# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Christopher John Pickett' 'David L. Hughes' 'Xiaoming Liu' 'Cedric Tard' _publ_contact_author_name 'Prof Christopher John Pickett' _publ_contact_author_address ; Department of Biological Chemistry John Innes Centre Norwich Research Park Norwich NR4 7UH UNITED KINGDOM ; _publ_contact_author_email CHRIS.PICKETT@BBSRC.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; A Novel {FeI-FeII-FeII-FeI} Iron Thiolate Carbonyl Assembly which Electrocatalyses Hydrogen Evolution ; data_cedric3 _database_code_depnum_ccdc_archive 'CCDC 246858' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 Fe4 O8 S6' _chemical_formula_structural '[(Fe2(CO)4{(SCH2)3CMe})2]' _chemical_formula_sum 'C18 H18 Fe4 O8 S6' _chemical_formula_weight 778.08 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.837(2) _cell_length_b 12.119(2) _cell_length_c 14.101(3) _cell_angle_alpha 101.85(3) _cell_angle_beta 105.13(3) _cell_angle_gamma 114.56(3) _cell_volume 1378.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'wafer-thin needle' _exptl_crystal_colour 'deep red,' _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 2.558 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7931 _diffrn_reflns_av_R_equivalents 0.0978 _diffrn_reflns_av_sigmaI/netI 0.1145 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4696 _reflns_number_gt 3056 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _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^)+(0.0563P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4696 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 0.39925(11) 0.70558(10) 0.57162(7) 0.0406(3) Uani 1 1 d . . . Fe2 Fe 0.52478(10) 0.92146(9) 0.54576(7) 0.0377(2) Uani 1 1 d . . . S1 S 0.26488(18) 0.81454(17) 0.53691(12) 0.0398(4) Uani 1 1 d . . . C11 C 0.2473(7) 0.8924(7) 0.6550(5) 0.0406(16) Uani 1 1 d . . . H11A H 0.1676 0.9192 0.6337 0.049 Uiso 1 1 calc R . . H11B H 0.2049 0.8276 0.6858 0.049 Uiso 1 1 calc R . . S2 S 0.59825(19) 0.89443(17) 0.70030(12) 0.0405(4) Uani 1 1 d . . . C12 C 0.5276(8) 0.9710(7) 0.7869(5) 0.0441(16) Uani 1 1 d . . . H12A H 0.4827 0.9123 0.8219 0.053 Uiso 1 1 calc R . . H12B H 0.6223 1.0488 0.8409 0.053 Uiso 1 1 calc R . . C1 C 0.4014(7) 1.0099(7) 0.7408(5) 0.0415(16) Uani 1 1 d . . . C13 C 0.4712(8) 1.1269(7) 0.7045(5) 0.0415(16) Uani 1 1 d . . . H13A H 0.5368 1.2050 0.7670 0.050 Uiso 1 1 calc R . . H13B H 0.3806 1.1336 0.6639 0.050 Uiso 1 1 calc R . . C14 C 0.3570(8) 1.0584(7) 0.8308(5) 0.0478(17) Uani 1 1 d . . . H14A H 0.4522 1.1324 0.8860 0.072 Uiso 1 1 calc R . . H14B H 0.3137 0.9905 0.8576 0.072 Uiso 1 1 calc R . . H14C H 0.2771 1.0827 