Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ahmed, Moawia O.' 'Kaldis, John H.' 'Mathur, Pradeep' 'McGlinchey, Michael J.' _publ_contact_author_name 'Prof Pradeep Mathur' _publ_contact_author_address ; Chemistry Indian Institute of Technology Bombay Powai Bombay 400 076 INDIA ; _publ_contact_author_email 'MATHUR@CHEM.IITB.AC.IN' _publ_section_title ; ? ; data_1 _database_code_CSD 168671 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H20 Fe3 Mo2 O8 S2' _chemical_formula_weight 980.05 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Mo' 'Mo' -1.6832 0.6857 '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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2463(9) _cell_length_b 18.9432(9) _cell_length_c 17.4513(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.538(5) _cell_angle_gamma 90.00 _cell_volume 3383.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5776 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max .32 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.924 _exptl_crystal_density_method ? _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 2.151 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.472290 _exptl_absorpt_correction_T_max 0.719342 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25378 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5776 _reflns_number_observed 4253 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXTL-V.5.03 Sheldrick, 1994' _computing_structure_refinement 'SHELXL-V.5.03 Sheldrick, 1994' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 23 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00052(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5753 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_obs 0.0286 _refine_ls_wR_factor_all 0.0627 _refine_ls_wR_factor_obs 0.0563 _refine_ls_goodness_of_fit_all 0.966 _refine_ls_goodness_of_fit_obs 1.032 _refine_ls_restrained_S_all 0.973 _refine_ls_restrained_S_obs 1.032 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo -0.17667(3) 0.16891(2) 0.65097(2) 0.03125(9) Uani 1 d . . Mo2 Mo 0.08508(3) 0.17628(2) 0.66578(2) 0.03261(9) Uani 1 d . . Fe1 Fe -0.03523(5) 0.14543(3) 0.52234(3) 0.03362(14) Uani 1 d . . Fe2 Fe -0.06930(5) 0.26836(3) 0.75662(3) 0.03243(13) Uani 1 d . . Fe3 Fe 0.04013(5) 0.39135(3) 0.75665(3) 0.04047(15) Uani 1 d . . S1 S -0.03538(9) 0.07317(5) 0.62401(5) 0.0391(2) Uani 1 d . . S2 S -0.05538(9) 0.15483(5) 0.76893(5) 0.0376(2) Uani 1 d . . C1 C -0.0559(3) 0.2307(2) 0.5909(2) 0.0287(8) Uani 1 d . . C2 C 0.0245(3) 0.2899(2) 0.6020(2) 0.0310(8) Uani 1 d . . C3 C 0.1088(3) 0.3268(2) 0.5460(2) 0.0352(9) Uani 1 d . . C4 C 0.0904(4) 0.3989(2) 0.5369(2) 0.0491(10) Uani 1 d . . H4 H 0.0286(4) 0.4218(2) 0.5655(2) 0.059 Uiso 1 calc R . C5 C 0.1624(5) 0.4379(3) 0.4858(2) 0.0661(13) Uani 1 d . . H5 H 0.1478(5) 0.4861(3) 0.4798(2) 0.079 Uiso 1 calc R . C6 C 0.2558(5) 0.4044(3) 0.4440(2) 0.0648(13) Uani 1 d . . H6 H 0.3045(5) 0.4301(3) 0.4100(2) 0.078 Uiso 1 calc R . C7 C 0.2766(4) 0.3335(2) 0.4527(2) 0.0561(12) Uani 1 d . . H7 H 0.3406(4) 0.3111(2) 0.4253(2) 0.067 Uiso 1 calc R . C8 C 0.2024(4) 0.2948(2) 0.5023(2) 0.0455(10) Uani 1 d . . H8 H 0.2156(4) 0.2464(2) 0.5064(2) 0.055 Uiso 1 calc R . C9 C -0.0125(3) 0.3311(2) 0.6689(2) 0.0318(8) Uani 1 d . . C10 C -0.1195(3) 0.3612(2) 0.6975(2) 0.0323(8) Uani 1 d . . C11 C -0.2434(3) 0.3916(2) 0.6674(2) 0.0372(9) Uani 1 d . . C12 C -0.3246(4) 0.4311(2) 0.7126(2) 0.0458(10) Uani 1 d . . H12 H -0.2985(4) 0.4402(2) 0.7633(2) 0.055 Uiso 1 calc R . C13 C -0.4422(4) 0.4569(2) 0.6842(3) 0.0597(12) Uani 1 d . . H13 H -0.4956(4) 0.4828(2) 0.7155(3) 0.072 Uiso 1 calc R . C14 C -0.4804(5) 0.4440(3) 0.6083(3) 0.0702(14) Uani 1 d . . H14 H -0.5606(5) 0.4608(3) 0.5889(3) 0.084 Uiso 1 calc R . C15 C -0.4019(5) 0.4068(2) 0.5615(3) 0.0665(13) Uani 1 d . . H15 H -0.4280(5) 0.3992(2) 0.5105(3) 0.080 Uiso 1 calc R . C16 C -0.2834(4) 0.3806(2) 0.5902(2) 0.0476(10) Uani 1 d . . H16 H -0.2299(4) 0.3555(2) 0.5582(2) 0.057 Uiso 1 calc R . C17 C 0.2999(4) 0.1592(3) 0.6267(3) 0.0597(13) Uani 1 d . . H17 H 0.3257(4) 0.1542(3) 0.5735(3) 0.072 Uiso 1 calc R . C18 C 0.2707(4) 0.1038(3) 0.6756(3) 0.0639(13) Uani 1 d . . H18 H 