# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1738 data_1 _publ_contact_author_name 'Eugenio Coronado-97' _publ_contact_author_address ; Dept. de Qumica Inorganica, Universidad de Valencia, Dr. Moliner 50, 46100-Burjasot (Spain). e-mail: eugenio.coronado@uv.es ; _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H36 Fe2 O28 S28' _chemical_formula_weight 2142.20 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.487(2) _cell_length_b 21.118(11) _cell_length_c 17.514(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.56(2) _cell_angle_gamma 90.00 _cell_volume 3866(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type ? _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 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7560 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0968 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.97 _reflns_number_total 6974 _reflns_number_gt 3647 _reflns_threshold_expression >4sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 4sigma(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^)+(0.0690P)^2^+0.7363P] 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 6974 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1492 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.0976 _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 Fe Fe 0.32046(9) 0.19053(5) 0.32000(5) 0.0459(2) Uani 1 1 d . . . O1 O 0.1611(4) 0.1929(2) 0.2483(2) 0.0523(11) Uani 1 1 d . . . O2 O 0.1868(4) 0.2009(2) 0.3954(2) 0.0533(11) Uani 1 1 d . . . O3 O 0.3254(4) 0.0963(2) 0.3138(3) 0.0560(12) Uani 1 1 d . . . O4 O 0.4680(4) 0.1730(2) 0.3992(2) 0.0532(11) Uani 1 1 d . . . O5 O 0.3572(5) 0.2841(2) 0.3254(2) 0.0561(12) Uani 1 1 d . . . O6 O 0.4292(4) 0.2002(2) 0.2300(2) 0.0526(11) Uani 1 1 d . . . O7 O -0.0513(5) 0.1954(3) 0.2459(3) 0.0683(14) Uani 1 1 d . . . O8 O -0.0199(5) 0.2209(3) 0.4026(3) 0.094(2) Uani 1 1 d . . . O9 O 0.4315(4) 0.0119(2) 0.3595(3) 0.0707(14) Uani 1 1 d . . . O10 O 0.5911(5) 0.0950(2) 0.4464(3) 0.0672(14) Uani 1 1 d . . . O11 O 0.4588(4) 0.3608(2) 0.2693(3) 0.0619(13) Uani 1 1 d . . . O12 O 0.5163(5) 0.2734(3) 0.1590(3) 0.0767(16) Uani 1 1 d . . . C101 C 0.0552(7) 0.1969(3) 0.2787(3) 0.0471(16) Uani 1 1 d . . . C102 C 0.0719(7) 0.2063(3) 0.3665(4) 0.0550(18) Uani 1 1 d . . . C103 C 0.4148(6) 0.0692(3) 0.3567(4) 0.0471(15) Uani 1 1 d . . . C104 C 0.5002(6) 0.1151(3) 0.4057(3) 0.0431(15) Uani 1 1 d . . . C105 C 0.4237(6) 0.3064(3) 0.2745(4) 0.0476(15) Uani 1 1 d . . . C106 C 0.4609(6) 0.2565(4) 0.2149(4) 0.0506(17) Uani 1 1 d . . . S11 S 0.50255(18) 0.07737(11) -0.08029(10) 0.0649(5) Uani 1 1 d . . . S12 S 0.53720(18) 0.07396(10) 0.08555(10) 0.0626(5) Uani 1 1 d . . . C1 C 0.5089(6) 0.0329(3) 0.0015(4) 0.0559(18) Uani 1 1 d . . . C2 C 0.5300(8) 0.1482(4) -0.0342(5) 0.074(2) Uani 1 1 d . . . H2 H 0.5355 0.1860 -0.0610 0.050 Uiso 1 1 calc . . . C3 C 0.5429(7) 0.1463(4) 0.0419(4) 0.065(2) Uani 1 1 d . . . H3 H 0.5547 0.1832 0.0705 0.050 Uiso 1 1 calc . . . S21 S 0.19106(17) 0.11279(8) -0.05478(8) 0.0465(4) Uani 1 1 d . . . S22 S 0.21495(16) 0.08129(9) 0.10876(9) 0.0513(4) Uani 1 1 d . . . S23 S 0.13932(17) -0.03454(8) -0.09684(9) 0.0491(4) Uani 1 1 d . . . S24 S 0.16174(17) -0.06703(9) 0.06601(9) 0.0538(4) Uani 1 1 d . . . C21 C 0.1866(6) 0.0546(3) 0.0153(3) 0.0430(15) Uani 1 1 d . . . C22 C 0.1650(5) -0.0082(3) -0.0032(3) 0.0390(14) Uani 1 1 d . . . C23 C 0.2164(7) 0.1744(3) 0.0095(4) 0.0513(17) Uani 1 1 d . . . H23 H 0.2233 0.2161 -0.0070 0.050 Uiso 1 1 calc . . . C24 C 0.2256(6) 0.1600(3) 0.0827(3) 0.0514(17) Uani 1 1 d . . . H24 H 0.2376 0.1914 0.1198 0.050 Uiso 1 1 calc . . . C25 C 0.1133(7) -0.1125(3) -0.0719(4) 0.0541(17) Uani 1 1 d . . . H25 H 0.0936 -0.1432 -0.1090 0.050 Uiso 1 1 calc . . . C26 C 0.1225(7) -0.1266(3) 0.0011(4) 0.062(2) Uani 1 1 d . . . H26 H 0.1082 -0.1677 0.0175 0.050 Uiso 1 1 calc . . . S31 S -0.05379(17) 0.14445(8) 0.77350(9) 0.0497(4) Uani 1 1 d . . . S32 S -0.18402(16) 0.03724(9) 0.69901(10) 0.0545(4) Uani 1 1 d . . . S33 S 0.21819(15) 0.07814(8) 0.75248(8) 0.0481(4) Uani 1 1 d . . . S34 S 0.08657(19) -0.03104(9) 0.68251(11) 0.0633(5) Uani 1 1 d . . . C31 C -0.0407(6) 0.0725(3) 0.7316(3) 0.0427(14) Uani 1 1 d . . . C32 