0.8052 0.072 Uiso 1 1 calc R . . S3 S 0.59444(18) 1.12794(17) 0.62612(12) 0.0393(4) Uani 1 1 d . . . C4 C 0.3200(9) 0.6243(7) 0.6519(6) 0.0509(18) Uani 1 1 d . . . O4 O 0.2746(7) 0.5773(6) 0.7102(4) 0.0753(17) Uani 1 1 d . . . C5 C 0.2535(9) 0.5808(7) 0.4471(5) 0.0468(17) Uani 1 1 d . . . O5 O 0.1531(6) 0.4990(5) 0.3682(4) 0.0582(14) Uani 1 1 d . . . C6 C 0.5529(8) 0.6647(7) 0.5641(5) 0.0439(16) Uani 1 1 d . . . O6 O 0.6545(6) 0.6422(5) 0.5580(4) 0.0571(14) Uani 1 1 d . . . C7 C 0.7128(8) 0.9454(7) 0.5416(5) 0.0465(17) Uani 1 1 d . . . O7 O 0.8319(6) 0.9519(5) 0.5361(4) 0.0564(14) Uani 1 1 d . . . Fe1A Fe 0.21604(10) 0.33631(10) 0.11120(7) 0.0404(3) Uani 1 1 d . . . Fe2A Fe 0.01912(10) 0.40630(9) 0.02582(7) 0.0375(3) Uani 1 1 d . . . S1A S 0.27831(18) 0.48614(18) 0.03297(12) 0.0402(4) Uani 1 1 d . . . C11A C 0.2801(7) 0.4170(7) -0.0934(5) 0.0457(18) Uani 1 1 d . . . H11C H 0.3331 0.4878 -0.1162 0.055 Uiso 1 1 calc R . . H11D H 0.3466 0.3763 -0.0829 0.055 Uiso 1 1 calc R . . S2A S -0.00758(18) 0.20845(17) -0.03744(12) 0.0409(4) Uani 1 1 d . . . C12A C 0.0320(8) 0.1952(7) -0.1571(5) 0.0420(16) Uani 1 1 d . . . H12C H 0.0977 0.1535 -0.1553 0.050 Uiso 1 1 calc R . . H12D H -0.0713 0.1361 -0.2156 0.050 Uiso 1 1 calc R . . C1A C 0.1147(7) 0.3162(6) -0.1836(5) 0.0398(15) Uani 1 1 d . . . C13A C 0.0060(8) 0.3764(7) -0.2135(5) 0.0448(17) Uani 1 1 d . . . H13C H -0.0700 0.3247 -0.2857 0.054 Uiso 1 1 calc R . . H13D H 0.0749 0.4623 -0.2120 0.054 Uiso 1 1 calc R . . S3A S -0.11124(18) 0.39292(17) -0.13546(12) 0.0394(4) Uani 1 1 d . . . C14A C 0.1477(8) 0.2721(7) -0.2819(5) 0.0469(18) Uani 1 1 d . . . H14D H 0.2013 0.3457 -0.3006 0.070 Uiso 1 1 calc R . . H14E H 0.0468 0.2088 -0.3393 0.070 Uiso 1 1 calc R . . H14F H 0.2157 0.2343 -0.2668 0.070 Uiso 1 1 calc R . . C4A C 0.3348(9) 0.2604(8) 0.0903(5) 0.0492(18) Uani 1 1 d . . . O4A O 0.4051(6) 0.2085(6) 0.0723(4) 0.0624(15) Uani 1 1 d . . . C5A C 0.3580(8) 0.4667(8) 0.2303(5) 0.0449(18) Uani 1 1 d . . . O5A O 0.4562(6) 0.5565(6) 0.3063(4) 0.0581(14) Uani 1 1 d . . . C6A C 0.1098(8) 0.2407(7) 0.1780(5) 0.0483(18) Uani 1 1 d . . . O6A O 0.0392(6) 0.1795(6) 0.2190(4) 0.0678(16) Uani 1 1 d . . . C7A C -0.1499(8) 0.3316(7) 0.0595(5) 0.0443(17) Uani 1 1 d . . . O7A O -0.2544(6) 0.2768(5) 0.0845(4) 0.0570(13) 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 0.0425(5) 0.0466(6) 0.0426(5) 0.0183(5) 0.0202(4) 0.0274(5) Fe2 0.0367(5) 0.0447(6) 0.0399(5) 0.0158(4) 0.0180(4) 0.0252(4) S1 0.0387(8) 0.0468(10) 0.0424(9) 0.0162(8) 0.0196(7) 0.0263(8) C11 0.039(3) 0.050(4) 0.043(4) 0.016(3) 0.021(3) 0.028(3) S2 0.0411(8) 0.0498(10) 0.0386(8) 0.0161(8) 0.0173(7) 0.0281(8) C12 0.045(4) 