2676(10) 0.076(5) Uani 1 d . . H68A H 1.0002(9) -0.5363(11) -0.2903(10) 0.092 Uiso 1 calc R . C69 C 1.1064(10) -0.5440(8) -0.1992(8) 0.059(4) Uani 1 d . . H69A H 1.1207(10) -0.4868(8) -0.1646(8) 0.071 Uiso 1 calc R . C70 C 1.1509(8) -0.6080(9) -0.1881(6) 0.051(3) Uani 1 d . . H70A H 1.2027(8) -0.6043(9) -0.1439(6) 0.061 Uiso 1 calc R . C71 C 1.1156(8) -0.6762(8) -0.2482(7) 0.050(3) Uani 1 d . . H71A H 1.1375(8) -0.7295(8) -0.2545(7) 0.060 Uiso 1 calc R . C72 C 1.0438(8) -0.6568(9) -0.3005(6) 0.057(3) Uani 1 d . . H72A H 1.0078(8) -0.6921(9) -0.3500(6) 0.068 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0281(2) 0.0211(2) 0.0225(2) 0.00582(14) 0.00923(14) 0.01247(15) Pt2 0.0252(2) 0.0207(2) 0.0225(2) 0.00633(14) 0.00846(14) 0.00925(14) Pt3 0.0250(2) 0.0256(2) 0.0208(2) 0.00776(14) 0.00772(14) 0.00982(15) Pt4 0.0329(2) 0.0246(2) 0.0229(2) 0.00606(14) 0.0096(2) 0.0125(2) Fe1 0.0225(6) 0.0187(6) 0.0271(7) 0.0080(5) 0.0096(5) 0.0085(5) Fe2 0.0233(6) 0.0200(6) 0.0236(6) 0.0037(5) 0.0082(5) 0.0090(5) Fe3 0.0245(6) 0.0198(6) 0.0213(6) 0.0051(5) 0.0086(5) 0.0074(5) Fe4 0.0249(7) 0.0209(6) 0.0236(6) 0.0066(5) 0.0097(5) 0.0070(5) Fe5 0.0249(7) 0.0316(7) 0.0266(7) 0.0046(6) 0.0105(6) 0.0110(6) Fe6 0.0228(6) 0.0303(7) 0.0249(7) 0.0084(6) 0.0102(5) 0.0057(6) Fe7 0.0222(6) 0.0232(6) 0.0219(6) 0.0082(5) 0.0090(5) 0.0071(5) Fe8 0.0218(6) 0.0190(6) 0.0365(7) 0.0091(5) 0.0117(6) 0.0067(5) S1 0.0299(12) 0.0287(12) 0.0422(14) 0.0115(11) 0.0140(11) 0.0155(10) S2 0.0309(13) 0.0235(12) 0.0443(14) 0.0121(10) 0.0151(11) 0.0140(10) S3 0.0314(13) 0.0200(11) 0.0427(14) 0.0079(10) 0.0137(11) 0.0119(10) S4 0.0325(13) 0.0251(12) 0.0379(13) 0.0117(10) 0.0142(11) 0.0173(10) S5 0.0272(12) 0.0239(12) 0.0346(13) 0.0088(10) 0.0101(10) 0.0101(10) S6 0.0314(12) 0.0221(11) 0.0333(13) 0.0076(10) 0.0120(10) 0.0108(10) S7 0.0292(12) 0.0265(12) 0.0325(12) 0.0113(10) 0.0130(10) 0.0128(10) S8 0.0271(12) 0.0253(12) 0.0324(13) 0.0101(10) 0.0094(10) 0.0117(10) S9 0.0280(12) 0.0321(13) 0.0320(13) 0.0106(10) 0.0123(10) 0.0133(10) S10 0.0289(12) 0.0302(12) 0.0316(13) 0.0148(10) 0.0107(10) 0.0129(10) S11 0.0259(12) 0.0314(12) 0.0287(12) 0.0123(10) 0.0092(10) 0.0125(10) S12 0.0291(12) 0.0271(12) 0.0346(13) 0.0097(10) 0.0125(10) 0.0125(10) S13 0.0328(13) 0.0303(12) 0.0299(12) 0.0102(10) 0.0099(10) 0.0138(10) S14 0.0427(14) 0.0306(13) 0.0436(15) 0.0140(11) 0.0220(12) 0.0202(12) S15 0.0368(14) 0.0318(13) 0.0395(14) 0.0129(11) 0.0146(11) 0.0187(11) S16 0.0329(13) 0.0257(12) 0.0395(14) 0.0116(10) 0.0136(11) 0.0148(10) S17 0.0267(11) 0.0201(11) 0.0289(12) 0.0082(9) 0.0112(10) 0.0072(9) S18 0.0291(12) 0.0179(10) 0.0263(11) 0.0056(9) 0.0090(9) 0.0107(9) S19 0.0249(11) 0.0244(11) 0.0216(11) 0.0038(9) 0.0106(9) 0.0055(9) S20 0.0252(11) 0.0267(12) 0.0226(11) 0.0050(9) 0.0107(9) 0.0064(9) S21 0.0313(13) 0.0297(13) 0.0258(12) 0.0064(10) 0.0073(10) -0.0043(10) S22 0.0266(11) 0.0199(11) 0.0248(11) 0.0079(9) 0.0064(9) 0.0060(9) S23 0.0255(12) 0.0239(11) 0.0366(13) 0.0089(10) 0.0175(10) 0.0077(9) S24 0.0233(11) 0.0244(11) 0.0285(12) 0.0120(9) 0.0127(9) 0.0105(9) N1 0.035(5) 0.047(6) 0.091(8) 0.014(5) 0.033(5) 0.012(5) N2 0.047(6) 0.037(6) 0.068(7) 0.014(5) 0.024(5) 0.017(5) N3 0.048(6) 0.022(4) 0.071(7) 0.008(4) 0.025(5) 0.009(4) N4 0.047(5) 0.028(5) 0.059(6) 0.018(4) 0.034(5) 0.020(4) N5 0.028(5) 0.047(5) 0.054(6) 0.008(4) 0.021(4) 0.006(4) N6 0.047(6) 0.034(5) 0.048(6) 0.018(4) 0.007(5) 0.006(4) N7 0.032(5) 0.053(6) 0.054(6) 0.009(5) 0.017(4) 0.009(4) N8 0.068(7) 0.028(5) 0.045(6) 0.009(4) 0.023(5) 0.014(5) N9 0.033(5) 0.057(6) 0.063(7) 0.019(5) 0.016(5) 0.010(5) N10 0.044(6) 0.059(6) 0.046(6) 0.012(5) 0.021(5) 0.009(5) N10 0.055(6) 0.033(5) 0.048(6) 0.019(4) 0.019(5) 0.019(4) N11 0.057(6) 0.037(5) 0.060(6) 0.021(5) 0.023(5) 0.021(5) N13 0.052(6) 0.058(6) 0.044(6) 0.029(5) 0.016(5) 0.017(5) N14 0.082(8) 0.052(6) 0.087(8) 0.037(6) 0.063(7) 0.033(6) N15 0.050(6) 0.053(6) 0.052(6) 0.014(5) 0.031(5) 0.023(5) N16 0.043(6) 0.060(7) 0.096(8) 0.047(6) 0.032(6) 0.026(5) C1 0.026(5) 0.034(5) 0.025(5) 0.002(4) 0.009(4) 0.011(4) C2 0.037(6) 0.031(5) 0.056(7) 0.014(5) 0.022(5) 0.023(5) C3 0.031(5) 0.019(5) 0.032(5) 0.004(4) 0.009(4) 0.004(4) C4 0.026(5) 0.028(6) 0.040(6) 0.004(4) 0.006(4) 0.009(4) C5 0.034(5) 0.030(5) 0.024(5) 0.007(4) 0.015(4) 0.015(4) C6 0.043(6) 0.025(5) 0.041(6) 0.008(4) 0.019(5) 0.018(5) C7 0.031(5) 0.027(5) 0.025(5) 0.009(4) 0.015(4) 0.017(4) C8 0.047(6) 0.030(6) 0.029(5) 0.008(4) 0.023(5) 0.024(5) C9 0.025(5) 0.028(5) 0.020(4) 0.004(4) 0.004(4) 0.006(4) C10 0.041(6) 0.026(5) 0.031(5) 0.007(4) 0.014(5) 0.015(5) C11 0.030(5) 0.019(4) 0.027(5) 0.006(4) 0.011(4) 0.005(4) C12 0.028(5) 0.040(6) 0.021(5) 0.008(4) 0.000(4) 0.003(4) C13 0.032(5) 0.028(5) 0.021(5) 0.003(4) 0.015(4) 0.008(4) C14 0.040(6) 0.029(5) 0.036(6) 0.007(4) 0.015(5) 0.010(5) C15 0.031(5) 0.024(5) 0.028(5) 0.007(4) 0.010(4) 0.015(4) C16 0.041(6) 0.028(5) 0.027(5) 0.008(4) 0.016(4) 0.012(5) C17 0.036(5) 0.033(5) 0.018(5) 0.008(4) 0.005(4) 0.010(4) C18 0.037(6) 0.039(6) 0.029(5) 0.014(4) 0.013(5) 0.016(5) C19 0.031(5) 0.037(5) 0.026(5) 0.012(4) 0.012(4) 0.017(4) C20 0.015(4) 0.038(6) 0.024(5) 0.010(4) 0.004(4) 0.005(4) C21 0.027(5) 0.022(5) 0.016(4) 0.005(4) 0.002(4) 0.002(4) C22 0.029(5) 0.034(5) 0.033(5) 0.011(4) 0.012(4) 0.011(4) C23 0.025(5) 0.030(5) 0.023(5) 0.000(4) 0.007(4) 0.009(4) C24 0.025(5) 0.030(5) 0.028(5) 0.004(4) 0.004(4) 0.008(4) C25 0.031(5) 0.041(6) 0.017(5) 0.007(4) 0.008(4) 0.009(4) C26 0.038(6) 0.035(6) 0.039(6) 0.013(5) 0.014(5) 0.017(5) C27 0.043(6) 0.030(5) 0.020(5) 0.007(4) 0.013(4) 0.016(4) C28 0.060(7) 0.036(6) 0.033(6) 0.007(5) 0.030(5) 0.021(5) C29 0.030(5) 0.027(5) 0.020(5) -0.001(4) 0.004(4) 0.007(4) C30 0.035(6) 0.038(6) 0.027(5) -0.003(4) 0.005(5) 0.018(5) C31 0.034(5) 0.031(5) 0.027(5) 0.008(4) 0.010(4) 0.012(4) C32 0.037(6) 0.034(6) 0.054(7) 0.022(5) 0.020(5) 0.020(5) C33 0.028(6) 0.047(7) 0.058(7) -0.008(6) 0.025(5) -0.017(5) C34 0.026(5) 0.062(7) 0.067(8) 0.034(6) 0.029(5) 0.025(5) C35 0.045(6) 0.035(6) 0.057(7) 0.001(5) 0.037(6) 0.003(5) C36 0.028(5) 0.074(8) 0.050(7) 0.034(6) 0.025(5) 0.013(6) C37 0.052(7) 0.027(6) 0.109(11) 0.038(7) 0.059(8) 0.022(5) C38 0.042(6) 0.027(5) 0.026(5) 0.008(4) 0.009(4) 0.015(4) C39 0.048(6) 0.032(5) 0.020(5) 0.001(4) 0.003(4) 0.020(5) C40 0.039(6) 0.019(5) 0.035(6) -0.005(4) -0.002(5) 0.004(4) C41 0.023(5) 0.050(7) 0.035(6) 0.003(5) 0.004(4) 0.009(5) C42 0.054(7) 0.041(6) 0.022(5) 0.007(4) 0.004(5) 0.028(5) C43 0.049(7) 0.031(6) 0.025(5) -0.005(4) 0.011(5) -0.010(5) C44 0.033(5) 0.019(5) 0.053(7) 0.009(4) 0.019(5) 0.006(4) C45 0.078(9) 0.019(5) 0.046(7) 0.001(5) 0.029(6) -0.015(6) C46 0.058(8) 0.023(5) 0.059(8) 0.026(5) 0.000(6) 0.001(5) C47 0.049(7) 0.027(5) 0.063(8) 0.001(5) 0.028(6) 0.013(5) C48 0.032(6) 0.047(7) 0.051(7) 0.027(6) -0.006(5) 0.011(5) C49 0.066(8) 0.057(8) 0.038(7) -0.003(6) -0.002(6) 0.047(7) C50 0.040(7) 0.102(11) 0.074(9) 0.061(9) 0.030(7) 0.046(8) C51 0.028(6) 0.029(6) 0.071(9) 0.016(6) -0.003(6) 0.003(5) C52 0.044(6) 0.060(7) 0.027(5) 0.015(5) 0.005(5) 0.032(6) C53 0.028(5) 0.073(8) 0.034(6) 0.024(5) 0.011(4) 0.028(6) C54 0.023(5) 0.063(8) 0.033(6) 0.005(5) -0.004(4) 0.005(5) C55 0.033(6) 0.059(7) 0.030(6) 0.004(5) 0.008(5) 0.018(5) C56 0.025(5) 0.063(8) 0.036(6) 0.018(5) 0.007(5) -0.002(5) C57 0.064(8) 0.046(7) 0.031(6) 0.016(5) 