C 0.0756(6) 0.0423(3) 0.7235(3) 0.0445(15) Uani 1 1 d . . . C33 C -0.2185(7) 0.1474(3) 0.7624(4) 0.0553(18) Uani 1 1 d . . . H33 H -0.2644 0.1816 0.7794 0.050 Uiso 1 1 calc . . . C34 C -0.2756(6) 0.0979(4) 0.7283(4) 0.0571(18) Uani 1 1 d . . . H34 H -0.3643 0.0963 0.7205 0.050 Uiso 1 1 calc . . . C35 C 0.3101(7) 0.0166(4) 0.7246(4) 0.066(2) Uani 1 1 d . . . H35 H 0.3989 0.0180 0.7313 0.050 Uiso 1 1 calc . . . C36 C 0.2502(8) -0.0327(4) 0.6934(5) 0.073(2) Uani 1 1 d . . . H36 H 0.2954 -0.0676 0.6777 0.050 Uiso 1 1 calc . . . S41 S -0.01825(16) 0.21863(7) 0.61301(9) 0.0454(4) Uani 1 1 d . . . S42 S -0.14405(16) 0.11792(8) 0.52263(9) 0.0497(4) Uani 1 1 d . . . S43 S 0.25428(16) 0.15936(8) 0.59381(9) 0.0480(4) Uani 1 1 d . . . S44 S 0.14102(17) 0.05307(8) 0.50888(10) 0.0542(4) Uani 1 1 d . . . C41 C -0.0033(6) 0.1507(3) 0.5610(3) 0.0391(14) Uani 1 1 d . . . C42 C 0.1165(6) 0.1236(3) 0.5541(3) 0.0403(14) Uani 1 1 d . . . C43 C -0.1829(7) 0.2214(3) 0.5985(4) 0.0525(17) Uani 1 1 d . . . H43 H -0.2297 0.2538 0.6190 0.050 Uiso 1 1 calc . . . C44 C -0.2400(6) 0.1755(3) 0.5570(4) 0.0522(17) Uani 1 1 d . . . H44 H -0.3284 0.1745 0.5469 0.050 Uiso 1 1 calc . . . C45 C 0.3557(6) 0.1012(4) 0.5677(4) 0.0550(18) Uani 1 1 d . . . H45 H 0.4435 0.1038 0.5798 0.050 Uiso 1 1 calc . . . C46 C 0.3038(7) 0.0525(3) 0.5296(4) 0.0530(17) Uani 1 1 d . . . H46 H 0.3537 0.0190 0.5146 0.050 Uiso 1 1 calc . . . O101 O -0.3043(7) 0.1558(4) 0.2101(4) 0.124(2) Uani 1 1 d . . . O102 O -0.2878(6) 0.2375(3) 0.3659(4) 0.108(2) 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 Fe 0.0493(6) 0.0489(6) 0.0388(4) -0.0004(4) -0.0014(4) -0.0043(5) O1 0.052(3) 0.067(3) 0.037(2) -0.002(2) -0.004(2) 0.002(2) O2 0.053(3) 0.068(3) 0.039(2) 0.003(2) 0.006(2) -0.004(2) O3 0.056(3) 0.046(3) 0.062(3) -0.005(2) -0.013(2) -0.007(2) O4 0.057(3) 0.055(3) 0.045(2) -0.003(2) -0.009(2) -0.006(2) O5 0.069(3) 0.048(3) 0.053(3) 0.000(2) 0.012(2) -0.007(2) O6 0.051(3) 0.058(3) 0.050(2) -0.004(2) 0.009(2) 0.000(2) O7 0.049(3) 0.093(4) 0.060(3) 0.012(3) -0.007(2) -0.011(3) O8 0.068(4) 0.161(6) 0.054(3) 0.013(4) 0.017(3) -0.001(4) O9 0.051(3) 0.058(3) 0.101(4) -0.015(3) -0.007(3) 0.006(3) O10 0.056(3) 0.070(3) 0.073(3) -0.015(3) -0.014(3) 0.012(3) O11 0.051(3) 0.050(3) 0.086(4) 0.005(3) 0.013(3) -0.006(2) O12 0.080(4) 0.082(4) 0.071(3) 0.004(3) 0.026(3) -0.012(3) C101 0.053(4) 0.042(4) 0.045(3) 0.010(3) -0.002(3) -0.003(3) C102 0.048(4) 0.066(5) 0.050(4) 0.016(4) 0.000(3) -0.013(4) C103 0.039(4) 0.049(4) 0.053(4) -0.001(3) 0.008(3) 0.001(3) C104 0.032(3) 0.051(4) 0.047(3) -0.007(3) 0.005(3) -0.005(3) C105 0.038(3) 0.044(4) 0.059(4) 0.003(3) -0.008(3) 0.003(3) C106 0.040(4) 0.063(5) 0.048(4) 0.006(3) 0.001(3) 0.000(3) S11 0.0565(11) 0.0885(15) 0.0487(9) 0.0098(10) -0.0022(8) 0.0007(11) S12 0.0537(11) 0.0818(14) 0.0510(9) -0.0037(10) -0.0038(8) 0.0015(10) C1 0.034(3) 0.085(5) 0.048(3) 0.005(4) -0.003(3) 0.009(4) C2 0.063(5) 0.076(6) 0.081(5) 0.015(5) -0.008(4) -0.011(4) C3 0.057(5) 0.059(5) 0.075(5) -0.006(4) -0.010(4) -0.003(4) S21 0.0564(10) 0.0478(10) 0.0348(7) 0.0009(7) 0.0002(7) -0.0027(8) S22 0.0540(10) 0.0648(11) 0.0348(7) -0.0018(8) 0.0019(7) -0.0022(9) S23 0.0568(10) 0.0482(10) 0.0420(8) -0.0023(7) 0.0022(8) -0.0011(8) S24 0.0587(10) 0.0554(11) 0.0477(9) 0.0109(8) 0.0065(8) 0.0028(9) C21 0.040(3) 0.053(4) 0.036(3) 0.003(3) 0.005(3) -0.005(3) C22 0.036(3) 0.044(4) 0.037(3) 0.003(3) 0.000(2) 0.000(3) C23 0.061(4) 0.041(4) 0.053(4) -0.005(3) 0.008(3) 0.001(3) C24 0.056(4) 0.052(4) 0.045(3) -0.013(3) 0.001(3) 0.002(3) C25 0.052(4) 0.040(4) 0.070(4) -0.005(3) 0.002(4) 0.001(3) C26 0.063(5) 0.048(4) 0.076(5) 0.010(4) 0.012(4) 0.002(4) S31 0.0531(10) 0.0494(10) 0.0461(8) -0.0020(8) 0.0019(8) 0.0008(8) S32 0.0434(10) 0.0540(11) 0.0660(11) -0.0013(9) 0.0037(8) -0.0082(8) S33 0.0420(9) 0.0616(11) 0.0408(8) 0.0008(8) 0.0043(7) -0.0037(8) S34 0.0657(12) 0.0537(11) 0.0707(11) -0.0112(9) 0.0071(10) 0.0025(10) C31 0.040(3) 0.050(4) 0.039(3) 0.004(3) 0.003(3) -0.004(3) C32 0.050(4) 0.051(4) 0.033(3) 0.007(3) 0.007(3) -0.006(3) C33 0.052(4) 0.057(5) 0.058(4) 0.005(4) 0.010(3) 0.016(4) C34 0.039(4) 0.074(5) 0.060(4) 0.007(4) 0.014(3) 0.004(4) C35 0.048(4) 0.096(6) 0.054(4) 0.002(4) 