0.057(5) 0.036(3) 0.017(3) 0.019(3) 0.028(3) C1 0.041(3) 0.048(4) 0.041(4) 0.015(3) 0.017(3) 0.027(3) C13 0.047(4) 0.050(4) 0.030(3) 0.009(3) 0.018(3) 0.027(3) C14 0.051(4) 0.051(4) 0.047(4) 0.014(3) 0.028(3) 0.027(3) S3 0.0379(8) 0.0441(10) 0.0412(9) 0.0135(8) 0.0185(7) 0.0238(7) C4 0.054(4) 0.053(5) 0.060(5) 0.025(4) 0.034(4) 0.029(4) O4 0.092(4) 0.075(4) 0.067(4) 0.036(3) 0.048(3) 0.033(4) C5 0.056(4) 0.056(5) 0.047(4) 0.021(4) 0.029(4) 0.037(4) O5 0.059(3) 0.058(3) 0.054(3) 0.011(3) 0.013(3) 0.036(3) C6 0.050(4) 0.052(4) 0.036(4) 0.020(3) 0.017(3) 0.029(4) O6 0.058(3) 0.063(3) 0.062(3) 0.019(3) 0.023(2) 0.042(3) C7 0.047(4) 0.052(5) 0.044(4) 0.013(3) 0.015(3) 0.030(4) O7 0.047(3) 0.068(4) 0.064(3) 0.019(3) 0.029(2) 0.035(3) Fe1A 0.0359(5) 0.0546(6) 0.0417(5) 0.0208(5) 0.0188(4) 0.0281(5) Fe2A 0.0312(4) 0.0495(6) 0.0390(5) 0.0152(4) 0.0157(4) 0.0252(4) S1A 0.0320(8) 0.0543(11) 0.0433(9) 0.0190(8) 0.0170(7) 0.0270(8) C11A 0.038(3) 0.068(5) 0.043(4) 0.020(4) 0.020(3) 0.035(4) S2A 0.0367(8) 0.0462(10) 0.0437(9) 0.0147(8) 0.0177(7) 0.0234(7) C12A 0.038(3) 0.045(4) 0.044(4) 0.008(3) 0.018(3) 0.024(3) C1A 0.037(3) 0.045(4) 0.043(4) 0.014(3) 0.018(3) 0.024(3) C13A 0.039(3) 0.061(5) 0.040(3) 0.012(3) 0.014(3) 0.033(3) S3A 0.0339(8) 0.0528(10) 0.0362(8) 0.0138(8) 0.0130(6) 0.0270(8) C14A 0.053(4) 0.061(5) 0.037(4) 0.016(3) 0.022(3) 0.036(4) C4A 0.055(4) 0.067(5) 0.047(4) 0.032(4) 0.026(3) 0.040(4) O4A 0.068(3) 0.090(4) 0.064(3) 0.035(3) 0.035(3) 0.059(3) C5A 0.045(4) 0.066(5) 0.021(3) 0.006(3) 0.009(3) 0.031(4) O5A 0.057(3) 0.078(4) 0.051(3) 0.025(3) 0.025(3) 0.040(3) C6A 0.039(4) 0.054(5) 0.046(4) 0.013(4) 0.010(3) 0.025(3) O6A 0.054(3) 0.088(5) 0.062(3) 0.036(3) 0.029(3) 0.027(3) C7A 0.037(3) 0.045(4) 0.048(4) 0.008(3) 0.012(3) 0.026(3) O7A 0.049(3) 0.067(4) 0.066(3) 0.029(3) 0.036(3) 0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C4 1.772(8) . ? Fe1 C5 1.794(8) . ? Fe1 C6 1.796(6) . ? Fe1 S2 2.254(2) . ? Fe1 S1 2.2603(18) . ? Fe1 Fe2 2.5384(16) . ? Fe2 C7 1.768(7) . ? Fe2 S3 2.224(2) 2_676 ? Fe2 S3 2.241(2) . ? Fe2 S2 2.246(2) . ? Fe2 S1 2.290(2) . ? Fe2 Fe2 2.642(2) 2_676 ? S1 C11 1.826(6) . ? C11 C1 1.526(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? S2 C12 1.830(6) . ? C12 C1 1.542(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C1 C14 1.531(8) . ? C1 C13 1.554(10) . ? C13 S3 1.840(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? S3 Fe2 2.224(2) 2_676 ? C4 O4 1.171(9) . ? C5 O5 1.164(8) . ? C6 O6 1.158(7) . ? C7 O7 1.166(7) . ? Fe1A C5A 1.766(7) . ? Fe1A C4A 1.805(7) . ? Fe1A C6A 1.810(9) . ? Fe1A S2A 2.249(2) . ? Fe1A S1A 2.267(2) . ? Fe1A Fe2A 2.5474(14) . ? Fe2A C7A 