# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jingping Qu' _publ_contact_author_email QUJP@CHEM.DLUT.EDU.CN _publ_section_title ; Insertion Reactions of CS2, COS, PhNCS at Thiolate-Bridged Diiron Centers ; loop_ _publ_author_name 'Jingping Qu.' 'Yanhui Chen.' 'Pingping Chen.' 'Shuoyi Chen.' 'Yang Li.' ; Litao Liu ; 'Ying Peng.' 'Jinfeng Zhao.' # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 737810' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H40 Fe2 S4' _chemical_formula_weight 568.50 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 18.9893(6) _cell_length_b 12.8536(6) _cell_length_c 11.2639(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.964(4) _cell_angle_gamma 90.00 _cell_volume 2745.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5368 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5902 _exptl_absorpt_correction_T_max 0.7170 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11074 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2420 _reflns_number_gt 2119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.8589P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2420 _refine_ls_number_parameters 227 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.427119(14) 0.21749(2) 0.16142(2) 0.04141(13) Uani 1 1 d . . . S1 S 0.54162(3) 0.27085(4) 0.14859(4) 0.04481(16) Uani 1 1 d . . . S2 S 0.45570(3) 0.05920(4) 0.19537(5) 0.05469(17) Uani 1 1 d . . . C1 C 0.3857(8) 0.3271(18) 0.038(3) 0.067(5) Uani 0.511(13) 1 d PD A 1 C2 C 0.3830(10) 0.228(3) -0.0106(13) 0.067(5) Uani 0.511(13) 1 d PD A 1 C3 C 0.3390(10) 0.1672(10) 0.057(2) 0.055(3) Uani 0.511(13) 1 d PD A 1 C4 C 0.3168(7) 0.228(2) 0.1501(12) 0.063(4) Uani 0.511(13) 1 d PD A 1 C5 C 0.3453(13) 0.3259(15) 0.137(2) 0.062(5) Uani 0.511(13) 1 d PD A 1 C6 C 0.4241(5) 0.4186(11) -0.0105(17) 0.243(14) Uani 0.511(13) 1 d PD A 1 H6A H 0.3933 0.4555 -0.0662 0.364 Uiso 0.511(13) 1 calc PR A 1 H6B H 0.4647 0.3947 -0.0498 0.364 Uiso 0.511(13) 1 calc PR A 1 H6C H 0.4388 0.4641 0.0537 0.364 Uiso 0.511(13) 1 calc PR A 1 C7 C 0.4166(6) 0.1930(16) -0.1222(7) 0.251(15) Uani 0.511(13) 1 d PD A 1 H7A H 0.3851 0.2064 -0.1898 0.377 Uiso 0.511(13) 1 calc PR A 1 H7B H 0.4264 0.1198 -0.1172 0.377 Uiso 0.511(13) 1 calc PR A 1 H7C H 0.4599 0.2304 -0.1306 0.377 Uiso 0.511(13) 1 calc PR A 1 C8 C 0.3173(7) 0.0581(7) 0.0296(14) 0.169(8) Uani 0.511(13) 1 d PD A 1 H8A H 0.2750 0.0584 -0.0211 0.253 Uiso 0.511(13) 1 calc PR A 1 H8B H 0.3086 0.0221 0.1021 0.253 Uiso 0.511(13) 1 calc PR A 1 H8C H 0.3542 0.0234 -0.0100 0.253 Uiso 0.511(13) 1 calc PR A 1 C9 C 0.2670(4) 0.1926(15) 0.2411(10) 0.205(11) Uani 0.511(13) 1 d PD A 1 H9A H 0.2194 0.2058 0.2123 0.308 Uiso 0.511(13) 1 calc PR A 1 H9B H 0.2767 0.2301 0.3138 0.308 Uiso 0.511(13) 1 calc PR A 1 H9C H 0.2731 0.1194 0.2553 0.308 Uiso 0.511(13) 1 calc PR A 1 C10 C 0.3306(9) 0.4174(10) 0.2157(12) 0.240(14) Uani 0.511(13) 1 d PD A 1 H10A H 0.2895 0.4536 0.1846 0.361 Uiso 0.511(13) 1 calc PR A 1 H10B H 0.3703 0.4638 0.2183 0.361 Uiso 0.511(13) 1 calc PR A 1 H10C H 0.3228 0.3931 0.2945 0.361 Uiso 0.511(13) 1 calc PR A 1 C1' C 0.3955(8) 0.293(3) -0.0033(14) 0.059(4) Uani 0.489(13) 1 d PD A 2 C2' C 0.3628(14) 0.1939(19) 0.004(2) 0.065(6) Uani 0.489(13) 1 d PD A 2 C3' C 0.3208(7) 0.1955(19) 0.106(3) 0.062(5) Uani 0.489(13) 1 d PD A 2 C4' C 0.3246(9) 0.294(3) 0.1630(14) 0.068(4) Uani 0.489(13) 1 d PD A 2 C5' C 0.3720(11) 0.3515(8) 0.0944(19) 0.046(3) Uani 0.489(13) 1 d PD A 2 C6' C 0.4374(6) 0.3315(14) -0.0973(9) 0.175(9) Uani 0.489(13) 1 d PD A 2 H6'A H 0.4070 0.3606 -0.1594 0.262 Uiso 0.489(13) 1 calc PR A 2 H6'B H 0.4639 0.2751 -0.1286 0.262 Uiso 0.489(13) 1 calc PR A 2 H6'C H 0.4692 0.3841 -0.0664 0.262 Uiso 0.489(13) 1 calc PR A 2 C7' C 0.3681(9) 0.1087(11) -0.0804(14) 0.268(17) Uani 0.489(13) 1 d PD A 2 H7'A H 0.3327 0.1169 -0.1436 0.402 Uiso 0.489(13) 1 calc PR A 2 H7'B H 0.3612 0.0437 -0.0406 0.402 Uiso 0.489(13) 1 calc PR A 2 H7'C H 0.4140 0.1095 -0.1124 0.402 Uiso 0.489(13) 1 calc PR A 2 C8' C 0.2757(6) 0.1096(12) 0.1476(17) 0.248(15) Uani 0.489(13) 1 d PD A 2 H8'A H 0.2292 0.1156 0.1105 0.372 Uiso 0.489(13) 1 calc PR A 2 H8'B H 0.2730 0.1140 0.2323 0.372 Uiso 0.489(13) 1 calc PR A 2 H8'C H 0.2958 0.0439 0.1270 0.372 Uiso 0.489(13) 1 calc PR A 2 C9' C 0.2910(7) 0.3301(15) 0.2670(9) 0.211(11) Uani 0.489(13) 1 d PD A 2 H9'A H 0.2464 0.3613 0.2438 0.316 Uiso 0.489(13) 1 calc PR A 2 H9'B H 0.3206 0.3806 0.3079 0.316 Uiso 0.489(13) 1 calc PR A 2 H9'C H 0.2834 0.2723 0.3189 0.316 Uiso 0.489(13) 1 calc PR A 2 C10' C 0.3902(7) 0.4661(6) 0.1161(13) 0.149(7) Uani 0.489(13) 1 d PD A 2 H10D H 0.3559 0.5090 0.0741 0.224 Uiso 0.489(13) 1 calc PR A 2 H10E H 0.4361 0.4804 0.0881 0.224 Uiso 0.489(13) 1 calc PR A 2 H10F H 0.3900 0.4807 0.1996 0.224 Uiso 0.489(13) 1 calc PR A 2 C11 C 0.6249(3) 0.2418(3) -0.0452(3) 0.1254(15) Uani 1 1 d . A . H11A H 0.6458 0.1926 -0.0970 0.188 Uiso 1 1 calc R . . H11B H 0.6614 0.2822 -0.0051 0.188 Uiso 1 1 calc R . . H11C H 0.5939 0.2870 -0.0910 0.188 Uiso 1 1 calc R . . C12 C 0.58495(15) 0.1861(2) 0.0426(2) 0.0706(7) Uani 1 1 d . . . H12A H 0.6167 0.1394 0.0869 0.085 Uiso 1 1 calc R A . H12B H 0.5492 0.1440 0.0010 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0367(2) 0.0455(2) 0.0418(2) 0.00017(11) 0.00022(13) 0.00006(11) S1 0.0396(3) 0.0533(3) 0.0422(3) 0.0028(2) 0.0072(2) 0.0011(2) S2 0.0567(3) 0.0442(3) 0.0616(3) -0.0019(2) -0.0113(2) -0.0031(2) C1 0.042(7) 0.081(11) 0.079(14) 0.038(9) -0.001(8) 0.000(7) C2 0.053(8) 0.099(17) 0.048(4) 0.003(9) -0.011(5) 0.005(7) C3 0.046(6) 0.054(5) 0.064(8) -0.006(5) -0.013(5) 0.002(4) C4 0.046(4) 0.088(11) 0.054(6) -0.007(6) -0.003(4) 0.014(7) C5 0.042(10) 0.074(9) 0.070(12) -0.021(9) -0.010(7) 0.023(6) C6 0.103(9) 0.218(17) 0.39(3) 0.26(2) -0.118(14) -0.094(11) C7 0.145(12) 0.56(4) 0.045(4) -0.072(11) -0.028(5) 0.169(19) C8 0.148(12) 0.085(5) 0.257(18) -0.015(8) -0.141(12) -0.018(6) C9 0.041(4) 0.43(3) 0.146(10) 0.132(15) 0.027(6) 0.031(10) C10 0.32(2) 0.181(13) 0.205(15) -0.147(12) -0.179(16) 0.204(16) C1' 0.041(5) 0.097(12) 0.040(5) 0.007(6) 0.001(4) 0.011(7) C2' 0.062(13) 0.058(8) 0.071(14) -0.022(7) -0.030(10) 0.012(6) C3' 0.036(7) 0.061(9) 0.087(14) 0.019(7) -0.016(8) -0.013(7) C4' 0.031(6) 0.119(13) 0.055(5) 0.012(8) 0.010(4) 0.016(7) C5' 0.037(7) 0.047(3) 0.054(8) 0.006(4) 0.001(5) 0.005(3) C6' 0.088(6) 0.36(3) 0.078(7) 0.108(10) 0.013(5) 0.020(12) C7' 0.30(2) 0.211(16) 0.27(2) -0.203(16) -0.23(2) 0.194(17) C8' 0.093(9) 0.226(18) 0.41(3) 0.25(2) -0.131(14) -0.116(11) C9' 0.139(11) 0.40(3) 0.095(6) 0.032(12) 0.039(7) 0.194(16) C10' 0.173(12) 0.054(4) 0.208(14) 0.004(6) -0.105(11) -0.004(5) C11 0.145(4) 0.149(3) 0.089(2) -0.004(2) 0.073(3) 0.004(3) C12 0.0703(16) 0.0861(18) 0.0575(14) -0.0106(12) 0.0230(12) 0.0138(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 2.075(15) . ? Fe1 C5 2.095(9) . ? Fe1 C4 2.096(13) . ? Fe1 C3 2.096(11) . ? Fe1 C3' 2.102(9) . ? Fe1 C1 2.106(10) . ? Fe1 C2' 2.120(15) . ? Fe1 C5' 2.134(10) . ? Fe1 S2 2.1351(6) . ? Fe1 C1' 2.153(18) . ? Fe1 C4' 2.183(18) . ? Fe1 S1 2.2916(6) . ? S1 C12 1.841(2) . ? S1 Fe1 2.2959(6) 2_655 ? S2 S2 2.0324(11) 2_655 ? C1 C2 1.384(13) . ? C1 C5 1.387(10) . ? C1 C6 1.499(12) . ? C2 C3 1.400(13) . ? C2 C7 1.508(17) . ? C3 C4 1.386(11) . ? C3 C8 1.491(15) . ? C4 C5 1.386(14) . ? C4 C9 1.498(17) . ? C5 C10 1.510(12) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C1' C5' 1.420(10) . ? C1' C2' 1.425(14) . ? C1' C6' 1.444(19) . ? C2' C3' 1.427(12) . ? C2' C7' 1.458(15) . ? C3' C4' 1.423(14) . ? C3' C8' 1.489(11) . ? C4' C5' 1.422(9) . ? C4' C9' 1.439(19) . ? C5' C10' 1.529(13) . ? C6' H6'A 0.9600 . ? C6' H6'B 0.9600 . ? C6' H6'C 0.9600 . ? C7' H7'A 0.9600 . ? C7' H7'B 0.9600 . ? C7' H7'C 0.9600 . ? C8' H8'A 0.9600 . ? C8' H8'B 0.9600 . ? C8' H8'C 0.9600 . ? C9' H9'A 0.9600 . ? C9' H9'B 0.9600 . ? C9' H9'C 0.9600 . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11 C12 1.465(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C5 64.6(5) . . ? C2 Fe1 C4 65.5(6) . . ? C5 Fe1 C4 38.6(4) . . ? C2 Fe1 C3 39.2(3) . . ? C5 Fe1 C3 64.2(4) . . ? C4 Fe1 C3 38.6(3) . . ? C2 Fe1 C3' 52.8(5) . . ? C5 Fe1 C3' 49.9(4) . . ? C4 Fe1 C3' 18.0(5) . . ? C3 Fe1 C3' 20.7(5) . . ? C2 Fe1 C1 38.6(4) . . ? C5 Fe1 C1 38.6(3) . . ? C4 Fe1 C1 65.2(5) . . ? C3 Fe1 C1 64.9(5) . . ? C3' Fe1 C1 64.7(4) . . ? C2 Fe1 C2' 16.7(4) . . ? C5 Fe1 C2' 66.0(5) . . ? C4 Fe1 C2' 55.1(5) . . ? C3 Fe1 C2' 23.0(5) . . ? C3' Fe1 C2' 39.5(3) . . ? C1 Fe1 C2' 50.5(5) . . ? C2 Fe1 C5' 56.6(5) . . ? C5 Fe1 C5' 21.4(4) . . ? C4 Fe1 C5' 57.2(5) . . ? C3 Fe1 C5' 71.8(5) . . ? C3' Fe1 C5' 63.7(4) . . ? C1 Fe1 C5' 20.9(5) . . ? C2' Fe1 C5' 64.5(5) . . ? C2 Fe1 S2 108.5(9) . . ? C5 Fe1 S2 146.9(9) . . ? C4 Fe1 S2 108.3(8) . . ? C3 Fe1 S2 89.7(4) . . ? C3' Fe1 S2 99.0(6) . . ? C1 Fe1 S2 147.0(10) . . ? C2' Fe1 S2 98.3(6) . . ? C5' Fe1 S2 161.5(3) . . ? C2 Fe1 C1' 23.8(4) . . ? C5 Fe1 C1' 54.0(5) . . ? C4 Fe1 C1' 71.7(6) . . ? C3 Fe1 C1' 58.5(5) . . ? C3' Fe1 C1' 65.3(5) . . ? C1 Fe1 C1' 17.9(5) . . ? C2' Fe1 C1' 38.9(4) . . ? C5' Fe1 C1' 38.7(3) . . ? S2 Fe1 C1' 130.0(8) . . ? C2 Fe1 C4' 70.2(6) . . ? C5 Fe1 C4' 17.3(4) . . ? C4 Fe1 C4' 23.6(4) . . ? C3 Fe1 C4' 57.1(6) . . ? C3' Fe1 C4' 38.7(4) . . ? C1 Fe1 C4' 53.2(5) . . ? C2' Fe1 C4' 66.2(6) . . ? C5' Fe1 C4' 38.4(3) . . ? S2 Fe1 C4' 130.4(10) . . ? C1' Fe1 C4' 66.0(6) . . ? C2 Fe1 S1 105.1(7) . . ? C5 Fe1 S1 119.5(9) . . ? C4 Fe1 S1 157.8(8) . . ? C3 Fe1 S1 142.1(8) . . ? C3' Fe1 S1 157.1(6) . . ? C1 Fe1 S1 94.6(3) . . ? C2' Fe1 S1 119.8(10) . . ? C5' Fe1 S1 100.7(6) . . ? S2 Fe1 S1 93.63(2) . . ? C1' Fe1 S1 91.9(5) . . ? C4' Fe1 S1 135.6(10) . . ? C12 S1 Fe1 108.73(10) . . ? C12 S1 Fe1 108.95(9) . 2_655 ? Fe1 S1 Fe1 92.99(2) . 2_655 ? S2 S2 Fe1 107.654(16) 2_655 . ? C2 C1 C5 107.1(9) . . ? C2 C1 C6 126(3) . . ? C5 C1 C6 127(3) . . ? C2 C1 Fe1 69.5(7) . . ? C5 C1 Fe1 70.3(5) . . ? C6 C1 Fe1 126.3(6) . . ? C1 C2 C3 108.1(13) . . ? C1 C2 C7 126(3) . . ? C3 C2 C7 125(3) . . ? C1 C2 Fe1 71.9(7) . . ? C3 C2 Fe1 71.2(8) . . ? C7 C2 Fe1 126.2(10) . . ? C4 C3 C2 108.2(15) . . ? C4 C3 C8 126(3) . . ? C2 C3 C8 125(3) . . ? C4 C3 Fe1 70.7(8) . . ? C2 C3 Fe1 69.6(8) . . ? C8 C3 Fe1 127.7(8) . . ? C3 C4 C5 107.0(11) . . ? C3 C4 C9 125(3) . . ? C5 C4 C9 128(3) . . ? C3 C4 Fe1 70.7(8) . . ? C5 C4 Fe1 70.7(6) . . ? C9 C4 Fe1 127.2(9) . . ? C4 C5 C1 109.4(7) . . ? C4 C5 C10 124(3) . . ? C1 C5 C10 126(3) . . ? C4 C5 Fe1 70.7(6) . . ? C1 C5 Fe1 71.1(5) . . ? C10 C5 Fe1 126.7(6) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5' C1' C2' 105.8(14) . . ? C5' C1' C6' 127(3) . . ? C2' C1' C6' 127(3) . . ? C5' C1' Fe1 69.9(9) . . ? C2' C1' Fe1 69.3(9) . . ? C6' C1' Fe1 130.2(10) . . ? C1' C2' C3' 107.3(11) . . ? C1' C2' C7' 126(3) . . ? C3' C2' C7' 126(3) . . ? C1' C2' Fe1 71.8(9) . . ? C3' C2' Fe1 69.6(7) . . ? C7' C2' Fe1 126.6(10) . . ? C4' C3' C2' 111.0(8) . . ? C4' C3' C8' 122(3) . . ? C2' C3' C8' 127(4) . . ? C4' C3' Fe1 73.7(8) . . ? C2' C3' Fe1 70.9(7) . . ? C8' C3' Fe1 124.3(7) . . ? C5' C4' C3' 103.5(11) . . ? C5' C4' C9' 127(3) . . ? C3' C4' C9' 130(3) . . ? C5' C4' Fe1 68.9(9) . . ? C3' C4' Fe1 67.5(8) . . ? C9' C4' Fe1 125.8(11) . . ? C1' C5' C4' 112.4(15) . . ? C1' C5' C10' 124(3) . . ? C4' C5' C10' 124(3) . . ? C1' C5' Fe1 71.4(10) . . ? C4' C5' Fe1 72.7(10) . . ? C10' C5' Fe1 128.2(8) . . ? C1' C6' H6'A 109.5 . . ? C1' C6' H6'B 109.5 . . ? H6'A C6' H6'B 109.5 . . ? C1' C6' H6'C 109.5 . . ? H6'A C6' H6'C 109.5 . . ? H6'B C6' H6'C 109.5 . . ? C2' C7' H7'A 109.5 . . ? C2' C7' H7'B 109.5 . . ? H7'A C7' H7'B 109.5 . . ? C2' C7' H7'C 109.5 . . ? H7'A C7' H7'C 109.5 . . ? H7'B C7' H7'C 109.5 . . ? C3' C8' H8'A 109.5 . . ? C3' C8' H8'B 109.5 . . ? H8'A C8' H8'B 109.5 . . ? C3' C8' H8'C 109.5 . . ? H8'A C8' H8'C 109.5 . . ? H8'B C8' H8'C 109.5 . . ? C4' C9' H9'A 109.5 . . ? C4' C9' H9'B 109.5 . . ? H9'A C9' H9'B 109.5 . . ? C4' C9' H9'C 109.5 . . ? H9'A C9' H9'C 109.5 . . ? H9'B C9' H9'C 109.5 . . ? C5' C10' H10D 109.5 . . ? C5' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C5' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C11 C12 S1 114.4(2) . . ? C11 C12 H12A 108.7 . . ? S1 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 . . ? S1 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.231 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.049 # Attachment '2a.