0.006(3) 0.008(4) C36 0.061(5) 0.082(6) 0.076(5) -0.016(5) 0.015(4) 0.021(5) S41 0.0459(9) 0.0395(9) 0.0503(8) -0.0042(7) 0.0012(7) -0.0039(7) S42 0.0485(10) 0.0498(10) 0.0496(9) -0.0093(8) -0.0033(8) -0.0053(8) S43 0.0451(9) 0.0492(10) 0.0490(9) -0.0008(8) -0.0016(7) -0.0047(8) S44 0.0574(11) 0.0514(11) 0.0540(9) -0.0112(8) 0.0054(8) 0.0006(9) C41 0.046(4) 0.039(3) 0.032(3) 0.005(3) -0.004(3) -0.006(3) C42 0.043(3) 0.042(4) 0.035(3) 0.001(3) -0.003(3) -0.006(3) C43 0.054(4) 0.045(4) 0.059(4) 0.003(3) 0.009(3) 0.005(3) C44 0.045(4) 0.061(5) 0.050(4) 0.003(3) -0.004(3) -0.005(3) C45 0.042(4) 0.074(5) 0.049(4) 0.007(4) 0.010(3) 0.006(4) C46 0.056(4) 0.049(4) 0.055(4) 0.002(3) 0.015(3) 0.011(4) O101 0.112(6) 0.121(6) 0.139(6) -0.014(5) 0.019(5) 0.007(5) O102 0.093(5) 0.123(6) 0.106(5) 0.050(4) 0.001(4) -0.014(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 Fe O3 1.994(5) . ? Fe O1 2.009(4) . ? Fe O2 2.012(4) . ? Fe O5 2.013(5) . ? Fe O6 2.027(4) . ? Fe O4 2.028(4) . ? O1 C101 1.273(7) . ? O2 C102 1.275(8) . ? O3 C103 1.289(7) . ? O4 C104 1.272(7) . ? O5 C105 1.266(7) . ? O6 C106 1.268(8) . ? O7 C101 1.215(8) . ? O8 C102 1.232(8) . ? O9 C103 1.223(8) . ? O10 C104 1.221(8) . ? O11 C105 1.213(7) . ? O12 C106 1.231(7) . ? C101 C102 1.547(8) . ? C103 C104 1.536(9) . ? C105 C106 1.553(9) . ? S11 C1 1.709(7) . ? S11 C2 1.714(9) . ? S12 C3 1.712(8) . ? S12 C1 1.714(7) . ? C1 C1 1.404(14) 3_655 ? C2 C3 1.329(10) . ? S21 C23 1.728(7) . ? S21 C21 1.740(6) . ? S22 C24 1.730(7) . ? S22 C21 1.734(6) . ? S23 C25 1.730(7) . ? S23 C22 1.733(6) . ? S24 C26 1.723(8) . ? S24 C22 1.737(6) . ? C21 C22 1.380(9) . ? C23 C24 1.315(8) . ? C25 C26 1.310(9) . ? S31 C31 1.698(6) . ? S31 C33 1.724(7) . ? S32 C34 1.705(7) . ? S32 C31 1.733(6) . ? S33 C35 1.712(8) . ? S33 C32 1.716(6) . ? S34 C36 1.712(8) . ? S34 C32 1.715(6) . ? C31 C32 1.393(8) . ? C33 C34 1.323(10) . ? C35 C36 1.311(11) . ? S41 C41 1.714(6) . ? S41 C43 1.726(7) . ? S42 C41 1.717(6) . ? S42 C44 1.717(7) . ? S43 C45 1.711(7) . ? S43 C42 1.726(6) . ? S44 C42 1.717(6) . ? S44 C46 1.717(7) . ? C41 C42 1.394(8) . ? C43 C44 1.326(9) . ? C45 C46 1.319(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe O1 90.84(19) . . ? O3 Fe O2 99.61(19) . . ? O1 Fe O2 79.59(18) . . ? O3 Fe O5 167.46(19) . . ? O1 Fe O5 98.7(2) . . ? O2 Fe O5 90.17(18) . . ? O3 Fe O6 92.27(19) . . ? O1 Fe O6 90.15(17) . . ? O2 Fe O6 164.35(19) . . ? O5 Fe O6 79.65(18) . . ? O3 Fe O4 80.45(19) . . ? O1 Fe O4 169.50(19) . . ? O2 Fe O4 96.00(18) . . ? O5 Fe O4 90.80(19) . . ? O6 Fe O4 95.99(18) . . ? C101 O1 Fe 116.8(4) . . ? C102 O2 Fe 115.8(4) . . ? C103 O3 Fe 115.6(4) . . ? C104 O4 Fe 114.8(4) . . ? C105 O5 Fe 116.5(4) . . ? C106 O6 Fe 115.4(4) . . ? O7 C101 O1 126.9(6) . . ? O7 C101 C102 120.0(6) . . ? O1 C101 C102 113.0(6) . . ? O8 C102 O2 124.9(6) . . ? O8 C102 C101 120.7(6) . . ? O2 C102 C101 114.3(6) . . ? O9 C103 O3 124.0(6) . . ? O9 C103 C104 121.8(6) . . ? O3 C103 C104 114.2(6) . . ? O10 C104 O4 125.2(6) . . ? O10 C104 C103 120.0(6) . . ? O4 C104 C103 114.7(6) . . ? O11 C105 O5 126.4(6) . . ? O11 C105 C106 119.9(6) . . ? O5 C105 C106 113.7(6) . . ? O12 C106 O6 125.9(7) . . ? O12 C106 C105 119.8(7) . . ? O6 C106 C105 114.3(6) . . ? C1 S11 C2 95.2(4) . . ? C3 S12 C1 94.4(4) . . ? C1 C1 S11 121.1(7) 3_655 . ? C1 C1 S12 123.1(7) 3_655 . ? S11 C1 S12 115.8(4) . . ? C3 C2 S11 116.5(6) . . ? C2 C3 S12 118.1(6) . . ? C23 S21 C21 94.8(3) . . ? C24 S22 C21 94.2(3) . . ? C25 S23 C22 94.7(3) . . ? C26 S24 C22 94.5(3) . . ? C22 C21 S22 123.1(4) . . ? C22 C21 S21 121.8(4) . . ? S22 C21 S21 115.1(4) . . ? C21 C22 S23 122.7(4) . . ? C21 C22 S24 122.4(4) . . ? S23 C22 S24 114.9(4) . . ? C24 C23 S21 117.2(5) . . ? C23 C24 S22 118.6(5) . . ? C26 C25 S23 117.6(6) . . ? C25 C26 S24 118.2(6) . . ? C31 S31 C33 95.7(3) . . ? C34 S32 C31 94.2(3) . . ? C35 S33 C32 94.4(4) . . ? C36 S34 C32 94.1(4) . . ? C32 C31 S31 123.7(5) . . ? C32 C31 S32 120.9(5) . . ? S31 C31 S32 115.4(4) . . ? C31 C32 S34 122.9(5) . . ? C31 C32 S33 121.2(5) . . ? S34 C32 S33 115.9(4) . . ? C34 C33 S31 115.8(5) . . ? C33 C34 S32 119.0(5) . . ? C36 C35 S33 117.3(6) . . ? C35 C36 S34 118.2(6) . . ? C41 S41 C43 94.7(3) . . ? C41 S42 C44 95.0(3) . . ? C45 