1.774(8) . ? Fe2A S3A 2.2352(19) . ? Fe2A S3A 2.241(2) 2_565 ? Fe2A S2A 2.256(2) . ? Fe2A S1A 2.2852(18) . ? Fe2A Fe2A 2.660(2) 2_565 ? S1A C11A 1.814(6) . ? C11A C1A 1.545(8) . ? C11A H11C 0.9700 . ? C11A H11D 0.9700 . ? S2A C12A 1.819(6) . ? C12A C1A 1.530(10) . ? C12A H12C 0.9700 . ? C12A H12D 0.9700 . ? C1A C14A 1.545(8) . ? C1A C13A 1.547(8) . ? C13A S3A 1.828(6) . ? C13A H13C 0.9700 . ? C13A H13D 0.9700 . ? S3A Fe2A 2.241(2) 2_565 ? C14A H14D 0.9600 . ? C14A H14E 0.9600 . ? C14A H14F 0.9600 . ? C4A O4A 1.152(8) . ? C5A O5A 1.172(8) . ? C6A O6A 1.152(9) . ? C7A O7A 1.158(8) . ? 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 C4 Fe1 C5 97.1(4) . . ? C4 Fe1 C6 103.2(3) . . ? C5 Fe1 C6 92.4(3) . . ? C4 Fe1 S2 98.0(3) . . ? C5 Fe1 S2 164.4(3) . . ? C6 Fe1 S2 87.6(2) . . ? C4 Fe1 S1 105.3(2) . . ? C5 Fe1 S1 86.5(2) . . ? C6 Fe1 S1 151.5(2) . . ? S2 Fe1 S1 86.13(7) . . ? C4 Fe1 Fe2 145.8(2) . . ? C5 Fe1 Fe2 109.1(3) . . ? C6 Fe1 Fe2 97.4(2) . . ? S2 Fe1 Fe2 55.53(6) . . ? S1 Fe1 Fe2 56.65(6) . . ? C7 Fe2 S3 94.5(2) . 2_676 ? C7 Fe2 S3 99.5(2) . . ? S3 Fe2 S3 107.44(7) 2_676 . ? C7 Fe2 S2 88.5(2) . . ? S3 Fe2 S2 159.66(8) 2_676 . ? S3 Fe2 S2 91.82(8) . . ? C7 Fe2 S1 159.0(2) . . ? S3 Fe2 S1 84.44(8) 2_676 . ? S3 Fe2 S1 100.83(7) . . ? S2 Fe2 S1 85.60(8) . . ? C7 Fe2 Fe1 104.9(3) . . ? S3 Fe2 Fe1 104.13(8) 2_676 . ? S3 Fe2 Fe1 138.03(6) . . ? S2 Fe2 Fe1 55.80(7) . . ? S1 Fe2 Fe1 55.54(6) . . ? C7 Fe2 Fe2 101.9(3) . 2_676 ? S3 Fe2 Fe2 54.01(6) 2_676 2_676 ? S3 Fe2 Fe2 53.43(6) . 2_676 ? S2 Fe2 Fe2 144.72(7) . 2_676 ? S1 Fe2 Fe2 94.46(7) . 2_676 ? Fe1 Fe2 Fe2 146.74(6) . 2_676 ? C11 S1 Fe1 110.8(2) . . ? C11 S1 Fe2 110.9(2) . . ? Fe1 S1 Fe2 67.81(6) . . ? C1 C11 S1 117.3(4) . . ? C1 C11 H11A 108.0 . . ? S1 C11 H11A 108.0 . . ? C1 C11 H11B 108.0 . . ? S1 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? C12 S2 Fe2 108.6(2) . . ? C12 S2 Fe1 113.9(2) . . ? Fe2 S2 Fe1 68.68(6) . . ? C1 C12 S2 119.9(4) . . ? C1 C12 H12A 107.4 . . ? S2 C12 H12A 107.4 . . ? C1 C12 H12B 107.4 . . ? S2 C12 H12B 107.4 . . ? H12A C12 H12B 106.9 . . ? C11 C1 C14 107.9(5) . . ? C11 C1 C12 110.8(5) . . ? C14 C1 C12 106.6(5) . . ? C11 C1 C13 113.0(5) . . ? C14 C1 C13 105.1(5) . . ? C12 C1 C13 113.0(5) . . ? C1 C13 S3 118.9(4) . . ? C1 C13 H13A 107.6 . . ? S3 C13 H13A 107.6 . . ? C1 C13 H13B 107.6 . . ? S3 C13 H13B 107.6 . . ? H13A C13 H13B 107.0 . . ? C1 C14 H14A 109.5 . . ? C1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 S3 Fe2 117.0(2) . 