0.010(5) 0.014(6) C58 0.091(11) 0.063(9) 0.154(16) 0.081(11) 0.101(12) 0.061(9) C59 0.057(9) 0.041(8) 0.129(16) -0.048(9) -0.032(10) 0.022(7) C60 0.141(16) 0.160(18) 0.053(9) 0.062(11) 0.065(11) 0.137(15) C61 0.034(7) 0.067(9) 0.130(14) 0.068(10) 0.025(8) 0.026(7) C62 0.098(11) 0.070(10) 0.049(8) 0.030(7) 0.018(8) 0.057(9) C63 0.033(6) 0.019(5) 0.061(7) 0.011(5) 0.012(5) 0.010(4) C64 0.047(6) 0.028(5) 0.037(6) 0.018(5) 0.010(5) -0.001(5) C65 0.023(5) 0.026(5) 0.057(7) 0.006(5) 0.018(5) 0.000(4) C66 0.022(5) 0.026(5) 0.032(5) 0.007(4) -0.004(4) -0.002(4) C67 0.039(6) 0.024(5) 0.032(5) -0.002(4) 0.015(5) 0.001(4) C68 0.055(8) 0.101(11) 0.158(16) 0.113(12) 0.081(10) 0.062(8) C69 0.063(8) 0.030(6) 0.094(11) 0.008(7) 0.061(8) -0.005(6) C70 0.030(6) 0.074(9) 0.043(7) 0.011(6) 0.014(5) 0.009(6) C71 0.053(7) 0.041(6) 0.086(9) 0.033(7) 0.052(7) 0.022(6) C72 0.041(7) 0.073(9) 0.048(7) 0.017(7) 0.025(6) -0.006(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 Pt1 S2 2.261(2) . ? Pt1 S4 2.266(2) . ? Pt1 S1 2.266(2) . ? Pt1 S3 2.274(2) . ? Pt2 S7 2.263(2) . ? Pt2 S6 2.266(2) . ? Pt2 S5 2.271(2) . ? Pt2 S8 2.273(2) . ? Pt3 S10 2.266(2) . ? Pt3 S12 2.267(2) . ? Pt3 S9 2.272(2) . ? Pt3 S11 2.274(2) . ? Pt4 S15 2.265(2) . ? Pt4 S13 2.270(2) . ? Pt4 S16 2.270(2) . ? Pt4 S14 2.272(2) . ? Fe1 C35 2.081(10) . ? Fe1 C33 2.103(9) . ? Fe1 C36 2.108(10) . ? Fe1 C37 2.118(9) . ? Fe1 C34 2.124(9) . ? Fe1 S17 2.158(2) . ? Fe1 S20 2.208(2) . ? Fe1 S18 2.263(2) . ? Fe1 Fe2 2.673(2) . ? Fe1 Fe4 2.703(2) . ? Fe2 C39 2.081(9) . ? Fe2 C38 2.081(9) . ? Fe2 C42 2.117(9) . ? Fe2 C40 2.121(9) . ? Fe2 C41 2.145(9) . ? Fe2 S17 2.149(2) . ? Fe2 S18 2.187(2) . ? Fe2 S19 2.240(2) . ? Fe3 C46 2.078(10) . ? Fe3 C47 2.083(10) . ? Fe3 C43 2.085(9) . ? Fe3 C45 2.111(10) . ? Fe3 C44 2.114(9) . ? Fe3 S20 2.161(2) . ? Fe3 S19 2.177(2) . ? Fe3 S18 2.254(2) . ? Fe3 Fe4 2.652(2) . ? Fe4 C49 2.064(10) . ? Fe4 C48 2.096(10) . ? Fe4 C50 2.107(11) . ? Fe4 C52 2.130(9) . ? Fe4 C51 2.141(10) . ? Fe4 S20 2.167(2) . ? Fe4 S17 2.207(2) . ? Fe4 S19 2.259(2) . ? Fe5 C55 2.071(10) . ? Fe5 C54 2.107(10) . ? Fe5 C56 2.126(10) . ? Fe5 C53 2.145(9) . ? Fe5 C57 2.155(11) . ? Fe5 S24 2.170(2) . ? Fe5 S23 2.196(3) . ? Fe5 S21 2.232(3) . ? Fe5 Fe7 2.663(2) . ? Fe6 C60 2.066(12) . ? Fe6 C61 2.084(11) . ? Fe6 C62 2.104(12) . ? Fe6 C59 2.108(13) . ? Fe6 C58 2.139(11) . ? Fe6 S22 2.175(3) . ? Fe6 S21 2.220(3) . ? Fe6 S23 2.222(3) . ? Fe6 Fe8 2.643(2) . ? Fe6 Fe7 2.896(2) . ? Fe7 C66 2.096(8) . ? Fe7 C67 2.097(9) . ? Fe7 C64 2.113(9) . ? Fe7 C63 2.116(9) . ? Fe7 C65 2.125(9) . ? Fe7 S23 2.173(3) . ? Fe7 S22 2.214(2) . ? Fe7 S24 2.224(2) . ? Fe8 C70 2.091(10) . ? Fe8 C69 2.102(10) . ? Fe8 C71 2.102(10) . ? Fe8 C72 2.110(11) . ? Fe8 C68 2.112(10) . ? Fe8 S21 2.171(3) . ? Fe8 S22 2.196(2) . ? Fe8 S24 2.238(2) . ? S1 C1 1.710(10) . ? S2 C3 1.706(9) . ? S3 C5 1.721(9) . ? S4 C7 1.720(9) . ? S5 C9 1.712(9) . ? S6 C11 1.715(9) . ? S7 C13 1.716(9) . ? S8 C15 1.713(9) . ? S9 C17 1.729(9) . ? S10 C19 1.720(9) . ? S11 C21 1.724(8) . ? S12 C23 1.724(9) . ? S13 C25 1.723(10) . ? S14 C27 1.709(10) . ? S15 C29 1.711(9) . ? S16 C31 1.719(10) . ? N1 C2 1.148(12) . ? N2 C4 1.157(12) . ? N3 C6 1.149(12) . ? N4 C8 1.135(12) . ? N5 C10 1.141(12) . ? N6 C12 1.154(12) . ? N7 C14 1.163(12) . ? N8 C16 1.139(12) . ? N9 C18 1.150(12) . ? N10 C22 1.137(12) . ? N10 C20 1.132(12) . ? N11 C24 1.131(12) . ? N13 C26 1.149(13) . ? N14 C28 1.137(13) . ? N15 C30 1.130(12) . ? N16 C32 1.144(13) . ? C1 C3 1.391(12) . ? C1 C2 1.434(13) . ? C3 C4 1.424(13) . ? C5 C7 1.352(12) . ? C5 C6 1.440(13) . ? C7 C8 1.449(13) . ? C9 C11 1.388(12) . ? C9 C10 1.443(13) . ? C11 C12 1.428(13) . ? C13 C15 1.367(12) . ? C13 C14 1.448(13) . ? C15 C16 1.432(13) . ? C17 C19 1.397(13) . ? C17 C18 1.420(13) . ? C19 C20 1.439(13) . ? C21 C23 1.367(12) . ? C21 C22 1.426(12) . ? C23 C24 1.451(13) . ? C25 C27 1.400(13) . ? C25 C26 1.434(13) . ? C27 C28 1.426(14) . ? C29 C31 1.384(13) . ? C29 C30 1.438(14) . ? C31 C32 1.442(13) . ? C33 C34 1.39(2) . ? C33 C37 1.41(2) . ? C34 C35 1.39(2) . ? C35 C36 1.40(2) . ? C36 C37 1.39(2) . ? C38 C42 1.406(14) . ? C38 C39 1.415(13) . ? C39 C40 1.415(14) . ? C40 C41 1.404(14) . ? C41 C42 1.405(14) . ? C43 C44 1.385(14) . ? C43 C47 1.386(15) . ? C44 C45 1.393(15) . ? C45 C46 1.40(2) . ? C46 C47 1.39(2) . ? C48 C52 1.386(15) . ? C48 C49 1.41(2) . ? C49 C50 1.40(2) . ? C50 C51 1.36(2) . ? C51 C52 1.39(2) . ? C53 C57 1.396(15) . ? C53 C54 1.42(2) . ? C54 C55 1.419(14) . ? C55 C56 1.400(15) . ? C56 C57 1.41(2) . ? C58 C62 1.33(2) . ? C58 C59 1.37(2) . ? C59 C60 1.38(2) . ? C60 C61 1.38(2) . ? C61 C62 1.34(2) . ? C63 C64 1.399(15) . ? C63 C67 1.406(14) . ? C64 C65 1.409(14) . ? C65 C66 1.411(14) . ? C66 C67 1.414(13) . ? C68 C69 1.37(2) . ? C68 C72 1.43(2) . ? C69 C70 1.35(2) . ? C70 C71 1.35(2) . ? C71 C72 1.41(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Pt1 S4 174.57(9) . . ? S2 Pt1 S1 89.95(8) . . ? S4 Pt1 S1 89.69(8) . . ? S2 Pt1 S3 90.20(8) . . ? S4 Pt1 S3 90.06(8) . . ? S1 Pt1 S3 178.87(9) . . ? S7 Pt2 S6 88.89(8) . . ? S7 Pt2 S5 179.04(8) . . ? S6 Pt2 S5 90.31(8) . . ? S7 Pt2 S8 90.21(8) . . ? S6 Pt2 S8 179.09(8) . . ? S5 Pt2 S8 90.59(8) . . ? S10 Pt3 S12 178.95(9) . . ? S10 Pt3 S9 89.80(8) . . ? S12 Pt3 S9 89.82(8) . . ? S10 Pt3 S11 90.61(8) . . ? S12 Pt3 S11 89.75(8) . . ? S9 Pt3 S11 179.08(8) . . ? S15 Pt4 S13 175.77(9) . . ? S15 Pt4 S16 89.97(9) . . ? S13 Pt4 S16 90.53(8) . . ? S15 Pt4 S14 89.23(9) . . ? S13 Pt4 S14 90.10(9) . . ? S16 Pt4 S14 177.66(9) . . ? C35 Fe1 C33 64.4(4) . . ? C35 Fe1 C36 39.0(4) . . ? C33 Fe1 C36 64.9(4) . . ? C35 Fe1 C37 64.5(4) . . ? C33 Fe1 C37 38.9(5) . . ? C36 Fe1 C37 38.4(4) . . ? C35 Fe1 C34 38.7(4) . . ? C33 Fe1 C34 38.5(4) . . ? C36 Fe1 C34 65.4(4) . . ? C37 Fe1 C34 64.9(4) . . ? C35 Fe1 S17 151.4(3) . . ? C33 Fe1 S17 95.6(3) . . ? C36 Fe1 S17 115.1(3) . . ? C37 Fe1 S17 87.0(3) . . ? C34 Fe1 S17 132.1(3) . . ? C35 Fe1 S20 91.1(3) . . ? C33 Fe1 S20 154.1(3) . . ? C36 Fe1 S20 91.0(3) . . ? C37 Fe1 S20 124.3(4) . . ? C34 Fe1 S20 124.1(3) . . ? S17 Fe1 S20 103.69(9) . . ? C35 Fe1 S18 106.7(3) . . ? C33 Fe1 S18 114.7(4) . . ? C36 Fe1 S18 144.6(3) . . ? C37 Fe1 S18 153.5(4) . . ? C34 Fe1 S18 92.3(3) . . ? S17 Fe1 S18 100.25(9) . . ? S20 Fe1 S18 78.94(9) . . ? C35 Fe1 Fe2 147.0(3) . . ? C33 Fe1 Fe2 99.5(3) . . ? C36 Fe1 Fe2 160.1(3) . . ? C37 Fe1 Fe2 121.8(4) . . ? C34 Fe1 Fe2 110.8(3) . . ? S17 Fe1 Fe2 51.50(7) . . ? S20 Fe1 Fe2 106.01(7) . . ? S18 Fe1 Fe2 51.79(6) . . ? C35 Fe1 Fe4 135.1(3) . . ? C33 Fe1 Fe4 143.6(4) . . ? C36 Fe1 Fe4 109.4(3) . . ? C37 Fe1 Fe4 113.4(3) . . ? C34 Fe1 Fe4 173.7(3) . . ? S17 Fe1 Fe4 52.55(7) . . ? S20 Fe1 Fe4 51.17(7) . . ? S18 Fe1 Fe4 90.65(7) . . ? Fe2 Fe1 Fe4 75.32(5) . . ? C39 Fe2 C38 39.8(3) . . ? C39 Fe2 C42 65.1(4) . . ? C38 Fe2 C42 39.1(4) . . ? C39 Fe2 C40 39.4(4) . . ? C38 Fe2 C40 66.4(4) . . ? C42 Fe2 C40 64.7(4) . . ? C39 Fe2 C41 65.2(4) . . ? C38 Fe2 C41 65.8(4) . . ? C42 Fe2 C41 38.5(4) . . ? C40 Fe2 C41 38.4(4) . . ? C39 Fe2 S17 100.8(3) . . ? C38 Fe2 S17 138.8(3) . . ? C42 Fe2 S17 153.1(3) . . ? C40 Fe2 S17 89.7(3) . . ? C41 Fe2 S17 115.5(3) . . ? C39 Fe2 S18 156.2(3) . . ? C38 Fe2 S18 117.0(3) . . ? C42 Fe2 S18 92.9(3) . . ? C40 Fe2 S18 140.2(3) . . ? C41 Fe2 S18 103.8(3) . . ? S17 Fe2 S18 102.99(9) . . ? C39 Fe2 S19 101.2(3) . . ? C38 Fe2 S19 