S43 C42 95.5(3) . . ? C42 S44 C46 95.2(3) . . ? C42 C41 S41 120.6(4) . . ? C42 C41 S42 123.6(5) . . ? S41 C41 S42 115.7(4) . . ? C41 C42 S44 124.4(4) . . ? C41 C42 S43 121.2(4) . . ? S44 C42 S43 114.5(4) . . ? C44 C43 S41 117.3(5) . . ? C43 C44 S42 117.3(5) . . ? C46 C45 S43 117.0(5) . . ? C45 C46 S44 117.7(5) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.510 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.097 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H40 Fe2 O22 S20' _chemical_formula_weight 1793.73 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.777(5) _cell_length_b 13.900(5) _cell_length_c 13.457(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 107.400(5) _cell_angle_gamma 90.000(5) _cell_volume 3530(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type ? _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 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3380 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.1394 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.91 _reflns_number_total 3221 _reflns_number_gt 1485 _reflns_threshold_expression >6sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 6sigma(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^)+(0.0843P)^2^+13.7918P] 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 SHELXL _refine_ls_extinction_coef 0.0007(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3221 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1861 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1872 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.003 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 0.0000 0.30335(13) -0.5000 0.0437(5) Uani 1 2 d S . . O1 O -0.0507(3) 0.4189(4) -0.5901(4) 0.0478(14) Uani 1 1 d . . . O2 O 0.0504(3) 0.2184(4) -0.3862(4) 0.0507(15) Uani 1 1 d . . . O3 O -0.0746(3) 0.2934(4) -0.4320(4) 0.0529(15) Uani 1 1 d . . . O4 O 0.0363(3) 0.1415(5) -0.2472(5) 0.077(2) Uani 1 1 d . . . O5 O -0.0960(3) 0.2270(6) -0.2933(5) 0.080(2) Uani 1 1 d . . . C1 C -0.0290(5) 0.5000 -0.5509(8) 0.037(3) Uani 1 2 d S . . C2 C 0.0157(4) 0.1948(7) -0.3229(7) 0.052(2) Uani 1 1 d . . . C3 C -0.0587(4) 0.2408(7) -0.3494(7) 0.053(2) Uani 1 1 d . . . S1 S 0.16641(10) 0.37763(18) -0.20809(16) 0.0520(6) Uani 1 1 d . . . S2 S 0.32025(10) 0.3808(2) -0.15053(17) 0.0583(7) Uani 1 1 d . . . S3 S 0.17672(11) 0.37697(18) 0.03805(17) 0.0544(6) Uani 1 1 d . . . S4 S 0.33058(11) 0.37816(17) 0.09069(16) 0.0524(6) Uani 1 1 d . . . S5 S -0.02260(13) 0.3831(2) -0.11483(18) 0.0675(8) Uani 1 1 d . . . C11 C 0.2458(4) 0.3785(6) -0.1105(6) 0.047(2) Uani 1 1 d . . . C12 C 0.2501(4) 0.3791(6) -0.0050(7) 0.0463(19) Uani 1 1 d . . . C13 C 0.2042(4) 0.3722(7) -0.3061(6) 0.061(3) Uani 1 1 d . . . H13 H 0.1767 0.3676 -0.3754 0.050 Uiso 1 1 calc . . . C14 C 0.2751(5) 0.3747(8) -0.2794(7) 0.067(3) Uani 1 1 d . . . H14 H 0.2988 0.3731 -0.3296 0.050 Uiso 1 1 calc . . . C15 C 0.2239(5) 0.3721(7) 0.1660(6) 0.060(2) Uani 1 1 d . . . H15 H 0.2010 0.3693 0.2171 0.050 Uiso 1 1 calc . . . C16 C 0.2952(5) 0.3721(7) 0.1922(6) 0.061(2) Uani 1 1 d . . . H16 H 0.3234 0.3691 0.2611 0.050 Uiso 1 1 calc . . . C21 C 0.0000 0.4513(9) 0.0000 0.059(4) Uani 1 2 d S . . C22 C -0.0094(5) 0.2730(7) -0.0507(7) 0.065(3) Uani 1 1 d . . . H22 H -0.0155 0.2155 -0.0878 0.050 Uiso 1 1 calc . . . C101 C -0.1655(7) 0.0000 -0.5290(10) 0.066(4) Uani 1 2 d S . . C201 C -0.0880(7) 0.0000 -0.5008(13) 0.090(5) Uani 1 2 d S . . C102 C -0.2048(6) 0.0860(8) -0.5439(7) 0.074(3) Uani 1 1 d . . . H102 H -0.1815 0.1450 -0.5357 0.050 Uiso 1 1 calc . . . C103 C -0.2773(7) 0.0832(12) -0.5705(9) 0.105(5) Uani 1 1 d . . . H103 H -0.3017 0.1413 -0.5790 0.050 Uiso 1 1 calc . . . C104 C -0.3158(10) 0.0000 -0.5854(14) 0.115(9) Uani 1 2 d S . . H104 H -0.3650 0.0000 -0.6044 0.050 Uiso 1 2 calc S . . O100 O -0.0564(5) 0.0000 -0.2066(8) 0.086(3) Uani 1 2 d S . . 