2_676 ? C13 S3 Fe2 107.7(2) . . ? Fe2 S3 Fe2 72.56(7) 2_676 . ? O4 C4 Fe1 175.9(7) . . ? O5 C5 Fe1 176.7(6) . . ? O6 C6 Fe1 177.4(7) . . ? O7 C7 Fe2 175.2(6) . . ? C5A Fe1A C4A 99.8(3) . . ? C5A Fe1A C6A 92.5(3) . . ? C4A Fe1A C6A 99.3(3) . . ? C5A Fe1A S2A 160.9(2) . . ? C4A Fe1A S2A 99.0(2) . . ? C6A Fe1A S2A 87.8(2) . . ? C5A Fe1A S1A 86.0(3) . . ? C4A Fe1A S1A 104.0(3) . . ? C6A Fe1A S1A 156.5(2) . . ? S2A Fe1A S1A 86.20(8) . . ? C5A Fe1A Fe2A 105.7(2) . . ? C4A Fe1A Fe2A 145.7(2) . . ? C6A Fe1A Fe2A 102.0(2) . . ? S2A Fe1A Fe2A 55.70(5) . . ? S1A Fe1A Fe2A 56.31(5) . . ? C7A Fe2A S3A 99.1(2) . . ? C7A Fe2A S3A 95.0(2) . 2_565 ? S3A Fe2A S3A 107.09(7) . 2_565 ? C7A Fe2A S2A 88.0(2) . . ? S3A Fe2A S2A 91.65(8) . . ? S3A Fe2A S2A 160.25(7) 2_565 . ? C7A Fe2A S1A 159.1(2) . . ? S3A Fe2A S1A 100.90(8) . . ? S3A Fe2A S1A 84.76(8) 2_565 . ? S2A Fe2A S1A 85.61(7) . . ? C7A Fe2A Fe1A 104.7(2) . . ? S3A Fe2A Fe1A 137.66(6) . . ? S3A Fe2A Fe1A 105.08(6) 2_565 . ? S2A Fe2A Fe1A 55.44(6) . . ? S1A Fe2A Fe1A 55.64(6) . . ? C7A Fe2A Fe2A 101.9(2) . 2_565 ? S3A Fe2A Fe2A 53.65(6) . 2_565 ? S3A Fe2A Fe2A 53.44(5) 2_565 2_565 ? S2A Fe2A Fe2A 144.80(7) . 2_565 ? S1A Fe2A Fe2A 94.70(7) . 2_565 ? Fe1A Fe2A Fe2A 147.18(6) . 2_565 ? C11A S1A Fe1A 110.2(3) . . ? C11A S1A Fe2A 111.1(2) . . ? Fe1A S1A Fe2A 68.05(7) . . ? C1A C11A S1A 117.4(4) . . ? C1A C11A H11C 108.0 . . ? S1A C11A H11C 108.0 . . ? C1A C11A H11D 108.0 . . ? S1A C11A H11D 108.0 . . ? H11C C11A H11D 107.2 . . ? C12A S2A Fe1A 114.1(2) . . ? C12A S2A Fe2A 108.1(2) . . ? Fe1A S2A Fe2A 68.86(7) . . ? C1A C12A S2A 120.7(4) . . ? C1A C12A H12C 107.2 . . ? S2A C12A H12C 107.2 . . ? C1A C12A H12D 107.2 . . ? S2A C12A H12D 107.2 . . ? H12C C12A H12D 106.8 . . ? C12A C1A C11A 110.7(6) . . ? C12A C1A C14A 106.8(5) . . ? C11A C1A C14A 107.6(5) . . ? C12A C1A C13A 113.1(5) . . ? C11A C1A C13A 111.7(5) . . ? C14A C1A C13A 106.5(5) . . ? C1A C13A S3A 119.4(5) . . ? C1A C13A H13C 107.5 . . ? S3A C13A H13C 107.5 . . ? C1A C13A H13D 107.5 . . ? S3A C13A H13D 107.5 . . ? H13C C13A H13D 107.0 . . ? C13A S3A Fe2A 107.3(2) . . ? C13A S3A Fe2A 116.4(3) . 2_565 ? Fe2A S3A Fe2A 72.91(7) . 2_565 ? C1A C14A H14D 109.5 . . ? C1A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C1A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? O4A C4A Fe1A 176.8(7) . . ? O5A C5A Fe1A 176.5(7) . . ? O6A C6A Fe1A 178.6(6) . . ? O7A C7A Fe2A 174.1(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Fe1 Fe2 C7 122.5(5) . . . . ? C5 Fe1 Fe2 C7 -99.4(3) . . . . ? C6 Fe1 Fe2 C7 -4.3(3) . . . . ? S2 Fe1 Fe2 C7 77.7(2) . . . . ? S1 Fe1 Fe2 C7 -171.6(2) . . . . ? C4 Fe1 Fe2 S3 -138.8(4) . . . 2_676 ? C5 Fe1 Fe2 S3 -0.7(2) . . . 2_676 ? C6 Fe1 Fe2 S3 94.4(2) . . . 2_676 ? S2 Fe1 Fe2 S3 176.37(7) . . . 2_676 ? S1 Fe1 Fe2 S3 -72.91(7) . . . 