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 749168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H45 Fe2 S5' _chemical_formula_weight 641.63 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9506(2) _cell_length_b 15.2338(2) _cell_length_c 16.6540(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.6590(10) _cell_angle_gamma 90.00 _cell_volume 2988.93(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9158 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 32.18 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 1.335 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22845 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6830 _reflns_number_gt 5787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+1.9451P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6830 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.14328(3) 0.743933(19) 0.198785(19) 0.02309(9) Uani 1 1 d . . . Fe2 Fe -0.10905(3) 0.689114(19) 0.202918(18) 0.01833(8) Uani 1 1 d . . . S2 S 0.06119(4) 0.63724(3) 0.26413(3) 0.01743(11) Uani 1 1 d . A . S4 S -0.12012(4) 0.79561(3) 0.28984(3) 0.02009(12) Uani 1 1 d . A . S5 S -0.01455(5) 0.95833(3) 0.36756(3) 0.02246(12) Uani 1 1 d . A . S3 S 0.12416(4) 0.85023(3) 0.28344(3) 0.01912(11) Uani 1 1 d . A . S1 S -0.02707(11) 0.77914(11) 0.11812(7) 0.0241(3) Uani 0.718(3) 1 d P A 1 S1' S -0.0109(3) 0.7480(2) 0.1199(2) 0.0241(3) Uani 0.282(3) 1 d P A 2 C1 C 0.3216(2) 0.76790(18) 0.2185(2) 0.0482(9) Uani 1 1 d . A . C2 C 0.30192(19) 0.67658(15) 0.21805(15) 0.0280(5) Uani 1 1 d . A . C3 C 0.2382(2) 0.65380(14) 0.14031(14) 0.0259(5) Uani 1 1 d . A . C4 C 0.2196(3) 0.73126(19) 0.09313(18) 0.0507(9) Uani 1 1 d . A . C5 C 0.2696(3) 0.80200(17) 0.1424(2) 0.0647(12) Uani 1 1 d . A . C6 C 0.3913(3) 0.8181(3) 0.2873(3) 0.0949(18) Uani 1 1 d . . . H22A H 0.4689 0.8202 0.2791 0.142 Uiso 1 1 calc R A . H22B H 0.3872 0.7892 0.3380 0.142 Uiso 1 1 calc R . . H22C H 0.3622 0.8767 0.2886 0.142 Uiso 1 1 calc R . . C7 C 0.3465(2) 0.6106(2) 0.28270(16) 0.0428(7) Uani 1 1 d . . . H4A H 0.4211 0.5922 0.2758 0.064 Uiso 1 1 calc R A . H4B H 0.2968 0.5607 0.2782 0.064 Uiso 1 1 calc R . . H4C H 0.3500 0.6369 0.3355 0.064 Uiso 1 1 calc R . . C8 C 0.2078(2) 0.56257(16) 0.11299(17) 0.0359(6) Uani 1 1 d . . . H10A H 0.2681 0.5378 0.0889 0.054 Uiso 1 1 calc R A . H10B H 0.1393 0.5634 0.0735 0.054 Uiso 1 1 calc R . . H10C H 0.1963 0.5277 0.1589 0.054 Uiso 1 1 calc R . . C9 C 0.1644(4) 0.7358(3) 0.00580(19) 0.0992(19) Uani 1 1 d . . . H21A H 0.2208 0.7285 -0.0284 0.149 Uiso 1 1 calc R A . H21B H 0.1281 0.7918 -0.0049 0.149 Uiso 1 1 calc R . . H21C H 0.1087 0.6900 -0.0054 0.149 Uiso 1 1 calc R . . C10 C 0.2769(5) 0.8958(2) 0.1142(4) 0.134(3) Uani 1 1 d . . . H20A H 0.3446 0.9033 0.0910 0.201 Uiso 1 1 calc R A . H20B H 0.2789 0.9348 0.1598 0.201 Uiso 1 1 calc R . . H20C H 0.2117 0.9091 0.0739 0.201 Uiso 1 1 calc R . . C11 C -0.2841(2) 0.68554(17) 0.15451(19) 0.0415(7) Uani 1 1 d . A . C12 C -0.2224(2) 0.64453(16) 0.09812(15) 0.0349(6) Uani 1 1 d . A . C13 C -0.16226(18) 0.57273(14) 0.13817(13) 0.0226(4) Uani 1 1 d . A . C14 C -0.19209(19) 0.56680(15) 0.21744(14) 0.0262(5) Uani 1 1 d . A . C15 C -0.2660(2) 0.63658(18) 0.22701(17) 0.0367(6) Uani 1 1 d . A . C16 C -0.3632(3) 0.7629(2) 0.1379(3) 0.0836(16) Uani 1 1 d . . . H24A H -0.4376 0.7427 0.1144 0.125 Uiso 1 1 calc R A . H24B H -0.3355 0.8023 0.1008 0.125 Uiso 1 1 calc R . . H24C H -0.3669 0.7930 0.1881 0.125 Uiso 1 1 calc R . . C17 C -0.2262(3) 0.6675(2) 0.01009(18) 0.0606(10) Uani 1 1 d . . . H25A H -0.2879 0.6369 -0.0225 0.091 Uiso 1 1 calc R A . H25B H -0.1561 0.6507 -0.0065 0.091 Uiso 1 1 calc R . . H25C H -0.2371 0.7297 0.0029 0.091 Uiso 1 1 calc R . . C18 C -0.0903(2) 0.50823(18) 0.10333(18) 0.0410(7) Uani 1 1 d . . . H5A H -0.1371 0.4620 0.0769 0.062 Uiso 1 1 calc R A . H5B H -0.0352 0.4840 0.1462 0.062 Uiso 1 1 calc R . . H5C H -0.0520 0.5371 0.0644 0.062 Uiso 1 1 calc R . . C19 C -0.1612(3) 0.49127(19) 0.27359(19) 0.0480(8) Uani 1 1 d . . . H3A H -0.2189 0.4469 0.2630 0.072 Uiso 1 1 calc R A . H3B H -0.1550 0.5109 0.3289 0.072 Uiso 1 1 calc R . . H3C H -0.0898 0.4673 0.2650 0.072 Uiso 1 1 calc R . . C20 C -0.3229(3) 0.6511(3) 0.2999(2) 0.0694(12) Uani 1 1 d . . . H23A H -0.3929 0.6189 0.2932 0.104 Uiso 1 1 calc R A . H23B H -0.3383 0.7125 0.3050 0.104 Uiso 1 1 calc R . . H23C H -0.2739 0.6312 0.3481 0.104 Uiso 1 1 calc R . . C21 C -0.0640(4) 0.8971(2) 0.1223(2) 0.0339(8) Uani 0.718(3) 1 d P A 1 H2A H -0.1066 0.9071 0.1662 0.041 Uiso 0.718(3) 1 calc PR A 1 H2B H 0.0048 0.9320 0.1330 0.041 Uiso 0.718(3) 1 calc PR A 1 C21' C -0.0579(10) 0.8620(6) 0.1017(7) 0.0339(8) Uani 0.282(3) 1 d P A 2 H2'A H -0.1392 0.8614 0.1012 0.041 Uiso 0.282(3) 1 calc PR A 2 H2'B H -0.0249 0.8942 0.1502 0.041 Uiso 0.282(3) 1 calc PR A 2 C22 C -0.1341(6) 0.9245(4) 0.0423(3) 0.0781(17) Uani 0.718(3) 1 d P A 1 H27A H -0.1531 0.9855 0.0445 0.117 Uiso 0.718(3) 1 calc PR A 1 H27B H -0.2024 0.8902 0.0323 0.117 Uiso 0.718(3) 1 calc PR A 1 H27C H -0.0913 0.9150 -0.0009 0.117 Uiso 0.718(3) 1 calc PR A 1 C22' C -0.0420(15) 0.9132(10) 0.0382(8) 0.0781(17) Uani 0.282(3) 1 d P A 2 H27D H -0.0750 0.9699 0.0434 0.117 Uiso 0.282(3) 1 calc PR A 2 H27E H -0.0775 0.8863 -0.0118 0.117 Uiso 0.282(3) 1 calc PR A 2 H27F H 0.0378 0.9196 0.0378 0.117 Uiso 0.282(3) 1 calc PR A 2 C23 C 0.09231(19) 0.65672(14) 0.37428(13) 0.0225(4) Uani 1 1 d . . . H17A H 0.1717 0.6437 0.3937 0.027 Uiso 1 1 calc R A . H17B H 0.0804 0.7184 0.3846 0.027 Uiso 1 1 calc R . . C24 C 0.0205(3) 0.60248(18) 0.42208(15) 0.0395(6) Uani 1 1 d . A . H13A H 0.0410 0.6156 0.4790 0.059 Uiso 1 1 calc R . . H13B H 0.0330 0.5413 0.4133 0.059 Uiso 1 1 calc R . . H13C H -0.0582 0.6161 0.4043 0.059 Uiso 1 1 calc R . . C25 C -0.00422(18) 0.86077(13) 0.31191(12) 0.0183(4) Uani 1 1 d . . . C26 C -0.10669(18) 0.92743(14) 0.43908(13) 0.0221(4) Uani 1 1 d . . . H18A H -0.1251 0.9794 0.4679 0.027 Uiso 1 1 calc R A . H18B H -0.1770 0.9040 0.4091 0.027 Uiso 1 1 calc R . . C27 C -0.0534(2) 0.85979(15) 0.50028(14) 0.0284(5) Uani 1 1 d . A . H16A H -0.1053 0.8456 0.5365 0.043 Uiso 1 1 calc R . . H16B H 0.0153 0.8831 0.5310 0.043 Uiso 1 1 calc R . . H16C H -0.0363 0.8078 0.4721 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0354(2) 0.01486(14) 0.02253(17) -0.00176(11) 0.01518(14) -0.00004(12) Fe2 0.01739(16) 0.01758(15) 0.01881(16) -0.00537(11) -0.00041(11) 0.00044(11) S2 0.0173(2) 0.0163(2) 0.0186(2) -0.00104(18) 0.00267(19) -0.00085(18) S4 0.0173(2) 0.0191(2) 0.0240(3) -0.0070(2) 0.0036(2) -0.00116(19) S5 0.0259(3) 0.0170(2) 0.0263(3) -0.0073(2) 0.0096(2) -0.0025(2) S3 0.0192(3) 0.0175(2) 0.0215(3) -0.00556(19) 0.0059(2) -0.00222(19) S1 0.0301(5) 0.0256(7) 0.0167(3) -0.0026(5) 0.0040(3) -0.0066(5) S1' 0.0301(5) 0.0256(7) 0.0167(3) -0.0026(5) 0.0040(3) -0.0066(5) C1 0.0398(15) 0.0353(14) 0.081(2) -0.0289(15) 0.0446(16) -0.0175(12) C2 0.0224(11) 0.0308(11) 0.0344(13) -0.0093(10) 0.0149(10) -0.0060(9) C3 0.0330(12) 0.0224(10) 0.0248(11) -0.0008(9) 0.0122(10) 0.0078(9) C4 0.083(2) 0.0416(15) 0.0380(15) 0.0153(12) 0.0413(16) 0.0359(16) C5 0.098(3) 0.0203(12) 0.099(3) 0.0091(15) 0.085(3) 0.0099(14) C6 0.0383(19) 0.087(3) 0.172(5) -0.095(3) 0.054(2) -0.0368(19) C7 0.0226(12) 0.071(2) 0.0343(14) 0.0034(14) 0.0042(10) 0.0076(13) C8 0.0285(13) 0.0341(13) 0.0445(15) -0.0172(11) 0.0049(11) 0.0061(11) C9 0.158(4) 0.120(3) 0.0320(17) 0.037(2) 0.051(2) 0.110(3) C10 0.210(6) 0.0282(16) 0.218(6) 0.033(3) 0.189(5) 0.025(2) C11 0.0256(13) 0.0297(12) 0.0602(19) -0.0234(13) -0.0187(12) 0.0047(10) C12 0.0406(14) 0.0289(12) 0.0285(13) -0.0056(10) -0.0138(11) -0.0099(11) C13 0.0193(10) 0.0212(10) 0.0265(11) -0.0098(9) 0.0013(9) -0.0048(8) C14 0.0213(11) 0.0279(11) 0.0287(12) -0.0057(9) 0.0021(9) -0.0117(9) C15 0.0183(11) 0.0455(14) 0.0470(16) -0.0267(13) 0.0077(11) -0.0104(10) C16 0.055(2) 0.0459(18) 0.128(4) -0.042(2) -0.050(2) 0.0259(16) C17 0.088(3) 0.0523(18) 0.0303(15) 0.0017(14) -0.0215(16) -0.0269(18) C18 0.0274(13) 0.0388(14) 0.0580(18) -0.0298(13) 0.0105(12) -0.0083(11) C19 0.0537(18) 0.0396(15) 0.0464(17) 0.0070(13) -0.0043(14) -0.0267(14) C20 0.0402(17) 0.095(3) 0.082(3) -0.057(2) 0.0365(17) -0.0356(18) C21 0.051(2) 0.020(2) 0.028(2) 0.0032(15) -0.0019(16) 0.0048(18) C21' 0.051(2) 0.020(2) 0.028(2) 0.0032(15) -0.0019(16) 0.0048(18) C22 0.099(4) 0.081(3) 0.044(3) 0.010(2) -0.016(3) 0.035(3) C22' 0.099(4) 0.081(3) 0.044(3) 0.010(2) -0.016(3) 0.035(3) C23 0.0232(11) 0.0257(10) 0.0175(10) 0.0006(8) 0.0008(8) -0.0015(9) C24 0.0570(17) 0.0388(14) 0.0234(12) 0.0004(10) 0.0094(12) -0.0165(13) C25 0.0207(10) 0.0164(9) 0.0180(10) -0.0036(8) 0.0036(8) 0.0012(8) C26 0.0200(10) 0.0235(10) 0.0244(11) -0.0067(9) 0.0078(9) 0.0004(8) C27 0.0323(13) 0.0262(11) 0.0278(12) -0.0040(9) 0.0080(10) 0.0008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 S1' 2.077(4) . ? Fe1 C5 2.102(3) . ? Fe1 C3 2.119(2) . ? Fe1 C4 2.122(2) . ? Fe1 C2 2.132(2) . ? Fe1 C1 2.133(3) . ? Fe1 S3 2.1840(6) . ? Fe1 S2 2.2687(6) . ? Fe1 S1 2.3063(14) . ? Fe2 C11 2.113(2) . ? Fe2 C13 2.117(2) . ? Fe2 C12 2.133(2) . ? Fe2 C15 2.139(2) . ? Fe2 C14 2.144(2) . ? Fe2 S1' 2.153(4) . ? Fe2 S4 2.1930(6) . ? Fe2 S2 2.2598(6) . ? Fe2 S1 2.3020(13) . ? S2 C23 1.834(2) . ? S4 C25 1.694(2) . ? S5 C25 1.7668(19) . ? S5 C26 1.815(2) . ? S3 C25 1.688(2) . ? S1 C21 1.855(4) . ? S1' C21' 1.835(10) . ? C1 C2 1.411(3) . ? C1 C5 1.413(5) . ? C1 C6 1.507(5) . ? C2 C3 1.430(3) . ? C2 C7 1.503(4) . ? C3 C4 1.415(3) . ? C3 C8 1.488(3) . ? C4 C5 1.424(5) . ? C4 C9 1.494(5) . ? C5 C10 1.512(4) . ? C6 H22A 0.9600 . ? C6 H22B 0.9600 . ? C6 H22C 0.9600 . ? C7 H4A 0.9600 . ? C7 H4B 0.9600 . ? C7 H4C 0.9600 . ? C8 H10A 0.9600 . ? C8 H10B 0.9600 . ? C8 H10C 0.9600 . ? C9 H21A 0.9600 . ? C9 H21B 0.9600 . ? C9 H21C 0.9600 . ? C10 H20A 0.9600 . ? C10 H20B 0.9600 . ? C10 H20C 0.9600 . ? C11 C15 1.405(4) . ? C11 C12 1.431(4) . ? C11 C16 1.508(4) . ? C12 C13 1.413(3) . ? C12 C17 1.500(4) . ? C13 C14 1.427(3) . ? C13 C18 1.487(3) . ? C14 C15 1.408(3) . ? C14 C19 1.490(4) . ? C15 C20 1.504(4) . ? C16 H24A 0.9600 . ? C16 H24B 0.9600 . ? C16 H24C 0.9600 . ? C17 H25A 0.9600 . ? C17 H25B 0.9600 . ? C17 H25C 0.9600 . ? C18 H5A 0.9600 . ? C18 H5B 0.9600 . ? C18 H5C 0.9600 . ? C19 H3A 0.9600 . ? C19 H3B 0.9600 . ? C19 H3C 0.9600 . ? C20 H23A 0.9600 . ? C20 H23B 0.9600 . ? C20 H23C 0.9600 . ? C21 C22 1.509(6) . ? C21 H2A 0.9700 . ? C21 H2B 0.9700 . ? C21' C22' 1.353(18) . ? C21' H2'A 0.9700 . ? C21' H2'B 0.9700 . ? C22 H27A 0.9600 . ? C22 H27B 0.9600 . ? C22 H27C 0.9600 . ? C22' H27D 0.9600 . ? C22' H27E 0.9600 . ? C22' H27F 0.9600 . ? C23 C24 1.511(3) . ? C23 H17A 0.9700 . ? C23 H17B 0.9700 . ? C24 H13A 0.9600 . ? C24 H13B 0.9600 . ? C24 H13C 0.9600 . ? C26 C27 1.513(3) . ? C26 H18A 0.9700 . ? C26 H18B 0.9700 . ? C27 H16A 0.9600 . ? C27 H16B 0.9600 . ? C27 H16C 0.9600 . ? 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' Fe1 C5 109.42(16) . . ? S1' Fe1 C3 102.43(12) . . ? C5 Fe1 C3 65.65(9) . . ? S1' Fe1 C4 86.41(14) . . ? C5 Fe1 C4 39.40(14) . . ? C3 Fe1 C4 38.97(9) . . ? S1' Fe1 C2 141.43(12) . . ? C5 Fe1 C2 65.34(12) . . ? C3 Fe1 C2 39.32(9) . . ? C4 Fe1 C2 65.55(11) . . ? S1' Fe1 C1 148.21(14) . . ? C5 Fe1 C1 38.98(15) . . ? C3 Fe1 C1 65.39(10) . . ? C4 Fe1 C1 65.53(14) . . ? C2 Fe1 C1 38.63(10) . . ? S1' Fe1 S3 102.02(10) . . ? C5 Fe1 S3 97.87(9) . . ? C3 Fe1 S3 154.04(7) . . ? C4 Fe1 S3 135.13(9) . . ? C2 Fe1 S3 116.51(7) . . ? C1 Fe1 S3 89.08(7) . . ? S1' Fe1 S2 85.15(10) . . ? C5 Fe1 S2 156.43(9) . . ? C3 Fe1 S2 93.67(6) . . ? C4 Fe1 S2 127.82(9) . . ? C2 Fe1 S2 91.62(6) . . ? C1 Fe1 S2 123.39(10) . . ? S3 Fe1 S2 96.95(2) . . ? S1' Fe1 S1 11.97(8) . . ? C5 Fe1 S1 105.77(13) . . ? C3 Fe1 S1 111.78(8) . . ? C4 Fe1 S1 89.89(10) . . ? C2 Fe1 S1 151.07(7) . . ? C1 Fe1 S1 144.23(11) . . ? S3 Fe1 S1 91.48(4) . . ? S2 Fe1 S1 92.04(4) . . ? C11 Fe2 C13 65.82(9) . . ? C11 Fe2 C12 39.41(11) . . ? C13 Fe2 C12 38.84(9) . . ? C11 Fe2 C15 38.58(12) . . ? C13 Fe2 C15 65.42(9) . . ? C12 Fe2 C15 65.02(11) . . ? C11 Fe2 C14 64.73(10) . . ? C13 Fe2 C14 39.13(8) . . ? C12 Fe2 C14 64.73(9) . . ? C15 Fe2 C14 38.40(9) . . ? C11 Fe2 S1' 112.14(14) . . ? C13 Fe2 S1' 99.87(11) . . ? C12 Fe2 S1' 86.95(12) . . ? C15 Fe2 S1' 149.98(13) . . ? C14 Fe2 S1' 138.33(11) . . ? C11 Fe2 S4 96.05(7) . . ? C13 Fe2 S4 155.46(6) . . ? C12 Fe2 S4 132.49(8) . . ? C15 Fe2 S4 90.06(7) . . ? C14 Fe2 S4 119.22(6) . . ? S1' Fe2 S4 102.43(10) . . ? C11 Fe2 S2 157.22(8) . . ? C13 Fe2 S2 96.18(6) . . ? C12 Fe2 S2 131.13(8) . . ? C15 Fe2 S2 122.43(8) . . ? C14 Fe2 S2 92.51(7) . . ? S1' Fe2 S2 83.64(11) . . ? S4 Fe2 S2 96.34(2) . . ? C11 Fe2 S1 106.10(10) . . ? C13 Fe2 S1 107.99(7) . . ? C12 Fe2 S1 87.98(8) . . ? C15 Fe2 S1 144.59(9) . . ? C14 Fe2 S1 147.11(7) . . ? S1' Fe2 S1 12.60(8) . . ? S4 Fe2 S1 92.48(4) . . ? S2 Fe2 S1 92.38(4) . . ? C23 S2 Fe2 114.26(7) . . ? C23 S2 Fe1 109.42(7) . . ? Fe2 S2 Fe1 87.83(2) . . ? C25 S4 Fe2 116.05(7) . . ? C25 S5 C26 103.28(10) . . ? C25 S3 Fe1 116.76(7) . . ? C21 S1 Fe2 115.19(14) . . ? C21 S1 Fe1 113.30(14) . . ? Fe2 S1 Fe1 85.93(5) . . ? C21' S1' Fe1 110.3(4) . . ? C21' S1' Fe2 108.4(4) . . ? Fe1 S1' Fe2 95.90(15) . . ? C2 C1 C5 108.1(3) . . ? C2 C1 C6 125.0(4) . . ? C5 C1 C6 126.8(3) . . ? C2 C1 Fe1 70.66(14) . . ? C5 C1 Fe1 69.32(19) . . ? C6 C1 Fe1 127.89(19) . . ? C1 C2 C3 107.9(3) . . ? C1 C2 C7 128.1(3) . . ? C3 C2 C7 123.9(2) . . ? C1 C2 Fe1 70.70(16) . . ? C3 C2 Fe1 69.85(13) . . ? C7 C2 Fe1 128.94(16) . . ? C4 C3 C2 108.1(2) . . ? C4 C3 C8 127.0(2) . . ? C2 C3 C8 124.7(2) . . ? C4 C3 Fe1 70.63(13) . . ? C2 C3 Fe1 70.83(13) . . ? C8 C3 Fe1 128.57(17) . . ? C3 C4 C5 107.4(3) . . ? C3 C4 C9 125.6(3) . . ? C5 C4 C9 126.9(3) . . ? C3 C4 Fe1 70.40(13) . . ? C5 C4 Fe1 69.53(15) . . ? C9 C4 Fe1 128.5(3) . . ? C1 C5 C4 108.5(2) . . ? C1 C5 C10 125.9(4) . . ? C4 C5 C10 125.2(4) . . ? C1 C5 Fe1 71.69(15) . . ? C4 C5 Fe1 71.07(16) . . ? C10 C5 Fe1 128.3(2) . . ? C1 C6 H22A 109.5 . . ? C1 C6 H22B 109.5 . . ? H22A C6 H22B 109.5 . . ? C1 C6 H22C 109.5 . . ? H22A C6 H22C 109.5 . . ? H22B C6 H22C 109.5 . . ? C2 C7 H4A 109.5 . . ? C2 C7 H4B 109.5 . . ? H4A C7 H4B 109.5 . . ? C2 C7 H4C 109.5 . . ? H4A C7 H4C 109.5 . . ? H4B C7 H4C 109.5 . . ? C3 C8 H10A 109.5 . . ? C3 C8 H10B 109.5 . . ? H10A C8 H10B 109.5 . . ? C3 C8 H10C 109.5 . . ? H10A C8 H10C 109.5 . . ? H10B C8 H10C 109.5 . . ? C4 C9 H21A 109.5 . . ? C4 C9 H21B 109.5 . . ? H21A C9 H21B 109.5 . . ? C4 C9 H21C 109.5 . . ? H21A C9 H21C 109.5 . . ? H21B C9 H21C 109.5 . . ? C5 C10 H20A 109.5 . . ? C5 C10 H20B 109.5 . . ? H20A C10 H20B 109.5 . . ? C5 C10 H20C 109.5 . . ? H20A C10 H20C 109.5 . . ? H20B C10 H20C 109.5 . . ? C15 C11 C12 108.1(2) . . ? C15 C11 C16 125.0(3) . . ? C12 C11 C16 126.7(3) . . ? C15 C11 Fe2 71.72(14) . . ? C12 C11 Fe2 71.06(14) . . ? C16 C11 Fe2 126.9(2) . . ? C13 C12 C11 107.8(2) . . ? C13 C12 C17 124.9(3) . . ? C11 C12 C17 127.2(3) . . ? C13 C12 Fe2 69.97(12) . . ? C11 C12 Fe2 69.54(14) . . ? C17 C12 Fe2 129.5(2) . . ? C12 C13 C14 107.4(2) . . ? C12 C13 C18 127.5(2) . . ? C14 C13 C18 124.8(2) . . ? C12 C13 Fe2 71.19(12) . . ? C14 C13 Fe2 71.46(12) . . ? C18 C13 Fe2 127.48(16) . . ? C15 C14 C13 108.4(2) . . ? C15 C14 C19 127.3(2) . . ? C13 C14 C19 123.8(2) . . ? C15 C14 Fe2 70.61(14) . . ? C13 C14 Fe2 69.41(12) . . ? C19 C14 Fe2 132.19(17) . . ? C11 C15 C14 108.2(2) . . ? C11 C15 C20 126.2(3) . . ? C14 C15 C20 125.4(3) . . ? C11 C15 Fe2 69.70(15) . . ? C14 C15 Fe2 70.99(13) . . ? C20 C15 Fe2 128.75(18) . . ? C11 C16 H24A 109.5 . . ? C11 C16 H24B 109.5 . . ? H24A C16 H24B 109.5 . . ? C11 C16 H24C 109.5 . . ? H24A C16 H24C 109.5 . . ? H24B C16 H24C 109.5 . . ? C12 C17 H25A 109.5 . . ? C12 C17 H25B 109.5 . . ? H25A C17 H25B 109.5 . . ? C12 C17 H25C 109.5 . . ? H25A C17 H25C 109.5 . . ? H25B C17 H25C 109.5 . . ? C13 C18 H5A 109.5 . . ? C13 C18 H5B 109.5 . . ? H5A C18 H5B 109.5 . . ? C13 C18 H5C 109.5 . . ? H5A C18 H5C 109.5 . . ? H5B C18 H5C 109.5 . . ? C14 C19 H3A 109.5 . . ? C14 C19 H3B 109.5 . . ? H3A C19 H3B 109.5 . . ? C14 C19 H3C 109.5 . . ? H3A C19 H3C 109.5 . . ? H3B C19 H3C 109.5 . . ? C15 C20 H23A 109.5 . . ? C15 C20 H23B 109.5 . . ? H23A C20 H23B 109.5 . . ? C15 C20 H23C 109.5 . . ? H23A C20 H23C 109.5 . . ? H23B C20 H23C 109.5 . . ? C22 C21 S1 109.5(3) . . ? C22 C21 H2A 109.8 . . ? S1 C21 H2A 109.8 . . ? C22 C21 H2B 109.8 . . ? S1 C21 H2B 109.8 . . ? H2A C21 H2B 108.2 . . ? C22' C21' S1' 126.5(10) . . ? C22' C21' H2'A 105.7 . . ? S1' C21' H2'A 105.7 . . ? C22' C21' H2'B 105.7 . . ? S1' C21' H2'B 105.7 . . ? H2'A C21' H2'B 106.1 . . ? C21 C22 H27A 109.5 . . ? C21 C22 H27B 109.5 . . ? H27A C22 H27B 109.5 . . ? C21 C22 H27C 109.5 . . ? H27A C22 H27C 109.5 . . ? H27B C22 H27C 109.5 . . ? C21' C22' H27D 109.5 . . ? C21' C22' H27E 109.5 . . ? H27D C22' H27E 109.5 . . ? C21' C22' H27F 109.5 . . ? H27D C22' H27F 109.5 . . ? H27E C22' H27F 109.5 . . ? C24 C23 S2 113.63(16) . . ? C24 C23 H17A 108.8 . . ? S2 C23 H17A 108.8 . . ? C24 C23 H17B 108.8 . . ? S2 C23 H17B 108.8 . . ? H17A C23 H17B 107.7 . . ? C23 C24 H13A 109.5 . . ? C23 C24 H13B 109.5 . . ? H13A C24 H13B 109.5 . . ? C23 C24 H13C 109.5 . . ? H13A C24 H13C 109.5 . . ? H13B C24 H13C 109.5 . . ? S3 C25 S4 129.22(12) . . ? S3 C25 S5 111.97(11) . . ? S4 C25 S5 118.70(12) . . ? C27 C26 S5 112.67(15) . . ? C27 C26 H18A 109.1 . . ? S5 C26 H18A 109.1 . . ? C27 C26 H18B 109.1 . . ? S5 C26 H18B 109.1 . . ? H18A C26 H18B 107.8 . . ? C26 C27 H16A 109.5 . . ? C26 C27 H16B 109.5 . . ? H16A C27 H16B 109.5 . . ? C26 C27 H16C 109.5 . . ? H16A C27 H16C 109.5 . . ? H16B C27 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.518 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.072 # Attachment '2b.cif' data_2b _database_code_depnum_ccdc_archive 'CCDC 749169' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H39 Fe2 S5' _chemical_formula_weight 599.55 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.2519(6) _cell_length_b 16.6115(6) _cell_length_c 22.6704(9) _cell_angle_alpha 70.051(2) _cell_angle_beta 89.969(2) _cell_angle_gamma 83.232(2) _cell_volume 5707.