0.2735(4) 0.0534(3) 0.6630(3) 0.077 Uiso 1 calc R . C19 C 0.2513(4) 0.1327(3) 0.7495(3) 0.0638(13) Uani 1 d . . H19 H 0.2388(4) 0.1057(3) 0.7966(3) 0.077 Uiso 1 calc R . C20 C 0.2666(4) 0.2066(3) 0.7445(2) 0.0562(12) Uani 1 d . . H20 H 0.2670(4) 0.2398(3) 0.7876(2) 0.067 Uiso 1 calc R . C21 C 0.2969(3) 0.2232(3) 0.6684(2) 0.0559(12) Uani 1 d . . H21 H 0.3216(3) 0.2698(3) 0.6495(2) 0.067 Uiso 1 calc R . C22 C -0.3770(3) 0.2007(2) 0.5899(2) 0.0515(11) Uani 1 d . . H22 H -0.3886(3) 0.2301(2) 0.5438(2) 0.062 Uiso 1 calc R . C23 C -0.3700(4) 0.1259(3) 0.5918(3) 0.0607(13) Uani 1 d . . H23 H -0.3759(4) 0.0946(3) 0.5471(3) 0.073 Uiso 1 calc R . C24 C -0.3704(4) 0.1043(2) 0.6690(3) 0.0578(12) Uani 1 d . . H24 H -0.3750(4) 0.0555(2) 0.6871(3) 0.069 Uiso 1 calc R . C25 C -0.3753(4) 0.1645(2) 0.7148(2) 0.0472(10) Uani 1 d . . H25 H -0.3841(4) 0.1650(2) 0.7705(2) 0.057 Uiso 1 calc R . C26 C -0.3824(3) 0.2241(2) 0.6659(2) 0.0462(10) Uani 1 d . . H26 H -0.3958(3) 0.2730(2) 0.6821(2) 0.055 Uiso 1 calc R . C27 C 0.1101(4) 0.1088(2) 0.4835(2) 0.0455(10) Uani 1 d . . O27 O 0.2001(3) 0.0842(2) 0.4577(2) 0.0677(9) Uani 1 d . . C28 C -0.1505(4) 0.0889(2) 0.4702(2) 0.0443(10) Uani 1 d . . O28 O -0.2214(3) 0.0524(2) 0.4377(2) 0.0653(9) Uani 1 d . . C29 C -0.0573(4) 0.2150(2) 0.4527(2) 0.0448(10) Uani 1 d . . O29 O -0.0765(3) 0.2581(2) 0.4077(2) 0.0668(9) Uani 1 d . . C30 C -0.2167(4) 0.2870(2) 0.8034(2) 0.0400(9) Uani 1 d . . O30 O -0.3104(3) 0.3005(2) 0.8339(2) 0.0582(8) Uani 1 d . . C31 C 0.0384(4) 0.2838(2) 0.8390(2) 0.0455(10) Uani 1 d . . O31 O 0.0971(3) 0.2785(2) 0.8976(2) 0.0651(9) Uani 1 d . . C32 C 0.0412(4) 0.4741(2) 0.7098(2) 0.0589(12) Uani 1 d . . O32 O 0.0381(4) 0.5275(2) 0.6783(2) 0.0961(13) Uani 1 d . . C33 C -0.0009(4) 0.4280(2) 0.8488(2) 0.0465(10) Uani 1 d . . O33 O -0.0247(3) 0.4497(2) 0.9078(2) 0.0678(9) Uani 1 d . . C34 C 0.2143(4) 0.3824(2) 0.7677(2) 0.0554(11) Uani 1 d . . O34 O 0.3255(3) 0.3787(2) 0.7731(2) 0.0928(12) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0252(2) 0.0385(2) 0.0303(2) 0.00153(14) 0.00418(12) -0.00361(13) Mo2 0.0248(2) 0.0462(2) 0.0267(2) -0.00151(14) -0.00013(12) 0.00370(14) Fe1 0.0324(3) 0.0410(3) 0.0275(3) -0.0034(2) 0.0013(2) -0.0015(2) Fe2 0.0307(3) 0.0420(3) 0.0248(3) 0.0000(2) 0.0040(2) -0.0009(2) Fe3 0.0384(3) 0.0489(4) 0.0342(3) -0.0080(2) 0.0017(2) -0.0104(3) S1 0.0435(6) 0.0388(6) 0.0353(5) 0.0004(4) 0.0027(4) 0.0022(4) S2 0.0426(6) 0.0434(6) 0.0272(5) 0.0047(4) 0.0052(4) 0.0033(4) C1 0.025(2) 0.042(2) 0.020(2) 0.0000(15) -0.0010(13) 0.002(2) C2 0.026(2) 0.041(2) 0.025(2) 0.000(2) 0.0013(14) -0.003(2) C3 0.036(2) 0.045(2) 0.025(2) 0.001(2) 0.0033(15) -0.013(2) C4 0.048(3) 0.059(3) 0.042(2) 0.005(2) 0.016(2) 0.000(2) C5 0.081(4) 0.060(3) 0.059(3) 0.018(2) 0.018(3) -0.011(3) C6 0.074(3) 0.077(4) 0.045(3) 0.003(2) 0.023(2) -0.030(3) C7 0.055(3) 0.068(3) 0.047(3) -0.015(2) 0.026(2) -0.021(2) C8 0.045(3) 0.053(3) 0.040(2) -0.012(2) 0.017(2) -0.016(2) C9 0.030(2) 0.036(2) 0.029(2) 0.002(2) 0.0036(15) -0.009(2) C10 0.031(2) 0.035(2) 0.031(2) -0.001(2) 0.005(2) -0.009(2) C11 0.034(2) 0.037(2) 0.041(2) 0.006(2) 0.004(2) -0.008(2) C12 0.042(3) 0.043(2) 0.053(3) 0.001(2) 0.011(2) -0.003(2) C13 0.041(3) 0.052(3) 0.087(4) 0.006(3) 0.015(2) 0.010(2) C14 0.047(3) 0.063(3) 0.099(4) 0.024(3) -0.011(3) 0.006(2) C15 0.065(3) 0.066(3) 0.066(3) 0.010(3) -0.020(3) -0.006(3) C16 0.046(3) 0.049(3) 0.047(3) 0.006(2) -0.004(2) -0.003(2) C17 0.022(2) 0.106(4) 0.052(3) -0.021(3) 0.000(2) 0.010(2) C18 0.036(3) 0.076(4) 0.079(4) -0.004(3) -0.011(2) 0.024(2) C19 0.039(3) 0.097(4) 0.054(3) 0.005(3) -0.017(2) 0.027(3) C20 0.027(2) 0.087(4) 0.053(3) -0.018(2) -0.015(2) 0.009(2) C21 0.020(2) 0.085(4) 0.062(3) -0.006(3) -0.005(2) -0.004(2) C22 0.026(2) 0.078(3) 0.050(3) 0.004(2) -0.004(2) -0.006(2) C23 0.028(2) 0.088(4) 0.066(3) -0.030(3) 0.006(2) -0.018(2) C24 0.037(3) 0.050(3) 0.088(4) -0.003(3) 0.016(2) -0.017(2) C25 0.033(2) 0.060(3) 0.050(3) 0.004(2) 0.014(2) -0.009(2) C26 0.019(2) 0.055(3) 0.065(3) -0.003(2) 0.005(2) -0.002(2) C27 0.048(3) 0.051(3) 0.038(2) 0.001(2) 0.006(2) -0.002(2) O27 0.055(2) 0.082(2) 0.068(2) -0.009(2) 0.024(2) 0.013(2) C28 0.048(3) 0.050(3) 0.035(2) -0.004(2) 