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 0.0447(9) 0.0363(11) 0.0491(10) 0.000 0.0127(7) 0.000 O1 0.053(3) 0.034(3) 0.048(3) -0.007(3) 0.000(3) -0.006(3) O2 0.056(3) 0.039(4) 0.058(4) 0.010(3) 0.019(3) 0.002(3) O3 0.049(3) 0.054(4) 0.058(4) 0.006(3) 0.019(3) 0.007(3) O4 0.080(4) 0.073(5) 0.066(4) 0.029(4) 0.006(3) -0.006(4) O5 0.066(4) 0.107(6) 0.075(4) 0.012(4) 0.033(3) -0.015(4) C1 0.031(5) 0.047(8) 0.035(6) 0.000 0.014(4) 0.000 C2 0.049(4) 0.044(5) 0.057(5) 0.002(5) 0.004(4) -0.011(5) C3 0.053(5) 0.046(6) 0.059(6) -0.008(5) 0.017(4) -0.015(4) S1 0.0458(11) 0.0583(16) 0.0508(12) 0.0010(12) 0.0127(9) 0.0035(12) S2 0.0454(11) 0.0764(19) 0.0546(13) 0.0111(14) 0.0173(9) 0.0107(12) S3 0.0524(12) 0.0571(16) 0.0570(13) -0.0004(13) 0.0212(10) 0.0007(12) S4 0.0515(11) 0.0529(15) 0.0495(12) 0.0019(12) 0.0099(9) 0.0036(12) S5 0.0756(15) 0.0703(19) 0.0570(14) -0.0041(14) 0.0207(12) 0.0001(15) C11 0.050(4) 0.045(6) 0.049(5) 0.007(5) 0.019(4) 0.007(4) C12 0.044(4) 0.039(5) 0.060(5) 0.007(5) 0.022(3) 0.006(4) C13 0.061(5) 0.076(7) 0.049(5) 0.001(5) 0.019(4) 0.017(5) C14 0.066(6) 0.076(8) 0.066(6) 0.010(6) 0.029(5) 0.024(6) C15 0.075(6) 0.062(7) 0.049(5) -0.013(5) 0.027(4) -0.004(6) C16 0.076(6) 0.057(6) 0.047(5) -0.004(5) 0.015(4) -0.002(6) C21 0.052(6) 0.073(10) 0.046(7) 0.000 0.007(5) 0.000 C22 0.067(6) 0.057(7) 0.073(6) -0.005(5) 0.024(6) 0.002(5) C101 0.067(8) 0.072(11) 0.064(9) 0.000 0.030(7) 0.000 C201 0.055(8) 0.093(13) 0.117(14) 0.000 0.020(8) 0.000 C102 0.097(8) 0.074(8) 0.057(6) 0.011(6) 0.030(5) 0.028(6) C103 0.094(9) 0.152(16) 0.073(8) 0.015(9) 0.032(7) 0.056(9) C104 0.079(13) 0.21(3) 0.066(11) 0.000 0.041(10) 0.000 O100 0.098(7) 0.077(8) 0.106(8) 0.000 0.064(6) 0.000 _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 O2 1.954(6) 2_554 ? Fe1 O2 1.954(6) . ? Fe1 O3 1.960(5) 2_554 ? Fe1 O3 1.960(5) . ? Fe1 O1 2.081(6) 2_554 ? Fe1 O1 2.081(6) . ? O1 C1 1.264(6) . ? O2 C2 1.286(9) . ? O3 C3 1.288(10) . ? O4 C2 1.227(10) . ? O5 C3 1.219(9) . ? C1 O1 1.264(6) 6_565 ? C1 C1 1.501(19) 5_564 ? C2 C3 1.545(12) . ? S1 C13 1.701(8) . ? S1 C11 1.719(8) . ? S2 C14 1.699(9) . ? S2 C11 1.714(8) . ? S3 C15 1.697(9) . ? S3 C12 1.715(8) . ? S4 C16 1.713(9) . ? S4 C12 1.723(8) . ? S5 C22 1.738(9) . ? S5 C21 1.754(7) . ? C11 C12 1.396(11) . ? C13 C14 1.341(12) . ? C15 C16 1.347(12) . ? C21 C21 1.35(3) 5_565 ? C21 S5 1.754(7) 2 ? C22 C22 1.302(17) 2 ? C101 C102 1.407(11) 6 ? C101 C102 1.407(11) . ? C101 C201 1.465(18) . ? C102 C103 1.370(15) . ? C103 C104 1.366(16) . ? C104 C103 1.366(16) 6 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O2 105.7(3) 2_554 . ? O2 Fe1 O3 82.5(2) 2_554 2_554 ? O2 Fe1 O3 92.6(2) . 2_554 ? O2 Fe1 O3 92.6(2) 2_554 . ? O2 Fe1 O3 82.5(2) . . ? O3 Fe1 O3 171.9(4) 2_554 . ? O2 Fe1 O1 165.2(2) 2_554 2_554 ? O2 Fe1 O1 88.0(2) . 2_554 ? O3 Fe1 O1 91.6(2) 2_554 2_554 ? O3 Fe1 O1 94.7(2) . 2_554 ? O2 Fe1 O1 88.0(2) 2_554 . ? O2 Fe1 O1 165.2(2) . . ? O3 Fe1 O1 94.7(2) 2_554 . ? O3 Fe1 O1 91.6(2) . . ? O1 Fe1 O1 78.9(3) 2_554 . ? C1 O1 Fe1 113.6(5) . . ? C2 O2 Fe1 115.2(5) . . ? C3 O3 Fe1 114.8(5) . . ? O1 C1 O1 126.2(9) . 6_565 ? O1 C1 C1 116.9(5) . 5_564 ? O1 C1 C1 116.9(5) 6_565 5_564 ? O4 C2 O2 126.4(8) . . ? O4 C2 C3 120.0(9) . . ? O2 C2 C3 113.6(8) . . ? O5 C3 O3 126.0(8) . . ? O5 C3 C2 120.2(9) . . ? O3 C3 C2 113.8(8) . . ? C13 S1 C11 94.6(4) . . ? C14 S2 C11 94.7(4) . . ? C15 S3 C12 94.6(4) . . ? C16 S4 C12 95.1(4) . . ? C22 S5 C21 94.5(5) . . ? C12 C11 S2 121.5(6) . . ? C12 C11 S1 122.8(6) . . ? S2 C11 S1 115.7(5) . . ? C11 C12 S4 121.4(6) . . ? C11 C12 S3 122.9(6) . . ? S4 C12 S3 115.7(5) . . ? C14 C13 S1 117.3(7) . . ? C13 C14 S2 117.6(7) . . ? C16 C15 S3 118.7(7) . . ? C15 C16 S4 115.9(6) . . ? C21 C21 S5 122.8(4) 5_565 . ? C21 C21 S5 122.8(4) 5_565 2 ? S5 C21 S5 114.5(7) . 2 ? C22 C22 S5 118.3(3) 2 . ? C102 C101 C102 116.3(13) 6 . ? C102 C101 C201 121.8(7) 6 . ? C102 C101 C201 121.8(7) . . ? C103 C102 C101 120.2(12) . . ? C104 C103 C102 123.8(15) . . ? C103 C104 C103 115.7(18) . 6 ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 1.246 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.103 #===END data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H61 Fe2 N1 O24 S16' _chemical_formula_weight 1768.72 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6100(10) _cell_length_b 14.0850(10) _cell_length_c 14.2530(10) _cell_angle_alpha 118.1100(10) _cell_angle_beta 90.6600(10) _cell_angle_gamma 114.1000(10) _cell_volume 1815.