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5904 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.20 _exptl_crystal_description block _exptl_crystal_colour blue-purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46198 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18553 _reflns_number_gt 7737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00006(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 18553 _refine_ls_number_parameters 1118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.91285(5) 0.72994(6) 0.10293(4) 0.0404(2) Uani 1 1 d . . . Fe2 Fe 1.94713(5) 0.79022(5) 0.22659(4) 0.0382(2) Uani 1 1 d . . . Fe3 Fe 2.58730(5) 0.27009(5) 0.46793(4) 0.0405(2) Uani 1 1 d . . . Fe4 Fe 2.55287(5) 0.20982(5) 0.62172(4) 0.0383(2) Uani 1 1 d . . . Fe5 Fe 2.05287(5) 0.20997(5) 0.27337(4) 0.0385(2) Uani 1 1 d . . . Fe6 Fe 2.08723(5) 0.27024(6) 0.39697(4) 0.0407(2) Uani 1 1 d . . . Fe7 Fe 2.58719(5) 0.27007(5) -0.03213(4) 0.0408(2) Uani 1 1 d . . . Fe8 Fe 2.55289(5) 0.20989(5) 0.12166(4) 0.0385(2) Uani 1 1 d . . . S1 S 2.01990(9) 0.71790(10) 0.17109(8) 0.0440(4) Uani 1 1 d . . . S2 S 1.87114(10) 0.84168(10) 0.13535(8) 0.0490(5) Uani 1 1 d . . . S3 S 1.84025(10) 0.63590(11) 0.16501(9) 0.0560(5) Uani 1 1 d . . . S4 S 1.87168(11) 0.69197(11) 0.27733(8) 0.0544(5) Uani 1 1 d . . . S5 S 1.76155(12) 0.56033(13) 0.28032(10) 0.0770(7) Uani 1 1 d . . . S6 S 2.48008(9) 0.28238(10) 0.52988(7) 0.0444(4) Uani 1 1 d . . . S7 S 2.62883(10) 0.15813(10) 0.55618(8) 0.0499(5) Uani 1 1 d . . . S8 S 2.65986(10) 0.36421(11) 0.48294(8) 0.0557(5) Uani 1 1 d . . . S9 S 2.62822(10) 0.30806(11) 0.62321(8) 0.0541(5) Uani 1 1 d . . . S10 S 2.73867(12) 0.43987(13) 0.56053(10) 0.0776(7) Uani 1 1 d . . . S11 S 1.97999(9) 0.28237(10) 0.32888(8) 0.0438(4) Uani 1 1 d . . . S12 S 2.12847(10) 0.15813(10) 0.36486(8) 0.0502(5) Uani 1 1 d . . . S13 S 2.15984(10) 0.36419(11) 0.33498(8) 0.0556(5) Uani 1 1 d . . . S14 S 2.12840(10) 0.30800(11) 0.22279(8) 0.0539(5) Uani 1 1 d . . . S15 S 2.23866(12) 0.43992(13) 0.21973(10) 0.0775(7) Uani 1 1 d . . . S16 S 2.48017(9) 0.28227(10) 0.03002(7) 0.0439(4) Uani 1 1 d . . . S17 S 2.62857(10) 0.15829(10) 0.05604(8) 0.0495(5) Uani 1 1 d . . . S18 S 2.65985(10) 0.36407(11) -0.01712(8) 0.0556(5) Uani 1 1 d . . . S19 S 2.62828(10) 0.30815(11) 0.12316(8) 0.0538(5) Uani 1 1 d . . . S20 S 2.73853(12) 0.43985(13) 0.06016(10) 0.0769(6) Uani 1 1 d . . . C1 C 1.8792(5) 0.8073(5) 0.0086(3) 0.073(2) Uani 1 1 d . . . C2 C 1.8564(4) 0.7248(6) 0.0200(3) 0.070(2) Uani 1 1 d . . . C3 C 1.9272(4) 0.6626(4) 0.0373(3) 0.060(2) Uani 1 1 d . . . C4 C 1.9955(4) 0.7061(4) 0.0362(3) 0.0533(19) Uani 1 1 d . . . C5 C 1.9681(4) 0.7950(5) 0.0198(3) 0.058(2) Uani 1 1 d . . . C6 C 1.8195(5) 0.8889(5) -0.0154(4) 0.145(4) Uani 1 1 d . . . H6A H 1.8177 0.9103 -0.0605 0.217 Uiso 1 1 calc R . . H6B H 1.8375 0.9314 0.0000 0.217 Uiso 1 1 calc R . . H6C H 1.7652 0.8771 -0.0009 0.217 Uiso 1 1 calc R . . C7 C 1.7716(4) 0.6991(6) 0.0110(4) 0.128(4) Uani 1 1 d . . . H7A H 1.7635 0.7028 -0.0319 0.192 Uiso 1 1 calc R . . H7B H 1.7292 0.7372 0.0209 0.192 Uiso 1 1 calc R . . H7C H 1.7687 0.6409 0.0382 0.192 Uiso 1 1 calc R . . C8 C 1.9356(5) 0.5667(4) 0.0513(4) 0.105(3) Uani 1 1 d . . . H8A H 1.9415 0.5548 0.0129 0.157 Uiso 1 1 calc R . . H8B H 1.8871 0.5443 0.0715 0.157 Uiso 1 1 calc R . . H8C H 1.9836 0.5396 0.0786 0.157 Uiso 1 1 calc R . . C9 C 2.0873(4) 0.6718(5) 0.0456(4) 0.098(3) Uani 1 1 d . . . H9A H 2.1082 0.6683 0.0068 0.147 Uiso 1 1 calc R . . H9B H 2.0947 0.6154 0.0772 0.147 Uiso 1 1 calc R . . H9C H 2.1169 0.7100 0.0586 0.147 Uiso 1 1 calc R . . C10 C 2.0185(5) 0.8684(5) 0.0093(3) 0.116(4) Uani 1 1 d . . . H10A H 2.0371 0.8859 -0.0329 0.175 Uiso 1 1 calc R . . H10B H 2.0656 0.8501 0.0383 0.175 Uiso 1 1 calc R . . H10C H 1.9850 0.9161 0.0157 0.175 Uiso 1 1 calc R . . C11 C 1.9243(4) 0.8629(6) 0.2859(5) 0.078(3) Uani 1 1 d . . . C12 C 1.9889(5) 0.7983(5) 0.3122(3) 0.078(3) Uani 1 1 d . . . C13 C 2.0526(4) 0.8081(4) 0.2718(3) 0.063(2) Uani 1 1 d . . . C14 C 2.0302(4) 0.8812(5) 0.2180(3) 0.0559(19) Uani 1 1 d . . . C15 C 1.9513(5) 0.9159(4) 0.2274(4) 0.072(2) Uani 1 1 d . . . C16 C 1.8446(5) 0.8737(7) 0.3196(5) 0.190(6) Uani 1 1 d . . . H16A H 1.8510 0.9107 0.3434 0.285 Uiso 1 1 calc R . . H16B H 1.8333 0.8183 0.3474 0.285 Uiso 1 1 calc R . . H16C H 1.7994 0.8988 0.2892 0.285 Uiso 1 1 calc R . . C17 C 1.9973(6) 0.7272(6) 0.3770(3) 0.152(4) Uani 1 1 d . . . H17A H 2.0191 0.7489 0.4072 0.228 Uiso 1 1 calc R . . H17B H 2.0342 0.6786 0.3753 0.228 Uiso 1 1 calc R . . H17C H 1.9438 0.7097 0.3893 0.228 Uiso 1 1 calc R . . C18 C 2.1389(4) 0.7596(6) 0.2787(5) 0.143(4) Uani 1 1 d . . . H18A H 2.1750 0.7827 0.3005 0.215 Uiso 1 1 calc R . . H18B H 2.1593 0.7656 0.2379 0.215 Uiso 1 1 calc R . . H18C H 2.1370 0.6996 0.3021 0.215 Uiso 1 1 calc R . . C19 C 2.0785(6) 0.9229(6) 0.1608(4) 0.154(5) Uani 1 1 d . . . H19A H 2.1115 0.9623 0.1693 0.232 Uiso 1 1 calc R . . H19B H 2.0406 0.9538 0.1258 0.232 Uiso 1 1 calc R . . H19C H 2.1140 0.8791 0.1511 0.232 Uiso 1 1 calc R . . C20 C 1.8980(5) 0.9972(5) 0.1881(4) 0.126(3) Uani 1 1 d . . . H20A H 1.9120 1.0450 0.1991 0.189 Uiso 1 1 calc R . . H20B H 1.8406 0.9907 0.1957 0.189 Uiso 1 1 calc R . . H20C H 1.9074 1.0078 0.1444 0.189 Uiso 1 1 calc R . . C21 C 2.0478(4) 0.6054(4) 0.2195(3) 0.075(2) Uani 1 1 d . . . H21A H 2.0930 0.6007 0.2481 0.112 Uiso 1 1 calc R . . H21B H 2.0642 0.5722 0.1931 0.112 Uiso 1 1 calc R . . H21C H 2.0009 0.5838 0.2427 0.112 Uiso 1 1 calc R . . C22 C 1.7596(3) 0.8465(5) 0.1494(3) 0.087(3) Uani 1 1 d . . . H22A H 1.7287 0.8686 0.1099 0.130 Uiso 1 1 calc R . . H22B H 1.7454 0.8838 0.1732 0.130 Uiso 1 1 calc R . . H22C H 1.7465 0.7896 0.1725 0.130 Uiso 1 1 calc R . . C23 C 1.8293(4) 0.6341(4) 0.2401(3) 0.0534(19) Uani 1 1 d . . . C24 C 1.7753(4) 0.5505(4) 0.3607(3) 0.088(3) Uani 1 1 d . . . H24A H 1.7400 0.5108 0.3859 0.132 Uiso 1 1 calc R . . H24B H 1.7612 0.6059 0.3650 0.132 Uiso 1 1 calc R . . H24C H 1.8321 0.5294 0.3745 0.132 Uiso 1 1 calc R . . C25 C 2.6240(5) 0.1983(5) 0.4097(3) 0.067(2) Uani 1 1 d . . . C26 C 2.6425(4) 0.2820(5) 0.3800(3) 0.0565(19) Uani 1 1 d . . . C27 C 2.5668(4) 0.3371(5) 0.3692(3) 0.062(2) Uani 1 1 d . . . C28 C 2.5026(4) 0.2884(5) 0.3918(3) 0.059(2) Uani 1 1 d . . . C29 C 2.5359(5) 0.2009(5) 0.4187(3) 0.065(2) Uani 1 1 d . . . C30 C 2.6790(5) 0.1131(5) 0.4285(3) 0.123(4) Uani 1 1 d . . . H30A H 2.6848 0.0941 0.3930 0.185 Uiso 1 1 calc R . . H30B H 2.6546 0.0710 0.4618 0.185 Uiso 1 1 calc R . . H30C H 2.7326 0.1199 0.4425 0.185 Uiso 1 1 calc R . . C31 C 2.7283(4) 0.3034(6) 0.3595(3) 0.113(3) Uani 1 1 d . . . H31A H 2.7349 0.3039 0.3173 0.170 Uiso 1 1 calc R . . H31B H 2.7692 0.2607 0.3871 0.170 Uiso 1 1 calc R . . H31C H 2.7352 0.3592 0.3612 0.170 Uiso 1 1 calc R . . C32 C 2.5638(5) 0.4330(5) 0.3343(3) 0.107(3) Uani 1 1 d . . . H32A H 2.5536 0.4449 0.2903 0.161 Uiso 1 1 calc R . . H32B H 2.6158 0.4514 0.3408 0.161 Uiso 1 1 calc R . . H32C H 2.5200 0.4635 0.3498 0.161 Uiso 1 1 calc R . . C33 C 2.4125(4) 0.3276(5) 0.3815(3) 0.103(3) Uani 1 1 d . . . H33A H 2.3908 0.3254 0.3427 0.154 Uiso 1 1 calc R . . H33B H 2.4082 0.3865 0.3796 0.154 Uiso 1 1 calc R . . H33C H 2.3812 0.2956 0.4156 0.154 Uiso 1 1 calc R . . C34 C 2.4824(5) 0.1314(5) 0.4434(3) 0.113(3) Uani 1 1 d . . . H34A H 2.4683 0.1106 0.4106 0.169 Uiso 1 1 calc R . . H34B H 2.4326 0.1538 0.4584 0.169 Uiso 1 1 calc R . . H34C H 2.5115 0.0850 0.4774 0.169 Uiso 1 1 calc R . . C35 C 2.5036(5) 0.2055(4) 0.7091(3) 0.068(2) Uani 1 1 d . . . C36 C 2.5718(4) 0.1437(5) 0.7182(3) 0.066(2) Uani 1 1 d . . . C37 C 2.5557(5) 0.0833(4) 0.6885(3) 0.070(2) Uani 1 1 d . . . C38 C 2.4760(5) 0.1141(4) 0.6594(3) 0.065(2) Uani 1 1 d . . . C39 C 2.4449(4) 0.1869(5) 0.6731(3) 0.067(2) Uani 1 1 d . . . C40 C 2.4992(7) 0.2741(5) 0.7394(4) 0.170(5) Uani 1 1 d . . . H40A H 2.4728 0.2543 0.7788 0.255 Uiso 1 1 calc R . . H40B H 2.4677 0.3261 0.7122 0.255 Uiso 1 1 calc R . . H40C H 2.5542 0.2854 0.7464 0.255 Uiso 1 1 calc R . . C41 C 2.6537(5) 0.1290(7) 0.7569(4) 0.168(5) Uani 1 1 d . . . H41A H 2.6455 0.0970 0.8002 0.252 Uiso 1 1 calc R . . H41B H 2.6707 0.1837 0.7536 0.252 Uiso 1 1 calc R . . H41C H 2.6958 0.0971 0.7411 0.252 Uiso 1 1 calc R . . C42 C 2.6038(6) 0.0017(4) 0.6866(4) 0.195(6) Uani 1 1 d . . . H42A H 2.5935 -0.0456 0.7233 0.292 Uiso 1 1 calc R . . H42B H 2.6620 0.0073 0.6856 0.292 Uiso 1 1 calc R . . H42C H 2.5869 -0.0090 0.6497 0.292 Uiso 1 1 calc R . . C43 C 2.4221(6) 0.0774(5) 0.6227(4) 0.137(4) Uani 1 1 d . . . H43A H 2.3919 0.0353 0.6513 0.205 Uiso 1 1 calc R . . H43B H 2.4565 0.0506 0.5984 0.205 Uiso 1 1 calc R . . H43C H 2.3838 0.1231 0.5950 0.205 Uiso 1 1 calc R . . C44 C 2.3601(4) 0.2399(6) 0.6573(4) 0.151(4) Uani 1 1 d . . . H44A H 2.3226 0.2148 0.6892 0.226 Uiso 1 1 calc R . . H44B H 2.3396 0.2406 0.6175 0.226 Uiso 1 1 calc R . . H44C H 2.3646 0.2979 0.6553 0.226 Uiso 1 1 calc R . . C45 C 2.7404(3) 0.1537(5) 0.5725(3) 0.086(3) Uani 1 1 d . . . H45A H 2.7576 0.1059 0.6101 0.130 Uiso 1 1 calc R . . H45B H 2.7511 0.2064 0.5779 0.130 Uiso 1 1 calc R . . H45C H 2.7708 0.1464 0.5380 0.130 Uiso 1 1 calc R . . C46 C 2.4521(4) 0.3946(4) 0.5220(3) 0.077(2) Uani 1 1 d . . . H46A H 2.4069 0.3992 0.5484 0.116 Uiso 1 1 calc R . . H46B H 2.4358 0.4277 0.4791 0.116 Uiso 1 1 calc R . . H46C H 2.4990 0.4163 0.5344 0.116 Uiso 1 1 calc R . . C47 C 2.6707(4) 0.3661(4) 0.5576(3) 0.0507(18) Uani 1 1 d . . . C48 C 2.7249(4) 0.4500(5) 0.6361(3) 0.089(3) Uani 1 1 d . . . H48A H 2.7600 0.4899 0.6412 0.134 Uiso 1 1 calc R . . H48B H 2.7391 0.3947 0.6682 0.134 Uiso 1 1 calc R . . H48C H 2.6680 0.4709 0.6394 0.134 Uiso 1 1 calc R . . C49 C 2.0561(5) 0.0836(5) 0.2695(4) 0.070(2) Uani 1 1 d . . . C50 C 1.9767(5) 0.1134(5) 0.2839(3) 0.068(2) Uani 1 1 d . . . C51 C 1.9460(4) 0.1860(5) 0.2343(4) 0.071(2) Uani 1 1 d . . . C52 C 2.0040(5) 0.2046(4) 0.1891(3) 0.066(2) Uani 1 1 d . . . C53 C 2.0720(5) 0.1427(5) 0.2099(3) 0.068(2) Uani 1 1 d . . . C54 C 2.1026(6) 0.0020(4) 0.3126(5) 0.190(6) Uani 1 1 d . . . H54A H 2.0920 -0.0452 0.2995 0.285 Uiso 1 1 calc R . . H54B H 2.0847 -0.0083 0.3546 0.285 Uiso 1 1 calc R . . H54C H 2.1609 0.0068 0.3115 0.285 Uiso 1 1 calc R . . C55 C 1.9220(5) 0.0771(5) 0.3387(4) 0.129(4) Uani 1 1 d . . . H55A H 1.8915 0.0356 0.3307 0.194 Uiso 1 1 calc R . . H55B H 1.8841 0.1231 0.3434 0.194 Uiso 1 1 calc R . . H55C H 1.9560 0.0497 0.3764 0.194 Uiso 1 1 calc R . . C56 C 1.8605(5) 0.2404(6) 0.2221(5) 0.147(4) Uani 1 1 d . . . H56A H 1.8231 0.2147 0.2032 0.221 Uiso 1 1 calc R . . H56B H 1.8655 0.2978 0.1944 0.221 Uiso 1 1 calc R . . H56C H 1.8394 0.2426 0.2612 0.221 Uiso 1 1 calc R . . C57 C 2.0006(6) 0.2735(6) 0.1237(3) 0.160(5) Uani 1 1 d . . . H57A H 1.9751 0.2532 0.0941 0.240 Uiso 1 1 calc R . . H57B H 2.0559 0.2847 0.1115 0.240 Uiso 1 1 calc R . . H57C H 1.9688 0.3256 0.1243 0.240 Uiso 1 1 calc R . . C58 C 2.1533(5) 0.1289(7) 0.1786(5) 0.174(5) Uani 1 1 d . . . H58A H 2.1457 0.0963 0.1518 0.261 Uiso 1 1 calc R . . H58B H 2.1958 0.0979 0.2104 0.261 Uiso 1 1 calc R . . H58C H 2.1696 0.1839 0.1542 0.261 Uiso 1 1 calc R . . C59 C 2.0351(5) 0.2012(5) 0.4808(3) 0.060(2) Uani 1 1 d . . . C60 C 2.0033(4) 0.2884(5) 0.4645(3) 0.060(2) Uani 1 1 d . . . C61 C 2.0673(4) 0.3377(4) 0.4623(3) 0.060(2) Uani 1 1 d . . . C62 C 2.1419(4) 0.2815(5) 0.4797(3) 0.060(2) Uani 1 1 d . . . C63 C 2.1236(5) 0.1986(5) 0.4904(3) 0.067(2) Uani 1 1 d . . . C64 C 1.9813(5) 0.1312(5) 0.4908(3) 0.113(3) Uani 1 1 d . . . H64A H 1.9654 0.1118 0.5337 0.170 Uiso 1 1 calc R . . H64B H 2.0113 0.0838 0.4817 0.170 Uiso 1 1 calc R . . H64C H 1.9326 0.1529 0.4635 0.170 Uiso 1 1 calc R . . C65 C 1.9126(4) 0.3273(6) 0.4549(3) 0.105(3) Uani 1 1 d . . . H65A H 1.8912 0.3268 0.4945 0.158 Uiso 1 1 calc R . . H65B H 1.8814 0.2939 0.4381 0.158 Uiso 1 1 calc R . . H65C H 1.9081 0.3856 0.4262 0.158 Uiso 1 1 calc R . . C66 C 2.0642(5) 0.4334(5) 0.4493(4) 0.108(3) Uani 1 1 d . . . H66A H 2.0549 0.4452 0.4875 0.162 Uiso 1 1 calc R . . H66B H 2.0199 0.4639 0.4191 0.162 Uiso 1 1 calc R . . H66C H 2.1159 0.4520 0.4329 0.162 Uiso 1 1 calc R . . C67 C 2.2281(4) 0.3043(6) 0.4887(4) 0.112(3) Uani 1 1 d . . . H67A H 2.2355 0.3036 0.5309 0.168 Uiso 1 1 calc R . . H67B H 2.2338 0.3608 0.4597 0.168 Uiso 1 1 calc R . . H67C H 2.2693 0.2628 0.4812 0.168 Uiso 1 1 calc R . . C68 C 2.1793(5) 0.1141(5) 0.5151(3) 0.127(4) Uani 1 1 d . . . H68A H 2.1848 0.0960 0.5601 0.191 Uiso 1 1 calc R . . H68B H 2.2330 0.1212 0.4977 0.191 Uiso 1 1 calc R . . H68C H 2.1557 0.0712 0.5033 0.191 Uiso 1 1 calc R . . C69 C 1.9519(4) 0.3945(4) 0.2805(3) 0.076(2) Uani 1 1 d . . . H69A H 1.9067 0.3990 