95.1(3) . . ? C42 Fe2 S19 124.7(3) . . ? C40 Fe2 S19 136.2(3) . . ? C41 Fe2 S19 160.8(3) . . ? S17 Fe2 S19 79.13(9) . . ? S18 Fe2 S19 83.45(9) . . ? C39 Fe2 Fe1 147.5(3) . . ? C38 Fe2 Fe1 168.7(3) . . ? C42 Fe2 Fe1 130.1(3) . . ? C40 Fe2 Fe1 114.7(3) . . ? C41 Fe2 Fe1 107.6(3) . . ? S17 Fe2 Fe1 51.78(7) . . ? S18 Fe2 Fe1 54.40(7) . . ? S19 Fe2 Fe1 91.15(7) . . ? C46 Fe3 C47 39.0(4) . . ? C46 Fe3 C43 65.3(4) . . ? C47 Fe3 C43 38.8(4) . . ? C46 Fe3 C45 39.2(5) . . ? C47 Fe3 C45 65.1(4) . . ? C43 Fe3 C45 64.8(4) . . ? C46 Fe3 C44 65.2(4) . . ? C47 Fe3 C44 64.8(4) . . ? C43 Fe3 C44 38.5(4) . . ? C45 Fe3 C44 38.5(4) . . ? C46 Fe3 S20 136.5(4) . . ? C47 Fe3 S20 99.7(3) . . ? C43 Fe3 S20 90.5(3) . . ? C45 Fe3 S20 154.6(3) . . ? C44 Fe3 S20 117.4(3) . . ? C46 Fe3 S19 119.0(4) . . ? C47 Fe3 S19 156.2(3) . . ? C43 Fe3 S19 135.8(3) . . ? C45 Fe3 S19 91.4(3) . . ? C44 Fe3 S19 99.9(3) . . ? S20 Fe3 S19 103.72(9) . . ? C46 Fe3 S18 96.1(3) . . ? C47 Fe3 S18 105.1(3) . . ? C43 Fe3 S18 140.8(3) . . ? C45 Fe3 S18 122.4(4) . . ? C44 Fe3 S18 160.2(3) . . ? S20 Fe3 S18 80.13(9) . . ? S19 Fe3 S18 83.34(9) . . ? C46 Fe3 Fe4 169.0(4) . . ? C47 Fe3 Fe4 144.5(3) . . ? C43 Fe3 Fe4 111.9(3) . . ? C45 Fe3 Fe4 129.8(4) . . ? C44 Fe3 Fe4 105.7(3) . . ? S20 Fe3 Fe4 52.32(7) . . ? S19 Fe3 Fe4 54.70(7) . . ? S18 Fe3 Fe4 92.17(7) . . ? C49 Fe4 C48 39.6(5) . . ? C49 Fe4 C50 39.3(5) . . ? C48 Fe4 C50 65.8(5) . . ? C49 Fe4 C52 64.3(4) . . ? C48 Fe4 C52 38.3(4) . . ? C50 Fe4 C52 63.8(4) . . ? C49 Fe4 C51 64.0(4) . . ? C48 Fe4 C51 64.3(4) . . ? C50 Fe4 C51 37.4(5) . . ? C52 Fe4 C51 37.9(4) . . ? C49 Fe4 S20 154.0(3) . . ? C48 Fe4 S20 116.6(4) . . ? C50 Fe4 S20 133.5(4) . . ? C52 Fe4 S20 90.0(3) . . ? C51 Fe4 S20 98.7(4) . . ? C49 Fe4 S17 89.4(3) . . ? C48 Fe4 S17 90.6(3) . . ? C50 Fe4 S17 123.0(4) . . ? C52 Fe4 S17 125.0(3) . . ? C51 Fe4 S17 152.3(3) . . ? S20 Fe4 S17 103.42(9) . . ? C49 Fe4 S19 104.0(4) . . ? C48 Fe4 S19 142.4(4) . . ? C50 Fe4 S19 90.9(3) . . ? C52 Fe4 S19 152.2(3) . . ? C51 Fe4 S19 114.6(3) . . ? S20 Fe4 S19 100.84(9) . . ? S17 Fe4 S19 77.56(9) . . ? C49 Fe4 Fe3 146.2(4) . . ? C48 Fe4 Fe3 162.3(3) . . ? C50 Fe4 Fe3 110.5(4) . . ? C52 Fe4 Fe3 124.0(3) . . ? C51 Fe4 Fe3 101.8(3) . . ? S20 Fe4 Fe3 52.10(7) . . ? S17 Fe4 Fe3 104.94(8) . . ? S19 Fe4 Fe3 51.89(6) . . ? C49 Fe4 Fe1 134.3(4) . . ? C48 Fe4 Fe1 110.1(3) . . ? C50 Fe4 Fe1 173.4(4) . . ? C52 Fe4 Fe1 116.5(3) . . ? C51 Fe4 Fe1 146.6(4) . . ? S20 Fe4 Fe1 52.53(7) . . ? S17 Fe4 Fe1 50.92(7) . . ? S19 Fe4 Fe1 89.97(7) . . ? Fe3 Fe4 Fe1 74.97(5) . . ? C55 Fe5 C54 39.7(4) . . ? C55 Fe5 C56 38.9(4) . . ? C54 Fe5 C56 66.1(4) . . ? C55 Fe5 C53 64.7(4) . . ? C54 Fe5 C53 39.1(4) . . ? C56 Fe5 C53 64.3(4) . . ? C55 Fe5 C57 64.6(4) . . ? C54 Fe5 C57 65.3(4) . . ? C56 Fe5 C57 38.4(4) . . ? C53 Fe5 C57 37.9(4) . . ? C55 Fe5 S24 155.5(3) . . ? C54 Fe5 S24 117.9(3) . . ? C56 Fe5 S24 135.0(3) . . ? C53 Fe5 S24 91.1(3) . . ? C57 Fe5 S24 99.3(3) . . ? C55 Fe5 S23 101.1(3) . . ? C54 Fe5 S23 138.5(3) . . ? C56 Fe5 S23 90.9(3) . . ? C53 Fe5 S23 154.3(3) . . ? C57 Fe5 S23 117.4(3) . . ? S24 Fe5 S23 102.90(10) . . ? C55 Fe5 S21 98.8(3) . . ? C54 Fe5 S21 93.0(3) . . ? C56 Fe5 S21 133.7(3) . . ? C53 Fe5 S21 123.7(3) . . ? C57 Fe5 S21 158.3(3) . . ? S24 Fe5 S21 91.20(10) . . ? S23 Fe5 S21 78.11(9) . . ? C55 Fe5 Fe7 145.9(3) . . ? C54 Fe5 Fe7 168.1(3) . . ? C56 Fe5 Fe7 112.8(3) . . ? C53 Fe5 Fe7 129.1(3) . . ? C57 Fe5 Fe7 106.1(3) . . ? S24 Fe5 Fe7 53.63(7) . . ? S23 Fe5 Fe7 52.07(7) . . ? S21 Fe5 Fe7 95.48(8) . . ? C60 Fe6 C61 38.8(6) . . ? C60 Fe6 C62 63.2(5) . . ? C61 Fe6 C62 37.2(5) . . ? C60 Fe6 C59 38.6(7) . . ? C61 Fe6 C59 64.0(6) . . ? C62 Fe6 C59 62.5(6) . . ? C60 Fe6 C58 63.3(5) . . ? C61 Fe6 C58 62.4(5) . . ? C62 Fe6 C58 36.5(5) . . ? C59 Fe6 C58 37.6(7) . . ? C60 Fe6 S22 149.5(5) . . ? C61 Fe6 S22 111.3(5) . . ? C62 Fe6 S22 88.4(4) . . ? C59 Fe6 S22 137.7(7) . . ? C58 Fe6 S22 101.0(5) . . ? C60 Fe6 S21 107.8(6) . . ? C61 Fe6 S21 146.2(5) . . ? C62 Fe6 S21 150.1(5) . . ? C59 Fe6 S21 92.3(4) . . ? C58 Fe6 S21 113.7(5) . . ? S22 Fe6 S21 102.45(10) . . ? C60 Fe6 S23 92.7(5) . . ? C61 Fe6 S23 95.5(4) . . ? C62 Fe6 S23 128.8(5) . . ? C59 Fe6 S23 124.6(7) . . ? C58 Fe6 S23 155.3(3) . . ? S22 Fe6 S23 97.37(9) . . ? S21 Fe6 S23 77.82(9) . . ? C60 Fe6 Fe8 152.1(7) . . ? C61 Fe6 Fe8 159.1(5) . . ? C62 Fe6 Fe8 122.5(4) . . ? C59 Fe6 Fe8 116.1(6) . . ? C58 Fe6 Fe8 104.0(3) . . ? S22 Fe6 Fe8 53.16(7) . . ? S21 Fe6 Fe8 52.15(7) . . ? S23 Fe6 Fe8 100.15(8) . . ? C60 Fe6 Fe7 133.4(6) . . ? C61 Fe6 Fe7 110.8(4) . . ? C62 Fe6 Fe7 117.8(4) . . ? C59 Fe6 Fe7 171.7(7) . . ? C58 Fe6 Fe7 147.1(5) . . ? S22 Fe6 Fe7 49.30(7) . . ? S21 Fe6 Fe7 89.52(8) . . ? S23 Fe6 Fe7 48.07(7) . . ? Fe8 Fe6 Fe7 71.19(5) . . ? C66 Fe7 C67 39.4(4) . . ? C66 Fe7 C64 65.2(4) . . ? C67 Fe7 C64 65.3(4) . . ? C66 Fe7 C63 65.4(4) . . ? C67 Fe7 C63 39.0(4) . . ? C64 Fe7 C63 38.6(4) . . ? C66 Fe7 C65 39.0(4) . . ? C67 Fe7 C65 65.7(4) . . ? C64 Fe7 C65 38.8(4) . . ? C63 Fe7 C65 65.1(4) . . ? C66 Fe7 S23 114.2(3) . . ? C67 Fe7 S23 152.1(3) . . ? C64 Fe7 S23 98.0(3) . . ? C63 Fe7 S23 135.0(3) . . ? C65 Fe7 S23 87.2(3) . . ? C66 Fe7 S22 92.6(3) . . ? C67 Fe7 S22 93.4(3) . . ? C64 Fe7 S22 156.7(3) . . ? C63 Fe7 S22 127.1(3) . . ? C65 Fe7 S22 125.3(3) . . ? S23 Fe7 S22 97.66(9) . . ? C66 Fe7 S24 143.8(3) . . ? C67 Fe7 S24 105.2(3) . . ? C64 Fe7 S24 113.0(3) . . ? C63 Fe7 S24 90.7(3) . . ? C65 Fe7 S24 151.8(3) . . ? S23 Fe7 S24 101.89(9) . . ? S22 Fe7 S24 80.32(9) . . ? C66 Fe7 Fe5 161.4(3) . . ? C67 Fe7 Fe5 148.3(3) . . ? C64 Fe7 Fe5 101.1(3) . . ? C63 Fe7 Fe5 112.5(3) . . ? C65 Fe7 Fe5 122.4(3) . . ? S23 Fe7 Fe5 52.85(7) . . ? S22 Fe7 Fe5 102.06(8) . . ? S24 Fe7 Fe5 51.79(7) . . ? C66 Fe7 Fe6 110.6(3) . . ? C67 Fe7 Fe6 135.5(3) . . ? C64 Fe7 Fe6 144.3(3) . . ? C63 Fe7 Fe6 174.5(3) . . ? C65 Fe7 Fe6 114.5(3) . . ? S23 Fe7 Fe6 49.52(7) . . ? S22 Fe7 Fe6 48.14(7) . . ? S24 Fe7 Fe6 90.96(7) . . ? Fe5 Fe7 Fe6 72.50(5) . . ? C70 Fe8 C69 37.7(5) . . ? C70 Fe8 C71 37.7(4) . . ? C69 Fe8 C71 63.5(4) . . ? C70 Fe8 C72 64.6(4) . . ? C69 Fe8 C72 65.0(5) . . ? C71 Fe8 C72 39.0(5) . . ? C70 Fe8 C68 63.5(5) . . ? C69 Fe8 C68 37.9(5) . . ? C71 Fe8 C68 64.5(4) . . ? C72 Fe8 C68 39.6(5) . . ? C70 Fe8 S21 101.8(3) . . ? C69 Fe8 S21 89.0(3) . . ? C71 Fe8 S21 138.5(4) . . ? C72 Fe8 S21 151.8(4) . . ? C68 Fe8 S21 112.7(5) . . ? C70 Fe8 S22 154.6(3) . . ? C69 Fe8 S22 139.1(5) . . ? C71 Fe8 S22 117.9(4) . . ? C72 Fe8 S22 91.1(3) . . ? C68 Fe8 S22 102.9(5) . . ? S21 Fe8 S22 103.36(10) . . ? C70 Fe8 S24 102.7(4) . . ? C69 Fe8 S24 139.0(4) . . ? C71 Fe8 S24 91.1(3) . . ? C72 Fe8 S24 115.5(4) . . ? C68 Fe8 S24 154.1(4) . . ? S21 Fe8 S24 91.01(10) . . ? S22 Fe8 S24 80.40(9) . . ? C70 Fe8 Fe6 148.7(4) . . ? C69 Fe8 Fe6 115.0(4) . . ? C71 Fe8 Fe6 165.1(4) . . ? C72 Fe8 Fe6 126.2(4) . . ? C68 Fe8 Fe6 104.8(3) . . ? S21 Fe8 Fe6 53.84(7) . . ? S22 Fe8 Fe6 52.43(7) . . ? S24 Fe8 Fe6 97.54(7) . . ? C1 S1 Pt1 102.9(3) . . ? C3 S2 Pt1 103.0(3) . . ? C5 S3 Pt1 102.1(3) . . ? C7 S4 Pt1 102.2(3) . . ? C9 S5 Pt2 102.3(3) . . ? C11 S6 Pt2 102.9(3) . . ? C13 S7 Pt2 102.4(3) . . ? C15 S8 Pt2 102.2(3) . . ? C17 S9 Pt3 103.6(3) . . ? C19 S10 Pt3 103.4(3) . . ? C21 S11 Pt3 102.8(3) . . ? C23 S12 Pt3 103.0(3) . . ? C25 S13 Pt4 102.8(3) . . ? C27 S14 Pt4 103.1(3) . . ? C29 S15 Pt4 103.1(3) . . ? C31 S16 Pt4 102.4(3) . . ? Fe2 