0.000(2) 0.000(2) O28 0.065(2) 0.070(2) 0.060(2) -0.017(2) -0.015(2) -0.014(2) C29 0.042(2) 0.058(3) 0.034(2) -0.009(2) -0.002(2) -0.010(2) O29 0.087(2) 0.065(2) 0.046(2) 0.017(2) -0.020(2) -0.012(2) C30 0.045(3) 0.040(2) 0.036(2) 0.002(2) 0.006(2) -0.001(2) O30 0.054(2) 0.066(2) 0.057(2) 0.0018(15) 0.029(2) 0.0101(15) C31 0.047(3) 0.053(3) 0.037(2) -0.007(2) 0.004(2) 0.000(2) O31 0.070(2) 0.087(2) 0.036(2) -0.0015(15) -0.017(2) 0.000(2) C32 0.074(3) 0.056(3) 0.046(3) -0.008(2) -0.007(2) -0.024(2) O32 0.151(4) 0.061(2) 0.074(2) 0.004(2) -0.019(2) -0.038(2) C33 0.037(2) 0.055(3) 0.047(3) -0.004(2) -0.003(2) -0.004(2) O33 0.076(2) 0.078(2) 0.050(2) -0.022(2) 0.010(2) 0.009(2) C34 0.047(3) 0.066(3) 0.053(3) -0.016(2) 0.006(2) -0.017(2) O34 0.039(2) 0.127(3) 0.113(3) -0.018(2) 0.011(2) -0.016(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 Mo1 C1 2.029(3) . ? Mo1 C23 2.339(4) . ? Mo1 C22 2.349(4) . ? Mo1 C24 2.364(4) . ? Mo1 C25 2.365(4) . ? Mo1 S2 2.3721(9) . ? Mo1 C26 2.377(4) . ? Mo1 S1 2.3806(10) . ? Mo1 Mo2 2.6867(5) . ? Mo1 Fe1 2.7614(6) . ? Mo1 Fe2 2.8246(6) . ? Mo2 C1 2.166(3) . ? Mo2 C20 2.335(4) . ? Mo2 C21 2.344(4) . ? Mo2 C19 2.345(4) . ? Mo2 C18 2.346(4) . ? Mo2 C17 2.355(4) . ? Mo2 S2 2.3888(10) . ? Mo2 S1 2.4064(10) . ? Mo2 C2 2.490(3) . ? Mo2 Fe1 2.8025(5) . ? Mo2 Fe2 2.8774(6) . ? Fe1 C29 1.800(4) . ? Fe1 C27 1.802(4) . ? Fe1 C28 1.810(4) . ? Fe1 C1 2.027(3) . ? Fe1 S1 2.2410(10) . ? Fe2 C30 1.784(4) . ? Fe2 C31 1.796(4) . ? Fe2 C9 2.044(3) . ? Fe2 C10 2.092(3) . ? Fe2 S2 2.1653(11) . ? Fe2 Fe3 2.5856(7) . ? Fe3 C32 1.768(5) . ? Fe3 C34 1.794(5) . ? Fe3 C33 1.818(4) . ? Fe3 C9 1.966(3) . ? Fe3 C10 1.979(3) . ? Fe3 C31 2.493(4) . ? C1 C2 1.400(4) . ? C2 C9 1.467(5) . ? C2 C3 1.504(5) . ? C3 C4 1.389(5) . ? C3 C8 1.390(5) . ? C4 C5 1.394(5) . ? C5 C6 1.383(6) . ? C6 C7 1.367(6) . ? C7 C8 1.386(5) . ? C9 C10 1.351(5) . ? C10 C11 1.470(5) . ? C11 C12 1.390(5) . ? C11 C16 1.405(5) . ? C12 C13 1.373(5) . ? C13 C14 1.387(6) . ? C14 C15 1.366(6) . ? C15 C16 1.385(5) . ? C17 C18 1.393(6) . ? C17 C21 1.416(6) . ? C18 C19 1.423(6) . ? C19 C20 1.413(6) . ? C20 C21 1.412(6) . ? C22 C26 1.401(5) . ? C22 C23 1.420(6) . ? C23 C24 1.407(6) . ? C24 C25 1.394(5) . ? C25 C26 1.416(5) . ? C27 O27 1.143(4) . ? C28 O28 1.135(4) . ? C29 O29 1.144(4) . ? C30 O30 1.147(4) . ? C31 O31 1.169(4) . ? C32 O32 1.151(5) . ? C33 O33 1.145(4) . ? C34 O34 1.142(5) . ? 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 Mo1 C23 119.80(15) . . ? C1 Mo1 C22 99.09(13) . . ? C23 Mo1 C22 35.27(14) . . ? C1 Mo1 C24 154.44(14) . . ? C23 Mo1 C24 34.81(14) . . ? C22 Mo1 C24 58.09(15) . . ? C1 Mo1 C25 145.23(14) . . ? C23 Mo1 C25 57.71(14) . . ? C22 Mo1 C25 58.00(14) . . ? C24 Mo1 C25 34.28(13) . . ? C1 Mo1 S2 101.84(8) . . ? C23 Mo1 S2 138.12(13) . . ? C22 Mo1 S2 146.75(11) . . ? C24 Mo1 S2 103.72(12) . . ? C25 Mo1 S2 90.91(10) . . ? C1 Mo1 C26 111.53(13) . . ? C23 Mo1 C26 57.58(14) . . ? C22 Mo1 C26 34.48(13) . . ? C24 Mo1 C26 57.26(14) . . ? C25 Mo1 C26 34.74(13) . . ? S2 Mo1 C26 112.80(10) . . ? C1 Mo1 S1 86.98(10) . . ? C23 Mo1 S1 99.08(12) . . ? C22 Mo1 S1 129.24(11) . . ? C24 Mo1 S1 98.84(11) . . ? C25 Mo1 S1 127.57(10) . . ? S2 Mo1 S1 77.65(3) . . ? C26 Mo1 S1 155.02(10) . . ? C1 Mo1 Mo2 52.45(8) . . ? C23 Mo1 Mo2 151.97(11) . . ? C22 Mo1 Mo2 151.49(11) . . ? C24 Mo1 Mo2 148.70(11) . . ? C25 Mo1 Mo2 146.40(10) . . ? S2 Mo1 Mo2 55.94(2) . . ? C26 Mo1 Mo2 148.52(10) . . ? S1 Mo1 Mo2 56.31(2) . . ? C1 Mo1 Fe1 47.06(9) . . ? C23 Mo1 Fe1 92.86(11) . . ? C22 Mo1 Fe1 98.74(10) . . ? C24 Mo1 Fe1 119.92(11) . . ? C25 Mo1 Fe1 150.57(10) . . ? S2 Mo1 Fe1 114.44(3) . . ? C26 Mo1 Fe1 131.26(10) . . ? S1 Mo1 Fe1 51.02(3) . . ? Mo2 Mo1 Fe1 61.898(14) . . ? C1 Mo1 Fe2 73.95(9) . . ? C23 Mo1 Fe2 144.90(11) . . ? C22 Mo1 Fe2 115.61(11) . . ? C24 Mo1 Fe2 124.28(11) . . ? C25 Mo1 Fe2 91.99(10) . . ? S2 Mo1 Fe2 48.29(3) . . ? C26 Mo1 Fe2 87.54(9) . . ? S1 Mo1 Fe2 114.48(3) . . ? Mo2 Mo1 Fe2 62.886(14) . . ? Fe1 Mo1 Fe2 115.77(2) . . ? C1 Mo2 C20 136.9(2) . . ? C1 Mo2 C21 115.08(14) . . ? C20 Mo2 C21 35.13(14) . . ? C1 Mo2 C19 172.1(2) . . ? C20 Mo2 C19 35.14(15) . . ? C21 Mo2 C19 58.3(2) . . ? C1 Mo2 C18 147.11(15) . . ? C20 Mo2 C18 