2_676 ? C4 Fe1 Fe2 S3 -0.9(4) . . . . ? C5 Fe1 Fe2 S3 137.2(2) . . . . ? C6 Fe1 Fe2 S3 -127.7(2) . . . . ? S2 Fe1 Fe2 S3 -45.71(9) . . . . ? S1 Fe1 Fe2 S3 65.01(10) . . . . ? C4 Fe1 Fe2 S2 44.8(4) . . . . ? C5 Fe1 Fe2 S2 -177.1(2) . . . . ? C6 Fe1 Fe2 S2 -82.0(2) . . . . ? S1 Fe1 Fe2 S2 110.72(8) . . . . ? C4 Fe1 Fe2 S1 -65.9(4) . . . . ? C5 Fe1 Fe2 S1 72.2(2) . . . . ? C6 Fe1 Fe2 S1 167.3(2) . . . . ? S2 Fe1 Fe2 S1 -110.72(8) . . . . ? C4 Fe1 Fe2 Fe2 -94.9(4) . . . 2_676 ? C5 Fe1 Fe2 Fe2 43.2(2) . . . 2_676 ? C6 Fe1 Fe2 Fe2 138.3(2) . . . 2_676 ? S2 Fe1 Fe2 Fe2 -139.76(12) . . . 2_676 ? S1 Fe1 Fe2 Fe2 -29.04(10) . . . 2_676 ? C4 Fe1 S1 C11 43.0(3) . . . . ? C5 Fe1 S1 C11 139.4(3) . . . . ? C6 Fe1 S1 C11 -132.0(5) . . . . ? S2 Fe1 S1 C11 -54.3(2) . . . . ? Fe2 Fe1 S1 C11 -104.9(2) . . . . ? C4 Fe1 S1 Fe2 147.9(3) . . . . ? C5 Fe1 S1 Fe2 -115.7(2) . . . . ? C6 Fe1 S1 Fe2 -27.1(4) . . . . ? S2 Fe1 S1 Fe2 50.61(6) . . . . ? C7 Fe2 S1 C11 128.1(6) . . . . ? S3 Fe2 S1 C11 -143.8(3) 2_676 . . . ? S3 Fe2 S1 C11 -37.1(3) . . . . ? S2 Fe2 S1 C11 53.9(3) . . . . ? Fe1 Fe2 S1 C11 104.8(3) . . . . ? Fe2 Fe2 S1 C11 -90.7(2) 2_676 . . . ? C7 Fe2 S1 Fe1 23.3(6) . . . . ? S3 Fe2 S1 Fe1 111.37(7) 2_676 . . . ? S3 Fe2 S1 Fe1 -141.90(7) . . . . ? S2 Fe2 S1 Fe1 -50.88(6) . . . . ? Fe2 Fe2 S1 Fe1 164.51(6) 2_676 . . . ? Fe1 S1 C11 C1 71.7(6) . . . . ? Fe2 S1 C11 C1 -1.6(6) . . . . ? C7 Fe2 S2 C12 141.7(3) . . . . ? S3 Fe2 S2 C12 -119.3(3) 2_676 . . . ? S3 Fe2 S2 C12 42.3(3) . . . . ? S1 Fe2 S2 C12 -58.4(3) . . . . ? Fe1 Fe2 S2 C12 -109.1(3) . . . . ? Fe2 Fe2 S2 C12 33.1(3) 2_676 . . . ? C7 Fe2 S2 Fe1 -109.2(2) . . . . ? S3 Fe2 S2 Fe1 -10.2(2) 2_676 . . . ? S3 Fe2 S2 Fe1 151.38(6) . . . . ? S1 Fe2 S2 Fe1 50.66(6) . . . . ? Fe2 Fe2 S2 Fe1 142.17(11) 2_676 . . . ? C4 Fe1 S2 C12 -54.8(3) . . . . ? C5 Fe1 S2 C12 112.0(8) . . . . ? C6 Fe1 S2 C12 -157.7(3) . . . . ? S1 Fe1 S2 C12 50.1(3) . . . . ? Fe2 Fe1 S2 C12 101.7(3) . . . . ? C4 Fe1 S2 Fe2 -156.4(2) . . . . ? C5 Fe1 S2 Fe2 10.3(7) . . . . ? C6 Fe1 S2 Fe2 100.6(2) . . . . ? S1 Fe1 S2 Fe2 -51.54(6) . . . . ? Fe2 S2 C12 C1 14.5(6) . . . . ? Fe1 S2 C12 C1 -59.8(6) . . . . ? S1 C11 C1 C14 179.8(5) . . . . ? S1 C11 C1 C12 -63.8(7) . . . . ? S1 C11 C1 C13 64.1(6) . . . . ? S2 C12 C1 C11 57.5(8) . . . . ? S2 C12 C1 C14 174.7(5) . . . . ? S2 C12 C1 C13 -70.4(7) . . . . ? C11 C1 C13 S3 -80.8(6) . . . . ? C14 C1 C13 S3 161.8(4) . . . . ? C12 C1 C13 S3 46.0(7) . . . . ? C1 C13 S3 Fe2 103.1(5) . . . 2_676 ? C1 C13 S3 Fe2 24.1(5) . . . . ? C7 Fe2 S3 C13 -148.7(3) . . . . ? S3 Fe2 S3 C13 113.5(2) 2_676 . . . ? S2 Fe2 S3 C13 -59.9(2) . . . . ? S1 Fe2 S3 C13 26.0(2) . . . . ? Fe1 Fe2 S3 C13 -23.5(2) . . . . ? Fe2 Fe2 S3 C13 113.5(2) 2_676 . . . ? C7 Fe2 S3 Fe2 97.8(2) . . . 