S17 Fe1 76.71(8) . . ? Fe2 S17 Fe4 97.88(9) . . ? Fe1 S17 Fe4 76.53(8) . . ? Fe2 S18 Fe3 96.00(9) . . ? Fe2 S18 Fe1 73.81(8) . . ? Fe3 S18 Fe1 92.36(9) . . ? Fe3 S19 Fe2 96.68(9) . . ? Fe3 S19 Fe4 73.41(8) . . ? Fe2 S19 Fe4 93.79(9) . . ? Fe3 S20 Fe4 75.58(8) . . ? Fe3 S20 Fe1 96.48(9) . . ? Fe4 S20 Fe1 76.30(8) . . ? Fe8 S21 Fe6 74.01(9) . . ? Fe8 S21 Fe5 88.90(10) . . ? Fe6 S21 Fe5 95.37(10) . . ? Fe6 S22 Fe8 74.41(8) . . ? Fe6 S22 Fe7 82.56(9) . . ? Fe8 S22 Fe7 94.20(9) . . ? Fe7 S23 Fe5 75.08(8) . . ? Fe7 S23 Fe6 82.41(9) . . ? Fe5 S23 Fe6 96.33(9) . . ? Fe5 S24 Fe7 74.58(8) . . ? Fe5 S24 Fe8 88.76(9) . . ? Fe7 S24 Fe8 92.77(9) . . ? C3 C1 C2 118.7(8) . . ? C3 C1 S1 121.9(7) . . ? C2 C1 S1 119.4(7) . . ? N1 C2 C1 174.3(10) . . ? C1 C3 C4 119.1(8) . . ? C1 C3 S2 122.0(7) . . ? C4 C3 S2 118.9(7) . . ? N2 C4 C3 177.7(10) . . ? C7 C5 C6 120.1(8) . . ? C7 C5 S3 122.6(7) . . ? C6 C5 S3 117.3(7) . . ? N3 C6 C5 176.4(10) . . ? C5 C7 C8 118.4(8) . . ? C5 C7 S4 122.8(7) . . ? C8 C7 S4 118.8(6) . . ? N4 C8 C7 176.9(10) . . ? C11 C9 C10 120.1(8) . . ? C11 C9 S5 122.9(7) . . ? C10 C9 S5 116.9(7) . . ? N5 C10 C9 179.0(11) . . ? C9 C11 C12 121.7(8) . . ? C9 C11 S6 121.6(7) . . ? C12 C11 S6 116.8(7) . . ? N6 C12 C11 179.1(11) . . ? C15 C13 C14 121.0(8) . . ? C15 C13 S7 122.6(7) . . ? C14 C13 S7 116.4(7) . . ? N7 C14 C13 179.2(10) . . ? C13 C15 C16 119.7(8) . . ? C13 C15 S8 122.6(7) . . ? C16 C15 S8 117.7(7) . . ? N8 C16 C15 176.9(11) . . ? C19 C17 C18 122.5(9) . . ? C19 C17 S9 120.9(7) . . ? C18 C17 S9 116.6(7) . . ? N9 C18 C17 178.3(10) . . ? C17 C19 C20 120.2(8) . . ? C17 C19 S10 122.3(7) . . ? C20 C19 S10 117.5(7) . . ? N10 C20 C19 178.5(10) . . ? C23 C21 C22 119.1(8) . . ? C23 C21 S11 122.2(7) . . ? C22 C21 S11 118.7(7) . . ? N10 C22 C21 176.9(10) . . ? C21 C23 C24 121.9(8) . . ? C21 C23 S12 122.2(7) . . ? C24 C23 S12 115.8(7) . . ? N11 C24 C23 178.5(10) . . ? C27 C25 C26 120.2(9) . . ? C27 C25 S13 121.8(7) . . ? C26 C25 S13 118.0(7) . . ? N13 C26 C25 178.5(10) . . ? C25 C27 C28 118.3(9) . . ? C25 C27 S14 122.0(7) . . ? C28 C27 S14 119.7(7) . . ? N14 C28 C27 176.5(10) . . ? C31 C29 C30 118.8(9) . . ? C31 C29 S15 121.6(7) . . ? C30 C29 S15 119.6(7) . . ? N15 C30 C29 177.2(11) . . ? C29 C31 C32 119.1(9) . . ? C29 C31 S16 122.6(7) . . ? C32 C31 S16 118.2(7) . . ? N16 C32 C31 176.7(11) . . ? C34 C33 C37 108.9(10) . . ? C34 C33 Fe1 71.6(6) . . ? C37 C33 Fe1 71.1(6) . . ? C35 C34 C33 106.3(10) . . ? C35 C34 Fe1 69.0(6) . . ? C33 C34 Fe1 69.9(5) . . ? C34 C35 C36 109.9(10) . . ? C34 C35 Fe1 72.3(6) . . ? C36 C35 Fe1 71.6(6) . . ? C37 C36 C35 107.0(10) . . ? C37 C36 Fe1 71.2(6) . . ? C35 C36 Fe1 69.4(6) . . ? C36 C37 C33 108.0(9) . . ? C36 C37 Fe1 70.4(6) . . ? C33 C37 Fe1 70.0(6) . . ? C42 C38 C39 106.5(9) . . ? C42 C38 Fe2 71.8(6) . . ? C39 C38 Fe2 70.1(5) . . ? C38 C39 C40 108.7(9) . . ? C38 C39 Fe2 70.1(5) . . ? C40 C39 Fe2 71.9(6) . . ? C41 C40 C39 107.6(9) . . ? C41 C40 Fe2 71.7(5) . . ? C39 C40 Fe2 68.8(5) . . ? C40 C41 C42 107.7(9) . . ? C40 C41 Fe2 69.9(5) . . ? C42 C41 Fe2 69.7(5) . . ? C41 C42 C38 109.5(9) . . ? C41 C42 Fe2 71.8(6) . . ? C38 C42 Fe2 69.0(5) . . ? C44 C43 C47 108.6(9) . . ? C44 C43 Fe3 71.9(5) . . ? C47 C43 Fe3 70.5(6) . . ? C43 C44 C45 108.0(10) . . ? C43 C44 Fe3 69.6(5) . . ? C45 C44 Fe3 70.6(6) . . ? C44 C45 C46 107.6(10) . . ? C44 C45 Fe3 70.9(6) . . ? C46 C45 Fe3 69.1(6) . . ? C47 C46 C45 107.8(10) . . ? C47 C46 Fe3 70.7(6) . . ? C45 C46 Fe3 71.7(6) . . ? C43 C47 C46 108.0(10) . . ? C43 C47 Fe3 70.6(6) . . ? C46 C47 Fe3 70.3(6) . . ? C52 C48 C49 106.1(10) . . ? C52 C48 Fe4 72.2(6) . . ? C49 C48 Fe4 69.0(6) . . ? C50 C49 C48 108.5(10) . . ? C50 C49 Fe4 72.0(6) . . ? C48 C49 Fe4 71.5(6) . . ? C51 C50 C49 107.2(10) . . ? C51 C50 Fe4 72.6(7) . . ? C49 C50 Fe4 68.6(6) . . ? C50 C51 C52 109.2(10) . . ? C50 C51 Fe4 69.9(6) . . ? C52 C51 Fe4 70.6(6) . . ? C51 C52 C48 108.9(11) . . ? C51 C52 Fe4 71.5(6) . . ? C48 C52 Fe4 69.5(6) . . ? C57 C53 C54 109.3(9) . . ? C57 C53 Fe5 71.4(6) . . ? C54 C53 Fe5 69.0(5) . . ? C55 C54 C53 105.3(10) . . ? C55 C54 Fe5 68.8(6) . . ? C53 C54 Fe5 71.9(6) . . ? C56 C55 C54 110.1(10) . . ? C56 C55 Fe5 72.7(6) . . ? C54 C55 Fe5 71.5(6) . . ? C55 C56 C57 107.0(9) . . ? C55 C56 Fe5 68.4(6) . . ? C57 C56 Fe5 71.9(6) . . ? C53 C57 C56 108.3(10) . . ? C53 C57 Fe5 70.7(6) . . ? C56 C57 Fe5 69.7(6) . . ? C62 C58 C59 108.1(13) . . ? C62 C58 Fe6 70.3(7) . . ? C59 C58 Fe6 69.9(8) . . ? C58 C59 C60 106.9(12) . . ? C58 C59 Fe6 72.4(7) . . ? C60 C59 Fe6 69.1(8) . . ? C61 C60 C59 107.4(13) . . ? C61 C60 Fe6 71.3(7) . . ? C59 C60 Fe6 72.4(8) . . ? C62 C61 C60 107.2(13) . . ? C62 C61 Fe6 72.2(8) . . ? C60 C61 Fe6 69.9(7) . . ? C58 C62 C61 110.3(13) . . ? C58 C62 Fe6 73.2(8) . . ? C61 C62 Fe6 70.5(7) . . ? C64 C63 C67 108.1(9) . . ? C64 C63 Fe7 70.6(5) . . ? C67 C63 Fe7 69.8(5) . . ? C63 C64 C65 108.8(9) . . ? C63 C64 Fe7 70.8(5) . . ? C65 C64 Fe7 71.0(5) . . ? C64 C65 C66 107.2(9) . . ? C64 C65 Fe7 70.1(5) . . ? C66 C65 Fe7 69.4(5) . . ? C65 C66 C67 108.3(8) . . ? C65 C66 Fe7 71.6(5) . . ? C67 C66 Fe7 70.3(5) . . ? C63 C67 C66 107.7(9) . . ? C63 C67 Fe7 71.2(5) . . ? C66 C67 Fe7 70.3(5) . . ? C69 C68 C72 107.9(10) . . ? C69 C68 Fe8 70.7(7) . . ? C72 C68 Fe8 70.1(6) . . ? C70 C69 C68 108.8(11) . . ? C70 C69 Fe8 70.7(7) . . ? C68 C69 Fe8 71.5(7) . . ? C71 C70 C69 109.5(11) . . ? C71 C70 Fe8 71.6(6) . . ? C69 C70 Fe8 71.6(6) . . ? C70 C71 C72 108.8(11) . . ? C70 C71 Fe8 70.7(6) . . ? C72 C71 Fe8 70.8(6) . . ? C71 C72 C68 104.9(11) . . ? C71 C72 Fe8 70.2(6) . . ? C68 C72 Fe8 70.3(7) . . ? _refine_diff_density_max 1.625 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.171 #=END data_5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H20 Fe4 N4 Pt S8' _chemical_formula_weight 1087.45 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1195(10) _cell_length_b 12.193(2) _cell_length_c 15.364(3) _cell_angle_alpha 104.153(10) _cell_angle_beta 94.414(8) _cell_angle_gamma 90.920(6) _cell_volume 1650.52(53) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 214 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 24.99 _exptl_crystal_description diamonds _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.188 _exptl_crystal_density_method ? _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 6.474 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.874 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7549 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5585 _reflns_number_observed 5489 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+4.7000P] 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 5585 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_obs 0.0308 _refine_ls_wR_factor_all 0.0830 _refine_ls_wR_factor_obs 0.0817 _refine_ls_goodness_of_fit_all 1.114 _refine_ls_goodness_of_fit_obs 1.106 _refine_ls_restrained_S_all 1.114 _refine_ls_restrained_S_obs 1.106 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.14297(2) 0.478729(14) 0.577327(11) 0.02114(8) Uani 1 d . . Fe1 Fe 0.60224(7) 0.21713(5) 0.70927(4) 0.01904(15) Uani 1 d . . Fe2 Fe 0.61398(7) 0.41842(5) 0.82637(4) 0.01887(15) Uani 1 d . . Fe3 Fe 0.91021(7) 0.26208(5) 0.84362(4) 0.01965(15) Uani 1 d . . Fe4 Fe 0.66707(7) 0.18316(5) 0.89506(4) 0.01803(14) Uani 1 d . . S1 S 0.00392(14) 0.55276(10) 0.69290(8) 0.0247(2) Uani 