58.6(2) . . ? C21 Mo2 C18 58.2(2) . . ? C19 Mo2 C18 35.32(14) . . ? C1 Mo2 C17 119.84(15) . . ? C20 Mo2 C17 58.27(15) . . ? C21 Mo2 C17 35.06(14) . . ? C19 Mo2 C17 58.0(2) . . ? C18 Mo2 C17 34.48(15) . . ? C1 Mo2 S2 97.34(9) . . ? C20 Mo2 S2 95.12(12) . . ? C21 Mo2 S2 129.64(11) . . ? C19 Mo2 S2 85.16(12) . . ? C18 Mo2 S2 111.03(13) . . ? C17 Mo2 S2 142.83(12) . . ? C1 Mo2 S1 83.35(9) . . ? C20 Mo2 S1 139.69(13) . . ? C21 Mo2 S1 140.87(11) . . ? C19 Mo2 S1 104.56(13) . . ? C18 Mo2 S1 87.15(12) . . ? C17 Mo2 S1 105.89(12) . . ? S2 Mo2 S1 76.83(3) . . ? C1 Mo2 C2 34.12(11) . . ? C20 Mo2 C2 103.10(15) . . ? C21 Mo2 C2 83.88(13) . . ? C19 Mo2 C2 137.99(15) . . ? C18 Mo2 C2 136.4(2) . . ? C17 Mo2 C2 102.0(2) . . ? S2 Mo2 C2 109.72(8) . . ? S1 Mo2 C2 116.89(8) . . ? C1 Mo2 Mo1 47.96(9) . . ? C20 Mo2 Mo1 146.65(11) . . ? C21 Mo2 Mo1 160.27(11) . . ? C19 Mo2 Mo1 137.40(13) . . ? C18 Mo2 Mo1 141.19(13) . . ? C17 Mo2 Mo1 155.04(10) . . ? S2 Mo2 Mo1 55.35(2) . . ? S1 Mo2 Mo1 55.41(2) . . ? C2 Mo2 Mo1 76.94(7) . . ? C1 Mo2 Fe1 45.98(9) . . ? C20 Mo2 Fe1 152.18(12) . . ? C21 Mo2 Fe1 117.84(11) . . ? C19 Mo2 Fe1 139.63(12) . . ? C18 Mo2 Fe1 105.45(12) . . ? C17 Mo2 Fe1 95.29(10) . . ? S2 Mo2 Fe1 112.44(3) . . ? S1 Mo2 Fe1 50.26(2) . . ? C2 Mo2 Fe1 71.94(7) . . ? Mo1 Mo2 Fe1 60.361(14) . . ? C1 Mo2 Fe2 71.07(9) . . ? C20 Mo2 Fe2 88.27(11) . . ? C21 Mo2 Fe2 106.90(11) . . ? C19 Mo2 Fe2 105.79(12) . . ? C18 Mo2 Fe2 141.10(12) . . ? C17 Mo2 Fe2 141.87(11) . . ? S2 Mo2 Fe2 47.44(3) . . ? S1 Mo2 Fe2 111.83(3) . . ? C2 Mo2 Fe2 65.78(8) . . ? Mo1 Mo2 Fe2 60.901(13) . . ? Fe1 Mo2 Fe2 112.81(2) . . ? C29 Fe1 C27 96.3(2) . . ? C29 Fe1 C28 91.9(2) . . ? C27 Fe1 C28 96.6(2) . . ? C29 Fe1 C1 78.59(15) . . ? C27 Fe1 C1 129.7(2) . . ? C28 Fe1 C1 133.3(2) . . ? C29 Fe1 S1 167.77(13) . . ? C27 Fe1 S1 95.27(13) . . ? C28 Fe1 S1 90.77(12) . . ? C1 Fe1 S1 90.91(9) . . ? C29 Fe1 Mo1 112.11(13) . . ? C27 Fe1 Mo1 147.13(12) . . ? C28 Fe1 Mo1 98.62(12) . . ? C1 Fe1 Mo1 47.12(9) . . ? S1 Fe1 Mo1 55.67(3) . . ? C29 Fe1 Mo2 119.21(11) . . ? C27 Fe1 Mo2 94.49(12) . . ? C28 Fe1 Mo2 145.50(12) . . ? C1 Fe1 Mo2 50.20(8) . . ? S1 Fe1 Mo2 55.66(3) . . ? Mo1 Fe1 Mo2 57.742(13) . . ? C30 Fe2 C31 96.0(2) . . ? C30 Fe2 C9 120.2(2) . . ? C31 Fe2 C9 108.6(2) . . ? C30 Fe2 C10 82.20(15) . . ? C31 Fe2 C10 112.7(2) . . ? C9 Fe2 C10 38.12(13) . . ? C30 Fe2 S2 101.82(12) . . ? C31 Fe2 S2 92.69(13) . . ? C9 Fe2 S2 129.24(10) . . ? C10 Fe2 S2 153.87(9) . . ? C30 Fe2 Fe3 101.37(12) . . ? C31 Fe2 Fe3 66.56(13) . . ? C9 Fe2 Fe3 48.54(9) . . ? C10 Fe2 Fe3 48.66(9) . . ? S2 Fe2 Fe3 150.26(4) . . ? C30 Fe2 Mo1 96.77(12) . . ? C31 Fe2 Mo1 146.96(13) . . ? C9 Fe2 Mo1 90.84(9) . . ? C10 Fe2 Mo1 99.14(9) . . ? S2 Fe2 Mo1 54.86(3) . . ? Fe3 Fe2 Mo1 139.24(2) . . ? C30 Fe2 Mo2 150.41(12) . . ? C31 Fe2 Mo2 101.90(12) . . ? C9 Fe2 Mo2 76.01(10) . . ? C10 Fe2 Mo2 111.56(10) . . ? S2 Fe2 Mo2 54.36(3) . . ? Fe3 Fe2 Mo2 107.30(2) . . ? Mo1 Fe2 Mo2 56.212(13) . . ? C32 Fe3 C34 96.1(2) . . ? C32 Fe3 C33 94.4(2) . . ? C34 Fe3 C33 102.1(2) . . ? C32 Fe3 C9 99.3(2) . . ? C34 Fe3 C9 105.4(2) . . ? C33 Fe3 C9 147.6(2) . . ? C32 Fe3 C10 92.1(2) . . ? C34 Fe3 C10 145.5(2) . . ? C33 Fe3 C10 110.7(2) . . ? C9 Fe3 C10 40.06(13) . . ? C32 Fe3 C31 172.4(2) . . ? C34 Fe3 C31 83.9(2) . . ? C33 Fe3 C31 78.1(2) . . ? C9 Fe3 C31 88.06(13) . . ? C10 Fe3 C31 92.17(13) . . ? C32 Fe3 Fe2 144.12(13) . . ? C34 Fe3 Fe2 110.13(14) . . ? C33 Fe3 Fe2 103.09(13) . . ? C9 Fe3 Fe2 51.18(10) . . ? C10 Fe3 Fe2 52.53(10) . . ? C31 Fe3 Fe2 41.38(9) . . ? Fe1 S1 Mo1 73.31(3) . . ? Fe1 S1 Mo2 74.08(3) . . ? Mo1 S1 Mo2 68.28(3) . . ? Fe2 S2 Mo1 76.85(3) . . ? Fe2 S2 Mo2 78.20(3) . . ? Mo1 S2 Mo2 68.71(3) . . ? C2 C1 Fe1 130.1(3) . . ? C2 C1 Mo1 139.4(2) . . ? Fe1 C1 Mo1 85.82(13) . . ? C2 C1 Mo2 85.7(2) . . ? Fe1 C1 Mo2 83.82(12) . . ? Mo1 C1 Mo2 79.58(11) . . ? C1 C2 C9 111.4(3) . . ? C1 C2 C3 129.3(3) . . ? C9 C2 C3 116.5(3) . . ? C1 C2 Mo2 60.2(2) . . ? C9 C2 Mo2 100.0(2) . . ? C3 C2 Mo2 123.5(2) . . ? C4 C3 C8 117.3(3) . . ? C4 C3 C2 116.9(3) . . ? C8 C3 C2 125.8(3) . . ? C3 C4 C5 121.5(4) . . ? C6 C5 C4 119.5(4) . . ? C7 C6 C5 120.0(4) . . ? C6 C7 C8 120.1(4) . . ? C7 C8 C3 121.6(4) . . ? C10 C9 C2 