0.2519 0.113 Uiso 1 1 calc R . . H69B H 1.9987 0.4162 0.2572 0.113 Uiso 1 1 calc R . . H69C H 1.9355 0.4277 0.3069 0.113 Uiso 1 1 calc R . . C70 C 2.2385(4) 0.1530(4) 0.3512(3) 0.083(2) Uani 1 1 d . . . H70A H 2.2555 0.1052 0.3375 0.124 Uiso 1 1 calc R . . H70B H 2.2687 0.1456 0.3895 0.124 Uiso 1 1 calc R . . H70C H 2.2495 0.2057 0.3195 0.124 Uiso 1 1 calc R . . C71 C 2.1708(4) 0.3661(4) 0.2598(3) 0.0503(18) Uani 1 1 d . . . C72 C 2.2243(4) 0.4496(4) 0.1393(3) 0.087(3) Uani 1 1 d . . . H72A H 2.2592 0.4896 0.1139 0.131 Uiso 1 1 calc R . . H72B H 2.1673 0.4703 0.1258 0.131 Uiso 1 1 calc R . . H72C H 2.2386 0.3942 0.1350 0.131 Uiso 1 1 calc R . . C73 C 2.5307(4) 0.2054(5) -0.0827(3) 0.057(2) Uani 1 1 d . . . C74 C 2.5048(4) 0.2938(5) -0.1109(3) 0.0547(19) Uani 1 1 d . . . C75 C 2.5729(4) 0.3374(5) -0.1312(3) 0.060(2) Uani 1 1 d . . . C76 C 2.6435(4) 0.2746(6) -0.1177(3) 0.073(3) Uani 1 1 d . . . C77 C 2.6204(5) 0.1924(5) -0.0875(3) 0.074(2) Uani 1 1 d . . . C78 C 2.4807(5) 0.1312(5) -0.0565(3) 0.120(4) Uani 1 1 d . . . H78A H 2.4616 0.1143 -0.0901 0.180 Uiso 1 1 calc R . . H78B H 2.4340 0.1487 -0.0359 0.180 Uiso 1 1 calc R . . H78C H 2.5148 0.0834 -0.0269 0.180 Uiso 1 1 calc R . . C79 C 2.4128(4) 0.3283(5) -0.1191(3) 0.099(3) Uani 1 1 d . . . H79A H 2.3924 0.3320 -0.1598 0.149 Uiso 1 1 calc R . . H79B H 2.4053 0.3846 -0.1155 0.149 Uiso 1 1 calc R . . H79C H 2.3829 0.2900 -0.0873 0.149 Uiso 1 1 calc R . . C80 C 2.5636(5) 0.4336(5) -0.1665(3) 0.108(3) Uani 1 1 d . . . H80A H 2.5585 0.4443 -0.2107 0.163 Uiso 1 1 calc R . . H80B H 2.6115 0.4569 -0.1575 0.163 Uiso 1 1 calc R . . H80C H 2.5149 0.4606 -0.1535 0.163 Uiso 1 1 calc R . . C81 C 2.7283(4) 0.3004(6) -0.1395(4) 0.127(4) Uani 1 1 d . . . H81A H 2.7370 0.2958 -0.1801 0.191 Uiso 1 1 calc R . . H81B H 2.7706 0.2629 -0.1101 0.191 Uiso 1 1 calc R . . H81C H 2.7307 0.3589 -0.1419 0.191 Uiso 1 1 calc R . . C82 C 2.6798(5) 0.1108(5) -0.0700(4) 0.141(4) Uani 1 1 d . . . H82A H 2.6804 0.0877 -0.1035 0.211 Uiso 1 1 calc R . . H82B H 2.6625 0.0694 -0.0325 0.211 Uiso 1 1 calc R . . H82C H 2.7344 0.1230 -0.0628 0.211 Uiso 1 1 calc R . . C83 C 2.4480(4) 0.1915(4) 0.1759(3) 0.064(2) Uani 1 1 d . . . C84 C 2.5115(5) 0.2018(5) 0.2111(3) 0.078(3) Uani 1 1 d . . . C85 C 2.5758(4) 0.1373(6) 0.2176(4) 0.080(3) Uani 1 1 d . . . C86 C 2.5496(5) 0.0845(4) 0.1860(4) 0.074(3) Uani 1 1 d . . . C87 C 2.4702(4) 0.1188(5) 0.1584(3) 0.0573(19) Uani 1 1 d . . . C88 C 2.3608(4) 0.2408(6) 0.1584(4) 0.139(4) Uani 1 1 d . . . H88A H 2.3243 0.2170 0.1915 0.208 Uiso 1 1 calc R . . H88B H 2.3407 0.2358 0.1202 0.208 Uiso 1 1 calc R . . H88C H 2.3626 0.3006 0.1526 0.208 Uiso 1 1 calc R . . C89 C 2.5013(6) 0.2732(6) 0.2398(4) 0.152(4) Uani 1 1 d . . . H89A H 2.4792 0.2515 0.2808 0.228 Uiso 1 1 calc R . . H89B H 2.4639 0.3211 0.2134 0.228 Uiso 1 1 calc R . . H89C H 2.5542 0.2917 0.2433 0.228 Uiso 1 1 calc R . . C90 C 2.6550(5) 0.1270(7) 0.2566(4) 0.198(6) Uani 1 1 d . . . H90A H 2.6487 0.0896 0.2988 0.297 Uiso 1 1 calc R . . H90B H 2.6658 0.1824 0.2569 0.297 Uiso 1 1 calc R . . H90C H 2.7005 0.1023 0.2387 0.297 Uiso 1 1 calc R . . C91 C 2.6016(5) 0.0026(4) 0.1865(4) 0.129(4) Uani 1 1 d . . . H91A H 2.5868 -0.0454 0.2209 0.194 Uiso 1 1 calc R . . H91B H 2.6592 0.0079 0.1911 0.194 Uiso 1 1 calc R . . H91C H 2.5917 -0.0067 0.1477 0.194 Uiso 1 1 calc R . . C92 C 2.4212(6) 0.0775(6) 0.1224(4) 0.152(5) Uani 1 1 d . . . H92A H 2.3878 0.0388 0.1507 0.228 Uiso 1 1 calc R . . H92B H 2.4586 0.0460 0.1029 0.228 Uiso 1 1 calc R . . H92C H 2.3860 0.1215 0.0907 0.228 Uiso 1 1 calc R . . C93 C 2.4518(4) 0.3946(4) 0.0218(3) 0.075(2) Uani 1 1 d . . . H93A H 2.4066 0.3992 0.0482 0.113 Uiso 1 1 calc R . . H93B H 2.4353 0.4275 -0.0212 0.113 Uiso 1 1 calc R . . H93C H 2.4985 0.4167 0.0340 0.113 Uiso 1 1 calc R . . C94 C 2.7390(4) 0.1537(4) 0.0725(3) 0.083(2) Uani 1 1 d . . . H94A H 2.7701 0.1316 0.0442 0.124 Uiso 1 1 calc R . . H94B H 2.7531 0.1164 0.1150 0.124 Uiso 1 1 calc R . . H94C H 2.7520 0.2106 0.0672 0.124 Uiso 1 1 calc R . . C95 C 2.6703(4) 0.3660(4) 0.0572(3) 0.0514(18) Uani 1 1 d . . . C96 C 2.7248(4) 0.4495(4) 0.1348(3) 0.087(3) Uani 1 1 d . . . H96A H 2.7601 0.4891 0.1402 0.131 Uiso 1 1 calc R . . H96B H 2.7388 0.3940 0.1668 0.131 Uiso 1 1 calc R . . H96C H 2.6680 0.4706 0.1381 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0410(5) 0.0447(6) 0.0381(6) -0.0160(5) 0.0043(4) -0.0102(4) Fe2 0.0433(5) 0.0398(6) 0.0328(6) -0.0128(5) 0.0029(4) -0.0098(4) Fe3 0.0413(5) 0.0450(6) 0.0359(6) -0.0133(5) 0.0008(4) -0.0099(4) Fe4 0.0441(5) 0.0397(6) 0.0329(6) -0.0127(5) 0.0029(4) -0.0110(4) Fe5 0.0436(5) 0.0404(6) 0.0336(6) -0.0137(5) 0.0024(4) -0.0104(4) Fe6 0.0418(5) 0.0454(6) 0.0379(6) -0.0167(5) 0.0046(5) -0.0105(4) Fe7 0.0412(5) 0.0458(6) 0.0365(6) -0.0138(5) 0.0017(5) -0.0106(4) Fe8 0.0433(5) 0.0405(6) 0.0330(6) -0.0127(5) 0.0024(4) -0.0096(4) S1 0.0424(9) 0.0472(11) 0.0434(11) -0.0176(9) 0.0007(8) -0.0034(8) S2 0.0638(11) 0.0435(11) 0.0413(11) -0.0187(10) -0.0107(9) -0.0009(9) S3 0.0651(12) 0.0546(12) 0.0605(13) -0.0284(11) 0.0160(10) -0.0285(9) S4 0.0668(12) 0.0579(13) 0.0425(12) -0.0171(10) 0.0175(10) -0.0239(9) S5 0.0844(15) 0.0655(14) 0.0853(17) -0.0207(13) 0.0375(13) -0.0423(11) S6 0.0439(9) 0.0480(11) 0.0394(11) -0.0131(9) -0.0002(8) -0.0035(8) S7 0.0647(11) 0.0436(11) 0.0366(11) -0.0095(9) 0.0095(9) -0.0011(9) S8 0.0634(11) 0.0552(12) 0.0470(12) -0.0085(10) 0.0025(10) -0.0290(9) S9 0.0658(12) 0.0579(12) 0.0455(12) -0.0208(10) -0.0011(10) -0.0250(10) S10 0.0832(15) 0.0656(15) 0.0889(17) -0.0221(13) -0.0103(13) -0.0416(12) S11 0.0438(9) 0.0480(11) 0.0404(11) -0.0169(9) 0.0011(8) -0.0034(8) S12 0.0642(11) 0.0429(11) 0.0449(12) -0.0184(10) -0.0086(9) -0.0019(9) S13 0.0639(11) 0.0556(12) 0.0595(13) -0.0283(11) 0.0163(10) -0.0291(9) S14 0.0656(11) 0.0573(12) 0.0432(12) -0.0172(10) 0.0174(10) -0.0258(9) S15 0.0835(14) 0.0688(15) 0.0863(17) -0.0236(13) 0.0384(13) -0.0428(12) S16 0.0432(9) 0.0484(11) 0.0395(11) -0.0151(9) 0.0000(8) -0.0037(8) S17 0.0636(11) 0.0426(11) 0.0379(11) -0.0099(9) 0.0094(9) -0.0013(9) S18 0.0651(12) 0.0549(12) 0.0442(12) -0.0071(10) 0.0015(10) -0.0284(9) S19 0.0660(12) 0.0574(12) 0.0453(12) -0.0216(10) -0.0022(10) -0.0248(10) S20 0.0846(15) 0.0704(15) 0.0819(17) -0.0230(13) -0.0092(13) -0.0433(12) C1 0.110(7) 0.066(5) 0.031(4) -0.009(4) 0.006(4) 0.013(5) C2 0.034(3) 0.133(7) 0.042(5) -0.036(5) -0.005(3) 0.010(4) C3 0.067(5) 0.080(5) 0.057(5) -0.045(4) 0.019(4) -0.038(4) C4 0.055(4) 0.067(5) 0.039(4) -0.024(4) 0.003(3) 0.009(4) C5 0.063(4) 0.084(6) 0.040(5) -0.029(4) 0.018(4) -0.033(4) C6 0.196(10) 0.122(8) 0.061(6) -0.001(6) -0.021(6) 0.107(7) C7 0.062(5) 0.263(12) 0.082(7) -0.080(7) 0.002(5) -0.051(7) C8 0.137(8) 0.091(7) 0.118(8) -0.071(6) 0.021(6) -0.035(6) C9 0.048(5) 0.163(8) 0.096(7) -0.068(6) 0.004(5) 0.010(5) C10 0.180(9) 0.124(8) 0.064(6) -0.033(6) 0.035(6) -0.091(7) C11 0.053(4) 0.096(7) 0.122(8) -0.083(6) 0.010(5) -0.013(4) C12 0.125(7) 0.099(7) 0.035(4) -0.037(5) 0.033(4) -0.062(5) C13 0.073(5) 0.057(4) 0.057(5) -0.021(4) -0.042(4) 0.008(4) C14 0.053(4) 0.075(5) 0.056(5) -0.038(4) 0.005(3) -0.026(3) C15 0.107(6) 0.033(4) 0.074(6) -0.016(4) -0.043(5) -0.008(4) C16 0.111(8) 0.302(15) 0.303(15) -0.269(14) 0.109(9) -0.092(9) C17 0.265(13) 0.156(10) 0.044(6) -0.021(6) 0.005(7) -0.099(9) C18 0.082(7) 0.174(10) 0.209(12) -0.125(9) -0.066(7) 0.028(7) C19 0.238(12) 0.202(11) 0.084(7) -0.078(7) 0.084(8) -0.178(10) C20 0.178(9) 0.069(6) 0.144(8) -0.058(6) -0.051(7) -0.001(6) C21 0.080(5) 0.052(5) 0.080(6) -0.016(5) -0.011(5) 0.018(4) C22 0.030(3) 0.124(7) 0.125(7) -0.078(6) -0.017(4) 0.025(4) C23 0.052(4) 0.046(4) 0.063(5) -0.014(4) 0.017(4) -0.020(3) C24 0.097(6) 0.073(6) 0.075(6) 0.004(5) 0.034(5) -0.025(5) C25 0.086(5) 0.075(6) 0.039(4) -0.028(4) 0.002(4) 0.024(4) C26 0.063(4) 0.080(5) 0.030(4) -0.017(4) 0.007(3) -0.027(4) C27 0.072(5) 0.068(5) 0.039(5) -0.014(4) -0.013(4) 0.012(4) C28 0.041(4) 0.102(6) 0.047(5) -0.038(5) 0.006(3) -0.024(4) C29 0.108(6) 0.059(5) 0.044(5) -0.030(4) 0.017(4) -0.036(4) C30 0.178(9) 0.124(8) 0.072(6) -0.062(6) -0.027(6) 0.054(7) C31 0.065(5) 0.211(10) 0.079(6) -0.059(7) 0.025(5) -0.048(6) C32 0.140(8) 0.094(7) 0.066(6) 0.004(6) -0.021(6) -0.022(6) C33 0.045(4) 0.189(10) 0.079(6) -0.060(7) -0.015(4) 0.012(5) C34 0.177(9) 0.114(8) 0.075(6) -0.044(6) 0.010(6) -0.086(7) C35 0.089(5) 0.061(5) 0.049(5) -0.015(4) 0.031(4) -0.003(4) C36 0.073(5) 0.096(6) 0.029(4) -0.012(4) 0.000(4) -0.038(4) C37 0.077(5) 0.053(5) 0.049(5) 0.018(4) 0.032(4) 0.010(4) C38 0.107(6) 0.058(5) 0.046(5) -0.026(4) 0.034(4) -0.046(4) C39 0.044(4) 0.105(6) 0.042(4) -0.005(4) 0.004(3) -0.027(4) C40 0.332(15) 0.118(8) 0.108(8) -0.081(7) 0.117(9) -0.087(9) C41 0.140(9) 0.254(13) 0.060(7) 0.037(7) -0.036(6) -0.104(9) C42 0.279(13) 0.047(6) 0.186(11) 0.030(6) 0.168(10) 0.052(7) C43 0.214(11) 0.152(9) 0.076(7) -0.040(6) 0.034(7) -0.146(8) C44 0.068(6) 0.198(11) 0.127(9) 0.006(8) 0.042(6) 0.027(7) C45 0.042(4) 0.129(7) 0.065(6) -0.014(5) -0.003(4) 0.021(4) C46 0.090(6) 0.048(5) 0.083(6) -0.017(4) 0.002(5) 0.014(4) C47 0.054(4) 0.046(4) 0.053(5) -0.014(4) -0.005(4) -0.020(3) C48 0.093(6) 0.097(6) 0.106(7) -0.064(6) -0.015(5) -0.027(5) C49 0.077(5) 0.061(5) 0.085(6) -0.048(5) -0.036(4) 0.010(4) C50 0.120(7) 0.054(5) 0.028(4) 0.001(4) 0.001(4) -0.052(5) C51 0.044(4) 0.115(7) 0.089(6) -0.075(6) 0.014(4) -0.026(4) C52 0.096(6) 0.055(5) 0.042(5) -0.011(4) -0.034(4) -0.004(4) C53 0.077(5) 0.099(6) 0.063(5) -0.061(5) 0.027(4) -0.041(5) C54 0.279(12) 0.039(5) 0.237(11) -0.046(6) -0.213(10) 0.046(6) C55 0.194(10) 0.149(8) 0.082(7) -0.051(6) 0.045(7) -0.132(8) C56 0.079(7) 0.176(10) 0.218(12) -0.119(10) -0.057(7) 0.020(7) C57 0.293(14) 0.137(9) 0.039(6) 0.002(6) -0.047(7) -0.084(9) C58 0.139(9) 0.265(13) 0.246(13) -0.221(12) 0.118(9) -0.116(9) C59 0.098(6) 0.053(5) 0.032(4) -0.013(4) 0.010(4) -0.023(4) C60 0.038(3) 0.109(6) 0.045(5) -0.036(5) 0.009(3) -0.026(4) C61 0.063(4) 0.067(5) 0.050(5) -0.028(4) 0.001(4) 0.013(4) C62 0.064(4) 0.086(5) 0.052(5) -0.045(4) 0.010(4) -0.029(4) C63 0.077(5) 0.080(6) 0.038(5) -0.023(4) -0.015(4) 0.028(4) C64 0.183(9) 0.110(7) 0.067(6) -0.031(6) 0.044(6) -0.094(7) C65 0.057(5) 0.198(10) 0.065(6) -0.057(6) 0.008(4) 0.004(6) C66 0.144(8) 0.081(7) 0.114(8) -0.053(6) 0.039(6) -0.011(6) C67 0.081(6) 0.189(9) 0.105(7) -0.088(7) 0.010(5) -0.054(6) C68 0.179(9) 0.139(8) 0.046(5) -0.034(6) -0.016(6) 0.053(7) C69 0.087(6) 0.055(5) 0.076(6) -0.018(5) -0.013(5) 0.013(4) C70 0.096(6) 0.090(6) 0.070(5) -0.047(5) -0.020(4) 0.022(5) C71 0.055(4) 0.042(4) 0.055(5) -0.014(4) 0.017(4) -0.017(3) C72 0.099(6) 0.073(6) 0.073(6) -0.001(5) 0.030(5) -0.019(5) C73 0.059(4) 0.082(6) 0.033(4) -0.017(4) -0.007(3) -0.028(4) C74 0.055(4) 0.069(5) 0.034(4) -0.015(4) -0.009(3) 0.009(4) C75 0.064(4) 0.082(5) 0.030(4) -0.006(4) 0.006(3) -0.040(4) C76 0.036(4) 0.136(8) 0.059(5) -0.053(5) 0.000(4) 0.007(4) C77 0.108(7) 0.066(5) 0.046(5) -0.026(4) -0.021(5) 0.016(5) C78 0.191(10) 0.122(8) 0.082(7) -0.050(6) 0.031(7) -0.109(7) C79 0.056(5) 0.174(9) 0.079(6) -0.063(6) -0.007(5) -0.003(6) C80 0.158(9) 0.086(7) 0.062(6) 0.007(5) 0.001(6) -0.040(6) C81 0.071(6) 0.263(12) 0.087(7) -0.097(8) 0.033(5) -0.060(7) C82 0.191(10) 0.120(8) 0.111(8) -0.077(7) -0.050(7) 0.097(7) C83 0.071(5) 0.058(4) 0.052(5) -0.013(4) 0.033(4) 0.010(3) C84 0.128(7) 0.097(6) 0.030(4) -0.034(4) 0.013(4) -0.059(5) C85 0.054(5) 0.097(7) 0.051(5) 0.026(5) -0.003(4) -0.013(4) C86 0.106(7) 0.037(5) 0.066(6) -0.002(4) 0.047(5) -0.009(4) C87 0.059(4) 0.071(5) 0.040(4) -0.009(4) 0.008(3) -0.031(4) C88 0.088(7) 0.169(10) 0.108(8) 0.004(7) 0.043(6) 0.028(7) C89 0.248(12) 0.166(10) 0.102(8) -0.102(8) 0.070(8) -0.094(9) C90 0.112(8) 0.327(16) 0.075(7) 0.061(9) -0.048(6) -0.106(9) C91 0.187(9) 0.063(6) 0.106(7) 0.008(5) 0.078(7) -0.005(6) C92 0.210(11) 0.220(11) 0.075(7) -0.067(8) 0.035(7) -0.174(9) C93 0.082(5) 0.056(5) 0.079(6) -0.021(5) -0.003(5) 0.017(4) C94 0.076(5) 0.090(6) 0.058(5) -0.005(5) 0.003(4) 0.024(4) C95 0.054(4) 0.042(4) 0.059(5) -0.014(4) -0.004(4) -0.019(3) C96 0.095(6) 0.058(5) 0.120(7) -0.041(5) -0.024(5) -0.019(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 Fe1 C5 2.089(6) . ? Fe1 C1 2.118(7) . ? Fe1 C2 2.125(6) . ? Fe1 C4 2.128(6) . ? Fe1 C3 2.142(6) . ? Fe1 S3 2.1785(18) . ? Fe1 S2 2.2537(16) . ? Fe1 S1 2.2726(18) . ? Fe2 C13 2.098(6) . ? Fe2 C11 2.099(7) . ? Fe2 C15 2.102(6) . ? Fe2 C14 2.104(6) . ? Fe2 C12 2.108(6) . ? Fe2 S4 2.1632(18) . ? Fe2 S2 2.2544(18) . ? Fe2 S1 2.2627(16) . ? Fe3 C29 2.090(6) . ? Fe3 C25 2.104(6) . ? Fe3 C28 2.124(6) . ? Fe3 C27 2.139(7) . ? Fe3 C26 2.143(6) . ? Fe3 S8 2.1792(17) . ? Fe3 S7 2.2547(19) . ? Fe3 S6 2.2715(17) . ? Fe4 C38 2.087(6) . ? Fe4 C36 2.089(6) . ? Fe4 C39 2.106(6) . ? Fe4 C35 2.119(6) . ? Fe4 C37 2.125(7) . ? Fe4 S9 2.1615(17) . ? Fe4 S7 2.2556(17) . ? Fe4 S6 2.2674(18) . ? Fe5 C51 2.089(6) . ? Fe5 C50 2.090(6) . ? Fe5 C52 2.103(6) . ? Fe5 C53 2.104(6) . ? Fe5 C49 2.125(6) . ? Fe5 S14 2.1607(18) . ? Fe5 S12 2.2555(18) . ? Fe5 S11 2.2646(16) . ? Fe6 C63 2.089(7) . ? Fe6 C59 2.093(7) . ? Fe6 C60 2.124(6) . ? Fe6 C61 2.146(6) . ? Fe6 C62 2.149(6) . ? Fe6 S13 2.1769(18) . ? Fe6 S12 2.2533(17) . ? Fe6 S11 2.2734(18) . ? Fe7 C73 2.095(6) . ? Fe7 C77 2.116(7) . ? Fe7 C76 2.126(7) . ? Fe7 C74 2.129(6) . ? Fe7 C75 2.140(6) . ? Fe7 S18 2.1787(17) . ? Fe7 S17 2.2518(19) . ? Fe7 S16 2.2716(17) . ? Fe8 C83 2.092(6) . ? Fe8 C87 2.099(6) . ? Fe8 C84 2.102(6) . ? Fe8 C85 2.103(7) . ? Fe8 C86 2.104(7) . ? Fe8 S19 2.1623(17) . ? Fe8 S17 2.2540(17) . ? Fe8 S16 2.2632(18) . ? S1 C21 1.817(6) . ? S2 C22 1.838(5) . ? S3 C23 1.702(6) . ? S4 C23 1.680(6) . ? S5 C23 1.760(6) . ? S5 C24 1.786(7) . ? S6 C46 1.813(6) . ? S7 C45 1.839(5) . ? S8 C47 1.713(6) . ? S9 C47 1.672(6) . ? S10 C47 1.762(5) . ? S10 C48 1.789(6) . ? S11 C69 1.813(6) . ? S12 C70 1.811(6) . ? S13 C71 1.702(6) . ? S14 C71 1.680(6) . ? S15 C71 1.762(6) . ? S15 C72 1.787(7) . ? S16 C93 1.814(6) . ? S17 C94 1.821(6) . ? S18 C95 1.704(6) . ? S19 C95 1.673(6) . ? S20 C96 1.765(7) . ? S20 C95 1.766(5) . ? C1 C2 1.399(9) . ? C1 C5 1.445(9) . ? C1 C6 1.504(9) . ? C2 C3 1.410(9) . ? C2 C7 1.524(8) . ? C3 C4 1.391(8) . ? C3 C8 1.504(8) . ? C4 C5 1.411(8) . ? C4 C9 1.520(8) . ? C5 C10 1.500(8) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.381(10) . ? C11 C15 1.422(10) . ? C11 C16 1.527(9) . ? C12 C13 1.367(9) . ? C12 C17 1.534(9) . ? C13 C14 1.408(8) . ? C13 C18 1.513(8) . ? C14 C15 1.390(9) . ? C14 C19 1.513(8) . ? C15 C20 1.508(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.392(9) . ? C25 C29 1.444(9) . ? C25 C30 1.508(9) . ? C26 C27 1.412(8) . ? C26 C31 1.513(8) . ? C27 C28 1.386(8) . ? C27 C32 1.512(9) . ? C28 C29 1.410(9) . ? C28 C33 1.516(8) . ? C29 C34 1.482(8) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C39 1.382(9) . ? C35 C36 1.383(9) . ? C35 C40 1.513(8) . ? C36 C37 1.432(9) . ? C36 C41 1.543(9) . ? C37 C38 1.411(9) . ? C37 C42 1.497(8) . ? C38 C39 1.388(9) . ? C38 C43 1.518(8) . ? C39 C44 1.517(9) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.406(9) . ? C49 C53 1.418(10) . ? C49 C54 1.490(9) . ? C50 C51 1.378(9) . ? C50 C55 1.519(8) . ? C51 C52 1.373(9) . ? C51 C56 1.536(9) . ? C52 C53 1.379(9) . ? C52 C57 1.529(9) . ? C53 C58 1.530(9) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.400(9) . ? C59 C63 1.448(9) . ? C59 C64 1.493(8) . ? C60 C61 1.390(8) . ? C60 C65 1.522(8) . ? C61 C62 1.407(8) . ? C61 C66 1.509(8) . ? C62 C63 1.383(9) . ? C62 C67 1.525(8) . ? C63 C68 1.506(9) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 C74 1.399(8) . ? C73 C77 1.458(9) . ? C73 C78 1.506(8) . ? C74 C75 1.386(8) . ? C74 C79 1.524(8) . ? C75 C76 1.414(9) . ? C75 C80 1.512(9) . ? C76 C77 1.398(10) . ? C76 C81 1.524(8) . ? C77 C82 1.500(9) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C83 C84 1.365(9) . ? C83 C87 1.405(8) . ? C83 C88 1.532(9) . ? C84 C85 1.375(10) . ? C84 C89 1.528(8) . ? C85 C86 1.407(10) . ? C85 C90 1.522(9) . ? C86 C87 1.402(9) . ? C86 C91 1.511(9) . ? C87 C92 1.510(8) . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? 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 C5 Fe1 C1 40.2(3) . . ? C5 Fe1 C2 65.2(3) . . ? C1 Fe1 C2 38.5(3) . . ? C5 Fe1 C4 39.1(2) . . ? C1 Fe1 C4 65.8(3) . . ? C2 Fe1 C4 64.1(2) . . ? C5 Fe1 C3 65.1(2) . . ? C1 Fe1 C3 65.4(3) . . ? C2 Fe1 C3 38.6(2) . . ? C4 Fe1 C3 38.0(2) . . ? C5 Fe1 S3 157.07(18) . . ? C1 Fe1 S3 125.7(3) . . ? C2 Fe1 S3 93.6(2) . . ? C4 Fe1 S3 125.2(2) . . ? C3 Fe1 S3 93.08(17) . . ? C5 Fe1 S2 99.8(2) . . ? C1 Fe1 S2 90.9(2) . . ? C2 Fe1 S2 119.0(2) . . ? C4 Fe1 S2 136.6(2) . . ? C3 Fe1 S2 155.9(2) . . ? S3 Fe1 S2 98.20(7) . . ? C5 Fe1 S1 98.10(19) . . ? C1 Fe1 S1 135.2(3) . . ? C2 Fe1 S1 155.65(17) . . ? C4 Fe1 S1 91.64(18) . . ? C3 Fe1 S1 119.4(2) . . ? S3 Fe1 S1 99.03(7) . . ? S2 Fe1 S1 79.76(6) . . ? C13 Fe2 C11 64.6(3) . . ? C13 Fe2 C15 64.4(3) . . ? C11 Fe2 C15 39.6(3) . . ? C13 Fe2 C14 39.1(2) . . ? C11 Fe2 C14 65.9(3) . . ? C15 Fe2 C14 38.6(2) . . ? C13 Fe2 C12 37.9(2) . . ? C11 Fe2 C12 38.3(3) . . ? C15 Fe2 C12 64.4(3) . . ? C14 Fe2 C12 65.0(2) . . ? C13 Fe2 S4 119.5(2) . . ? C11 Fe2 S4 94.4(2) . . ? C15 Fe2 S4 130.8(3) . . ? C14 Fe2 S4 154.96(19) . . ? C12 Fe2 S4 90.01(19) . . ? C13 Fe2 S2 142.8(2) . . ? C11 Fe2 S2 114.6(3) . . ? C15 Fe2 S2 91.2(2) . . ? C14 Fe2 S2 104.4(2) . . ? C12 Fe2 S2 152.6(3) . . ? S4 Fe2 S2 97.76(7) . . ? C13 Fe2 S1 94.5(2) . . ? C11 Fe2 S1 158.8(2) . . ? C15 Fe2 S1 130.2(3) . . ? C14 Fe2 S1 96.31(17) . . ? C12 Fe2 S1 124.9(3) . . ? S4 Fe2 S1 98.93(7) . . ? S2 Fe2 S1 79.96(6) . . ? C29 Fe3 C25 40.3(2) . . ? C29 Fe3 C28 39.1(2) . . ? C25 Fe3 C28 65.2(3) . . ? C29 Fe3 C27 65.0(3) . . ? C25 Fe3 C27 64.2(3) . . ? C28 Fe3 C27 37.9(2) . . ? C29 Fe3 C26 66.1(2) . . ? C25 Fe3 C26 38.3(2) . . ? C28 Fe3 C26 64.7(2) . . ? C27 Fe3 C26 38.5(2) . . ? C29 Fe3 S8 157.4(2) . . ? C25 Fe3 S8 123.2(2) . . ? C28 Fe3 S8 127.7(2) . . ? C27 Fe3 S8 94.8(2) . . ? C26 Fe3 S8 91.97(18) . . ? C29 Fe3 S7 97.9(2) . . ? C25 Fe3 S7 92.7(2) . . ? C28 Fe3 S7 133.9(2) . . ? C27 Fe3 S7 156.82(18) . . ? C26 Fe3 S7 121.6(2) . . ? S8 Fe3 S7 98.34(7) . . ? C29 Fe3 S6 99.2(2) . . ? C25 Fe3 S6 137.8(2) . . ? C28 Fe3 S6 90.40(17) . . ? C27 Fe3 S6 116.84(19) . . ? C26 Fe3 S6 154.26(19) . . ? S8 Fe3 S6 99.03(7) . . ? S7 Fe3 S6 79.89(6) . . ? C38 Fe4 C36 65.3(3) . . ? C38 Fe4 C39 38.7(2) . . ? C36 Fe4 C39 64.1(3) . . ? C38 Fe4 C35 65.0(3) . . ? C36 Fe4 C35 38.4(2) . . ? C39 Fe4 C35 38.2(2) . . ? C38 Fe4 C37 39.1(3) . . ? C36 Fe4 C37 39.7(3) . . ? C39 Fe4 C37 65.1(3) . . ? C35 Fe4 C37 65.7(3) . . ? C38 Fe4 S9 155.55(18) . . ? C36 Fe4 S9 92.98(19) . . ? C39 Fe4 S9 123.0(2) . . ? C35 Fe4 S9 91.2(2) . . ? C37 Fe4 S9 127.5(3) . . ? C38 Fe4 S7 102.16(19) . . ? C36 Fe4 S7 117.8(2) . . ? C39 Fe4 S7 139.2(2) . . ? C35 Fe4 S7 155.4(2) . . ? C37 Fe4 S7 90.89(19) . . ? S9 Fe4 S7 97.84(7) . . ? C38 Fe4 S6 98.4(2) . . ? C36 Fe4 S6 157.2(2) . . ? C39 Fe4 S6 93.07(19) . . ? C35 Fe4 S6 121.4(2) . . ? C37 Fe4 S6 133.7(2) . . ? S9 Fe4 S6 98.83(7) . . ? S7 Fe4 S6 79.96(6) . . ? C51 Fe5 C50 38.5(3) . . ? C51 Fe5 C52 38.3(2) . . ? C50 Fe5 C52 64.8(3) . . ? C51 Fe5 C53 64.0(3) . . ? C50 Fe5 C53 65.0(3) . . ? C52 Fe5 C53 38.3(3) . . ? C51 Fe5 C49 64.7(3) . . ? C50 Fe5 C49 39.0(3) . . ? C52 Fe5 C49 65.2(3) . . ? C53 Fe5 C49 39.2(3) . . ? C51 Fe5 S14 123.5(3) . . ? C50 Fe5 S14 155.66(19) . . ? C52 Fe5 S14 91.5(2) . . ? C53 Fe5 S14 93.2(2) . . ? C49 Fe5 S14 127.2(3) . . ? C51 Fe5 S12 138.6(3) . . ? C50 Fe5 S12 101.7(2) . . ? C52 Fe5 S12 154.97(19) . . ? C53 Fe5 S12 117.6(3) . . ? C49 Fe5 S12 90.9(2) . . ? S14 Fe5 S12 97.91(7) . . ? C51 Fe5 S11 93.18(17) . . ? C50 Fe5 S11 98.5(2) . . ? C52 Fe5 S11 121.6(2) . . ? C53 Fe5 S11 157.1(2) . . ? C49 Fe5 S11 133.8(3) . . ? S14 Fe5 S11 98.95(7) . . ? S12 Fe5 S11 79.91(6) . . ? C63 Fe6 C59 40.5(3) . . ? C63 Fe6 C60 64.9(3) . . ? C59 Fe6 C60 38.8(2) . . ? C63 Fe6 C61 64.3(3) . . ? C59 Fe6 C61 65.2(3) . . ? C60 Fe6 C61 38.0(2) . . ? C63 Fe6 C62 38.1(2) . . ? C59 Fe6 C62 65.8(3) . . ? C60 Fe6 C62 64.0(2) . . ? C61 Fe6 C62 38.2(2) . . ? C63 Fe6 S13 123.2(2) . . ? C59 Fe6 S13 157.52(19) . . ? C60 Fe6 S13 127.7(2) . . ? C61 Fe6 S13 94.5(2) . . ? C62 Fe6 S13 92.39(18) . . ? C63 Fe6 S12 92.44(19) . . ? C59 Fe6 S12 97.8(2) . . ? C60 Fe6 S12 133.8(2) . . ? C61 Fe6 S12 156.76(19) . . ? C62 Fe6 S12 121.6(2) . . ? S13 Fe6 S12 98.49(7) . . ? C63 Fe6 S11 137.6(2) . . ? C59 Fe6 S11 98.9(2) . . ? C60 Fe6 S11 90.84(17) . . ? C61 Fe6 S11 117.13(18) . . ? C62 Fe6 S11 154.07(18) . . ? S13 Fe6 S11 99.11(7) . . ? S12 Fe6 S11 79.77(6) . . ? C73 Fe7 C77 40.5(3) . . ? C73 Fe7 C76 65.3(3) . . ? C77 Fe7 C76 38.5(3) . . ? C73 Fe7 C74 38.7(2) . . ? C77 Fe7 C74 65.7(3) . . ? C76 Fe7 C74 63.9(2) . . ? C73 Fe7 C75 65.1(2) . . ? C77 Fe7 C75 65.6(3) . . ? C76 Fe7 C75 38.7(2) . . ? C74 Fe7 C75 37.9(2) . . ? C73 Fe7 S18 157.21(19) . . ? C77 Fe7 S18 125.9(3) . . ? C76 Fe7 S18 93.8(2) . . ? C74 Fe7 S18 125.1(2) . . ? C75 Fe7 S18 93.06(17) . . ? C73 Fe7 S17 99.9(2) . . ? C77 Fe7 S17 90.7(2) . . ? C76 Fe7 S17 118.9(2) . . ? C74 Fe7 S17 136.5(2) . . ? C75 Fe7 S17 155.9(2) . . ? S18 Fe7 S17 98.31(7) . . ? C73 Fe7 S16 97.67(19) . . ? C77 Fe7 S16 135.0(3) . . ? C76 Fe7 S16 155.60(18) . . ? C74 Fe7 S16 91.80(18) . . ? C75 Fe7 S16 119.40(19) . . ? S18 Fe7 S16 99.01(7) . . ? S17 Fe7 S16 79.74(6) . . ? C83 Fe8 C87 39.2(2) . . ? C83 Fe8 C84 38.0(3) . . ? C87 Fe8 C84 65.2(2) . . ? C83 Fe8 C85 64.4(3) . . ? C87 Fe8 C85 66.1(3) . . ? C84 Fe8 C85 38.2(3) . . ? C83 Fe8 C86 64.2(3) . . ? C87 Fe8 C86 39.0(3) . . ? C84 Fe8 C86 64.1(3) . . ? C85 Fe8 C86 39.1(3) . . ? C83 Fe8 S19 119.6(2) . . ? C87 Fe8 S19 155.14(19) . . ? C84 Fe8 S19 89.93(18) . . ? C85 Fe8 S19 94.3(2) . . ? C86 Fe8 S19 130.3(3) . . ? C83 Fe8 S17 142.5(2) . . ? C87 Fe8 S17 104.1(2) . . ? C84 Fe8 S17 152.6(3) . . ? C85 Fe8 S17 114.7(3) . . ? C86 Fe8 S17 91.41(19) . . ? S19 Fe8 S17 97.89(7) . . ? C83 Fe8 S16 94.7(2) . . ? C87 Fe8 S16 96.34(19) . . ? C84 Fe8 S16 125.0(3) . . ? C85 Fe8 S16 158.9(2) . . ? C86 Fe8 S16 130.9(3) . . ? S19 Fe8 S16 98.87(7) . . ? S17 Fe8 S16 79.87(6) . . ? C21 S1 Fe2 110.4(2) . . ? C21 S1 Fe1 109.9(2) . . ? Fe2 S1 Fe1 95.23(6) . . ? C22 S2 Fe1 110.2(2) . . ? C22 S2 Fe2 111.1(2) . . ? Fe1 S2 Fe2 95.99(7) . . ? C23 S3 Fe1 118.5(2) . . ? C23 S4 Fe2 119.8(2) . . ? C23 S5 C24 104.6(3) . . ? C46 S6 Fe4 110.4(2) . . ? C46 S6 Fe3 110.0(2) . . ? Fe4 S6 Fe3 95.12(6) . . ? C45 S7 Fe3 110.0(2) . . ? C45 S7 Fe4 111.0(2) . . ? Fe3 S7 Fe4 95.91(7) . . ? C47 S8 Fe3 118.4(2) . . ? C47 S9 Fe4 120.3(2) . . ? C47 S10 C48 104.4(3) . . ? C69 S11 Fe5 110.3(2) . . ? C69 S11 Fe6 110.1(2) . . ? Fe5 S11 Fe6 95.11(6) . . ? C70 S12 Fe6 110.0(2) . . ? C70 S12 Fe5 111.1(2) . . ? Fe6 S12 Fe5 95.92(7) . . ? C71 S13 Fe6 118.5(2) . . ? C71 S14 Fe5 120.0(2) . . ? C71 S15 C72 104.2(3) . . ? C93 S16 Fe8 110.7(2) . . ? C93 S16 Fe7 110.0(2) . . ? Fe8 S16 Fe7 95.22(6) . . ? C94 S17 Fe7 110.1(2) . . ? C94 S17 Fe8 110.7(2) . . ? Fe7 S17 Fe8 96.03(7) . . ? C95 S18 Fe7 118.3(2) . . ? C95 S19 Fe8 119.8(2) . . ? C96 S20 C95 104.2(3) . . ? C2 C1 C5 105.8(6) . . ? C2 C1 C6 123.7(8) . . ? C5 C1 C6 130.3(8) . . ? C2 C1 Fe1 71.0(4) . . ? C5 C1 Fe1 68.8(4) . . ? C6 C1 Fe1 128.3(5) . . ? C1 C2 C3 110.1(6) . . ? C1 C2 C7 129.0(8) . . ? C3 C2 C7 120.8(8) . . ? C1 C2 Fe1 70.5(4) . . ? C3 C2 Fe1 71.4(4) . . ? C7 C2 Fe1 128.7(5) . . ? C4 C3 C2 107.5(6) . . ? C4 C3 C8 122.1(7) . . ? C2 C3 C8 130.3(6) . . ? C4 C3 Fe1 70.4(3) . . ? C2 C3 Fe1 70.0(4) . . ? C8 C3 Fe1 127.7(5) . . ? C3 C4 C5 108.8(6) . . ? C3 C4 C9 129.6(7) . . ? C5 C4 C9 121.4(7) . . ? C3 C4 Fe1 71.6(4) . . ? C5 C4 Fe1 69.0(3) . . ? C9 C4 Fe1 128.5(5) . . ? C4 C5 C1 107.8(6) . . ? C4 C5 C10 128.9(7) . . ? C1 C5 C10 123.1(7) . . ? C4 C5 Fe1 72.0(4) . . ? C1 C5 Fe1 71.0(4) . . ? C10 C5 Fe1 126.5(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 106.4(6) . . ? C12 C11 C16 123.3(9) . . ? C15 C11 C16 130.1(9) . . ? C12 C11 Fe2 71.2(4) . . ? C15 C11 Fe2 70.3(4) . . ? C16 C11 Fe2 127.0(5) . . ? C13 C12 C11 109.3(7) . . ? C13 C12 C17 121.2(9) . . ? C11 C12 C17 129.4(8) . . ? C13 C12 Fe2 70.7(4) . . ? C11 C12 Fe2 70.5(4) . . ? C17 C12 Fe2 127.8(5) . . ? C12 C13 C14 109.2(6) . . ? C12 C13 C18 131.2(8) . . ? C14 C13 C18 119.4(8) . . ? C12 C13 Fe2 71.4(4) . . ? C14 C13 Fe2 70.6(3) . . ? C18 C13 Fe2 127.8(5) . . ? C15 C14 C13 106.2(6) . . ? C15 C14 C19 122.8(8) . . ? C13 C14 C19 130.9(7) . . ? C15 C14 Fe2 70.6(4) . . ? C13 C14 Fe2 70.2(4) . . ? C19 C14 Fe2 126.5(4) . . ? C14 C15 C11 108.8(7) . . ? C14 C15 C20 130.4(9) . . ? C11 C15 C20 120.7(9) . . ? C14 C15 Fe2 70.8(4) . . ? C11 C15 Fe2 70.1(4) . . ? C20 C15 Fe2 127.2(5) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S1 C21 H21A 109.5 . . ? S1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S4 C23 S3 129.3(4) . . ? S4 C23 S5 119.3(4) . . ? S3 C23 S5 111.4(3) . . ? S5 C24 H24A 109.5 . . ? S5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C29 108.9(6) . . ? C26 C25 C30 130.5(7) . . ? C29 C25 C30 120.4(7) . . ? C26 C25 Fe3 72.4(4) . . ? C29 C25 Fe3 69.4(3) . . ? C30 C25 Fe3 126.8(5) . . ? C25 C26 C27 107.0(6) . . ? C25 C26 C31 123.6(7) . . ? C27 C26 C31 129.2(7) . . ? C25 C26 Fe3 69.4(3) . . ? C27 C26 Fe3 70.6(4) . . ? C31 C26 Fe3 129.0(5) . . ? C28 C27 C26 109.4(6) . . ? C28 C27 C32 129.6(7) . . ? C26 C27 C32 120.9(7) . . ? C28 C27 Fe3 70.4(4) . . ? C26 C27 Fe3 70.9(4) . . ? C32 C27 Fe3 127.6(5) . . ? C27 C28 C29 108.8(6) . . ? C27 C28 C33 122.3(7) . . ? C29 C28 C33 128.7(7) . . ? C27 C28 Fe3 71.6(4) . . ? C29 C28 Fe3 69.2(4) . . ? C33 C28 Fe3 129.7(5) . . ? C28 C29 C25 105.9(6) . . ? C28 C29 C34 121.9(7) . . ? C25 C29 C34 131.8(8) . . ? C28 C29 Fe3 71.7(4) . . ? C25 C29 Fe3 70.4(4) . . ? C34 C29 Fe3 127.3(5) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C39 C35 C36 107.3(6) . . ? C39 C35 C40 130.5(8) . . ? C36 C35 C40 122.0(8) . . ? C39 C35 Fe4 70.4(4) . . ? C36 C35 Fe4 69.6(4) . . ? C40 C35 Fe4 128.2(5) . . ? C35 C36 C37 109.7(6) . . ? C35 C36 C41 130.6(8) . . ? C37 C36 C41 119.5(8) . . ? C35 C36 Fe4 72.0(4) . . ? C37 C36 Fe4 71.5(4) . . ? C41 C36 Fe4 126.3(5) . . ? C38 C37 C36 104.8(6) . . ? C38 C37 C42 122.2(9) . . ? C36 C37 C42 133.0(9) . . ? C38 C37 Fe4 69.0(4) . . ? C36 C37 Fe4 68.8(4) . . ? C42 C37 Fe4 127.8(5) . . ? C39 C38 C37 108.9(6) . . ? C39 C38 C43 119.9(8) . . ? C37 C38 C43 131.0(8) . . ? C39 C38 Fe4 71.4(4) . . ? C37 C38 Fe4 71.9(4) . . ? C43 C38 Fe4 126.4(5) . . ? C35 C39 C38 109.3(6) . . ? C35 C39 C44 120.9(8) . . ? C38 C39 C44 129.7(8) . . ? C35 C39 Fe4 71.4(4) . . ? C38 C39 Fe4 69.9(4) . . ? C44 C39 Fe4 127.4(5) . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? S7 C45 H45A 109.5 . . ? S7 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S7 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? S6 C46 H46A 109.5 . . ? S6 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? S6 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? S9 C47 S8 129.0(3) . . ? S9 C47 S10 119.9(4) . . ? S8 C47 S10 111.1(3) . . ? S10 C48 H48A 109.5 . . ? S10 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? S10 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C53 105.8(6) . . ? C50 C49 C54 120.5(9) . . ? C53 C49 C54 133.6(9) . . ? C50 C49 Fe5 69.2(4) . . ? C53 C49 Fe5 69.6(4) . . ? C54 C49 Fe5 128.0(5) . . ? C51 C50 C49 108.2(6) . . ? C51 C50 C55 119.5(8) . . ? C49 C50 C55 132.2(8) . . ? C51 C50 Fe5 70.7(4) . . ? C49 C50 Fe5 71.9(4) . . ? C55 C50 Fe5 126.6(5) . . ? C52 C51 C50 109.5(6) . . ? C52 C51 C56 119.6(8) . . ? C50 C51 C56 130.7(8) . . ? C52 C51 Fe5 71.4(4) . . ? C50 C51 Fe5 70.8(4) . . ? C56 C51 Fe5 127.3(5) . . ? C51 C52 C53 107.7(6) . . ? C51 C52 C57 131.5(8) . . ? C53 C52 C57 120.7(8) . . ? C51 C52 Fe5 70.3(4) . . ? C53 C52 Fe5 70.9(4) . . ? C57 C52 Fe5 127.8(5) . . ? C52 C53 C49 108.9(6) . . ? C52 C53 C58 131.0(8) . . ? C49 C53 C58 120.1(8) . . ? C52 C53 Fe5 70.8(4) . . ? C49 C53 Fe5 71.2(4) . . ? C58 C53 Fe5 125.9(5) . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C53 C58 H58A 109.5 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 C63 105.1(6) . . ? C60 C59 C64 122.9(7) . . ? C63 C59 C64 131.7(7) . . ? C60 C59 Fe6 71.8(4) . . ? C63 C59 Fe6 69.6(4) . . ? C64 C59 Fe6 127.4(5) . . ? C61 C60 C59 110.0(6) . . ? C61 C60 C65 122.2(7) . . ? C59 C60 C65 127.6(7) . . ? C61 C60 Fe6 71.9(3) . . ? C59 C60 Fe6 69.4(4) . . ? C65 C60 Fe6 129.0(5) . . ? C60 C61 C62 108.0(6) . . ? C60 C61 C66 129.9(7) . . ? C62 C61 C66 121.9(7) . . ? C60 C61 Fe6 70.1(4) . . ? C62 C61 Fe6 71.0(3) . . ? C66 C61 Fe6 127.7(5) . . ? C63 C62 C61 107.8(6) . . ? C63 C62 C67 124.4(7) . . ? C61 C62 C67 127.7(7) . . ? C63 C62 Fe6 68.6(4) . . ? C61 C62 Fe6 70.8(4) . . ? C67 C62 Fe6 128.2(5) . . ? C62 C63 C59 109.0(6) . . ? C62 C63 C68 129.4(8) . . ? C59 C63 C68 121.2(8) . . ? C62 C63 Fe6 73.3(4) . . ? C59 C63 Fe6 69.9(4) . . ? C68 C63 Fe6 127.8(5) . . ? C59 C64 H64A 109.5 . . ? C59 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C59 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C60 C65 H65A 109.5 . . ? C60 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C60 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C63 C68 H68A 109.5 . . ? C63 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C63 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? S11 C69 H69A 109.5 . . ? S11 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? S11 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? S12 C70 H70A 109.5 . . ? S12 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? S12 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? S14 C71 S13 129.2(4) . . ? S14 C71 S15 119.5(4) . . ? S13 C71 S15 111.3(3) . . ? S15 C72 H72A 109.5 . . ? S15 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? S15 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C77 107.3(6) . . ? C74 C73 C78 130.2(7) . . ? C77 C73 C78 122.2(7) . . ? C74 C73 Fe7 72.0(4) . . ? C77 C73 Fe7 70.5(4) . . ? C78 C73 Fe7 126.8(5) . . ? C75 C74 C73 109.8(6) . . ? C75 C74 C79 129.5(7) . . ? C73 C74 C79 120.6(7) . . ? C75 C74 Fe7 71.5(4) . . ? C73 C74 Fe7 69.3(3) . . ? C79 C74 Fe7 128.7(5) . . ? C74 C75 C76 107.1(6) . . ? C74 C75 C80 121.8(7) . . ? C76 C75 C80 130.9(7) . . ? C74 C75 Fe7 70.6(4) . . ? C76 C75 Fe7 70.1(4) . . ? C80 C75 Fe7 128.7(5) . . ? C77 C76 C75 110.1(6) . . ? C77 C76 C81 129.4(8) . . ? C75 C76 C81 120.4(8) . . ? C77 C76 Fe7 70.3(4) . . ? C75 C76 Fe7 71.2(4) . . ? C81 C76 Fe7 128.3(5) . . ? C76 C77 C73 105.6(6) . . ? C76 C77 C82 123.7(8) . . ? C73 C77 C82 130.5(8) . . ? C76 C77 Fe7 71.2(4) . . ? C73 C77 Fe7 69.0(4) . . ? C82 C77 Fe7 127.8(5) . . ? C73 C78 H78A 109.5 . . ? C73 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C73 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C74 C79 H79A 109.5 . . ? C74 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C74 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C75 C80 H80A 109.5 . . ? C75 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C75 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C76 C81 H81A 109.5 . . ? C76 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C76 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C77 C82 H82A 109.5 . . ? C77 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C77 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 C87 109.7(6) . . ? C84 C83 C88 130.9(7) . . ? C87 C83 C88 119.3(7) . . ? C84 C83 Fe8 71.4(4) . . ? C87 C83 Fe8 70.7(3) . . ? C88 C83 Fe8 127.5(5) . . ? C83 C84 C85 109.2(6) . . ? C83 C84 C89 120.3(8) . . ? C85 C84 C89 130.3(8) . . ? C83 C84 Fe8 70.6(3) . . ? C85 C84 Fe8 71.0(4) . . ? C89 C84 Fe8 127.8(5) . . ? C84 C85 C86 106.7(6) . . ? C84 C85 C90 123.1(9) . . ? C86 C85 C90 130.0(9) . . ? C84 C85 Fe8 70.9(4) . . ? C86 C85 Fe8 70.5(4) . . ? C90 C85 Fe8 127.1(5) . . ? C87 C86 C85 109.3(6) . . ? C87 C86 C91 128.4(8) . . ? C85 C86 C91 122.3(9) . . ? C87 C86 Fe8 70.3(4) . . ? C85 C86 Fe8 70.4(4) . . ? C91 C86 Fe8 127.1(5) . . ? C86 C87 C83 105.1(6) . . ? C86 C87 C92 124.1(8) . . ? C83 C87 C92 130.6(8) . . ? C86 C87 Fe8 70.7(4) . . ? C83 C87 Fe8 70.1(4) . . ? C92 C87 Fe8 127.0(5) . . ? C83 C88 H88A 109.5 . . ? C83 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C83 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C84 C89 H89A 109.5 . . ? C84 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C84 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C85 C90 H90A 109.5 . . ? C85 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C85 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C86 C91 H91A 109.5 . . ? C86 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C86 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C87 C92 H92A 109.5 . . ? C87 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C87 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? S16 C93 H93A 109.5 . . ? S16 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? S16 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? S17 C94 H94A 109.5 . . ? S17 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? S17 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? S19 C95 S18 129.6(3) . . ? S19 C95 S20 119.5(4) . . ? S18 C95 S20 111.0(3) . . ? S20 C96 H96A 109.5 . . ? S20 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? S20 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.612 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.055 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 749170' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Fe N S3' _chemical_formula_weight 448.49 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5932(15) _cell_length_b 15.484(2) _cell_length_c 15.385(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.014(12) _cell_angle_gamma 90.00 _cell_volume 2285.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2314 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 21.8 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12379 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4027 _reflns_number_gt 3114 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4027 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.71347(10) 0.34039(4) 0.83882(5) 0.0449(2) Uani 1 1 d . . . S1 S 1.5773(2) 0.43249(11) 0.58686(10) 0.0635(5) Uani 1 1 d . . . S2 S 1.76175(19) 0.46833(9) 0.89186(9) 0.0583(5) Uani 1 1 d . . . S3 S 1.80986(17) 0.35594(9) 0.70095(10) 0.0543(4) Uani 1 1 d . . . C12 C 1.3829(7) 0.4369(4) 0.8441(4) 0.0573(16) Uani 1 1 d . . . H12A H 1.4488 0.4526 0.8855 0.069 Uiso 1 1 calc R . . C2 C 1.6557(9) 0.2827(4) 0.9594(4) 0.064(2) Uani 1 1 d . . . C3 C 1.7963(9) 0.2821(4) 0.9491(4) 0.0610(17) Uani 1 1 d . . . C1 C 1.5975(8) 0.2346(5) 0.8919(6) 0.079(2) Uani 1 1 d . . . C5 C 1.7004(12) 0.2045(3) 0.8376(4) 0.079(2) Uani 1 1 d . . . C4 C 1.8294(9) 0.2329(5) 0.8743(6) 0.079(2) Uani 1 1 d . . . C19 C 1.6418(6) 0.3894(4) 0.6848(3) 0.0465(14) Uani 1 1 d . . . C11 C 1.4251(7) 0.3996(3) 0.7674(4) 0.0474(14) Uani 1 1 d . . . C14 C 1.1468(8) 0.4314(5) 0.7987(6) 0.077(2) Uani 1 1 d . . . H14A H 1.0530 0.4430 0.8083 0.092 Uiso 1 1 calc R . . C13 C 1.2415(8) 0.4513(4) 0.8599(5) 0.0665(18) Uani 1 1 d . . . H13A H 1.2129 0.4745 0.9127 0.080 Uiso 1 1 calc R . . C15 C 1.1882(8) 0.3941(5) 0.7219(5) 0.076(2) Uani 1 1 d . . . H15A H 1.1220 0.3793 0.6804 0.091 Uiso 1 1 calc R . . C16 C 1.3265(7) 0.3787(4) 0.7061(4) 0.0599(16) Uani 1 1 d . . . H16A H 1.3537 0.3539 0.6537 0.072 Uiso 1 1 calc R . . C7 C 1.5758(14) 0.3263(6) 1.0338(6) 0.137(4) Uani 1 1 d . . . H7A H 1.5635 0.2858 1.0805 0.205 Uiso 1 1 calc R . . H7B H 1.4862 0.3449 1.0132 0.205 Uiso 1 1 calc R . . H7C H 1.6275 0.3753 1.0543 0.205 Uiso 1 1 calc R . . C6 C 1.4422(10) 0.2166(6) 0.8827(9) 0.176(7) Uani 1 1 d . . . H6A H 1.4192 0.1645 0.9134 0.264 Uiso 1 1 calc R . . H6B H 1.4192 0.2100 0.8224 0.264 Uiso 1 1 calc R . . H6C H 1.3902 0.2639 0.9067 0.264 Uiso 1 1 calc R . . C8 C 1.8963(12) 0.3203(6) 1.0140(6) 0.133(5) Uani 1 1 d . . . H8A H 1.9165 0.2785 1.0583 0.199 Uiso 1 1 calc R . . H8B H 1.8551 0.3705 1.0401 0.199 Uiso 1 1 calc R . . H8C H 1.9811 0.3364 0.9850 0.199 Uiso 1 1 calc R . . C9 C 1.9746(12) 0.2126(8) 0.8474(9) 0.186(7) Uani 1 1 d . . . H9A H 2.0029 0.1589 0.8732 0.279 Uiso 1 1 calc R . . H9B H 2.0358 0.2578 0.8664 0.279 Uiso 1 1 calc R . . H9C H 1.9789 0.2078 0.7853 0.279 Uiso 1 1 calc R . . C10 C 1.684(2) 0.1461(4) 0.7631(5) 0.178(8) Uani 1 1 d . . . H10A H 1.6811 0.0874 0.7834 0.267 Uiso 1 1 calc R . . H10B H 1.7606 0.1533 0.7240 0.267 Uiso 1 1 calc R . . H10C H 1.5982 0.1592 0.7335 0.267 Uiso 1 1 calc R . . C17 C 1.7360(9) 0.5526(3) 0.8124(4) 0.075(2) Uani 1 1 d . . . H17A H 1.7854 0.5378 0.7595 0.090 Uiso 1 1 calc R . . H17B H 1.6375 0.5568 0.7985 0.090 Uiso 1 1 calc R . . C18 C 1.7860(9) 0.6375(4) 0.8442(5) 0.087(2) Uani 1 1 d . . . H18A H 1.7706 0.6805 0.8003 0.131 Uiso 1 1 calc R . . H18B H 1.8838 0.6339 0.8569 0.131 Uiso 1 1 calc R . . H18C H 1.7360 0.6529 0.8959 0.131 Uiso 1 1 calc R . . C21 C 1.8041(9) 0.5282(5) 0.5347(5) 0.095(3) Uani 1 1 d . . . H21A H 1.8853 0.5311 0.4983 0.143 Uiso 1 1 calc R . . H21B H 1.8314 0.5333 0.5945 0.143 Uiso 1 1 calc R . . H21D H 1.7418 0.5745 0.5200 0.143 Uiso 1 1 calc R . . C20 C 1.7338(8) 0.4458(4) 0.5212(4) 0.0651(18) Uani 1 1 d . . . H20A H 1.7982 0.3994 0.5347 0.078 Uiso 1 1 calc R . . H20B H 1.7088 0.4406 0.4603 0.078 Uiso 1 1 calc R . . N1 N 1.5680(5) 0.3797(3) 0.7556(3) 0.0461(11) Uani 1 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 Fe1 0.0565(5) 0.0398(4) 0.0384(4) 0.0020(3) -0.0065(4) 0.0005(4) S1 0.0638(11) 0.0780(11) 0.0486(8) 0.0149(8) -0.0090(8) 0.0032(9) S2 0.0799(12) 0.0456(7) 0.0496(8) -0.0029(6) -0.0138(9) -0.0053(8) S3 0.0519(10) 0.0607(9) 0.0504(8) 0.0020(6) -0.0033(8) 0.0099(8) C12 0.065(4) 0.052(3) 0.055(4) -0.002(3) -0.002(4) -0.005(3) C2 0.106(7) 0.046(4) 0.040(3) 0.006(3) -0.002(4) 0.003(4) C3 0.065(5) 0.060(4) 0.059(4) 0.021(3) -0.017(4) -0.008(4) C1 0.086(5) 0.062(5) 0.087(6) 0.037(4) -0.028(5) -0.023(4) C5 0.154(8) 0.038(3) 0.046(3) 0.004(3) 0.001(5) 0.006(5) C4 0.080(6) 0.069(5) 0.089(6) 0.042(4) 0.029(4) 0.033(4) C19 0.048(4) 0.051(3) 0.041(3) -0.011(2) -0.008(3) -0.004(3) C11 0.046(4) 0.045(3) 0.051(3) 0.006(3) -0.002(3) -0.003(3) C14 0.040(4) 0.082(5) 0.109(6) 0.001(4) 0.007(5) 0.004(4) C13 0.060(5) 0.061(4) 0.078(4) -0.005(3) 0.018(4) 0.008(3) C15 0.046(4) 0.091(5) 0.092(5) 0.004(5) -0.013(4) -0.009(4) C16 0.054(4) 0.068(4) 0.057(3) -0.002(3) 0.002(3) -0.011(3) C7 0.212(13) 0.113(7) 0.086(6) 0.023(6) 0.059(8) 0.030(8) C6 0.118(8) 0.125(8) 0.285(17) 0.118(10) -0.103(10) -0.076(7) C8 0.178(11) 0.096(6) 0.125(8) 0.060(6) -0.095(8) -0.047(7) C9 0.148(9) 0.166(11) 0.245(15) 0.119(11) 0.083(11) 0.101(9) C10 0.41(2) 0.054(4) 0.068(5) -0.007(4) -0.032(10) -0.038(8) C17 0.104(6) 0.048(3) 0.073(4) 0.007(3) -0.025(4) -0.004(4) C18 0.112(6) 0.048(3) 0.102(5) -0.004(3) 0.012(6) -0.009(4) C21 0.093(6) 0.088(5) 0.105(6) -0.006(4) 0.021(5) -0.010(5) C20 0.088(5) 0.060(3) 0.047(3) 0.004(3) 0.012(4) 0.006(4) N1 0.051(3) 0.043(2) 0.044(3) 0.003(2) -0.004(2) -0.005(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 Fe1 N1 1.989(5) . ? Fe1 C4 2.074(6) . ? Fe1 C3 2.079(6) . ? Fe1 C5 2.108(6) . ? Fe1 C2 2.131(6) . ? Fe1 C1 2.141(7) . ? Fe1 S2 2.1920(15) . ? Fe1 S3 2.3266(19) . ? S1 C19 1.760(5) . ? S1 C20 1.821(7) . ? S2 C17 1.806(6) . ? S3 C19 1.711(6) . ? C12 C11 1.375(9) . ? C12 C13 1.396(10) . ? C12 H12A 0.9300 . ? C2 C3 1.358(9) . ? C2 C1 1.394(10) . ? C2 C7 1.534(11) . ? C3 C4 1.415(10) . ? C3 C8 1.506(10) . ? C1 C5 1.375(11) . ? C1 C6 1.523(11) . ? C5 C4 1.430(11) . ? C5 C10 1.469(10) . ? C4 C9 1.487(12) . ? C19 N1 1.309(7) . ? C11 C16 1.374(8) . ? C11 N1 1.417(8) . ? C14 C13 1.344(10) . ? C14 C15 1.374(11) . ? C14 H14A 0.9300 . ? C13 H13A 0.9300 . ? C15 C16 1.369(10) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C17 C18 1.482(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 C20 1.458(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21D 0.9600 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 C4 142.3(3) . . ? N1 Fe1 C3 157.8(3) . . ? C4 Fe1 C3 39.8(3) . . ? N1 Fe1 C5 104.9(3) . . ? C4 Fe1 C5 40.0(3) . . ? C3 Fe1 C5 66.2(3) . . ? N1 Fe1 C2 120.4(3) . . ? C4 Fe1 C2 64.8(3) . . ? C3 Fe1 C2 37.6(3) . . ? C5 Fe1 C2 64.8(3) . . ? N1 Fe1 C1 96.6(2) . . ? C4 Fe1 C1 64.2(3) . . ? C3 Fe1 C1 63.6(3) . . ? C5 Fe1 C1 37.7(3) . . ? C2 Fe1 C1 38.1(3) . . ? N1 Fe1 S2 96.39(13) . . ? C4 Fe1 S2 120.9(3) . . ? C3 Fe1 S2 90.46(19) . . ? C5 Fe1 S2 156.7(2) . . ? C2 Fe1 S2 96.29(18) . . ? C1 Fe1 S2 131.2(3) . . ? N1 Fe1 S3 70.16(15) . . ? C4 Fe1 S3 96.3(2) . . ? C3 Fe1 S3 129.6(2) . . ? C5 Fe1 S3 96.8(2) . . ? C2 Fe1 S3 160.04(18) . . ? C1 Fe1 S3 129.3(3) . . ? S2 Fe1 S3 99.32(6) . . ? C19 S1 C20 103.2(3) . . ? C17 S2 Fe1 111.9(2) . . ? C19 S3 Fe1 77.8(2) . . ? C11 C12 C13 120.2(6) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C3 C2 C1 107.9(7) . . ? C3 C2 C7 125.9(8) . . ? C1 C2 C7 126.2(9) . . ? C3 C2 Fe1 69.1(4) . . ? C1 C2 Fe1 71.3(4) . . ? C7 C2 Fe1 126.5(5) . . ? C2 C3 C4 108.8(7) . . ? C2 C3 C8 123.5(8) . . ? C4 C3 C8 127.4(9) . . ? C2 C3 Fe1 73.3(4) . . ? C4 C3 Fe1 69.9(4) . . ? C8 C3 Fe1 127.8(5) . . ? C5 C1 C2 110.3(7) . . ? C5 C1 C6 125.8(10) . . ? C2 C1 C6 123.9(10) . . ? C5 C1 Fe1 69.8(4) . . ? C2 C1 Fe1 70.6(4) . . ? C6 C1 Fe1 127.8(5) . . ? C1 C5 C4 106.1(6) . . ? C1 C5 C10 127.2(11) . . ? C4 C5 C10 126.4(11) . . ? C1 C5 Fe1 72.5(4) . . ? C4 C5 Fe1 68.8(4) . . ? C10 C5 Fe1 129.0(5) . . ? C3 C4 C5 107.0(7) . . ? C3 C4 C9 123.4(11) . . ? C5 C4 C9 129.4(10) . . ? C3 C4 Fe1 70.3(4) . . ? C5 C4 Fe1 71.3(4) . . ? C9 C4 Fe1 126.8(6) . . ? N1 C19 S3 110.7(4) . . ? N1 C19 S1 124.5(4) . . ? S3 C19 S1 124.7(3) . . ? C16 C11 C12 119.1(6) . . ? C16 C11 N1 121.8(6) . . ? C12 C11 N1 119.0(6) . . ? C13 C14 C15 120.2(7) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C14 C13 C12 119.8(6) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C16 C15 C14 120.4(7) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C11 120.2(7) . . ? C15 C16 H16A 119.9 . . ? C11 C16 H16A 119.9 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C18 C17 S2 111.9(5) . . ? C18 C17 H17A 109.2 . . ? S2 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? S2 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21D 109.5 . . ? H21A C21 H21D 109.5 . . ? H21B C21 H21D 109.5 . . ? C21 C20 S1 113.7(5) . . ? C21 C20 H20A 108.8 . . ? S1 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? S1 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C19 N1 C11 127.2(5) . . ? C19 N1 Fe1 101.0(4) . . ? C11 N1 Fe1 131.6(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.580 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.075 # Attachment '6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 749171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H25 Fe N0 S4' _chemical_formula_weight 389.44 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4688(8) _cell_length_b 22.6674(18) _cell_length_c 9.6535(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.944(5) _cell_angle_gamma 90.00 _cell_volume 1830.