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 910 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type ? _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 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7648 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7268 _reflns_number_gt 4712 _reflns_threshold_expression >4sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-97 ' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 4sigma(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^)+(0.0556P)^2^+3.4195P] 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 SHELXL _refine_ls_extinction_coef 0.0006(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7268 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1553 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.721 _refine_ls_shift/su_mean 0.030 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 Fe Fe 0.11351(7) 0.18015(7) -0.04487(6) 0.0353(2) Uani 1 1 d . . . S1 S 0.35948(13) 0.05209(13) 0.14716(12) 0.0425(3) Uani 1 1 d . . . S2 S 0.62214(13) 0.11859(14) 0.23991(13) 0.0471(4) Uani 1 1 d . . . S3 S 0.45583(14) 0.16183(14) -0.00190(12) 0.0454(4) Uani 1 1 d . . . S4 S 0.72474(14) 0.23316(14) 0.08211(13) 0.0466(4) Uani 1 1 d . . . S5 S 0.72840(13) 0.47342(13) 0.37189(12) 0.0426(3) Uani 1 1 d . . . S6 S 0.49209(13) 0.43005(13) 0.25150(12) 0.0421(3) Uani 1 1 d . . . S7 S 0.55122(14) 0.34762(13) 0.49998(12) 0.0427(3) Uani 1 1 d . . . S8 S 0.32063(14) 0.30249(14) 0.36977(13) 0.0480(4) Uani 1 1 d . . . O1 O 0.0275(4) 0.2757(4) 0.0426(3) 0.0481(10) Uani 1 1 d . . . O2 O 0.2710(3) 0.3393(3) 0.0411(3) 0.0410(9) Uani 1 1 d . . . O3 O 0.2000(4) 0.0918(4) -0.1431(3) 0.0487(10) Uani 1 1 d . . . O4 O 0.0645(4) 0.1860(4) -0.1756(3) 0.0444(9) Uani 1 1 d . . . O5 O -0.0580(3) 0.0188(3) -0.0992(3) 0.0436(9) Uani 1 1 d . . . O6 O 0.1501(3) 0.1303(3) 0.0639(3) 0.0410(9) Uani 1 1 d . . . O7 O 0.0744(5) 0.4671(4) 0.1691(4) 0.0737(14) Uani 1 1 d . . . O8 O 0.3349(5) 0.5276(4) 0.1796(4) 0.0712(14) Uani 1 1 d . . . O9 O 0.2056(5) 0.0006(5) -0.3185(4) 0.0778(15) Uani 1 1 d . . . O10 O 0.0733(5) 0.1134(4) -0.3511(3) 0.0670(13) Uani 1 1 d . . . C1 C 0.1053(6) 0.3894(6) 0.1100(5) 0.0434(13) Uani 1 1 d . . . C2 C 0.2505(6) 0.4267(5) 0.1131(5) 0.0463(14) Uani 1 1 d . . . C3 C 0.1749(6) 0.0662(6) -0.2424(5) 0.0507(15) Uani 1 1 d . . . C4 C 0.0982(5) 0.1260(5) -0.2609(5) 0.0436(13) Uani 1 1 d . . . C5 C 0.0600(5) 0.0326(5) 0.0477(4) 0.0353(12) Uani 1 1 d . . . C11 C 0.5229(5) 0.1196(5) 0.1520(4) 0.0384(12) Uani 1 1 d . . . C12 C 0.5655(5) 0.1677(5) 0.0861(4) 0.0403(12) Uani 1 1 d . . . C13 C 0.3791(5) 0.0179(5) 0.2460(4) 0.0407(13) Uani 1 1 d . . . C14 C 0.5013(5) 0.0500(5) 0.2904(4) 0.0408(13) Uani 1 1 d . . . C15 C 0.5708(6) 0.2363(5) -0.0529(4) 0.0429(13) Uani 1 1 d . . . C16 C 0.6971(6) 0.2724(5) -0.0110(5) 0.0452(14) Uani 1 1 d . . . C17 C 0.2564(8) -0.0465(8) 0.2723(7) 0.0591(18) Uani 1 1 d . . . C18 C 0.5422(8) 0.0353(8) 0.3809(6) 0.0526(16) Uani 1 1 d . . . C19 C 0.5211(9) 0.2553(8) -0.1364(7) 0.0628(19) Uani 1 1 d . . . C20 C 0.8125(9) 0.3445(9) -0.0389(8) 0.0627(19) Uani 1 1 d . . . C21 C 0.5621(5) 0.4156(5) 0.3474(4) 0.0358(12) Uani 1 1 d . . . C22 C 0.4868(5) 0.3618(5) 0.4012(4) 0.0380(12) Uani 1 1 d . . . C23 C 0.7465(5) 0.5261(5) 0.2817(4) 0.0405(12) Uani 1 1 d . . . C24 C 0.6365(5) 0.5053(5) 0.2257(4) 0.0385(12) Uani 1 1 d . . . C25 C 0.4017(5) 0.2683(5) 0.5190(4) 0.0408(13) Uani 1 1 d . . . C26 C 0.2954(6) 0.2490(5) 0.4590(5) 0.0438(13) Uani 1 1 d . . . C27 C 0.8822(6) 0.5870(7) 0.2725(6) 0.0499(15) Uani 1 1 d . . . C28 C 0.6277(9) 0.5407(9) 0.1427(7) 0.0559(18) Uani 1 1 d . . . C29 C 0.4061(9) 0.2268(8) 0.5987(7) 0.0538(17) Uani 1 1 d . . . C30 C 0.1567(7) 0.1857(8) 0.4610(8) 0.0600(18) Uani 1 1 d . . . O51 O 0.1372(6) -0.1248(5) -0.5487(5) 0.0674(14) Uani 1 1 d . . . O52 O 0.2801(7) 0.7391(7) 0.3469(6) 0.094(2) Uani 1 1 d . . . N101 N 0.019(4) -0.229(4) -0.256(4) 0.27(2) Uani 0.50 1 d P . . C101 C 0.010(2) -0.309(3) -0.326(3) 0.114(9) Uani 0.50 1 d P . . C102 C 0.0045(9) -0.4019(13) -0.4086(9) 0.097(3) Uani 1 1 d . . . C103 C -0.0648(9) -0.5164(13) -0.4243(10) 0.092(3) Uani 1 1 d . . . C104 C 0.0710(9) -0.3862(13) -0.4860(11) 0.099(3) Uani 1 1 d . . . H1 H 0.191(9) -0.085(8) 0.218(7) 0.10(3) Uiso 