1 d . . S2 S 0.25947(14) 0.64939(11) 0.59609(9) 0.0274(3) Uani 1 d . . S3 S 0.28500(14) 0.41321(11) 0.46289(8) 0.0270(3) Uani 1 d . . S4 S 0.03095(14) 0.30394(10) 0.55241(8) 0.0257(3) Uani 1 d . . S5 S 0.48610(12) 0.26692(9) 0.83160(7) 0.0197(2) Uani 1 d . . S6 S 0.78917(12) 0.34232(9) 0.74359(7) 0.0199(2) Uani 1 d . . S7 S 0.75748(12) 0.36112(9) 0.93303(7) 0.0206(2) Uani 1 d . . S8 S 0.76921(12) 0.11884(9) 0.76951(7) 0.0198(2) Uani 1 d . . C1 C 0.0697(6) 0.6913(4) 0.7259(3) 0.0244(10) Uani 1 d . . C2 C 0.0032(6) 0.7639(5) 0.7992(4) 0.0302(11) Uani 1 d . . C3 C 0.1793(5) 0.7318(4) 0.6849(3) 0.0250(10) Uani 1 d . . C4 C 0.2319(6) 0.8485(4) 0.7153(4) 0.0301(11) Uani 1 d . . C5 C 0.2292(6) 0.2729(4) 0.4252(3) 0.0272(11) Uani 1 d . . C6 C 0.3051(6) 0.2091(5) 0.3520(4) 0.0342(12) Uani 1 d . . C7 C 0.1200(6) 0.2268(4) 0.4632(3) 0.0271(10) Uani 1 d . . C8 C 0.0717(7) 0.1106(5) 0.4293(4) 0.0338(12) Uani 1 d . . C9 C 0.5440(10) 0.0714(6) 0.6050(5) 0.065(3) Uani 1 d . . H9A H 0.5681(10) -0.0017(6) 0.6075(5) 0.078 Uiso 1 calc R . C10 C 0.6301(7) 0.1477(10) 0.5738(4) 0.074(3) Uani 1 d . . H10A H 0.7230(7) 0.1351(10) 0.5531(4) 0.089 Uiso 1 calc R . C11 C 0.5513(9) 0.2456(7) 0.5794(4) 0.058(2) Uani 1 d . . H11A H 0.5818(9) 0.3096(7) 0.5620(4) 0.070 Uiso 1 calc R . C12 C 0.4230(7) 0.2318(6) 0.6144(4) 0.046(2) Uani 1 d . . H12A H 0.3508(7) 0.2854(6) 0.6253(4) 0.055 Uiso 1 calc R . C13 C 0.4156(7) 0.1255(6) 0.6315(4) 0.046(2) Uani 1 d . . H13A H 0.3389(7) 0.0958(6) 0.6562(4) 0.056 Uiso 1 calc R . C14 C 0.4538(9) 0.5159(5) 0.7750(5) 0.060(2) Uani 1 d . . H14A H 0.3811(9) 0.4866(5) 0.7288(5) 0.072 Uiso 1 calc R . C15 C 0.5985(10) 0.5541(6) 0.7644(5) 0.059(2) Uani 1 d . . H15A H 0.6387(10) 0.5546(6) 0.7107(5) 0.070 Uiso 1 calc R . C16 C 0.6666(7) 0.5906(5) 0.8509(5) 0.049(2) Uani 1 d . . H16A H 0.7625(7) 0.6204(5) 0.8649(5) 0.058 Uiso 1 calc R . C17 C 0.5724(7) 0.5762(5) 0.9124(4) 0.0399(13) Uani 1 d . . H17A H 0.5937(7) 0.5945(5) 0.9745(4) 0.048 Uiso 1 calc R . C18 C 0.4407(7) 0.5302(5) 0.8675(5) 0.0422(14) Uani 1 d . . H18A H 0.3581(7) 0.5120(5) 0.8937(5) 0.051 Uiso 1 calc R . C19 C 1.0905(7) 0.1591(6) 0.8560(6) 0.061(2) Uani 1 d . . H19A H 1.0821(7) 0.0820(6) 0.8525(6) 0.073 Uiso 1 calc R . C20 C 1.0891(6) 0.2421(7) 0.9342(4) 0.053(2) Uani 1 d . . H20A H 1.0810(6) 0.2319(7) 0.9917(4) 0.064 Uiso 1 calc R . C21 C 1.1031(6) 0.3493(6) 0.9095(6) 0.068(3) Uani 1 d . . H21A H 1.1042(6) 0.4223(6) 0.9462(6) 0.082 Uiso 1 calc R . C22 C 1.1146(6) 0.3142(7) 0.8145(5) 0.051(2) Uani 1 d . . H22A H 1.1270(6) 0.3631(7) 0.7774(5) 0.061 Uiso 1 calc R . C23 C 1.1051(7) 0.2022(8) 0.7867(6) 0.063(2) Uani 1 d . . H23A H 1.1082(7) 0.1608(8) 0.7274(6) 0.076 Uiso 1 calc R . C24 C 0.6647(7) 0.1708(5) 1.0320(3) 0.0390(14) Uani 1 d . . H24A H 0.6914(7) 0.2294(5) 1.0825(3) 0.047 Uiso 1 calc R . C25 C 0.7582(6) 0.0893(5) 0.9876(4) 0.0373(13) Uani 1 d . . H25A H 0.8579(6) 0.0846(5) 1.0036(4) 0.045 Uiso 1 calc R . C26 C 0.6764(7) 0.0164(4) 0.9152(4) 0.0320(12) Uani 1 d . . H26A H 0.7122(7) -0.0452(4) 0.8750(4) 0.038 Uiso 1 calc R . C27 C 0.5301(6) 0.0525(5) 0.9136(4) 0.0344(12) Uani 1 d . . H27A H 0.4525(6) 0.0193(5) 0.8721(4) 0.041 Uiso 1 calc R . C28 C 0.5231(7) 0.1483(5) 0.9865(4) 0.0396(14) Uani 1 d . . H28A H 0.4398(7) 0.1893(5) 1.0018(4) 0.048 Uiso 1 calc R . N1 N -0.0511(6) 0.8212(4) 0.8586(3) 0.0404(11) Uani 1 d . . N2 N 0.2715(6) 0.9401(4) 0.7396(4) 0.0481(13) Uani 1 d . . N3 N 0.3684(6) 0.1615(5) 0.2940(4) 0.0473(13) Uani 1 d . . N4 N 0.0323(7) 0.0180(5) 0.4020(4) 0.0527(15) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02527(12) 0.02029(12) 0.01845(12) 0.00644(8) -0.00005(7) 0.00155(7) Fe1 0.0192(3) 0.0224(3) 0.0148(3) 0.0040(2) -0.0006(2) -0.0009(2) Fe2 0.0202(3) 0.0184(3) 0.0189(3) 0.0056(2) 0.0032(2) 0.0004(2) Fe3 0.0158(3) 0.0229(3) 0.0204(3) 0.0062(3) -0.0001(2) -0.0010(2) Fe4 0.0208(3) 0.0176(3) 0.0161(3) 0.0051(2) 0.0015(2) -0.0012(2) S1 0.0295(6) 0.0219(6) 0.0233(6) 0.0063(5) 0.0035(5) -0.0020(5) S2 0.0308(6) 0.0244(6) 0.0279(6) 0.0071(5) 0.0067(5) -0.0024(5) S3 0.0320(6) 0.0251(6) 0.0245(6) 0.0065(5) 0.0053(5) 0.0021(5) S4 0.0323(6) 0.0211(6) 0.0239(6) 0.0061(5) 0.0021(5) 0.0005(5) S5 0.0168(5) 0.0228(5) 0.0205(5) 0.0069(4) 0.0022(4) -0.0004(4) S6 0.0195(5) 0.0209(5) 0.0201(5) 0.0064(4) 0.0023(4) -0.0003(4) S7 0.0234(5) 0.0191(5) 0.0181(5) 0.0027(4) 0.0008(4) -0.0027(4) S8 0.0217(5) 0.0197(5) 0.0177(5) 0.0042(4) 0.0012(4) 0.0007(4) C1 0.032(3) 0.019(2) 0.020(2) 0.002(2) -0.002(2) -0.001(2) C2 0.031(3) 0.031(3) 0.027(3) 0.005(2) -0.001(2) -0.007(2) C3 0.026(2) 0.028(3) 0.022(2) 0.008(2) -0.004(2) -0.004(2) C4 0.030(3) 0.025(3) 0.033(3) 0.003(2) 0.003(2) -0.004(2) C5 0.036(3) 0.026(3) 0.018(2) 0.003(2) 0.000(2) 0.007(2) C6 0.040(3) 0.029(3) 0.033(3) 0.008(2) -0.002(2) 0.001(2) C7 0.034(3) 0.024(2) 0.024(3) 0.008(2) -0.002(2) 0.003(2) C8 0.049(3) 0.025(3) 0.027(3) 0.004(2) 0.008(2) -0.001(2) C9 0.096(6) 0.033(3) 0.044(4) -0.019(3) -0.048(4) 0.020(4) C10 0.033(3) 0.151(9) 0.016(3) -0.022(4) 0.000(2) -0.003(4) C11 0.074(5) 0.078(5) 0.025(3) 0.027(3) -0.020(3) -0.036(4) C12 0.043(3) 0.048(4) 0.036(3) -0.003(3) -0.022(3) 0.008(3) C13 0.044(3) 0.065(4) 0.025(3) 0.007(3) -0.013(2) -0.029(3) C14 0.076(5) 0.030(3) 0.059(4) -0.007(3) -0.038(4) 0.032(3) C15 0.101(6) 0.046(4) 0.049(4) 0.035(3) 0.048(4) 0.041(4) C16 0.045(3) 0.013(2) 0.089(5) 0.014(3) 0.009(3) 0.002(2) C17 0.056(4) 0.025(3) 0.035(3) 0.002(2) 0.002(3) 0.012(2) C18 0.037(3) 0.025(3) 0.067(4) 0.011(3) 0.019(3) 0.013(2) C19 0.028(3) 0.040(4) 0.107(7) 0.009(4) -0.013(4) 0.005(3) C20 0.019(3) 0.111(6) 0.040(3) 0.046(4) -0.009(2) -0.009(3) C21 0.014(3) 0.045(4) 0.112(7) -0.038(4) -0.015(3) -0.003(2) C22 0.018(3) 0.086(5) 0.067(4) 0.055(4) -0.002(3) -0.010(3) C23 0.026(3) 0.084(6) 0.067(5) -0.008(4) 0.006(3) 0.005(3) C24 0.072(4) 0.030(3) 0.016(2) 0.007(2) 0.006(2) -0.010(3) C25 0.040(3) 0.044(3) 0.035(3) 0.028(3) -0.009(2) -0.002(2) C26 0.056(3) 0.017(2) 0.027(3) 0.010(2) 0.013(2) 0.006(2) C27 0.036(3) 0.035(3) 0.038(3) 0.023(2) -0.005(2) -0.016(2) C28 0.047(3) 0.038(3) 0.049(3) 0.031(3) 0.028(3) 0.011(3) N1 0.043(3) 0.044(3) 0.029(3) -0.001(2) 0.007(2) 0.005(2) N2 0.044(3) 0.032(3) 0.063(4) 0.003(2) 0.003(3) -0.002(2) N3 0.061(3) 0.042(3) 0.035(3) -0.004(2) 0.019(3) -0.002(3) N4 0.076(4) 0.035(3) 0.042(3) -0.003(2) 0.019(3) -0.008(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 Pt1 S3 2.2592(12) . ? Pt1 S2 2.2650(13) . ? Pt1 S1 2.2749(12) . ? Pt1 S4 2.2810(12) . ? Fe1 C10 2.084(6) . ? Fe1 C9 2.110(6) . ? Fe1 C11 2.125(6) . ? Fe1 C13 2.132(5) . ? Fe1 C12 2.145(6) . ? Fe1 S5 2.1890(12) . ? Fe1 S6 2.2133(13) . ? Fe1 S8 2.2350(13) . ? Fe1 Fe2 2.6598(9) . ? Fe2 C16 2.081(6) . ? Fe2 C15 2.103(6) . ? Fe2 C17 2.109(5) . ? Fe2 C14 2.123(5) . ? Fe2 C18 2.134(5) . ? Fe2 S5 2.1902(13) . ? Fe2 S6 2.1941(13) . ? Fe2 S7 2.2684(13) . ? Fe3 C22 2.076(6) . ? Fe3 C21 2.095(5) . ? Fe3 C23 2.103(7) . ? Fe3 C19 2.110(6) . ? Fe3 C20 2.119(5) . ? Fe3 S8 2.1749(13) . ? Fe3 S7 2.1961(13) . ? Fe3 S6 2.2464(13) . ? Fe3 Fe4 2.6533(9) . ? Fe4 C27 2.096(5) . ? Fe4 C28 2.107(5) . ? Fe4 C26 2.132(5) . ? Fe4 C24 2.148(5) . ? Fe4 C25 2.160(5) . ? Fe4 S8 2.1826(13) . ? Fe4 S7 2.2310(13) . ? Fe4 S5 2.2384(13) . ? S1 C1 1.724(5) . ? S2 C3 1.707(5) . ? S3 C5 1.721(5) . ? S4 C7 1.729(5) . ? C1 C3 1.369(7) . ? C1 C2 1.433(7) . ? C2 N1 