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1392 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 24.8 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.269 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7382 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0991 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.24 _reflns_number_total 3317 _reflns_number_gt 1998 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3317 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.82385(9) 0.09798(3) 0.71921(9) 0.0276(2) Uani 1 1 d . . . S1 S 0.88325(17) 0.13623(6) 0.94860(16) 0.0347(4) Uani 1 1 d . . . S2 S 1.07537(16) 0.09445(6) 0.74197(16) 0.0317(3) Uani 1 1 d . . . S3 S 0.84618(17) 0.18127(5) 0.59964(16) 0.0325(4) Uani 1 1 d . . . S4 S 1.17070(18) 0.19650(6) 0.60813(18) 0.0390(4) Uani 1 1 d . . . C1 C 0.5865(6) 0.0834(2) 0.5489(6) 0.0278(12) Uani 1 1 d . . . C2 C 0.6040(6) 0.0655(2) 0.6948(6) 0.0284(12) Uani 1 1 d . . . C3 C 0.7191(6) 0.0185(2) 0.7515(6) 0.0296(13) Uani 1 1 d . . . C4 C 0.7716(6) 0.0085(2) 0.6383(6) 0.0318(13) Uani 1 1 d . . . C5 C 0.6926(6) 0.0491(2) 0.5123(6) 0.0281(12) Uani 1 1 d . . . C6 C 0.4723(6) 0.1297(2) 0.4443(6) 0.0381(14) Uani 1 1 d . . . H6A H 0.3712 0.1117 0.3768 0.057 Uiso 1 1 calc R . . H6B H 0.5151 0.1476 0.3818 0.057 Uiso 1 1 calc R . . H6C H 0.4576 0.1593 0.5075 0.057 Uiso 1 1 calc R . . C7 C 0.5152(7) 0.0884(2) 0.7767(7) 0.0411(15) Uani 1 1 d . . . H7A H 0.4189 0.0659 0.7450 0.062 Uiso 1 1 calc R . . H7B H 0.4885 0.1291 0.7498 0.062 Uiso 1 1 calc R . . H7C H 0.5809 0.0848 0.8880 0.062 Uiso 1 1 calc R . . C8 C 0.7691(7) -0.0145(2) 0.9027(6) 0.0375(14) Uani 1 1 d . . . H8A H 0.7020 -0.0485 0.8836 0.056 Uiso 1 1 calc R . . H8B H 0.7588 0.0108 0.9772 0.056 Uiso 1 1 calc R . . H8C H 0.8783 -0.0269 0.9438 0.056 Uiso 1 1 calc R . . C9 C 0.8901(7) -0.0376(2) 0.6466(7) 0.0379(14) Uani 1 1 d . . . H9A H 0.8350 -0.0738 0.6022 0.057 Uiso 1 1 calc R . . H9B H 0.9674 -0.0439 0.7541 0.057 Uiso 1 1 calc R . . H9C H 0.9435 -0.0242 0.5888 0.057 Uiso 1 1 calc R . . C10 C 0.7080(7) 0.0523(2) 0.3666(6) 0.0413(15) Uani 1 1 d . . . H10A H 0.6340 0.0253 0.2906 0.062 Uiso 1 1 calc R . . H10B H 0.8150 0.0419 0.3894 0.062 Uiso 1 1 calc R . . H10C H 0.6849 0.0917 0.3255 0.062 Uiso 1 1 calc R . . C11 C 1.0544(7) 0.1860(3) 1.0185(7) 0.0462(16) Uani 1 1 d . . . H11A H 1.1494 0.1640 1.0365 0.055 Uiso 1 1 calc R . . H11B H 1.0357 0.2159 0.9398 0.055 Uiso 1 1 calc R . . C12 C 1.0792(7) 0.2149(3) 1.1683(7) 0.0477(16) Uani 1 1 d . . . H12A H 1.1694 0.2410 1.2048 0.072 Uiso 1 1 calc R . . H12B H 1.0988 0.1852 1.2462 0.072 Uiso 1 1 calc R . . H12C H 0.9854 0.2369 1.1498 0.072 Uiso 1 1 calc R . . C13 C 1.0313(6) 0.1601(2) 0.6456(6) 0.0285(13) Uani 1 1 d . . . C14 C 1.0660(7) 0.2627(2) 0.5083(6) 0.0405(15) Uani 1 1 d . . . H14A H 1.1175 0.2787 0.4501 0.049 Uiso 1 1 calc R . . H14B H 0.9574 0.2522 0.4331 0.049 Uiso 1 1 calc R . . C15 C 1.0602(9) 0.3098(2) 0.6149(8) 0.061(2) Uani 1 1 d . . . H15A H 1.0030 0.3434 0.5537 0.091 Uiso 1 1 calc R . . H15B H 1.1671 0.3214 0.6881 0.091 Uiso 1 1 calc R . . H15C H 1.0068 0.2949 0.6711 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0283(4) 0.0234(4) 0.0332(4) 0.0008(3) 0.0163(3) -0.0001(3) S1 0.0378(9) 0.0349(7) 0.0363(8) -0.0049(6) 0.0213(7) -0.0054(6) S2 0.0310(8) 0.0289(7) 0.0377(8) 0.0036(6) 0.0182(6) 0.0036(6) S3 0.0322(8) 0.0266(7) 0.0406(8) 0.0042(6) 0.0187(7) 0.0018(6) S4 0.0376(9) 0.0361(8) 0.0508(9) 0.0067(7) 0.0271(7) -0.0019(7) C1 0.022(3) 0.020(3) 0.041(3) 0.000(2) 0.014(2) 0.002(2) C2 0.027(3) 0.025(3) 0.038(3) -0.003(2) 0.019(3) -0.004(2) C3 0.032(3) 0.024(3) 0.033(3) 0.001(2) 0.016(3) -0.006(2) C4 0.038(3) 0.020(3) 0.037(3) -0.004(2) 0.018(3) -0.004(2) C5 0.028(3) 0.021(3) 0.034(3) -0.002(2) 0.014(2) -0.004(2) C6 0.034(4) 0.038(3) 0.043(3) 0.002(3) 0.019(3) 0.001(3) C7 0.038(4) 0.036(3) 0.057(4) -0.004(3) 0.028(3) -0.001(3) C8 0.043(4) 0.032(3) 0.040(3) 0.001(3) 0.021(3) 0.002(3) C9 0.037(3) 0.023(3) 0.052(4) 0.001(3) 0.020(3) 0.001(2) C10 0.047(4) 0.039(3) 0.041(3) 0.000(3) 0.023(3) -0.001(3) C11 0.048(4) 0.047(4) 0.046(4) -0.011(3) 0.024(3) -0.015(3) C12 0.052(4) 0.047(4) 0.043(4) -0.010(3) 0.022(3) -0.016(3) C13 0.037(3) 0.030(3) 0.025(3) -0.002(2) 0.019(3) -0.006(2) C14 0.056(4) 0.036(3) 0.035(3) 0.003(3) 0.026(3) -0.008(3) C15 0.107(6) 0.030(3) 0.066(4) -0.006(3) 0.058(4) -0.003(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 Fe1 C1 2.097(5) . ? Fe1 C5 2.106(5) . ? Fe1 C2 2.114(5) . ? Fe1 C4 2.147(5) . ? Fe1 C3 2.149(5) . ? Fe1 S1 2.1919(16) . ? Fe1 S3 2.2738(15) . ? Fe1 S2 2.2883(16) . ? S1 C11 1.824(6) . ? S2 C13 1.699(5) . ? S3 C13 1.665(5) . ? S4 C13 1.733(5) . ? S4 C14 1.807(5) . ? C1 C2 1.399(7) . ? C1 C5 1.440(7) . ? C1 C6 1.506(7) . ? C2 C3 1.437(7) . ? C2 C7 1.492(7) . ? C3 C4 1.415(7) . ? C3 C8 1.506(7) . ? C4 C5 1.426(7) . ? C4 C9 1.506(7) . ? C5 C10 1.482(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.503(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C14 C15 1.503(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Fe1 C5 40.07(19) . . ? C1 Fe1 C2 38.81(19) . . ? C5 Fe1 C2 66.3(2) . . ? C1 Fe1 C4 65.60(19) . . ? C5 Fe1 C4 39.17(18) . . ? C2 Fe1 C4 65.4(2) . . ? C1 Fe1 C3 65.44(19) . . ? C5 Fe1 C3 65.7(2) . . ? C2 Fe1 C3 39.39(19) . . ? C4 Fe1 C3 38.5(2) . . ? C1 Fe1 S1 121.84(16) . . ? C5 Fe1 S1 157.57(16) . . ? C2 Fe1 S1 91.35(15) . . ? C4 Fe1 S1 130.37(15) . . ? C3 Fe1 S1 95.88(15) . . ? C1 Fe1 S3 93.03(14) . . ? C5 Fe1 S3 96.28(14) . . ? C2 Fe1 S3 123.60(14) . . ? C4 Fe1 S3 131.33(16) . . ? C3 Fe1 S3 158.28(14) . . ? S1 Fe1 S3 98.25(6) . . ? C1 Fe1 S2 138.97(16) . . ? C5 Fe1 S2 101.39(15) . . ? C2 Fe1 S2 157.59(14) . . ? C4 Fe1 S2 93.08(16) . . ? C3 Fe1 S2 119.14(15) . . ? S1 Fe1 S2 98.86(6) . . ? S3 Fe1 S2 74.79(5) . . ? C11 S1 Fe1 112.4(2) . . ? C13 S2 Fe1 86.52(19) . . ? C13 S3 Fe1 87.80(18) . . ? C13 S4 C14 103.1(3) . . ? C2 C1 C5 108.8(4) . . ? C2 C1 C6 125.9(5) . . ? C5 C1 C6 125.2(5) . . ? C2 C1 Fe1 71.3(3) . . ? C5 C1 Fe1 70.3(3) . . ? C6 C1 Fe1 125.8(3) . . ? C1 C2 C3 108.1(5) . . ? C1 C2 C7 127.0(5) . . ? C3 C2 C7 124.8(5) . . ? C1 C2 Fe1 69.9(3) . . ? C3 C2 Fe1 71.6(3) . . ? C7 C2 Fe1 126.2(4) . . ? C4 C3 C2 107.6(4) . . ? C4 C3 C8 127.2(5) . . ? C2 C3 C8 125.1(5) . . ? C4 C3 Fe1 70.7(3) . . ? C2 C3 Fe1 69.0(3) . . ? C8 C3 Fe1 126.9(3) . . ? C3 C4 C5 108.8(5) . . ? C3 C4 C9 126.3(5) . . ? C5 C4 C9 124.9(5) . . ? C3 C4 Fe1 70.8(3) . . ? C5 C4 Fe1 68.9(3) . . ? C9 C4 Fe1 126.6(4) . . ? C4 C5 C1 106.7(5) . . ? C4 C5 C10 126.5(5) . . ? C1 C5 C10 126.6(5) . . ? C4 C5 Fe1 72.0(3) . . ? C1 C5 Fe1 69.6(3) . . ? C10 C5 Fe1 126.7(4) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 S1 109.7(4) . . ? C12 C11 H11A 109.7 . . ? S1 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? S1 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S3 C13 S2 110.9(3) . . ? S3 C13 S4 128.1(3) . . ? S2 C13 S4 121.1(3) . . ? C15 C14 S4 114.4(4) . . ? C15 C14 H14A 108.7 . . ? S4 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? S4 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.864 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.108 # Attachment '7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 749172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 Fe O S3' _chemical_formula_weight 356.33 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.1525(4) _cell_length_b 9.3061(4) _cell_length_c 21.4965(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1630.90(13) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 6599 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 30.61 _exptl_crystal_description block _exptl_crystal_colour black-red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.4952 _exptl_absorpt_correction_T_max 0.5928 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9350 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3476 _reflns_number_gt 3343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0364P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.028(12) _refine_ls_number_reflns 3476 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0591 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.85876(3) 0.37721(3) 0.879700(12) 0.02723(8) Uani 1 1 d . . . S1 S 0.82975(7) 0.61679(6) 0.85770(3) 0.04323(13) Uani 1 1 d . . . S2 S 0.59680(6) 0.43185(5) 0.90861(2) 0.03333(11) Uani 1 1 d . . . S3 S 0.50611(7) 0.74638(6) 0.89108(3) 0.04618(14) Uani 1 1 d . . . C1 C 0.8632(3) 0.3112(2) 0.78616(9) 0.0398(5) Uani 1 1 d . . . C2 C 0.7780(2) 0.2074(2) 0.82146(10) 0.0375(5) Uani 1 1 d . . . C3 C 0.8834(2) 0.15581(19) 0.86854(9) 0.0320(4) Uani 1 1 d . . . C4 C 1.0388(2) 0.22614(19) 0.86110(8) 0.0297(4) Uani 1 1 d . . . C5 C 1.0272(2) 0.3231(2) 0.81079(8) 0.0335(4) Uani 1 1 d . . . C6 C 0.8025(4) 0.3911(4) 0.72994(12) 0.0716(9) Uani 1 1 d . . . H6A H 0.8208 0.3340 0.6934 0.107 Uiso 1 1 calc R . . H6B H 0.8607 0.4804 0.7262 0.107 Uiso 1 1 calc R . . H6C H 0.6873 0.4100 0.7343 0.107 Uiso 1 1 calc R . . C7 C 0.6054(3) 0.1582(3) 0.81057(14) 0.0615(8) Uani 1 1 d . . . H7A H 0.6056 0.0792 0.7818 0.092 Uiso 1 1 calc R . . H7B H 0.5422 0.2359 0.7936 0.092 Uiso 1 1 calc R . . H7C H 0.5579 0.1279 0.8493 0.092 Uiso 1 1 calc R . . C8 C 0.8478(3) 0.0388(2) 0.91454(12) 0.0520(6) Uani 1 1 d . . . H8A H 0.8707 -0.0528 0.8960 0.078 Uiso 1 1 calc R . . H8B H 0.7344 0.0429 0.9264 0.078 Uiso 1 1 calc R . . H8C H 0.9155 0.0514 0.9507 0.078 Uiso 1 1 calc R . . C9 C 1.1899(3) 0.1947(3) 0.89822(11) 0.0440(5) Uani 1 1 d . . . H9A H 1.2508 0.1191 0.8785 0.066 Uiso 1 1 calc R . . H9B H 1.1593 0.1654 0.9394 0.066 Uiso 1 1 calc R . . H9C H 1.2566 0.2796 0.9005 0.066 Uiso 1 1 calc R . . C10 C 1.1622(3) 0.4122(3) 0.78404(11) 0.0511(6) Uani 1 1 d . . . H10A H 1.2192 0.3578 0.7528 0.077 Uiso 1 1 calc R . . H10B H 1.2374 0.4386 0.8164 0.077 Uiso 1 1 calc R . . H10C H 1.1168 0.4974 0.7656 0.077 Uiso 1 1 calc R . . C11 C 0.6362(2) 0.60021(19) 0.88532(8) 0.0315(4) Uani 1 1 d . . . C12 C 0.3254(3) 0.6703(3) 0.92619(13) 0.0533(6) Uani 1 1 d . . . H12A H 0.2663 0.6142 0.8955 0.064 Uiso 1 1 calc R . . H12B H 0.3573 0.6065 0.9598 0.064 Uiso 1 1 calc R . . C13 C 0.2165(4) 0.7845(3) 0.95089(13) 0.0622(7) Uani 1 1 d . . . H13A H 0.1210 0.7415 0.9692 0.093 Uiso 1 1 calc R . . H13B H 0.1839 0.8471 0.9176 0.093 Uiso 1 1 calc R . . H13C H 0.2742 0.8389 0.9819 0.093 Uiso 1 1 calc R . . C14 C 0.9382(3) 0.4012(3) 0.95483(10) 0.0443(5) Uani 1 1 d . . . O1 O 0.9939(3) 0.4095(3) 1.00339(8) 0.0737(6) Uani 1 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 Fe1 0.02626(12) 0.02436(13) 0.03107(13) -0.00287(11) -0.00086(10) -0.00025(10) S1 0.0437(3) 0.0269(2) 0.0591(3) 0.0034(2) 0.0129(2) -0.0030(2) S2 0.0305(2) 0.0243(2) 0.0452(3) -0.0009(2) 0.00440(19) 0.00021(17) S3 0.0491(3) 0.0312(3) 0.0582(3) 0.0086(2) 0.0048(3) 0.0130(2) C1 0.0474(12) 0.0396(11) 0.0323(9) -0.0090(9) -0.0053(9) 0.0037(10) C2 0.0295(9) 0.0341(11) 0.0490(11) -0.0203(10) 0.0018(8) 0.0007(8) C3 0.0270(9) 0.0232(9) 0.0458(11) -0.0058(7) 0.0095(7) 0.0001(6) C4 0.0273(9) 0.0263(9) 0.0354(9) -0.0031(8) 0.0056(7) 0.0006(7) C5 0.0374(10) 0.0322(9) 0.0310(9) -0.0029(8) 0.0046(8) -0.0029(8) C6 0.101(2) 0.0680(19) 0.0462(13) -0.0036(14) -0.0321(14) 0.0093(18) C7 0.0281(10) 0.0591(16) 0.097(2) -0.0420(15) -0.0060(11) -0.0013(10) C8 0.0524(13) 0.0323(11) 0.0712(16) 0.0039(11) 0.0218(12) -0.0058(10) C9 0.0311(10) 0.0442(12) 0.0568(12) 0.0002(11) 0.0000(9) 0.0044(9) C10 0.0600(15) 0.0505(14) 0.0427(11) 0.0014(10) 0.0139(10) -0.0154(11) C11 0.0363(9) 0.0244(9) 0.0339(9) -0.0003(7) -0.0035(8) 0.0031(7) C12 0.0464(13) 0.0399(12) 0.0736(16) -0.0020(12) 0.0073(12) 0.0097(10) C13 0.0640(16) 0.0598(18) 0.0628(15) -0.0095(13) 0.0143(14) 0.0146(14) C14 0.0374(11) 0.0496(14) 0.0458(11) -0.0128(10) -0.0021(9) 0.0082(9) O1 0.0626(11) 0.1114(17) 0.0470(9) -0.0271(10) -0.0195(9) 0.0128(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 Fe1 C14 1.754(2) . ? Fe1 C4 2.0712(18) . ? Fe1 C5 2.0820(19) . ? Fe1 C3 2.0841(18) . ? Fe1 C1 2.1027(19) . ? Fe1 C2 2.1210(19) . ? Fe1 S2 2.2816(5) . ? Fe1 S1 2.2914(6) . ? S1 C11 1.693(2) . ? S2 C11 1.6758(19) . ? S3 C11 1.7291(19) . ? S3 C12 1.801(3) . ? C1 C2 1.412(3) . ? C1 C5 1.442(3) . ? C1 C6 1.503(3) . ? C2 C3 1.412(3) . ? C2 C7 1.498(3) . ? C3 C4 1.434(3) . ? C3 C8 1.499(3) . ? C4 C5 1.412(3) . ? C4 C9 1.497(3) . ? C5 C10 1.493(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C12 C13 1.483(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O1 1.141(3) . ? 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 C14 Fe1 C4 90.14(9) . . ? C14 Fe1 C5 116.25(9) . . ? C4 Fe1 C5 39.74(8) . . ? C14 Fe1 C3 101.30(10) . . ? C4 Fe1 C3 40.39(7) . . ? C5 Fe1 C3 67.38(8) . . ? C14 Fe1 C1 155.66(9) . . ? C4 Fe1 C1 66.72(8) . . ? C5 Fe1 C1 40.32(8) . . ? C3 Fe1 C1 66.39(8) . . ? C14 Fe1 C2 138.82(11) . . ? C4 Fe1 C2 66.44(7) . . ? C5 Fe1 C2 66.72(8) . . ? C3 Fe1 C2 39.23(8) . . ? C1 Fe1 C2 39.05(9) . . ? C14 Fe1 S2 93.80(7) . . ? C4 Fe1 S2 150.12(5) . . ? C5 Fe1 S2 149.91(6) . . ? C3 Fe1 S2 110.00(5) . . ? C1 Fe1 S2 109.99(6) . . ? C2 Fe1 S2 92.07(6) . . ? C14 Fe1 S1 96.00(8) . . ? C4 Fe1 S1 133.93(6) . . ? C5 Fe1 S1 99.00(6) . . ? C3 Fe1 S1 161.47(6) . . ? C1 Fe1 S1 95.08(6) . . ? C2 Fe1 S1 124.83(7) . . ? S2 Fe1 S1 75.09(2) . . ? C11 S1 Fe1 86.28(6) . . ? C11 S2 Fe1 87.00(7) . . ? C11 S3 C12 102.86(10) . . ? C2 C1 C5 108.17(18) . . ? C2 C1 C6 127.5(2) . . ? C5 C1 C6 124.2(2) . . ? C2 C1 Fe1 71.17(11) . . ? C5 C1 Fe1 69.07(10) . . ? C6 C1 Fe1 128.23(18) . . ? C1 C2 C3 108.55(17) . . ? C1 C2 C7 126.0(2) . . ? C3 C2 C7 125.5(2) . . ? C1 C2 Fe1 69.78(11) . . ? C3 C2 Fe1 68.97(10) . . ? C7 C2 Fe1 127.71(14) . . ? C2 C3 C4 107.60(17) . . ? C2 C3 C8 127.0(2) . . ? C4 C3 C8 125.17(19) . . ? C2 C3 Fe1 71.80(11) . . ? C4 C3 Fe1 69.32(10) . . ? C8 C3 Fe1 128.57(15) . . ? C5 C4 C3 108.57(17) . . ? C5 C4 C9 126.01(18) . . ? C3 C4 C9 125.32(18) . . ? C5 C4 Fe1 70.54(11) . . ? C3 C4 Fe1 70.29(10) . . ? C9 C4 Fe1 127.79(14) . . ? C4 C5 C1 107.08(17) . . ? C4 C5 C10 126.9(2) . . ? C1 C5 C10 125.77(19) . . ? C4 C5 Fe1 69.72(10) . . ? C1 C5 Fe1 70.61(11) . . ? C10 C5 Fe1 128.77(15) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S2 C11 S1 111.62(10) . . ? S2 C11 S3 126.64(12) . . ? S1 C11 S3 121.66(11) . . ? C13 C12 S3 110.99(19) . . ? C13 C12 H12A 109.4 . . ? S3 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? S3 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 Fe1 176.2(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.270 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.054 # Attachment '2b.cif' data_ds1 _database_code_depnum_ccdc_archive 'CCDC 753805' #TrackingRef '2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H39 Fe2 S5' _chemical_formula_sum 'C24 H39 Fe2 S5' _chemical_formula_weight 599.55 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' Fe Fe 0.3463 0.8444 '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' _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 31.2295(12) _cell_length_b 11.3352(4) _cell_length_c 16.2519(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.191(2) _cell_angle_gamma 90.00 _cell_volume 5707.