139.6(3) . . ? C10 C9 Fe3 70.5(2) . . ? C2 C9 Fe3 148.9(3) . . ? C10 C9 Fe2 72.9(2) . . ? C2 C9 Fe2 112.2(2) . . ? Fe3 C9 Fe2 80.27(12) . . ? C9 C10 C11 137.3(3) . . ? C9 C10 Fe3 69.5(2) . . ? C11 C10 Fe3 139.0(3) . . ? C9 C10 Fe2 69.0(2) . . ? C11 C10 Fe2 134.1(2) . . ? Fe3 C10 Fe2 78.81(12) . . ? C12 C11 C16 117.9(3) . . ? C12 C11 C10 122.4(3) . . ? C16 C11 C10 119.7(3) . . ? C13 C12 C11 121.7(4) . . ? C12 C13 C14 119.2(4) . . ? C15 C14 C13 120.9(4) . . ? C14 C15 C16 119.9(4) . . ? C15 C16 C11 120.5(4) . . ? C18 C17 C21 108.6(4) . . ? C18 C17 Mo2 72.4(2) . . ? C21 C17 Mo2 72.0(2) . . ? C17 C18 C19 108.0(4) . . ? C17 C18 Mo2 73.1(2) . . ? C19 C18 Mo2 72.3(2) . . ? C20 C19 C18 107.7(4) . . ? C20 C19 Mo2 72.1(2) . . ? C18 C19 Mo2 72.4(2) . . ? C21 C20 C19 107.9(4) . . ? C21 C20 Mo2 72.8(2) . . ? C19 C20 Mo2 72.8(2) . . ? C20 C21 C17 107.7(4) . . ? C20 C21 Mo2 72.1(2) . . ? C17 C21 Mo2 72.9(2) . . ? C26 C22 C23 107.2(4) . . ? C26 C22 Mo1 73.8(2) . . ? C23 C22 Mo1 72.0(2) . . ? C24 C23 C22 108.1(4) . . ? C24 C23 Mo1 73.6(2) . . ? C22 C23 Mo1 72.7(2) . . ? C25 C24 C23 108.3(4) . . ? C25 C24 Mo1 72.9(2) . . ? C23 C24 Mo1 71.6(2) . . ? C24 C25 C26 107.9(4) . . ? C24 C25 Mo1 72.8(2) . . ? C26 C25 Mo1 73.1(2) . . ? C22 C26 C25 108.5(4) . . ? C22 C26 Mo1 71.7(2) . . ? C25 C26 Mo1 72.2(2) . . ? O27 C27 Fe1 178.1(4) . . ? O28 C28 Fe1 178.7(4) . . ? O29 C29 Fe1 177.2(3) . . ? O30 C30 Fe2 178.4(3) . . ? O31 C31 Fe2 163.9(4) . . ? O31 C31 Fe3 124.0(3) . . ? Fe2 C31 Fe3 72.07(13) . . ? O32 C32 Fe3 177.9(4) . . ? O33 C33 Fe3 178.2(4) . . ? O34 C34 Fe3 177.7(4) . . ? _refine_diff_density_max 0.388 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.073 #===END data_3 _database_code_CSD 168672 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H20 Fe4 Mo2 O9 S2' _chemical_formula_weight 1063.91 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Mo' 'Mo' -1.6832 0.6857 '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 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 16.3700(5) _cell_length_b 15.7216(5) _cell_length_c 28.2246(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.1690(10) _cell_angle_gamma 90.00 _cell_volume 7171.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 6329 _cell_measurement_theta_min 1.46 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'square pris' _exptl_crystal_colour red _exptl_crystal_size_max .26 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.971 _exptl_crystal_density_method ? _exptl_crystal_F_000 4176 _exptl_absorpt_coefficient_mu 2.424 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.593250 _exptl_absorpt_correction_T_max 0.737047 _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26923 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6329 _reflns_number_observed 4448 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXTL-V.5.03 Sheldrick, 1994' _computing_structure_refinement 'SHELXL-V.5.03 Sheldrick, 1994' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000062(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6317 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_obs 0.0288 _refine_ls_wR_factor_all 0.0514 _refine_ls_wR_factor_obs 0.0463 _refine_ls_goodness_of_fit_all 0.947 _refine_ls_goodness_of_fit_obs 1.037 _refine_ls_restrained_S_all 0.951 _refine_ls_restrained_S_obs 1.037 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.11742(2) 0.03159(2) 0.137819(11) 0.02701(9) Uani 1 d . . Mo2 Mo 0.20320(2) 0.03041(2) 0.057860(12) 0.03176(9) Uani 1 d . . Fe1 Fe 0.29901(3) 0.01489(3) 0.14553(2) 0.03193(14) Uani 1 d . . Fe2 Fe 0.27526(3) -0.15037(3) 0.15551(2) 0.02832(13) Uani 1 d . . Fe3 Fe 0.15314(3) -0.24742(3) 0.15907(2) 0.02959(13) Uani 1 d . . Fe4 Fe 0.14412(3) -0.11852(3) 0.09300(2) 0.02666(13) Uani 1 d . . S1 S 0.21792(6) 0.12760(6) 0.12271(4) 0.0391(3) Uani 1 d . . S2 S 0.06744(5) -0.01116(6) 0.05882(3) 0.0333(2) Uani 1 d . . C1 C 0.2692(2) -0.0664(2) 0.08966(12) 0.0278(9) Uani 1 d . . C2 C 0.3432(2) -0.0929(2) 0.11436(12) 0.0278(8) Uani 1 d . . C3 C 0.4266(2) -0.1134(2) 0.10370(14) 0.0324(9) Uani 1 d . . C4 C 0.4366(2) -0.1365(2) 0.05732(15) 0.0466(11) Uani 1 d . . H4 H 0.3911(2) -0.1363(2) 0.03292(15) 0.056 Uiso 1 calc R . C5 C 0.5142(3) -0.1597(3) 0.0471(2) 0.0649(14) Uani 1 d . . H5 H 0.5200(3) -0.1753(3) 0.0160(2) 0.078 Uiso 1 calc R . C6 C 0.5816(3) -0.1599(3) 0.0823(2) 0.0656(14) Uani 1 d . . H6 H 0.6332(3) -0.1748(3) 0.0751(2) 0.079 Uiso 1 calc R . C7 C 0.5737(2) -0.1380(3) 0.1286(2) 0.0588(13) Uani 1 d . . H7 H 0.6196(2) -0.1390(3) 0.1527(2) 0.071 Uiso 1 calc R . C8 C 0.4968(2) -0.1145(2) 0.1392(2) 0.0470(11) Uani 1 d . . H8 H 0.4920(2) -0.0992(2) 0.1704(2) 0.056 Uiso 1 calc R . C9 C 0.1719(2) -0.0784(2) 0.16440(12) 0.0266(8) Uani 1 d . . C10 C 0.1802(2) -0.1433(2) 0.19832(12) 0.0268(8) Uani 1 d . . C11 C 0.1892(2) -0.1313(2) 0.25168(12) 0.0277(8) Uani 1 d . . C12 C 0.2205(2) -0.0561(2) 0.27290(14) 0.0390(10) Uani 1 d . . H12 H 0.2366(2) -0.0132(2) 0.25372(14) 0.047 Uiso 1 calc R . C13 C 0.2283(2) -0.0433(2) 0.32223(15) 0.0479(11) Uani 1 d . . H13 H 0.2499(2) 0.0076(2) 0.33555(15) 0.057 Uiso 1 calc R . C14 C 0.2040(2) -0.1059(3) 0.35156(14) 0.0439(11) Uani 1 d . . H14 H 0.2092(2) -0.0976(3) 0.38453(14) 0.053 Uiso 1 calc R . C15 C 0.1721(2) -0.1804(2) 0.33093(14) 0.0423(10) Uani 1 d . . H15 H 0.1549(2) -0.2227(2) 0.35015(14) 0.051 Uiso 1 calc R . C16 C 0.1654(2) -0.1935(2) 0.28189(14) 0.0387(10) Uani 1 d . . H16 H 0.1445(2) -0.2449(2) 0.26887(14) 0.046 Uiso 1 calc R . C17 C -0.0226(2) 0.0429(4) 0.1468(2) 0.0624(14) Uani 1 d . . H17 H -0.0697(2) 0.0194(4) 0.1249(2) 0.075 Uiso 1 calc R . C18 C 0.0093(3) 0.1255(3) 0.1449(2) 0.0643(14) Uani 1 d . . H18 H -0.0121(3) 0.1698(3) 0.1218(2) 0.077 Uiso 1 calc R . C19 C 0.0675(3) 0.1371(3) 0.1856(2) 0.0583(13) Uani 1 d . . H19 H 0.0955(3) 0.1909(3) 0.1954(2) 0.070 Uiso 1 calc R . C20 C 0.0733(2) 0.0638(3) 0.21241(15) 0.0496(11) Uani 1 d . . H20 H 0.1064(2) 0.0565(3) 0.24427(15) 0.060 Uiso 1 calc R . C21 C 0.0179(3) 0.0037(3) 0.1884(2) 0.0538(12) Uani 1 d . . H21 H 0.0047(3) -0.0520(3) 0.2007(2) 0.065 Uiso 1 calc R . C22 C 0.1897(4) 0.1306(4) -0.0042(2) 0.077(2) Uani 1 d . . H22 H 0.1551(4) 0.1818(4) -0.0062(2) 0.092 Uiso 1 calc R . C23 C 0.1665(3) 0.0523(4) -0.0257(2) 0.074(2) Uani 1 d . . H23 H 0.1130(3) 0.0388(4) -0.0451(2) 0.089 Uiso 1 calc R . C24 C 0.2376(4) -0.0004(3) -0.0189(2) 0.0709(15) Uani 1 d . . H24 H 0.2421(4) -0.0571(3) -0.0327(2) 0.085 Uiso 1 calc R . C25 C 0.3022(3) 0.0472(3) 0.0057(2) 0.0638(14) Uani 1 d . . H25 H 0.3602(3) 0.0292(3) 0.0127(2) 0.077 Uiso 1 calc R . C26 C 0.2730(4) 0.1270(3) 0.0146(2) 0.0713(15) Uani 1 d . . H26 H 0.3069(4) 0.1751(3) 0.0284(2) 0.086 Uiso 1 calc R . O27 O 0.3905(2) 0.0407(2) 0.24350(11) 0.0739(10) Uani 1 d . . C27 C 0.3512(2) 0.0301(3) 0.2066(2) 0.0465(11) Uani 1 d . . C28 C 0.3856(2) 0.0667(2) 0.12708(15) 0.0474(11) Uani 1 d . . O28 O 0.4413(2) 0.1002(2) 0.11448(12) 0.0723(10) Uani 1 d . . O29 O 0.3179(2) -0.3065(2) 0.10762(10) 0.0567(8) Uani 1 d . . C29 C 0.2945(2) -0.2494(2) 0.12752(14) 0.0394(10) Uani 1 d . . O30 O 0.4006(2) -0.1805(2) 0.24053(11) 0.0715(10) Uani 1 d . . C30 C 0.3529(2) -0.1677(2) 0.2067(2) 0.0443(11) Uani 1 d . . C31 C 0.2155(2) -0.3113(2) 0.20204(15) 0.0397(10) Uani 1 d . . O31 O 0.2586(2) -0.3509(2) 0.23023(11) 0.0606(9) Uani 1 d . . O32 O 0.1278(2) -0.3820(2) 0.08398(11) 0.0662(9) Uani 1 d . . C32 C 0.1380(2) -0.3296(2) 0.11272(15) 0.0404(10) Uani 1 d . . O33 O -0.0001(2) -0.2819(2) 0.19769(10) 0.0617(9) Uani 1 d . . C33 C 0.0580(2) -0.2666(2) 0.18203(13) 0.0345(9) Uani 1 d . . O34 O -0.0200(2) -0.1974(2) 0.08829(10) 0.0542(8) Uani 1 d . . C34 C 0.0483(2) -0.1738(2) 0.09656(13) 0.0368(10) Uani 1 d . . O35 O 0.1695(2) -0.2207(2) 0.00889(11) 0.0795(11) Uani 1 d . . C35 C 0.1599(2) -0.1822(2) 0.0420(2) 0.0434(10) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0263(2) 0.0291(2) 0.0258(2) 0.0002(2) 0.00491(14) 0.00124(14) Mo2 0.0323(2) 0.0370(2) 0.0269(2) 0.0081(2) 0.00771(15) -0.00030(15) Fe1 0.0281(3) 0.0361(3) 0.0314(3) -0.0064(3) 0.0041(2) -0.0041(2) Fe2 0.0238(3) 0.0364(3) 0.0248(3) 0.0010(2) 0.0041(2) -0.0027(2) Fe3 0.0308(3) 0.0276(3) 0.0311(4) 0.0003(2) 0.0072(2) -0.0028(2) Fe4 0.0270(3) 0.0313(3) 0.0215(3) -0.0019(2) 0.0034(2) -0.0031(2) S1 0.0388(6) 0.0303(6) 0.0491(7) -0.0002(5) 0.0098(5) -0.0035(4) S2 0.0300(5) 0.0425(6) 0.0263(6) 0.0042(5) 0.0009(4) 0.0007(4) C1 0.033(2) 0.030(2) 