2_676 ? S3 Fe2 S3 Fe2 0.0 2_676 . . 2_676 ? S2 Fe2 S3 Fe2 -173.39(7) . . . 2_676 ? S1 Fe2 S3 Fe2 -87.52(7) . . . 2_676 ? Fe1 Fe2 S3 Fe2 -137.06(9) . . . 2_676 ? C5 Fe1 C4 O4 -175(9) . . . . ? C6 Fe1 C4 O4 91(9) . . . . ? S2 Fe1 C4 O4 1(9) . . . . ? S1 Fe1 C4 O4 -87(9) . . . . ? Fe2 Fe1 C4 O4 -34(9) . . . . ? C4 Fe1 C5 O5 42(11) . . . . ? C6 Fe1 C5 O5 145(11) . . . . ? S2 Fe1 C5 O5 -125(11) . . . . ? S1 Fe1 C5 O5 -63(11) . . . . ? Fe2 Fe1 C5 O5 -116(11) . . . . ? C4 Fe1 C6 O6 -162(13) . . . . ? C5 Fe1 C6 O6 100(13) . . . . ? S2 Fe1 C6 O6 -64(13) . . . . ? S1 Fe1 C6 O6 13(13) . . . . ? Fe2 Fe1 C6 O6 -9(13) . . . . ? S3 Fe2 C7 O7 -78(7) 2_676 . . . ? S3 Fe2 C7 O7 174(7) . . . . ? S2 Fe2 C7 O7 82(7) . . . . ? S1 Fe2 C7 O7 8(8) . . . . ? Fe1 Fe2 C7 O7 28(7) . . . . ? Fe2 Fe2 C7 O7 -132(7) 2_676 . . . ? C5A Fe1A Fe2A C7A -98.0(3) . . . . ? C4A Fe1A Fe2A C7A 125.3(5) . . . . ? C6A Fe1A Fe2A C7A -1.9(3) . . . . ? S2A Fe1A Fe2A C7A 77.0(2) . . . . ? S1A Fe1A Fe2A C7A -172.0(2) . . . . ? C5A Fe1A Fe2A S3A 139.8(3) . . . . ? C4A Fe1A Fe2A S3A 3.2(5) . . . . ? C6A Fe1A Fe2A S3A -124.1(2) . . . . ? S2A Fe1A Fe2A S3A -45.23(11) . . . . ? S1A Fe1A Fe2A S3A 65.77(11) . . . . ? C5A Fe1A Fe2A S3A 1.4(2) . . . 2_565 ? C4A Fe1A Fe2A S3A -135.2(5) . . . 2_565 ? C6A Fe1A Fe2A S3A 97.5(2) . . . 2_565 ? S2A Fe1A Fe2A S3A 176.38(8) . . . 2_565 ? S1A Fe1A Fe2A S3A -72.61(8) . . . 2_565 ? C5A Fe1A Fe2A S2A -175.0(2) . . . . ? C4A Fe1A Fe2A S2A 48.4(5) . . . . ? C6A Fe1A Fe2A S2A -78.9(2) . . . . ? S1A Fe1A Fe2A S2A 111.00(8) . . . . ? C5A Fe1A Fe2A S1A 74.0(2) . . . . ? C4A Fe1A Fe2A S1A -62.6(5) . . . . ? C6A Fe1A Fe2A S1A 170.1(2) . . . . ? S2A Fe1A Fe2A S1A -111.00(8) . . . . ? C5A Fe1A Fe2A Fe2A 45.3(3) . . . 2_565 ? C4A Fe1A Fe2A Fe2A -91.3(5) . . . 2_565 ? C6A Fe1A Fe2A Fe2A 141.4(2) . . . 2_565 ? S2A Fe1A Fe2A Fe2A -139.71(12) . . . 2_565 ? S1A Fe1A Fe2A Fe2A -28.70(11) . . . 2_565 ? C5A Fe1A S1A C11A 142.7(3) . . . . ? C4A Fe1A S1A C11A 43.6(3) . . . . ? C6A Fe1A S1A C11A -130.3(6) . . . . ? S2A Fe1A S1A C11A -54.8(2) . . . . ? Fe2A Fe1A S1A C11A -105.4(2) . . . . ? C5A Fe1A S1A Fe2A -111.9(2) . . . . ? C4A Fe1A S1A Fe2A 149.0(2) . . . . ? C6A Fe1A S1A Fe2A -24.9(5) . . . . ? S2A Fe1A S1A Fe2A 50.61(6) . . . . ? C7A Fe2A S1A C11A 126.1(6) . . . . ? S3A Fe2A S1A C11A -37.2(3) . . . . ? S3A Fe2A S1A C11A -143.6(3) 2_565 . . . ? S2A Fe2A S1A C11A 53.6(3) . . . . ? Fe1A Fe2A S1A C11A 104.1(3) . . . . ? Fe2A Fe2A S1A C11A -91.1(3) 2_565 . . . ? C7A Fe2A S1A Fe1A 22.1(6) . . . . ? S3A Fe2A S1A Fe1A -141.29(7) . . . . ? S3A Fe2A S1A Fe1A 112.29(7) 2_565 . . . ? S2A Fe2A S1A Fe1A -50.45(6) . . . . ? Fe2A