1 1 d . . . H2 H 0.251(11) -0.114(10) 0.267(9) 0.16(5) Uiso 1 1 d . . . H3 H 0.265(8) -0.009(7) 0.349(7) 0.10(3) Uiso 1 1 d . . . H4 H 0.577(8) 0.108(7) 0.452(7) 0.10(3) Uiso 1 1 d . . . H5 H 0.599(8) 0.000(7) 0.360(6) 0.09(3) Uiso 1 1 d . . . H6 H 0.476(6) -0.013(6) 0.388(5) 0.047(19) Uiso 1 1 d . . . H7 H -0.458(8) -0.183(7) -0.811(7) 0.09(3) Uiso 1 1 d . . . H8 H -0.584(7) -0.288(7) -0.832(6) 0.08(2) Uiso 1 1 d . . . H9 H -0.482(7) -0.306(7) -0.893(6) 0.09(3) Uiso 1 1 d . . . H10 H 0.853(8) 0.415(7) 0.009(7) 0.08(3) Uiso 1 1 d . . . H11 H 0.866(7) 0.309(6) -0.050(6) 0.07(2) Uiso 1 1 d . . . H12 H 0.789(8) 0.329(7) -0.105(7) 0.10(3) Uiso 1 1 d . . . H13 H 0.873(5) 0.606(5) 0.219(4) 0.038(15) Uiso 1 1 d . . . H14 H 0.916(6) 0.533(6) 0.230(5) 0.056(18) Uiso 1 1 d . . . H15 H 0.943(6) 0.641(6) 0.344(5) 0.057(18) Uiso 1 1 d . . . H16 H 0.539(12) 0.519(10) 0.114(9) 0.16(5) Uiso 1 1 d . . . H17 H 0.640(8) 0.502(8) 0.089(7) 0.09(3) Uiso 1 1 d . . . H18 H 0.654(10) 0.608(9) 0.169(8) 0.11(5) Uiso 1 1 d . . . H19 H 0.440(10) 0.165(10) 0.569(8) 0.15(4) Uiso 1 1 d . . . H20 H 0.459(8) 0.286(8) 0.652(7) 0.09(3) Uiso 1 1 d . . . H21 H 0.333(7) 0.208(6) 0.618(6) 0.07(2) Uiso 1 1 d . . . H22 H 0.106(8) 0.130(7) 0.389(7) 0.09(3) Uiso 1 1 d . . . H23 H 0.121(9) 0.230(8) 0.472(7) 0.11(4) Uiso 1 1 d . . . H24 H 0.152(7) 0.138(7) 0.490(6) 0.09(3) Uiso 1 1 d . . . H103 H -0.130(8) 0.468(7) -0.381(7) 0.10(3) Uiso 1 1 d . . . H104 H 0.114(8) -0.295(7) -0.458(6) 0.09(3) Uiso 1 1 d . . . H51 H -0.081(8) 0.117(7) -0.425(7) 0.09(3) Uiso 1 1 d . . . H52 H -0.150(9) 0.085(8) -0.516(8) 0.11(4) Uiso 1 1 d . . . H53 H -0.242(7) 0.317(7) -0.298(6) 0.06(3) Uiso 1 1 d . . . H54 H -0.221(8) 0.244(8) -0.368(7) 0.09(3) Uiso 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 Fe 0.0306(4) 0.0419(5) 0.0376(4) 0.0249(4) 0.0071(3) 0.0157(3) S1 0.0349(7) 0.0457(8) 0.0452(8) 0.0229(7) 0.0068(6) 0.0185(6) S2 0.0352(7) 0.0627(10) 0.0572(9) 0.0407(8) 0.0111(6) 0.0233(7) S3 0.0456(8) 0.0487(8) 0.0474(8) 0.0279(7) 0.0047(6) 0.0234(7) S4 0.0420(8) 0.0575(9) 0.0552(9) 0.0374(8) 0.0136(7) 0.0264(7) S5 0.0348(7) 0.0456(8) 0.0501(8) 0.0276(7) 0.0050(6) 0.0182(6) S6 0.0342(7) 0.0473(8) 0.0481(8) 0.0288(7) 0.0048(6) 0.0173(6) S7 0.0419(8) 0.0427(8) 0.0461(8) 0.0263(7) 0.0045(6) 0.0185(6) S8 0.0338(7) 0.0513(9) 0.0536(9) 0.0317(7) 0.0011(6) 0.0103(6) O1 0.036(2) 0.053(2) 0.059(3) 0.032(2) 0.0176(19) 0.0195(19) O2 0.0296(18) 0.042(2) 0.055(2) 0.0298(19) 0.0109(17) 0.0155(17) O3 0.048(2) 0.064(3) 0.041(2) 0.027(2) 0.0096(18) 0.033(2) O4 0.043(2) 0.054(2) 0.046(2) 0.034(2) 0.0096(18) 0.0229(19) O5 0.0318(19) 0.055(2) 0.048(2) 0.035(2) -0.0020(16) 0.0129(17) O6 0.037(2) 0.040(2) 0.046(2) 0.0296(18) 0.0011(16) 0.0091(17) O7 0.083(3) 0.072(3) 0.070(3) 0.024(3) 0.023(3) 0.054(3) O8 0.059(3) 0.040(3) 0.090(4) 0.024(3) -0.004(3) 0.013(2) O9 0.079(3) 0.113(4) 0.044(3) 0.027(3) 0.017(2) 0.063(3) O10 0.074(3) 0.086(3) 0.042(2) 0.041(2) 0.004(2) 0.029(3) C1 0.045(3) 0.050(4) 0.048(3) 0.033(3) 0.012(3) 0.026(3) C2 0.049(3) 0.037(3) 0.057(4) 0.030(3) 0.008(3) 0.017(3) C3 0.041(3) 0.061(4) 0.041(3) 0.022(3) 0.006(3) 0.023(3) C4 0.034(3) 0.044(3) 0.043(3) 0.026(3) 0.000(2) 0.005(2) C5 0.033(3) 0.046(3) 0.035(3) 0.025(3) 0.007(2) 0.020(3) C11 0.032(3) 0.042(3) 0.038(3) 0.019(3) 0.003(2) 0.017(2) C12 0.040(3) 0.037(3) 0.044(3) 0.020(3) 0.008(2) 0.020(2) C13 0.037(3) 0.038(3) 0.038(3) 0.019(2) 0.011(2) 0.012(2) C14 0.049(3) 0.041(3) 0.038(3) 0.022(3) 0.009(2) 0.024(3) C15 0.053(3) 0.038(3) 0.042(3) 0.025(3) 0.003(3) 0.020(3) C16 0.052(3) 0.041(3) 0.042(3) 0.027(3) 0.007(3) 0.015(3) C17 0.051(4) 0.065(5) 0.058(5) 0.031(4) 0.020(4) 0.026(4) C18 0.058(4) 0.070(5) 0.049(4) 0.039(4) 0.021(3) 0.036(4) C19 0.067(5) 0.062(5) 0.060(5) 0.038(4) -0.001(4) 0.024(4) C20 0.070(5) 0.061(5) 0.059(5) 0.037(4) 0.009(4) 0.025(4) C21 0.030(3) 0.038(3) 0.044(3) 0.023(2) 0.005(2) 0.018(2) C22 0.031(3) 0.035(3) 0.044(3) 0.021(3) 0.002(2) 0.011(2) C23 0.045(3) 0.043(3) 0.044(3) 0.025(3) 0.015(2) 0.025(3) C24 0.040(3) 0.041(3) 0.039(3) 0.023(3) 0.011(2) 0.021(2) C25 0.048(3) 0.030(3) 0.039(3) 0.017(2) 0.011(2) 0.014(2) C26 0.046(3) 0.035(3) 0.046(3) 0.021(3) 0.009(3) 0.015(3) C27 0.037(3) 0.066(4) 