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5904 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour blue-purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22282 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5025 _reflns_number_gt 4322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+5.3169P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5025 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.135069(11) 0.92923(3) 0.41278(2) 0.04056(12) Uani 1 1 d . . . Fe2 Fe 0.104937(11) 0.65172(3) 0.44712(2) 0.03844(11) Uani 1 1 d . . . S1 S 0.14115(2) 0.79890(6) 0.51992(4) 0.04410(16) Uani 1 1 d . . . S2 S 0.07913(2) 0.80872(6) 0.37139(4) 0.04968(18) Uani 1 1 d . . . S3 S 0.18209(2) 0.85210(6) 0.34019(5) 0.0559(2) Uani 1 1 d . . . S4 S 0.15402(2) 0.59953(6) 0.37170(5) 0.05403(19) Uani 1 1 d . . . S5 S 0.21995(3) 0.65938(9) 0.26140(6) 0.0773(3) Uani 1 1 d . . . C1 C 0.09787(12) 1.0805(3) 0.3781(2) 0.0724(10) Uani 1 1 d . . . C2 C 0.13962(12) 1.0990(2) 0.35723(18) 0.0633(8) Uani 1 1 d . . . C3 C 0.16885(11) 1.0939(2) 0.42959(19) 0.0602(8) Uani 1 1 d . . . C4 C 0.14566(11) 1.0738(2) 0.49641(17) 0.0577(7) Uani 1 1 d . . . C5 C 0.10149(11) 1.0628(2) 0.4665(2) 0.0606(8) Uani 1 1 d . . . C6 C 0.05669(17) 1.0870(4) 0.3193(4) 0.128(2) Uani 1 1 d . . . H6A H 0.0461 1.1665 0.3167 0.21(3) Uiso 1 1 d R . . H6B H 0.0357 1.0364 0.3392 0.109(16) Uiso 1 1 d R . . H6C H 0.0618 1.0622 0.2651 0.23(4) Uiso 1 1 d R . . C7 C 0.1518(2) 1.1287(4) 0.2721(3) 0.1200(19) Uani 1 1 d . . . H7A H 0.1503 1.2125 0.2640 0.16(2) Uiso 1 1 d R . . H7B H 0.1322 1.0907 0.2302 0.19(3) Uiso 1 1 d R . . H7C H 0.1806 1.1019 0.2682 0.26(4) Uiso 1 1 d R . . C8 C 0.21685(14) 1.1148(4) 0.4357(4) 0.1067(15) Uani 1 1 d . . . H8A H 0.2225 1.1976 0.4425 0.19(3) Uiso 1 1 d R . . H8B H 0.2276 1.0877 0.3863 0.22(3) Uiso 1 1 d R . . H8C H 0.2310 1.0729 0.4826 0.32(6) Uiso 1 1 d R . . C9 C 0.1640(2) 1.0734(4) 0.5873(2) 0.0994(15) Uani 1 1 d . . . H9A H 0.1649 1.1526 0.6081 0.18(2) Uiso 1 1 d R . . H9B H 0.1926 1.0411 0.5936 0.18(3) Uiso 1 1 d R . . H9C H 0.1459 1.0264 0.6176 0.16(2) Uiso 1 1 d R . . C10 C 0.06535(17) 1.0469(4) 0.5181(4) 0.1168(18) Uani 1 1 d . . . H10A H 0.0563 1.1227 0.5357 0.117(15) Uiso 1 1 d R . . H10B H 0.0750 0.9997 0.5658 0.13(2) Uiso 1 1 d R . . H10C H 0.0416 1.0086 0.4857 0.25(4) Uiso 1 1 d R . . C11 C 0.07037(13) 0.4929(3) 0.4265(2) 0.0739(10) Uani 1 1 d . . . C12 C 0.10201(11) 0.4776(3) 0.4931(2) 0.0702(9) Uani 1 1 d . . . C13 C 0.09479(11) 0.5565(3) 0.55406(19) 0.0649(8) Uani 1 1 d . . . C14 C 0.05839(10) 0.6241(3) 0.5274(2) 0.0624(8) Uani 1 1 d . . . C15 C 0.04192(10) 0.5837(3) 0.4473(2) 0.0739(10) Uani 1 1 d . . . C16 C 0.0640(3) 0.4230(6) 0.3460(4) 0.181(4) Uani 1 1 d . . . H16A H 0.0463 0.3556 0.3529 0.22(3) Uiso 1 1 d R . . H16B H 0.0916 0.3974 0.3331 0.25(4) Uiso 1 1 d R . . H16C H 0.0504 0.4711 0.3018 0.37(7) Uiso 1 1 d R . . C17 C 0.1367(2) 0.3837(5) 0.4985(6) 0.152(3) Uani 1 1 d . . . H17A H 0.1262 0.3134 0.5219 0.22(3) Uiso 1 1 d R . . H17B H 0.1615 0.4120 0.5337 0.35(7) Uiso 1 1 d R . . H17C H 0.1446 0.3665 0.4446 0.32(6) Uiso 1 1 d R . . C18 C 0.1207(2) 0.5631(6) 0.6388(3) 0.143(2) Uani 1 1 d . . . H18A H 0.1085 0.5100 0.6755 0.20(3) Uiso 1 1 d R . . H18B H 0.1194 0.6422 0.6592 0.27(5) Uiso 1 1 d R . . H18C H 0.1502 0.5421 0.6358 0.37(7) Uiso 1 1 d R . . C19 C 0.0388(2) 0.7168(4) 0.5780(5) 0.143(2) Uani 1 1 d . . . H19A H 0.0189 0.6799 0.6102 0.17(2) Uiso 1 1 d R . . H19B H 0.0239 0.7742 0.5417 0.27(4) Uiso 1 1 d R . . H19C H 0.0612 0.7549 0.6143 0.24(4) Uiso 1 1 d R . . C20 C 0.00141(13) 0.6245(6) 0.3967(5) 0.152(3) Uani 1 1 d . . . H20A H -0.0224 0.5776 0.4097 0.20(3) Uiso 1 1 d R . . H20B H 0.0041 0.6170 0.3388 0.24(4) Uiso 1 1 d R . . H20C H -0.0035 0.7055 0.4094 0.20(3) Uiso 1 1 d R . . C21 C 0.19738(10) 0.7587(3) 0.5480(2) 0.0755(10) Uani 1 1 d . . . H21A H 0.1997 0.7036 0.5932 0.122(16) Uiso 1 1 d R . . H21B H 0.2139 0.8281 0.5645 0.117(15) Uiso 1 1 d R . . H21C H 0.2083 0.7231 0.5012 0.114(15) Uiso 1 1 d R . . C22 C 0.07661(15) 0.7781(3) 0.26026(19) 0.0826(11) Uani 1 1 d . . . H22A H 0.0683 0.8477 0.2295 0.141(19) Uiso 1 1 d R . . H22B H 0.0560 0.7174 0.2450 0.19(2) Uiso 1 1 d R . . H22C H 0.1043 0.7530 0.2480 0.088(13) Uiso 1 1 d R . . C23 C 0.18304(8) 0.7026(3) 0.32949(17) 0.0516(7) Uani 1 1 d . . . C24 C 0.22484(13) 0.5033(4) 0.2750(3) 0.0885(12) Uani 1 1 d . . . H24A H 0.2447 0.4727 0.2398 0.122(15) Uiso 1 1 d R . . H24B H 0.1971 0.4670 0.2609 0.116(16) Uiso 1 1 d R . . H24C H 0.2353 0.4864 0.3319 0.126(17) Uiso 1 1 d 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 Fe1 0.0453(2) 0.0366(2) 0.0411(2) -0.00176(14) 0.01030(15) -0.00168(15) Fe2 0.0401(2) 0.0330(2) 0.0435(2) -0.00029(14) 0.01035(15) -0.00027(14) S1 0.0481(4) 0.0402(3) 0.0434(3) -0.0004(3) 0.0036(3) -0.0018(3) S2 0.0435(4) 0.0403(3) 0.0639(4) 0.0103(3) 0.0016(3) -0.0048(3) S3 0.0549(4) 0.0533(4) 0.0649(4) -0.0077(3) 0.0291(3) -0.0107(3) S4 0.0576(4) 0.0428(4) 0.0661(4) -0.0102(3) 0.0250(3) 0.0025(3) S5 0.0673(5) 0.0890(6) 0.0840(6) -0.0255(5) 0.0424(5) -0.0003(4) C1 0.079(2) 0.0359(15) 0.094(2) -0.0038(15) -0.0217(19) 0.0080(15) C2 0.102(3) 0.0380(15) 0.0512(16) 0.0007(12) 0.0133(16) -0.0052(16) C3 0.075(2) 0.0421(15) 0.0652(18) -0.0068(13) 0.0146(16) -0.0141(14) C4 0.087(2) 0.0372(14) 0.0488(15) -0.0046(12) 0.0075(14) -0.0013(14) C5 0.071(2) 0.0344(14) 0.081(2) -0.0058(14) 0.0308(16) 0.0016(13) C6 0.119(4) 0.062(3) 0.181(6) -0.002(3) -0.070(4) 0.019(3) C7 0.235(7) 0.067(3) 0.065(2) 0.011(2) 0.048(3) -0.010(3) C8 0.084(3) 0.091(3) 0.148(4) -0.024(3) 0.028(3) -0.038(2) C9 0.176(5) 0.066(2) 0.051(2) -0.0104(17) -0.007(2) -0.001(3) C10 0.121(4) 0.064(2) 0.185(5) -0.010(3) 0.098(4) 0.011(3) C11 0.101(3) 0.0574(19) 0.069(2) -0.0136(16) 0.0333(19) -0.0400(19) C12 0.076(2) 0.0370(15) 0.101(3) 0.0137(17) 0.027(2) 0.0020(15) C13 0.080(2) 0.0573(18) 0.0574(17) 0.0186(15) 0.0072(15) -0.0150(16) C14 0.070(2) 0.0435(15) 0.082(2) 0.0078(15) 0.0402(17) -0.0034(14) C15 0.0465(17) 0.077(2) 0.096(3) 0.045(2) -0.0012(16) -0.0217(16) C16 0.282(8) 0.153(5) 0.126(5) -0.084(4) 0.102(5) -0.156(6) C17 0.146(5) 0.060(3) 0.265(8) 0.057(4) 0.086(6) 0.043(3) C18 0.184(6) 0.161(6) 0.074(3) 0.056(3) -0.027(3) -0.072(4) C19 0.180(5) 0.071(3) 0.213(5) -0.021(4) 0.159(5) -0.013(3) C20 0.056(3) 0.173(6) 0.217(7) 0.123(5) -0.024(3) -0.039(3) C21 0.0526(18) 0.082(2) 0.085(2) 0.005(2) -0.0168(17) 0.0021(18) C22 0.106(3) 0.078(2) 0.0563(19) 0.0085(18) -0.0206(19) -0.024(2) C23 0.0438(15) 0.0601(17) 0.0543(15) -0.0128(13) 0.0188(12) -0.0009(13) C24 0.072(2) 0.098(3) 0.098(3) -0.029(2) 0.023(2) 0.026(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 Fe1 C5 2.093(3) . ? Fe1 C1 2.108(3) . ? Fe1 C4 2.129(3) . ? Fe1 C2 2.138(3) . ? Fe1 C3 2.145(3) . ? Fe1 S3 2.1786(7) . ? Fe1 S2 2.2531(7) . ? Fe1 S1 2.2733(7) . ? Fe2 C14 2.095(3) . ? Fe2 C13 2.104(3) . ? Fe2 C11 2.104(3) . ? Fe2 C15 2.114(3) . ? Fe2 C12 2.117(3) . ? Fe2 S4 2.1615(7) . ? Fe2 S2 2.2547(7) . ? Fe2 S1 2.2643(7) . ? S1 C21 1.816(3) . ? S2 C22 1.831(3) . ? S3 C23 1.704(3) . ? S4 C23 1.677(3) . ? S5 C23 1.764(2) . ? S5 C24 1.787(4) . ? C1 C2 1.403(5) . ? C1 C5 1.441(5) . ? C1 C6 1.504(5) . ? C2 C3 1.397(5) . ? C2 C7 1.518(5) . ? C3 C4 1.397(4) . ? C3 C8 1.509(5) . ? C4 C5 1.410(5) . ? C4 C9 1.515(4) . ? C5 C10 1.499(5) . ? C6 H6A 0.9584 . ? C6 H6B 0.9573 . ? C6 H6C 0.9574 . ? C7 H7A 0.9596 . ? C7 H7B 0.9589 . ? C7 H7C 0.9589 . ? C8 H8A 0.9594 . ? C8 H8B 0.9583 . ? C8 H8C 0.9585 . ? C9 H9A 0.9592 . ? C9 H9B 0.9585 . ? C9 H9C 0.9584 . ? C10 H10A 0.9594 . ? C10 H10B 0.9587 . ? C10 H10C 0.9584 . ? C11 C12 1.383(5) . ? C11 C15 1.427(5) . ? C11 C16 1.520(5) . ? C12 C13 1.374(5) . ? C12 C17 1.514(5) . ? C13 C14 1.394(4) . ? C13 C18 1.509(5) . ? C14 C15 1.415(5) . ? C14 C19 1.509(5) . ? C15 C20 1.494(5) . ? C16 H16A 0.9590 . ? C16 H16B 0.9581 . ? C16 H16C 0.9584 . ? C17 H17A 0.9596 . ? C17 H17B 0.9584 . ? C17 H17C 0.9581 . ? C18 H18A 0.9597 . ? C18 H18B 0.9586 . ? C18 H18C 0.9582 . ? C19 H19A 0.9595 . ? C19 H19B 0.9583 . ? C19 H19C 0.9585 . ? C20 H20A 0.9593 . ? C20 H20B 0.9578 . ? C20 H20C 0.9576 . ? C21 H21A 0.9601 . ? C21 H21B 0.9599 . ? C21 H21C 0.9599 . ? C22 H22A 0.9534 . ? C22 H22B 0.9530 . ? C22 H22C 0.9532 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 C5 Fe1 C1 40.12(14) . . ? C5 Fe1 C4 39.00(12) . . ? C1 Fe1 C4 65.23(12) . . ? C5 Fe1 C2 65.69(12) . . ? C1 Fe1 C2 38.60(14) . . ? C4 Fe1 C2 64.11(11) . . ? C5 Fe1 C3 65.26(12) . . ? C1 Fe1 C3 64.66(13) . . ? C4 Fe1 C3 38.17(12) . . ? C2 Fe1 C3 38.06(12) . . ? C5 Fe1 S3 157.33(8) . . ? C1 Fe1 S3 124.59(12) . . ? C4 Fe1 S3 126.40(10) . . ? C2 Fe1 S3 92.73(9) . . ? C3 Fe1 S3 93.68(9) . . ? C5 Fe1 S2 98.78(9) . . ? C1 Fe1 S2 91.85(9) . . ? C4 Fe1 S2 135.25(10) . . ? C2 Fe1 S2 120.64(10) . . ? C3 Fe1 S2 156.39(9) . . ? S3 Fe1 S2 98.34(3) . . ? C5 Fe1 S1 98.56(9) . . ? C1 Fe1 S1 136.38(12) . . ? C4 Fe1 S1 91.14(8) . . ? C2 Fe1 S1 154.80(8) . . ? C3 Fe1 S1 118.39(9) . . ? S3 Fe1 S1 99.01(3) . . ? S2 Fe1 S1 79.74(3) . . ? C14 Fe2 C13 38.78(13) . . ? C14 Fe2 C11 65.75(12) . . ? C13 Fe2 C11 64.23(13) . . ? C14 Fe2 C15 39.27(14) . . ? C13 Fe2 C15 64.83(13) . . ? C11 Fe2 C15 39.56(14) . . ? C14 Fe2 C12 64.94(12) . . ? C13 Fe2 C12 37.99(13) . . ? C11 Fe2 C12 38.25(14) . . ? C15 Fe2 C12 65.03(13) . . ? C14 Fe2 S4 155.35(9) . . ? C13 Fe2 S4 121.27(10) . . ? C11 Fe2 S4 93.54(10) . . ? C15 Fe2 S4 128.86(12) . . ? C12 Fe2 S4 90.58(10) . . ? C14 Fe2 S2 103.27(9) . . ? C13 Fe2 S2 140.86(10) . . ? C11 Fe2 S2 116.55(12) . . ? C15 Fe2 S2 91.13(9) . . ? C12 Fe2 S2 154.24(11) . . ? S4 Fe2 S2 97.87(3) . . ? C14 Fe2 S1 97.16(9) . . ? C13 Fe2 S1 93.63(9) . . ? C11 Fe2 S1 157.86(9) . . ? C15 Fe2 S1 132.22(12) . . ? C12 Fe2 S1 122.90(11) . . ? S4 Fe2 S1 98.90(3) . . ? S2 Fe2 S1 79.90(3) . . ? C21 S1 Fe2 110.50(13) . . ? C21 S1 Fe1 109.93(13) . . ? Fe2 S1 Fe1 95.18(3) . . ? C22 S2 Fe1 110.22(13) . . ? C22 S2 Fe2 110.90(13) . . ? Fe1 S2 Fe2 96.01(3) . . ? C23 S3 Fe1 118.42(9) . . ? C23 S4 Fe2 119.94(10) . . ? C23 S5 C24 104.47(16) . . ? C2 C1 C5 107.6(3) . . ? C2 C1 C6 125.9(4) . . ? C5 C1 C6 126.4(5) . . ? C2 C1 Fe1 71.86(18) . . ? C5 C1 Fe1 69.39(16) . . ? C6 C1 Fe1 127.5(2) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 C7 124.4(4) . . ? C1 C2 C7 126.8(4) . . ? C3 C2 Fe1 71.24(17) . . ? C1 C2 Fe1 69.54(17) . . ? C7 C2 Fe1 128.4(3) . . ? C2 C3 C4 108.3(3) . . ? C2 C3 C8 126.0(4) . . ? C4 C3 C8 125.6(4) . . ? C2 C3 Fe1 70.69(17) . . ? C4 C3 Fe1 70.28(16) . . ? C8 C3 Fe1 127.8(3) . . ? C3 C4 C5 109.0(3) . . ? C3 C4 C9 126.0(4) . . ? C5 C4 C9 124.8(4) . . ? C3 C4 Fe1 71.55(16) . . ? C5 C4 Fe1 69.13(16) . . ? C9 C4 Fe1 129.0(2) . . ? C4 C5 C1 106.5(3) . . ? C4 C5 C10 126.2(4) . . ? C1 C5 C10 127.2(4) . . ? C4 C5 Fe1 71.87(16) . . ? C1 C5 Fe1 70.49(17) . . ? C10 C5 Fe1 126.7(2) . . ? C1 C6 H6A 109.7 . . ? C1 C6 H6B 108.9 . . ? H6A C6 H6B 109.4 . . ? C1 C6 H6C 110.0 . . ? H6A C6 H6C 109.4 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.3 . . ? C2 C7 H7B 109.7 . . ? H7A C7 H7B 109.4 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.1 . . ? C3 C8 H8B 110.1 . . ? H8A C8 H8B 109.4 . . ? C3 C8 H8C 109.3 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.9 . . ? H9A C9 H9B 109.4 . . ? C4 C9 H9C 109.2 . . ? H9A C9 H9C 109.4 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.3 . . ? C5 C10 H10B 109.7 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.4 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 108.1(3) . . ? C12 C11 C16 127.7(5) . . ? C15 C11 C16 124.1(5) . . ? C12 C11 Fe2 71.39(18) . . ? C15 C11 Fe2 70.62(17) . . ? C16 C11 Fe2 126.3(3) . . ? C13 C12 C11 108.5(3) . . ? C13 C12 C17 126.7(5) . . ? C11 C12 C17 124.7(5) . . ? C13 C12 Fe2 70.47(17) . . ? C11 C12 Fe2 70.36(18) . . ? C17 C12 Fe2 127.8(3) . . ? C12 C13 C14 109.6(3) . . ? C12 C13 C18 124.9(5) . . ? C14 C13 C18 125.4(5) . . ? C12 C13 Fe2 71.53(18) . . ? C14 C13 Fe2 70.29(16) . . ? C18 C13 Fe2 127.5(3) . . ? C13 C14 C15 107.2(3) . . ? C13 C14 C19 125.7(4) . . ? C15 C14 C19 126.9(4) . . ? C13 C14 Fe2 70.93(17) . . ? C15 C14 Fe2 71.09(17) . . ? C19 C14 Fe2 126.5(2) . . ? C14 C15 C11 106.6(3) . . ? C14 C15 C20 126.3(5) . . ? C11 C15 C20 127.0(5) . . ? C14 C15 Fe2 69.64(16) . . ? C11 C15 Fe2 69.83(17) . . ? C20 C15 Fe2 127.6(2) . . ? C11 C16 H16A 109.3 . . ? C11 C16 H16B 108.8 . . ? H16A C16 H16B 109.4 . . ? C11 C16 H16C 110.4 . . ? H16A C16 H16C 109.4 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.2 . . ? C12 C17 H17B 108.6 . . ? H17A C17 H17B 109.4 . . ? C12 C17 H17C 110.7 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.1 . . ? C13 C18 H18B 108.7 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 110.6 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.2 . . ? C14 C19 H19B 109.7 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.6 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 110.0 . . ? H20A C20 H20B 109.4 . . ? C15 C20 H20C 109.0 . . ? H20A C20 H20C 109.4 . . ? H20B C20 H20C 109.5 . . ? S1 C21 H21A 109.4 . . ? S1 C21 H21B 109.4 . . ? H21A C21 H21B 109.5 . . ? S1 C21 H21C 109.6 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.6 . . ? S2 C22 H22B 109.7 . . ? H22A C22 H22B 109.3 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.3 . . ? H22B C22 H22C 109.3 . . ? S4 C23 S3 129.34(15) . . ? S4 C23 S5 119.45(17) . . ? S3 C23 S5 111.20(15) . . ? S5 C24 H24A 109.6 . . ? S5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S5 C24 H24C 109.3 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.599 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.057