1.155(7) . ? C3 C4 1.446(7) . ? C4 N2 1.131(8) . ? C5 C7 1.372(8) . ? C5 C6 1.435(8) . ? C6 N3 1.140(8) . ? C7 C8 1.434(8) . ? C8 N4 1.145(8) . ? C9 C13 1.393(11) . ? C9 C10 1.401(13) . ? C10 C11 1.391(13) . ? C11 C12 1.349(10) . ? C12 C13 1.386(10) . ? C14 C18 1.404(10) . ? C14 C15 1.427(11) . ? C15 C16 1.387(11) . ? C16 C17 1.365(10) . ? C17 C18 1.376(9) . ? C19 C23 1.312(12) . ? C19 C20 1.369(11) . ? C20 C21 1.454(11) . ? C21 C22 1.430(11) . ? C22 C23 1.327(11) . ? C24 C25 1.402(9) . ? C24 C28 1.410(9) . ? C25 C26 1.397(8) . ? C26 C27 1.412(8) . ? C27 C28 1.414(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Pt1 S2 87.27(5) . . ? S3 Pt1 S1 177.41(4) . . ? S2 Pt1 S1 90.16(4) . . ? S3 Pt1 S4 90.08(5) . . ? S2 Pt1 S4 177.33(4) . . ? S1 Pt1 S4 92.48(4) . . ? C10 Fe1 C9 39.0(4) . . ? C10 Fe1 C11 38.6(4) . . ? C9 Fe1 C11 64.3(3) . . ? C10 Fe1 C13 64.4(3) . . ? C9 Fe1 C13 38.3(3) . . ? C11 Fe1 C13 63.2(3) . . ? C10 Fe1 C12 63.4(3) . . ? C9 Fe1 C12 63.6(2) . . ? C11 Fe1 C12 36.8(3) . . ? C13 Fe1 C12 37.8(3) . . ? C10 Fe1 S5 157.7(2) . . ? C9 Fe1 S5 123.5(3) . . ? C11 Fe1 S5 130.1(3) . . ? C13 Fe1 S5 93.5(2) . . ? C12 Fe1 S5 97.7(2) . . ? C10 Fe1 S6 99.9(3) . . ? C9 Fe1 S6 135.7(3) . . ? C11 Fe1 S6 94.1(2) . . ? C13 Fe1 S6 157.2(2) . . ? C12 Fe1 S6 121.3(2) . . ? S5 Fe1 S6 100.25(5) . . ? C10 Fe1 S8 98.5(3) . . ? C9 Fe1 S8 89.6(2) . . ? C11 Fe1 S8 135.4(3) . . ? C13 Fe1 S8 117.5(2) . . ? C12 Fe1 S8 153.0(2) . . ? S5 Fe1 S8 94.31(5) . . ? S6 Fe1 S8 79.80(5) . . ? C10 Fe1 Fe2 139.3(3) . . ? C9 Fe1 Fe2 166.0(2) . . ? C11 Fe1 Fe2 106.9(2) . . ? C13 Fe1 Fe2 128.8(2) . . ? C12 Fe1 Fe2 102.7(2) . . ? S5 Fe1 Fe2 52.62(3) . . ? S6 Fe1 Fe2 52.55(3) . . ? S8 Fe1 Fe2 103.80(4) . . ? C16 Fe2 C15 38.7(3) . . ? C16 Fe2 C17 38.0(3) . . ? C15 Fe2 C17 64.7(2) . . ? C16 Fe2 C14 64.5(3) . . ? C15 Fe2 C14 39.5(3) . . ? C17 Fe2 C14 64.0(2) . . ? C16 Fe2 C18 63.9(2) . . ? C15 Fe2 C18 65.3(2) . . ? C17 Fe2 C18 37.8(2) . . ? C14 Fe2 C18 38.5(3) . . ? C16 Fe2 S5 156.9(2) . . ? C15 Fe2 S5 139.2(3) . . ? C17 Fe2 S5 119.9(2) . . ? C14 Fe2 S5 102.6(2) . . ? C18 Fe2 S5 93.9(2) . . ? C16 Fe2 S6 102.2(2) . . ? C15 Fe2 S6 92.4(2) . . ? C17 Fe2 S6 137.8(2) . . ? C14 Fe2 S6 120.2(2) . . ? C18 Fe2 S6 157.2(2) . . ? S5 Fe2 S6 100.81(5) . . ? C16 Fe2 S7 103.9(2) . . ? C15 Fe2 S7 139.9(3) . . ? C17 Fe2 S7 94.2(2) . . ? C14 Fe2 S7 156.8(2) . . ? C18 Fe2 S7 118.8(2) . . ? S5 Fe2 S7 80.56(5) . . ? S6 Fe2 S7 81.06(5) . . ? C16 Fe2 Fe1 146.9(2) . . ? C15 Fe2 Fe1 113.2(2) . . ? C17 Fe2 Fe1 167.3(2) . . ? C14 Fe2 Fe1 106.0(2) . . ? C18 Fe2 Fe1 129.5(2) . . ? S5 Fe2 Fe1 52.58(3) . . ? S6 Fe2 Fe1 53.21(3) . . ? S7 Fe2 Fe1 94.30(4) . . ? C22 Fe3 C21 40.1(3) . . ? C22 Fe3 C23 37.0(3) . . ? C21 Fe3 C23 65.3(3) . . ? C22 Fe3 C19 61.9(3) . . ? C21 Fe3 C19 65.0(3) . . ? C23 Fe3 C19 36.3(3) . . ? C22 Fe3 C20 64.9(2) . . ? C21 Fe3 C20 40.4(3) . . ? C23 Fe3 C20 63.3(3) . . ? C19 Fe3 C20 37.8(3) . . ? C22 Fe3 S8 128.8(2) . . ? C21 Fe3 S8 157.8(2) . . ? C23 Fe3 S8 96.1(2) . . ? C19 Fe3 S8 92.8(2) . . ? C20 Fe3 S8 121.5(2) . . ? C22 Fe3 S7 127.8(2) . . ? C21 Fe3 S7 96.5(2) . . ? C23 Fe3 S7 161.8(2) . . ? C19 Fe3 S7 137.1(3) . . ? C20 Fe3 S7 103.0(2) . . ? S8 Fe3 S7 101.59(5) . . ? C22 Fe3 S6 92.9(2) . . ? C21 Fe3 S6 115.3(3) . . ? C23 Fe3 S6 106.0(3) . . ? C19 Fe3 S6 141.2(3) . . ? C20 Fe3 S6 155.3(2) . . ? S8 Fe3 S6 80.37(5) . . ? S7 Fe3 S6 81.51(5) . . ? C22 Fe3 Fe4 172.9(2) . . ? C21 Fe3 Fe4 135.4(3) . . ? C23 Fe3 Fe4 139.6(3) . . ? C19 Fe3 Fe4 111.9(2) . . ? C20 Fe3 Fe4 108.2(2) . . ? S8 Fe3 Fe4 52.62(3) . . ? S7 Fe3 Fe4 53.78(3) . . ? S6 Fe3 Fe4 94.20(4) . . ? C27 Fe4 C28 39.3(2) . . ? C27 Fe4 C26 39.0(2) . . ? C28 Fe4 C26 65.0(2) . . ? C27 Fe4 C24 65.1(2) . . ? C28 Fe4 C24 38.7(2) . . ? C26 Fe4 C24 64.1(2) . . ? C27 Fe4 C25 64.6(2) . . ? C28 Fe4 C25 64.4(2) . . ? C26 Fe4 C25 38.0(2) . . ? C24 Fe4 C25 38.0(2) . . ? C27 Fe4 S8 107.3(2) . . ? C28 Fe4 S8 146.6(2) . . ? C26 Fe4 S8 87.55(14) . . ? C24 Fe4 S8 143.8(2) . . ? C25 Fe4 S8 105.9(2) . . ? C27 Fe4 S7 152.4(2) . . ? C28 Fe4 S7 113.2(2) . . ? C26 Fe4 S7 148.0(2) . . ? C24 Fe4 S7 94.1(2) . . ? C25 Fe4 S7 110.7(2) . . ? S8 Fe4 S7 100.24(5) . . ? C27 Fe4 S5 94.6(2) . . ? C28 Fe4 S5 90.0(2) . . ? C26 Fe4 S5 130.4(2) . . ? C24 Fe4 S5 120.9(2) . . ? C25 Fe4 S5 154.3(2) . . ? S8 Fe4 S5 94.39(5) . . ? S7 Fe4 S5 80.34(5) . . ? C27 Fe4 Fe3 152.9(2) . . ? C28 Fe4 Fe3 156.5(2) . . ? C26 Fe4 Fe3 115.7(2) . . ? C24 Fe4 Fe3 118.7(2) . . ? C25 Fe4 Fe3 101.1(2) . . ? S8 Fe4 Fe3 52.36(4) . . ? S7 Fe4 Fe3 52.58(3) . . ? S5 Fe4 Fe3 103.87(4) . . ? C1 S1 Pt1 102.0(2) . . ? C3 S2 Pt1 102.8(2) . . ? C5 S3 Pt1 103.3(2) . . ? C7 S4 Pt1 102.1(2) . . ? Fe1 S5 Fe2 74.80(4) . . ? Fe1 S5 Fe4 85.28(4) . . ? Fe2 S5 Fe4 97.12(5) . . ? Fe2 S6 Fe1 74.24(4) . . ? Fe2 S6 Fe3 98.42(5) . . ? Fe1 S6 Fe3 95.82(5) . . ? Fe3 S7 Fe4 73.64(4) . . ? Fe3 S7 Fe2 97.70(5) . . ? Fe4 S7 Fe2 95.10(5) . . ? Fe3 S8 Fe4 75.02(4) . . ? Fe3 S8 Fe1 97.26(5) . . ? Fe4 S8 Fe1 85.51(4) . . ? C3 C1 C2 120.8(5) . . ? C3 C1 S1 122.6(4) . . ? C2 C1 S1 116.7(4) . . ? N1 C2 C1 179.1(6) . . ? C1 C3 C4 120.7(5) . . ? C1 C3 S2 122.5(4) . . ? C4 C3 S2 116.7(4) . . ? N2 C4 C3 179.1(6) . . ? C7 C5 C6 123.1(5) . . ? C7 C5 S3 121.8(4) . . ? C6 C5 S3 115.1(4) . . ? N3 C6 C5 177.7(6) . . ? C5 C7 C8 121.1(5) . . ? C5 C7 S4 122.7(4) . . ? C8 C7 S4 116.2(4) . . ? N4 C8 C7 179.5(7) . . ? C13 C9 C10 107.1(6) . . ? C13 C9 Fe1 71.7(3) . . ? C10 C9 Fe1 69.5(4) . . ? C11 C10 C9 107.6(6) . . ? C11 C10 Fe1 72.3(4) . . ? C9 C10 Fe1 71.5(4) . . ? C12 C11 C10 108.4(7) . . ? C12 C11 Fe1 72.4(4) . . ? C10 C11 Fe1 69.1(4) . . ? C11 C12 C13 109.3(6) . . ? C11 C12 Fe1 70.8(4) . . ? C13 C12 Fe1 70.6(3) . . ? C12 C13 C9 107.5(6) . . ? C12 C13 Fe1 71.6(3) . . ? C9 C13 Fe1 70.0(3) . . ? C18 C14 C15 107.7(6) . . ? C18 C14 Fe2 71.2(3) . . ? C15 C14 Fe2 69.5(3) . . ? C16 C15 C14 105.7(5) . . ? C16 C15 Fe2 69.8(3) . . ? C14 C15 Fe2 71.0(3) . . ? C17 C16 C15 110.0(6) . . ? C17 C16 Fe2 72.1(3) . . ? C15 C16 Fe2 71.5(4) . . ? C16 C17 C18 108.9(6) . . ? C16 C17 Fe2 69.9(3) . . ? C18 C17 Fe2 72.1(3) . . ? C17 C18 C14 107.6(6) . . ? C17 C18 Fe2 70.1(3) . . ? C14 C18 Fe2 70.3(3) . . ? C23 C19 C20 111.4(7) . . ? C23 C19 Fe3 71.6(4) . . ? C20 C19 Fe3 71.5(4) . . ? C19 C20 C21 106.3(6) . . ? C19 C20 Fe3 70.7(4) . . ? C21 C20 Fe3 68.9(3) . . ? C22 C21 C20 102.6(6) . . ? C22 C21 Fe3 69.2(3) . . ? C20 C21 Fe3 70.7(3) . . ? C23 C22 C21 110.4(7) . . ? C23 C22 Fe3 72.6(4) . . ? C21 C22 Fe3 70.7(3) . . ? C19 C23 C22 109.3(7) . . ? C19 C23 Fe3 72.1(4) . . ? C22 C23 Fe3 70.4(4) . . ? C25 C24 C28 107.9(5) . . ? C25 C24 Fe4 71.5(3) . . ? C28 C24 Fe4 69.1(3) . . ? C26 C25 C24 108.5(5) . . ? C26 C25 Fe4 69.9(3) . . ? C24 C25 Fe4 70.5(3) . . ? C25 C26 C27 108.2(5) . . ? C25 C26 Fe4 72.1(3) . . ? C27 C26 Fe4 69.1(3) . . ? C26 C27 C28 107.4(5) . . ? C26 C27 Fe4 71.9(3) . . ? C28 C27 Fe4 70.7(3) . . ? C24 C28 C27 108.0(5) . . ? C24 C28 Fe4 72.2(3) . . ? C27 C28 Fe4 69.9(3) . . ? _refine_diff_density_max 0.987 _refine_diff_density_min -1.376 _refine_diff_density_rms 0.183 #=END data_6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H40 Fe8N4 Pt1 S12' _chemical_formula_weight 1699.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5944(10) _cell_length_b 16.3005(15) _cell_length_c 15.6650(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.977(15) _cell_angle_gamma 90.00 _cell_volume 2655.