0.046(4) 0.030(3) 0.015(3) 0.022(3) C28 0.073(5) 0.060(5) 0.054(4) 0.034(4) 0.022(4) 0.041(4) C29 0.068(5) 0.058(5) 0.055(4) 0.039(4) 0.024(4) 0.034(4) C30 0.046(4) 0.060(5) 0.075(5) 0.041(4) 0.014(4) 0.019(4) O51 0.068(3) 0.086(4) 0.049(3) 0.030(3) 0.014(3) 0.043(3) O52 0.080(5) 0.071(4) 0.086(5) 0.015(4) 0.018(4) 0.027(4) N101 0.31(4) 0.37(5) 0.46(6) 0.37(5) 0.26(4) 0.26(4) C101 0.071(12) 0.13(2) 0.17(3) 0.09(2) 0.013(16) 0.058(15) C102 0.062(5) 0.144(10) 0.098(8) 0.078(8) 0.001(5) 0.043(7) C103 0.060(5) 0.143(10) 0.093(7) 0.088(8) 0.010(5) 0.034(6) C104 0.067(6) 0.139(10) 0.112(8) 0.094(8) 0.003(6) 0.033(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O2 1.970(4) . ? Fe O1 1.976(4) . ? Fe O3 1.982(4) . ? Fe O4 1.990(4) . ? Fe O6 2.081(3) . ? Fe O5 2.083(4) . ? S1 C11 1.723(5) . ? S1 C13 1.729(6) . ? S2 C11 1.702(5) . ? S2 C14 1.730(6) . ? S3 C12 1.726(5) . ? S3 C15 1.734(6) . ? S4 C12 1.712(6) . ? S4 C16 1.731(5) . ? S5 C21 1.716(5) . ? S5 C23 1.739(5) . ? S6 C21 1.716(5) . ? S6 C24 1.732(5) . ? S7 C22 1.716(5) . ? S7 C25 1.745(6) . ? S8 C22 1.712(5) . ? S8 C26 1.733(6) . ? O1 C1 1.285(7) . ? O2 C2 1.296(7) . ? O3 C3 1.281(7) . ? O4 C4 1.288(7) . ? O5 C5 1.244(6) 2 ? O6 C5 1.249(6) . ? O7 C1 1.222(7) . ? O8 C2 1.204(7) . ? O9 C3 1.220(7) . ? O10 C4 1.226(6) . ? C1 C2 1.541(8) . ? C3 C4 1.546(8) . ? C5 O5 1.244(6) 2 ? C5 C5 1.540(9) 2 ? C11 C12 1.386(8) . ? C13 C14 1.343(7) . ? C13 C17 1.507(9) . ? C14 C18 1.499(8) . ? C15 C16 1.360(8) . ? C15 C19 1.494(8) . ? C16 C20 1.505(10) . ? C21 C22 1.396(7) . ? C23 C24 1.343(7) . ? C23 C27 1.497(8) . ? C24 C28 1.501(9) . ? C25 C26 1.345(8) . ? C25 C29 1.512(8) . ? C26 C30 1.497(9) . ? N101 C101 1.06(5) . ? C101 C102 1.25(3) . ? C102 C104 1.404(14) . ? C102 C103 1.377(15) . ? C103 C104 1.337(15) 2_544 ? C104 C103 1.337(15) 2_544 ? 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 O2 Fe O1 82.31(16) . . ? O2 Fe O3 96.55(16) . . ? O1 Fe O3 173.67(17) . . ? O2 Fe O4 100.47(15) . . ? O1 Fe O4 92.59(16) . . ? O3 Fe O4 81.47(16) . . ? O2 Fe O6 90.46(14) . . ? O1 Fe O6 97.20(16) . . ? O3 Fe O6 89.02(15) . . ? O4 Fe O6 166.22(16) . . ? O2 Fe O5 166.43(15) . . ? O1 Fe O5 90.30(16) . . ? O3 Fe O5 92.01(16) . . ? O4 Fe O5 91.18(14) . . ? O6 Fe O5 79.14(13) . . ? C11 S1 C13 95.6(3) . . ? C11 S2 C14 96.5(3) . . ? C12 S3 C15 96.1(3) . . ? C12 S4 C16 96.1(3) . . ? C21 S5 C23 95.9(3) . . ? C21 S6 C24 95.9(3) . . ? C22 S7 C25 95.7(3) . . ? C22 S8 C26 95.8(3) . . ? C1 O1 Fe 114.6(3) . . ? C2 O2 Fe 114.7(3) . . ? C3 O3 Fe 115.2(4) . . ? C4 O4 Fe 114.7(3) . . ? C5 O5 Fe 113.9(3) 2 . ? C5 O6 Fe 113.9(3) . . ? O7 C1 O1 126.5(6) . . ? O7 C1 C2 119.1(6) . . ? O1 C1 C2 114.4(5) . . ? O8 C2 O2 124.7(6) . . ? O8 C2 C1 121.4(6) . . ? O2 C2 C1 113.8(5) . . ? O9 C3 O3 125.6(6) . . ? O9 C3 C4 120.6(5) . . ? O3 C3 C4 113.8(5) . . ? O10 C4 O4 125.5(6) . . ? O10 C4 C3 120.3(6) . . ? O4 C4 C3 114.2(5) . . ? O5 C5 O6 127.0(4) 2 . ? O5 C5 C5 116.6(6) 2 2 ? O6 C5 C5 116.4(5) . 2 ? C12 C11 S2 124.4(4) . . ? C12 C11 S1 120.8(4) . . ? S2 C11 S1 114.8(3) . . ? C11 C12 S4 124.4(4) . . ? C11 C12 S3 120.6(4) . . ? S4 C12 S3 115.0(3) . . ? C14 C13 C17 126.7(6) . . ? C14 C13 S1 117.0(4) . . ? C17 C13 S1 116.3(5) . . ? C13 C14 C18 126.3(6) . . ? C13 C14 S2 116.0(4) . . ? C18 C14 S2 117.7(5) . . ? C16 C15 C19 127.2(6) . . ? C16 C15 S3 116.0(4) . . ? C19 C15 S3 116.8(5) . . ? C15 C16 C20 124.7(6) . . ? C15 C16 S4 116.7(4) . . ? C20 C16 S4 118.6(5) . . ? C22 C21 S5 123.8(4) . . ? C22 C21 S6 121.1(4) . . ? S5 C21 S6 115.0(3) . . ? C21 C22 S8 121.2(4) . . ? C21 C22 S7 123.4(4) . . ? S8 C22 S7 115.4(3) . . ? C24 C23 C27 126.9(5) . . ? C24 C23 S5 116.4(4) . . ? C27 C23 S5 116.8(4) . . ? C23 C24 C28 125.9(6) . . ? C23 C24 S6 116.8(4) . . ? C28 C24 S6 117.4(5) . . ? C26 C25 C29 127.5(6) . . ? C26 C25 S7 116.0(4) . . ? C29 C25 S7 116.5(5) . . ? C25 C26 C30 126.8(6) . . ? C25 C26 S8 117.0(4) . . ? C30 C26 S8 116.2(5) . . ? N101 C101 C102 178(4) . . ? C101 C102 C104 118(2) . . ? C101 C102 C103 121.7(19) . . ? C104 C102 C103 120.3(12) . . ? C104 C103 C102 120.3(11) 2_544 . ? C103 C104 C102 119.4(12) 2_544 . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.467 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.099