0.022(2) -0.001(2) 0.011(2) -0.006(2) C2 0.025(2) 0.031(2) 0.028(2) 0.000(2) 0.006(2) -0.001(2) C3 0.027(2) 0.036(2) 0.035(3) -0.002(2) 0.009(2) -0.005(2) C4 0.039(2) 0.061(3) 0.041(3) -0.008(2) 0.008(2) -0.001(2) C5 0.053(3) 0.091(4) 0.057(4) -0.018(3) 0.030(3) -0.001(3) C6 0.036(3) 0.086(4) 0.080(4) 0.003(3) 0.025(3) 0.010(2) C7 0.024(2) 0.087(3) 0.065(4) 0.013(3) 0.007(2) 0.001(2) C8 0.033(2) 0.065(3) 0.043(3) 0.003(2) 0.007(2) -0.001(2) C9 0.027(2) 0.029(2) 0.024(2) -0.005(2) 0.002(2) -0.004(2) C10 0.027(2) 0.030(2) 0.024(2) -0.001(2) 0.006(2) -0.006(2) C11 0.028(2) 0.032(2) 0.022(2) 0.000(2) 0.003(2) 0.000(2) C12 0.047(2) 0.046(2) 0.026(3) 0.000(2) 0.011(2) -0.001(2) C13 0.060(3) 0.049(3) 0.036(3) -0.011(2) 0.008(2) -0.003(2) C14 0.045(2) 0.068(3) 0.019(2) 0.004(2) 0.007(2) 0.012(2) C15 0.044(2) 0.056(3) 0.029(3) 0.013(2) 0.010(2) 0.005(2) C16 0.043(2) 0.043(2) 0.031(3) 0.001(2) 0.009(2) -0.003(2) C17 0.021(2) 0.122(5) 0.047(3) -0.041(3) 0.012(2) -0.006(3) C18 0.058(3) 0.077(4) 0.063(4) 0.026(3) 0.025(3) 0.044(3) C19 0.059(3) 0.047(3) 0.075(4) -0.025(3) 0.030(3) 0.001(2) C20 0.046(3) 0.078(3) 0.028(3) -0.007(3) 0.016(2) 0.014(2) C21 0.059(3) 0.051(3) 0.064(4) -0.004(3) 0.046(3) -0.002(2) C22 0.101(5) 0.083(4) 0.055(4) 0.051(3) 0.037(3) 0.030(4) C23 0.049(3) 0.151(6) 0.022(3) 0.024(3) 0.005(2) -0.014(4) C24 0.110(5) 0.080(4) 0.032(3) 0.000(3) 0.041(3) -0.014(4) C25 0.058(3) 0.088(4) 0.053(4) 0.040(3) 0.033(3) 0.013(3) C26 0.092(4) 0.072(4) 0.054(4) 0.026(3) 0.025(3) -0.033(3) O27 0.053(2) 0.122(3) 0.042(2) -0.025(2) -0.005(2) -0.013(2) C27 0.040(2) 0.057(3) 0.045(3) -0.013(2) 0.012(2) -0.009(2) C28 0.043(3) 0.044(3) 0.054(3) -0.014(2) 0.005(2) -0.004(2) O28 0.055(2) 0.067(2) 0.100(3) -0.014(2) 0.029(2) -0.030(2) O29 0.049(2) 0.052(2) 0.075(2) -0.014(2) 0.027(2) 0.0066(14) C29 0.033(2) 0.045(2) 0.040(3) 0.010(2) 0.005(2) 0.000(2) O30 0.049(2) 0.103(3) 0.055(2) 0.020(2) -0.015(2) -0.003(2) C30 0.035(2) 0.057(3) 0.041(3) 0.012(2) 0.008(2) -0.002(2) C31 0.043(2) 0.027(2) 0.052(3) 0.004(2) 0.016(2) -0.002(2) O31 0.056(2) 0.053(2) 0.071(2) 0.025(2) 0.006(2) 0.0118(15) O32 0.075(2) 0.057(2) 0.070(2) -0.032(2) 0.021(2) -0.010(2) C32 0.041(2) 0.038(2) 0.045(3) -0.001(2) 0.013(2) -0.001(2) O33 0.038(2) 0.095(2) 0.057(2) -0.001(2) 0.023(2) -0.010(2) C33 0.037(2) 0.035(2) 0.029(3) -0.003(2) -0.003(2) 0.003(2) O34 0.032(2) 0.065(2) 0.060(2) 0.016(2) -0.0064(15) -0.0129(14) C34 0.038(2) 0.036(2) 0.037(3) 0.007(2) 0.007(2) 0.001(2) O35 0.097(3) 0.088(2) 0.060(3) -0.042(2) 0.034(2) -0.020(2) C35 0.040(2) 0.053(3) 0.037(3) -0.003(2) 0.007(2) -0.008(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 Mo1 C9 2.034(3) . ? Mo1 S1 2.3217(9) . ? Mo1 C18 2.338(4) . ? Mo1 S2 2.3475(10) . ? Mo1 C17 2.353(3) . ? Mo1 C19 2.364(4) . ? Mo1 C21 2.371(4) . ? Mo1 C20 2.387(4) . ? Mo1 Fe4 2.7453(5) . ? Mo1 Mo2 2.8416(4) . ? Mo1 Fe1 2.9574(6) . ? Mo2 C1 1.995(3) . ? Mo2 S2 2.3207(9) . ? Mo2 C22 2.339(4) . ? Mo2 C26 2.356(4) . ? Mo2 C23 2.363(4) . ? Mo2 S1 2.3669(10) . ? Mo2 C25 2.371(4) . ? Mo2 C24 2.375(4) . ? Mo2 Fe1 2.7214(6) . ? Mo2 Fe4 2.7763(5) . ? Fe1 C28 1.783(4) . ? Fe1 C27 1.814(5) . ? Fe1 C1 2.028(3) . ? Fe1 C2 2.090(3) . ? Fe1 S1 2.2461(11) . ? Fe1 Fe2 2.6487(7) . ? Fe2 C30 1.787(4) . ? Fe2 C29 1.796(4) . ? Fe2 C2 1.953(3) . ? Fe2 C9 2.083(3) . ? Fe2 C10 2.120(3) . ? Fe2 C1 2.269(3) . ? Fe2 Fe3 2.5296(6) . ? Fe2 Fe4 2.6008(7) . ? Fe3 C31 1.769(4) . ? Fe3 C33 1.805(4) . ? Fe3 C32 1.827(4) . ? Fe3 C10 1.987(3) . ? Fe3 Fe4 2.7418(7) . ? Fe4 C35 1.805(4) . ? Fe4 C34 1.810(4) . ? Fe4 C9 2.091(3) . ? Fe4 C1 2.221(3) . ? Fe4 S2 2.2292(10) . ? C1 C2 1.362(4) . ? C2 C3 1.481(4) . ? C3 C4 1.393(5) . ? C3 C8 1.399(5) . ? C4 C5 1.396(5) . ? C5 C6 1.362(6) . ? C6 C7 1.376(6) . ? C7 C8 1.388(5) . ? C9 C10 1.391(4) . ? C10 C11 1.502(4) . ? C11 C12 1.385(4) . ? C11 C16 1.394(4) . ? C12 C13 1.392(5) . ? C13 C14 1.383(5) . ? C14 C15 1.375(5) . ? C15 C16 1.386(5) . ? C17 C21 1.396(6) . ? C17 C18 1.404(6) . ? C18 C19 1.382(6) . ? C19 C20 1.374(5) . ? C20 C21 1.406(5) . ? C22 C26 1.382(6) . ? C22 C23 1.399(6) . ? C23 C24 1.417(6) . ? C24 C25 1.389(6) . ? C25 C26 1.380(6) . ? O27 C27 1.145(4) . ? C28 O28 1.157(4) . ? O29 C29 