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 156 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 25.01 _exptl_crystal_description diamonds _exptl_crystal_colour black _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.125 _exptl_crystal_density_method ? _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 5.253 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.925 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12487 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4657 _reflns_number_observed 4430 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+4.0000P] 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 4654 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_obs 0.0232 _refine_ls_wR_factor_all 0.0595 _refine_ls_wR_factor_obs 0.0573 _refine_ls_goodness_of_fit_all 1.116 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.120 _refine_ls_restrained_S_obs 1.107 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt -0.5000 0.0000 0.0000 0.02174(7) Uani 1 d S . Fe1 Fe -0.08447(4) -0.38559(3) -0.16662(3) 0.01577(10) Uani 1 d . . Fe2 Fe -0.13278(4) -0.21171(3) -0.06003(3) 0.01660(10) Uani 1 d . . Fe3 Fe -0.31628(4) -0.37385(3) -0.12448(3) 0.01486(10) Uani 1 d . . Fe4 Fe -0.26830(4) -0.22137(3) -0.21991(3) 0.01512(10) Uani 1 d . . S1 S -0.37429(8) 0.04465(5) 0.12693(5) 0.0264(2) Uani 1 d . . S2 S -0.44980(9) 0.11694(6) -0.06825(6) 0.0290(2) Uani 1 d . . S3 S -0.12564(7) -0.34884(5) -0.03962(5) 0.0183(2) Uani 1 d . . S4 S -0.33756(7) -0.24017(5) -0.09834(5) 0.0164(2) Uani 1 d . . S5 S -0.26616(7) -0.35508(5) -0.25222(4) 0.01561(15) Uani 1 d . . S6 S -0.06034(7) -0.24869(5) -0.17672(5) 0.0176(2) Uani 1 d . . N1 N -0.2411(3) 0.2347(2) 0.2324(2) 0.0419(8) Uani 1 d . . N2 N -0.2928(3) 0.3180(2) -0.0209(2) 0.0360(7) Uani 1 d . . C1 C -0.3372(3) 0.1441(2) 0.1010(2) 0.0242(7) Uani 1 d . . C2 C -0.2807(3) 0.1952(2) 0.1732(2) 0.0286(8) Uani 1 d . . C3 C -0.3647(3) 0.1734(2) 0.0180(2) 0.0254(7) Uani 1 d . . C4 C -0.3245(3) 0.2541(2) -0.0025(2) 0.0279(7) Uani 1 d . . C5 C 0.0444(5) -0.4791(3) -0.1125(3) 0.0492(13) Uani 1 d . . H14A H 0.0641(5) -0.4962(3) -0.0515(3) 0.059 Uiso 1 calc R . C6 C -0.0494(5) -0.5143(3) -0.1801(6) 0.077(2) Uani 1 d . . H17A H -0.1086(5) -0.5591(3) -0.1737(6) 0.092 Uiso 1 calc R . C7 C -0.0404(4) -0.4741(3) -0.2562(4) 0.0578(15) Uani 1 d . . H13A H -0.0925(4) -0.4857(3) -0.3136(4) 0.069 Uiso 1 calc R . C8 C 0.0535(4) -0.4179(3) -0.2393(2) 0.0385(10) Uani 1 d . . H16A H 0.0815(4) -0.3830(3) -0.2830(2) 0.046 Uiso 1 calc R . C9 C 0.1084(3) -0.4189(2) -0.1520(2) 0.0305(8) Uani 1 d . . H15A H 0.1825(3) -0.3864(2) -0.1236(2) 0.037 Uiso 1 calc R . C10 C 0.0239(4) -0.1779(3) 0.0350(3) 0.0390(10) Uani 1 d . . H23A H 0.1014(4) -0.2107(3) 0.0549(3) 0.047 Uiso 1 calc R . C11 C -0.0861(4) -0.1779(2) 0.0710(2) 0.0344(9) Uani 1 d . . H24A H -0.0999(4) -0.2117(2) 0.1202(2) 0.041 Uiso 1 calc R . C12 C -0.1712(4) -0.1201(3) 0.0283(3) 0.0418(10) Uani 1 d . . H5A H -0.2556(4) -0.1065(3) 0.0412(3) 0.050 Uiso 1 calc R . C13 C -0.1125(6) -0.0822(3) -0.0356(3) 0.0562(14) Uani 1 d . . H7A H -0.1490(6) -0.0381(3) -0.0752(3) 0.067 Uiso 1 calc R . C14 C 0.0080(5) -0.1185(3) -0.0304(3) 0.0492(12) Uani 1 d . . H6A H 0.0717(5) -0.1038(3) -0.0657(3) 0.059 Uiso 1 calc R . C15 C -0.4696(3) -0.4518(2) -0.1860(2) 0.0314(8) Uani 1 d . . H25A H -0.4999(3) -0.4577(2) -0.2489(2) 0.038 Uiso 1 calc R . C16 C -0.3766(4) -0.5007(2) -0.1341(3) 0.0375(10) Uani 1 d . . H4A H -0.3297(4) -0.5463(2) -0.1544(3) 0.045 Uiso 1 calc R . C17 C -0.3635(4) -0.4737(3) -0.0474(3) 0.0378(9) Uani 1 d . . H3A H -0.3072(4) -0.4977(3) 0.0033(3) 0.045 Uiso 1 calc R . C18 C -0.4485(3) -0.4078(2) -0.0463(2) 0.0291(8) Uani 1 d . . H2A H -0.4635(3) -0.3787(2) 0.0056(2) 0.035 Uiso 1 calc R . C19 C -0.5150(3) -0.3946(2) -0.1322(2) 0.0255(7) Uani 1 d . . H1A H -0.5839(3) -0.3546(2) -0.1505(2) 0.031 Uiso 1 calc R . C20 C -0.2622(4) -0.0965(2) -0.2613(2) 0.0346(9) Uani 1 d . . H8A H -0.2038(4) -0.0537(2) -0.2330(2) 0.042 Uiso 1 calc R . C21 C -0.2411(4) -0.1485(2) -0.3287(2) 0.0296(8) Uani 1 d . . H9A H -0.1643(4) -0.1487(2) -0.3551(2) 0.035 Uiso 1 calc R . C22 C -0.3487(4) -0.1993(2) -0.3528(2) 0.0339(8) Uani 1 d . . H10A H -0.3603(4) -0.2403(2) -0.3994(2) 0.041 Uiso 1 calc R . C23 C -0.4381(4) -0.1800(3) -0.3007(3) 0.0432(11) Uani 1 d . . H12A H -0.5240(4) -0.2038(3) -0.3052(3) 0.052 Uiso 1 calc R . C24 C -0.3837(4) -0.1157(3) -0.2432(3) 0.0436(11) Uani 1 d . . H11A H -0.4259(4) -0.0879(3) -0.2008(3) 0.052 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01809(10) 0.02095(11) 0.02738(11) 0.00332(7) 0.00736(7) 0.00392(6) Fe1 0.0135(2) 0.0140(2) 0.0199(2) -0.0006(2) 0.0034(2) 0.0028(2) Fe2 0.0149(2) 0.0151(2) 0.0205(2) -0.0034(2) 0.0051(2) -0.0013(2) Fe3 0.0146(2) 0.0126(2) 0.0183(2) 0.0005(2) 0.0053(2) -0.0017(2) Fe4 0.0140(2) 0.0130(2) 0.0194(2) 0.0030(2) 0.0056(2) 0.0017(2) S1 0.0262(4) 0.0259(5) 0.0276(4) 0.0050(3) 0.0063(3) 0.0022(3) S2 0.0310(4) 0.0269(5) 0.0286(4) 0.0054(3) 0.0046(3) -0.0022(4) S3 0.0190(4) 0.0180(4) 0.0174(3) 0.0005(3) 0.0021(3) 0.0014(3) S4 0.0154(3) 0.0142(4) 0.0211(3) -0.0002(3) 0.0074(3) 0.0005(3) S5 0.0151(3) 0.0152(4) 0.0168(3) 0.0000(3) 0.0037(3) 0.0006(3) S6 0.0141(3) 0.0161(4) 0.0239(4) -0.0010(3) 0.0067(3) 0.0002(3) N1 0.038(2) 0.047(2) 0.041(2) -0.008(2) 0.0089(15) -0.008(2) N2 0.036(2) 0.031(2) 0.040(2) 0.0037(14) 0.0054(14) -0.0025(14) C1 0.017(2) 0.024(2) 0.034(2) -0.0001(14) 0.0092(13) 0.0030(13) C2 0.019(2) 0.032(2) 0.037(2) 0.005(2) 0.0114(15) 0.0045(14) C3 0.021(2) 0.025(2) 0.032(2) 0.0025(14) 0.0083(14) 0.0041(13) C4 0.021(2) 0.029(2) 0.033(2) 0.0005(15) 0.0033(14) 0.0037(14) C5 0.059(3) 0.049(3) 0.048(2) 0.028(2) 0.033(2) 0.044(2) C6 0.028(2) 0.013(2) 0.196(8) -0.018(3) 0.039(4) 0.002(2) C7 0.035(2) 0.054(3) 0.076(3) -0.041(3) -0.010(2) 0.024(2) C8 0.041(2) 0.045(3) 0.034(2) 0.007(2) 0.018(2) 0.030(2) C9 0.016(2) 0.028(2) 0.046(2) -0.008(2) 0.0035(14) 0.0087(14) C10 0.025(2) 0.041(2) 0.047(2) -0.027(2) -0.004(2) -0.001(2) C11 0.045(2) 0.032(2) 0.025(2) -0.0114(15) 0.006(2) -0.011(2) C12 0.025(2) 0.040(2) 0.058(3) -0.034(2) 0.002(2) -0.001(2) C13 0.098(4) 0.015(2) 0.043(2) -0.007(2) -0.018(2) -0.003(2) C14 0.062(3) 0.044(3) 0.049(2) -0.028(2) 0.029(2) -0.037(2) C15 0.032(2) 0.032(2) 0.033(2) -0.0067(15) 0.0108(15) -0.020(2) C16 0.031(2) 0.017(2) 0.071(3) -0.005(2) 0.027(2) -0.0108(14) C17 0.026(2) 0.035(2) 0.051(2) 0.028(2) 0.005(2) -0.012(2) C18 0.028(2) 0.034(2) 0.029(2) -0.0052(14) 0.0166(14) -0.018(2) C19 0.0134(15) 0.025(2) 0.039(2) 0.0010(14) 0.0059(13) -0.0074(13) C20 0.056(2) 0.014(2) 0.033(2) 0.0088(14) 0.007(2) -0.003(2) C21 0.034(2) 0.029(2) 0.028(2) 0.0144(14) 0.0101(15) 0.005(2) C22 0.045(2) 0.027(2) 0.025(2) 0.0100(14) -0.006(2) 0.002(2) C23 0.025(2) 0.047(3) 0.054(2) 0.033(2) -0.002(2) 0.006(2) C24 0.058(3) 0.036(2) 0.043(2) 0.024(2) 0.025(2) 0.036(2) _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 Pt1 S1 2.2910(8) . ? Pt1 S1 2.2910(8) 3_455 ? Pt1 S2 2.2970(9) . ? Pt1 S2 2.2971(9) 3_455 ? Fe1 C8 2.084(3) . ? Fe1 C9 2.085(3) . ? Fe1 C5 2.113(4) . ? Fe1 C7 2.125(4) . ? Fe1 C6 2.147(4) . ? Fe1 S5 2.1835(8) . ? Fe1 S3 2.1993(8) . ? Fe1 S6 2.2551(9) . ? Fe1 Fe3 2.6685(6) . ? Fe2 C10 2.082(4) . ? Fe2 C11 2.091(3) . ? Fe2 C14 2.117(4) . ? Fe2 C12 2.127(4) . ? Fe2 C13 2.149(4) . ? Fe2 S4 2.1878(8) . ? Fe2 S6 2.1973(8) . ? Fe2 S3 2.2573(9) . ? Fe2 Fe4 2.6438(6) . ? Fe3 C18 2.103(3) . ? Fe3 C19 2.113(3) . ? Fe3 C17 2.141(3) . ? Fe3 C15 2.141(3) . ? Fe3 C16 2.161(3) . ? Fe3 S5 2.1874(8) . ? Fe3 S3 2.2338(8) . ? Fe3 S4 2.2365(8) . ? Fe4 C24 2.103(3) . ? Fe4 C23 2.104(4) . ? Fe4 C22 2.125(3) . ? Fe4 C21 2.141(3) . ? Fe4 C20 2.141(3) . ? Fe4 S4 2.1889(8) . ? Fe4 S6 2.2233(8) . ? Fe4 S5 2.2386(8) . ? S1 C1 1.734(3) . ? S2 C3 1.737(4) . ? N1 C2 1.141(5) . ? N2 C4 1.148(5) . ? C1 C3 1.364(5) . ? C1 C2 1.440(5) . ? C3 C4 1.438(5) . ? C5 C9 1.401(6) . ? C5 C6 1.426(8) . ? C6 C7 1.380(9) . ? C7 C8 1.340(7) . ? C8 C9 1.381(5) . ? C10 C11 1.388(5) . ? C10 C14 1.396(7) . ? C11 C12 1.385(6) . ? C12 C13 1.416(7) . ? C13 C14 1.396(7) . ? C15 C19 1.401(5) . ? C15 C16 1.402(6) . ? C16 C17 1.409(6) . ? C17 C18 1.403(6) . ? C18 C19 1.412(5) . ? C20 C24 1.405(6) . ? C20 C21 1.406(5) . ? C21 C22 1.401(5) . ? C22 C23 1.399(6) . ? C23 C24 1.429(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pt1 S1 180.0 . 