Fe2A S1A Fe1A 164.86(6) 2_565 . . . ? Fe1A S1A C11A C1A 72.1(5) . . . . ? Fe2A S1A C11A C1A -1.3(6) . . . . ? C5A Fe1A S2A C12A 115.9(8) . . . . ? C4A Fe1A S2A C12A -53.7(4) . . . . ? C6A Fe1A S2A C12A -152.8(3) . . . . ? S1A Fe1A S2A C12A 49.9(2) . . . . ? Fe2A Fe1A S2A C12A 101.0(2) . . . . ? C5A Fe1A S2A Fe2A 14.9(8) . . . . ? C4A Fe1A S2A Fe2A -154.8(3) . . . . ? C6A Fe1A S2A Fe2A 106.2(2) . . . . ? S1A Fe1A S2A Fe2A -51.12(6) . . . . ? C7A Fe2A S2A C12A 141.0(3) . . . . ? S3A Fe2A S2A C12A 41.9(2) . . . . ? S3A Fe2A S2A C12A -119.9(3) 2_565 . . . ? S1A Fe2A S2A C12A -58.9(2) . . . . ? Fe1A Fe2A S2A C12A -109.5(2) . . . . ? Fe2A Fe2A S2A C12A 33.0(2) 2_565 . . . ? C7A Fe2A S2A Fe1A -109.5(2) . . . . ? S3A Fe2A S2A Fe1A 151.42(7) . . . . ? S3A Fe2A S2A Fe1A -10.4(2) 2_565 . . . ? S1A Fe2A S2A Fe1A 50.61(6) . . . . ? Fe2A Fe2A S2A Fe1A 142.55(11) 2_565 . . . ? Fe1A S2A C12A C1A -59.1(5) . . . . ? Fe2A S2A C12A C1A 15.3(5) . . . . ? S2A C12A C1A C11A 56.4(6) . . . . ? S2A C12A C1A C14A 173.3(4) . . . . ? S2A C12A C1A C13A -69.9(6) . . . . ? S1A C11A C1A C12A -63.6(6) . . . . ? S1A C11A C1A C14A -180.0(5) . . . . ? S1A C11A C1A C13A 63.4(7) . . . . ? C12A C1A C13A S3A 43.7(7) . . . . ? C11A C1A C13A S3A -82.0(7) . . . . ? C14A C1A C13A S3A 160.7(5) . . . . ? C1A C13A S3A Fe2A 26.2(6) . . . . ? C1A C13A S3A Fe2A 105.3(5) . . . 2_565 ? C7A Fe2A S3A C13A -148.8(3) . . . . ? S3A Fe2A S3A C13A 113.1(3) 2_565 . . . ? S2A Fe2A S3A C13A -60.6(3) . . . . ? S1A Fe2A S3A C13A 25.3(3) . . . . ? Fe1A Fe2A S3A C13A -24.8(3) . . . . ? Fe2A Fe2A S3A C13A 113.1(3) 2_565 . . . ? C7A Fe2A S3A Fe2A 98.1(2) . . . 2_565 ? S3A Fe2A S3A Fe2A 0.0 2_565 . . 2_565 ? S2A Fe2A S3A Fe2A -173.66(7) . . . 2_565 ? S1A Fe2A S3A Fe2A -87.82(8) . . . 2_565 ? Fe1A Fe2A S3A Fe2A -137.87(10) . . . 2_565 ? C5A Fe1A C4A O4A -168(13) . . . . ? C6A Fe1A C4A O4A 97(13) . . . . ? S2A Fe1A C4A O4A 8(13) . . . . ? S1A Fe1A C4A O4A -80(13) . . . . ? Fe2A Fe1A C4A O4A -31(13) . . . . ? C4A Fe1A C5A O5A 77(9) . . . . ? C6A Fe1A C5A O5A 177(100) . . . . ? S2A Fe1A C5A O5A -92(9) . . . . ? S1A Fe1A C5A O5A -26(9) . . . . ? Fe2A Fe1A C5A O5A -80(9) . . . . ? C5A Fe1A C6A O6A 130(27) . . . . ? C4A Fe1A C6A O6A -130(27) . . . . ? S2A Fe1A C6A O6A -31(27) . . . . ? S1A Fe1A C6A O6A 44(28) . . . . ? Fe2A Fe1A C6A O6A 23(28) . . . . ? S3A Fe2A C7A O7A 134(5) . . . . ? S3A Fe2A C7A O7A -118(5) 2_565 . . . ? S2A Fe2A C7A O7A 43(5) . . . . ? S1A Fe2A C7A O7A -29(6) . . . . ? Fe1A Fe2A C7A O7A -11(6) . . . . ? Fe2A Fe2A C7A O7A -171(5) 2_565 . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.513 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.125