3_455 ? S1 Pt1 S2 89.57(3) . . ? S1 Pt1 S2 90.43(3) 3_455 . ? S1 Pt1 S2 90.43(3) . 3_455 ? S1 Pt1 S2 89.57(3) 3_455 3_455 ? S2 Pt1 S2 180.0 . 3_455 ? C8 Fe1 C9 38.70(14) . . ? C8 Fe1 C5 64.51(15) . . ? C9 Fe1 C5 39.0(2) . . ? C8 Fe1 C7 37.1(2) . . ? C9 Fe1 C7 64.0(2) . . ? C5 Fe1 C7 64.4(2) . . ? C8 Fe1 C6 63.1(2) . . ? C9 Fe1 C6 64.7(2) . . ? C5 Fe1 C6 39.1(2) . . ? C7 Fe1 C6 37.7(2) . . ? C8 Fe1 S5 110.49(11) . . ? C9 Fe1 S5 149.11(11) . . ? C5 Fe1 S5 146.8(2) . . ? C7 Fe1 S5 91.61(12) . . ? C6 Fe1 S5 108.1(2) . . ? C8 Fe1 S3 147.51(12) . . ? C9 Fe1 S3 109.29(10) . . ? C5 Fe1 S3 93.33(12) . . ? C7 Fe1 S3 152.7(2) . . ? C6 Fe1 S3 115.0(2) . . ? S5 Fe1 S3 100.95(3) . . ? C8 Fe1 S6 96.40(13) . . ? C9 Fe1 S6 98.28(11) . . ? C5 Fe1 S6 132.0(2) . . ? C7 Fe1 S6 125.7(2) . . ? C6 Fe1 S6 159.3(2) . . ? S5 Fe1 S6 80.21(3) . . ? S3 Fe1 S6 80.71(3) . . ? C8 Fe1 Fe3 158.02(12) . . ? C9 Fe1 Fe3 156.99(11) . . ? C5 Fe1 Fe3 120.48(12) . . ? C7 Fe1 Fe3 122.70(14) . . ? C6 Fe1 Fe3 106.18(13) . . ? S5 Fe1 Fe3 52.44(2) . . ? S3 Fe1 Fe3 53.58(2) . . ? S6 Fe1 Fe3 93.92(2) . . ? C10 Fe2 C11 38.8(2) . . ? C10 Fe2 C14 38.8(2) . . ? C11 Fe2 C14 64.6(2) . . ? C10 Fe2 C12 64.80(15) . . ? C11 Fe2 C12 38.3(2) . . ? C14 Fe2 C12 64.4(2) . . ? C10 Fe2 C13 64.8(2) . . ? C11 Fe2 C13 64.5(2) . . ? C14 Fe2 C13 38.2(2) . . ? C12 Fe2 C13 38.7(2) . . ? C10 Fe2 S4 150.02(12) . . ? C11 Fe2 S4 111.21(11) . . ? C14 Fe2 S4 146.4(2) . . ? C12 Fe2 S4 91.43(10) . . ? C13 Fe2 S4 108.5(2) . . ? C10 Fe2 S6 108.08(11) . . ? C11 Fe2 S6 146.51(11) . . ? C14 Fe2 S6 92.05(12) . . ? C12 Fe2 S6 150.92(13) . . ? C13 Fe2 S6 112.25(15) . . ? S4 Fe2 S6 101.47(3) . . ? C10 Fe2 S3 99.22(13) . . ? C11 Fe2 S3 97.27(11) . . ? C14 Fe2 S3 132.5(2) . . ? C12 Fe2 S3 127.51(14) . . ? C13 Fe2 S3 161.47(12) . . ? S4 Fe2 S3 80.42(3) . . ? S6 Fe2 S3 80.71(3) . . ? C10 Fe2 Fe4 155.30(13) . . ? C11 Fe2 Fe4 158.38(12) . . ? C14 Fe2 Fe4 118.88(13) . . ? C12 Fe2 Fe4 121.42(12) . . ? C13 Fe2 Fe4 104.18(11) . . ? S4 Fe2 Fe4 52.86(2) . . ? S6 Fe2 Fe4 53.72(2) . . ? S3 Fe2 Fe4 94.16(2) . . ? C18 Fe3 C19 39.13(14) . . ? C18 Fe3 C17 38.6(2) . . ? C19 Fe3 C17 64.75(14) . . ? C18 Fe3 C15 64.76(13) . . ? C19 Fe3 C15 38.45(14) . . ? C17 Fe3 C15 64.19(15) . . ? C18 Fe3 C16 64.38(15) . . ? C19 Fe3 C16 64.19(15) . . ? C17 Fe3 C16 38.2(2) . . ? C15 Fe3 C16 38.0(2) . . ? C18 Fe3 S5 150.96(10) . . ? C19 Fe3 S5 112.50(10) . . ? C17 Fe3 S5 138.21(13) . . ? C15 Fe3 S5 88.08(10) . . ? C16 Fe3 S5 100.97(12) . . ? C18 Fe3 S3 109.19(10) . . ? C19 Fe3 S3 147.30(10) . . ? C17 Fe3 S3 94.88(10) . . ? C15 Fe3 S3 153.99(11) . . ? C16 Fe3 S3 115.97(13) . . ? S5 Fe3 S3 99.75(3) . . ? C18 Fe3 S4 92.78(11) . . ? C19 Fe3 S4 91.86(10) . . ? C17 Fe3 S4 126.48(13) . . ? C15 Fe3 S4 124.47(11) . . ? C16 Fe3 S4 154.99(11) . . ? S5 Fe3 S4 94.69(3) . . ? S3 Fe3 S4 79.89(3) . . ? C18 Fe3 Fe1 150.66(11) . . ? C19 Fe3 Fe1 158.15(10) . . ? C17 Fe3 Fe1 114.20(11) . . ? C15 Fe3 Fe1 120.08(10) . . ? C16 Fe3 Fe1 100.84(11) . . ? S5 Fe3 Fe1 52.31(2) . . ? S3 Fe3 Fe1 52.40(2) . . ? S4 Fe3 Fe1 104.17(3) . . ? C24 Fe4 C23 39.7(2) . . ? C24 Fe4 C22 65.2(2) . . ? C23 Fe4 C22 38.6(2) . . ? C24 Fe4 C21 64.53(14) . . ? C23 Fe4 C21 64.70(15) . . ? C22 Fe4 C21 38.35(15) . . ? C24 Fe4 C20 38.7(2) . . ? C23 Fe4 C20 65.4(2) . . ? C22 Fe4 C20 64.66(15) . . ? C21 Fe4 C20 38.33(14) . . ? C24 Fe4 S4 89.17(11) . . ? C23 Fe4 S4 100.29(12) . . ? C22 Fe4 S4 137.57(11) . . ? C21 Fe4 S4 152.68(10) . . ? C20 Fe4 S4 115.52(11) . . ? C24 Fe4 S6 136.60(14) . . ? C23 Fe4 S6 158.68(11) . . ? C22 Fe4 S6 121.41(11) . . ? C21 Fe4 S6 94.43(10) . . ? C20 Fe4 S6 101.37(12) . . ? S4 Fe4 S6 100.61(3) . . ? C24 Fe4 S5 142.04(14) . . ? C23 Fe4 S5 102.75(14) . . ? C22 Fe4 S5 87.86(11) . . ? C21 Fe4 S5 110.56(11) . . ? C20 Fe4 S5 148.77(10) . . ? S4 Fe4 S5 94.59(3) . . ? S6 Fe4 S5 79.73(3) . . ? C24 Fe4 Fe2 107.97(13) . . ? C23 Fe4 Fe2 143.01(14) . . ? C22 Fe4 Fe2 164.20(11) . . ? C21 Fe4 Fe2 126.14(10) . . ? C20 Fe4 Fe2 100.82(10) . . ? S4 Fe4 Fe2 52.82(2) . . ? S6 Fe4 Fe2 52.82(2) . . ? S5 Fe4 Fe2 104.19(2) . . ? C1 S1 Pt1 102.37(12) . . ? C3 S2 Pt1 102.08(12) . . ? Fe1 S3 Fe3 74.02(3) . . ? Fe1 S3 Fe2 98.55(3) . . ? Fe3 S3 Fe2 95.41(3) . . ? Fe2 S4 Fe4 74.32(3) . . ? Fe2 S4 Fe3 97.33(3) . . ? Fe4 S4 Fe3 85.12(3) . . ? Fe1 S5 Fe3 75.25(3) . . ? Fe1 S5 Fe4 97.39(3) . . ? Fe3 S5 Fe4 85.10(3) . . ? Fe2 S6 Fe4 73.46(3) . . ? Fe2 S6 Fe1 98.68(3) . . ? Fe4 S6 Fe1 95.77(3) . . ? C3 C1 C2 121.9(3) . . ? C3 C1 S1 122.2(3) . . ? C2 C1 S1 115.9(3) . . ? N1 C2 C1 176.4(4) . . ? C1 C3 C4 120.9(3) . . ? C1 C3 S2 122.8(3) . . ? C4 C3 S2 116.3(2) . . ? N2 C4 C3 178.3(4) . . ? C9 C5 C6 106.4(4) . . ? C9 C5 Fe1 69.4(2) . . ? C6 C5 Fe1 71.7(2) . . ? C7 C6 C5 107.3(4) . . ? C7 C6 Fe1 70.3(3) . . ? C5 C6 Fe1 69.1(2) . . ? C8 C7 C6 109.0(4) . . ? C8 C7 Fe1 69.8(2) . . ? C6 C7 Fe1 72.0(3) . . ? C7 C8 C9 110.2(4) . . ? C7 C8 Fe1 73.1(3) . . ? C9 C8 Fe1 70.7(2) . . ? C8 C9 C5 107.2(4) . . ? C8 C9 Fe1 70.6(2) . . ? C5 C9 Fe1 71.6(2) . . ? C11 C10 C14 107.8(4) . . ? C11 C10 Fe2 70.9(2) . . ? C14 C10 Fe2 72.0(2) . . ? C12 C11 C10 108.8(4) . . ? C12 C11 Fe2 72.2(2) . . ? C10 C11 Fe2 70.2(2) . . ? C11 C12 C13 107.8(4) . . ? C11 C12 Fe2 69.4(2) . . ? C13 C12 Fe2 71.5(2) . . ? C14 C13 C12 107.1(4) . . ? C14 C13 Fe2 69.7(2) . . ? C12 C13 Fe2 69.8(2) . . ? C13 C14 C10 108.5(4) . . ? C13 C14 Fe2 72.1(2) . . ? C10 C14 Fe2 69.2(2) . . ? C19 C15 C16 108.2(3) . . ? C19 C15 Fe3 69.7(2) . . ? C16 C15 Fe3 71.7(2) . . ? C15 C16 C17 108.1(3) . . ? C15 C16 Fe3 70.2(2) . . ? C17 C16 Fe3 70.1(2) . . ? C18 C17 C16 107.8(3) . . ? C18 C17 Fe3 69.2(2) . . ? C16 C17 Fe3 71.7(2) . . ? C17 C18 C19 108.1(3) . . ? C17 C18 Fe3 72.2(2) . . ? C19 C18 Fe3 70.8(2) . . ? C15 C19 C18 107.8(3) . . ? C15 C19 Fe3 71.9(2) . . ? C18 C19 Fe3 70.0(2) . . ? C24 C20 C21 107.4(4) . . ? C24 C20 Fe4 69.2(2) . . ? C21 C20 Fe4 70.8(2) . . ? C22 C21 C20 108.7(3) . . ? C22 C21 Fe4 70.2(2) . . ? C20 C21 Fe4 70.8(2) . . ? C23 C22 C21 108.4(4) . . ? C23 C22 Fe4 69.9(2) . . ? C21 C22 Fe4 71.5(2) . . ? C22 C23 C24 107.3(4) . . ? C22 C23 Fe4 71.5(2) . . ? C24 C23 Fe4 70.1(2) . . ? C20 C24 C23 108.1(3) . . ? C20 C24 Fe4 72.1(2) . . ? C23 C24 Fe4 70.2(2) . . ? _refine_diff_density_max 0.686 _refine_diff_density_min -1.709 _refine_diff_density_rms 0.102 #=END