1.156(4) . ? O30 C30 1.150(4) . ? C31 O31 1.157(4) . ? O32 C32 1.150(4) . ? O33 C33 1.137(4) . ? O34 C34 1.165(4) . ? O35 C35 1.146(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Mo1 S1 109.79(9) . . ? C9 Mo1 C18 143.04(15) . . ? S1 Mo1 C18 99.98(14) . . ? C9 Mo1 S2 99.96(9) . . ? S1 Mo1 S2 99.30(4) . . ? C18 Mo1 S2 96.21(14) . . ? C9 Mo1 C17 113.7(2) . . ? S1 Mo1 C17 134.57(14) . . ? C18 Mo1 C17 34.84(14) . . ? S2 Mo1 C17 85.74(11) . . ? C9 Mo1 C19 123.9(2) . . ? S1 Mo1 C19 88.16(11) . . ? C18 Mo1 C19 34.18(14) . . ? S2 Mo1 C19 130.00(13) . . ? C17 Mo1 C19 56.94(15) . . ? C9 Mo1 C21 85.64(14) . . ? S1 Mo1 C21 143.64(11) . . ? C18 Mo1 C21 57.52(15) . . ? S2 Mo1 C21 110.49(13) . . ? C17 Mo1 C21 34.38(14) . . ? C19 Mo1 C21 56.86(14) . . ? C9 Mo1 C20 91.83(14) . . ? S1 Mo1 C20 110.30(12) . . ? C18 Mo1 C20 56.66(15) . . ? S2 Mo1 C20 142.17(11) . . ? C17 Mo1 C20 56.76(14) . . ? C19 Mo1 C20 33.61(13) . . ? C21 Mo1 C20 34.37(13) . . ? C9 Mo1 Fe4 49.18(9) . . ? S1 Mo1 Fe4 107.75(3) . . ? C18 Mo1 Fe4 139.52(15) . . ? S2 Mo1 Fe4 51.19(2) . . ? C17 Mo1 Fe4 110.11(12) . . ? C19 Mo1 Fe4 163.93(11) . . ? C21 Mo1 Fe4 107.08(10) . . ? C20 Mo1 Fe4 132.98(12) . . ? C9 Mo1 Mo2 92.53(9) . . ? S1 Mo1 Mo2 53.42(3) . . ? C18 Mo1 Mo2 123.28(11) . . ? S2 Mo1 Mo2 52.08(2) . . ? C17 Mo1 Mo2 134.36(12) . . ? C19 Mo1 Mo2 135.79(12) . . ? C21 Mo1 Mo2 161.91(12) . . ? C20 Mo1 Mo2 163.60(11) . . ? Fe4 Mo1 Mo2 59.565(13) . . ? C9 Mo1 Fe1 61.36(9) . . ? S1 Mo1 Fe1 48.54(3) . . ? C18 Mo1 Fe1 144.64(15) . . ? S2 Mo1 Fe1 103.80(2) . . ? C17 Mo1 Fe1 169.71(12) . . ? C19 Mo1 Fe1 117.06(11) . . ? C21 Mo1 Fe1 135.89(13) . . ? C20 Mo1 Fe1 113.33(10) . . ? Fe4 Mo1 Fe1 74.078(15) . . ? Mo2 Mo1 Fe1 55.933(13) . . ? C1 Mo2 S2 103.35(9) . . ? C1 Mo2 C22 146.1(2) . . ? S2 Mo2 C22 102.8(2) . . ? C1 Mo2 C26 116.9(2) . . ? S2 Mo2 C26 137.06(15) . . ? C22 Mo2 C26 34.2(2) . . ? C1 Mo2 C23 126.4(2) . . ? S2 Mo2 C23 87.76(11) . . ? C22 Mo2 C23 34.6(2) . . ? C26 Mo2 C23 57.0(2) . . ? C1 Mo2 S1 99.41(10) . . ? S2 Mo2 S1 98.77(3) . . ? C22 Mo2 S1 97.5(2) . . ? C26 Mo2 S1 89.24(13) . . ? C23 Mo2 S1 131.0(2) . . ? C1 Mo2 C25 89.39(14) . . ? S2 Mo2 C25 142.12(14) . . ? C22 Mo2 C25 56.8(2) . . ? C26 Mo2 C25 33.95(14) . . ? C23 Mo2 C25 57.0(2) . . ? S1 Mo2 C25 114.36(15) . . ? C1 Mo2 C24 93.7(2) . . ? S2 Mo2 C24 108.67(15) . . ? C22 Mo2 C24 57.5(2) . . ? C26 Mo2 C24 56.8(2) . . ? C23 Mo2 C24 34.8(2) . . ? S1 Mo2 C24 145.87(13) . . ? C25 Mo2 C24 34.03(15) . . ? C1 Mo2 Fe1 47.94(10) . . ? S2 Mo2 Fe1 112.23(3) . . ? C22 Mo2 Fe1 135.5(2) . . ? C26 Mo2 Fe1 105.81(13) . . ? C23 Mo2 Fe1 159.74(11) . . ? S1 Mo2 Fe1 51.82(3) . . ? C25 Mo2 Fe1 102.84(13) . . ? C24 Mo2 Fe1 128.7(2) . . ? C1 Mo2 Fe4 52.44(9) . . ? S2 Mo2 Fe4 50.92(2) . . ? C22 Mo2 Fe4 147.0(2) . . ? C26 Mo2 Fe4 162.63(14) . . ? C23 Mo2 Fe4 115.56(15) . . ? S1 Mo2 Fe4 105.46(3) . . ? C25 Mo2 Fe4 128.84(13) . . ? C24 Mo2 Fe4 107.52(12) . . ? Fe1 Mo2 Fe4 77.44(2) . . ? C1 Mo2 Mo1 87.04(9) . . ? S2 Mo2 Mo1 52.93(2) . . ? C22 Mo2 Mo1 126.18(12) . . ? C26 Mo2 Mo1 138.55(14) . . ? C23 Mo2 Mo1 135.40(12) . . ? S1 Mo2 Mo1 51.97(2) . . ? C25 Mo2 Mo1 164.85(14) . . ? C24 Mo2 Mo1 160.97(14) . . ? Fe1 Mo2 Mo1 64.187(14) . . ? Fe4 Mo2 Mo1 58.492(13) . . ? C28 Fe1 C27 86.6(2) . . ? C28 Fe1 C1 99.49(15) . . ? C27 Fe1 C1 147.2(2) . . ? C28 Fe1 C2 84.45(14) . . ? C27 Fe1 C2 111.4(2) . . ? C1 Fe1 C2 38.60(12) . . ? C28 Fe1 S1 90.95(13) . . ? C27 Fe1 S1 109.60(13) . . ? C1 Fe1 S1 102.48(10) . . ? C2 Fe1 S1 138.32(10) . . ? C28 Fe1 Fe2 128.06(12) . . ? C27 Fe1 Fe2 94.79(13) . . ? C1 Fe1 Fe2 56.18(9) . . ? C2 Fe1 Fe2 46.86(9) . . ? S1 Fe1 Fe2 135.59(3) . . ? C28 Fe1 Mo2 93.62(13) . . ? C27 Fe1 Mo2 165.53(13) . . ? C1 Fe1 Mo2 46.92(10) . . ? C2 Fe1 Mo2 82.98(10) . . ? S1 Fe1 Mo2 55.93(3) . . ? Fe2 Fe1 Mo2 96.40(2) . . ? C28 Fe1 Mo1 140.74(13) . . ? C27 Fe1 Mo1 111.95(11) . . ? C1 Fe1 Mo1 83.35(9) . . ? C2 Fe1 Mo1 116.86(9) . . ? S1 Fe1 Mo1 50.78(2) . . ? Fe2 Fe1 Mo1 86.10(2) . . ? Mo2 Fe1 Mo1 59.881(13) . . ? C30 Fe2 C29 94.1(2) . . ? C30 Fe2 C2 98.8(2) . . ? C29 Fe2 C2 89.05(15) . . ? C30 Fe2 C9 118.2(2) . . ? C29 Fe2 C9 136.59(14) . . ? C2 Fe2 C9 111.74(13) . . ? C30 Fe2 C10 92.3(2) . . ? C29 Fe2 C10 119.49(14) . . ? C2 Fe2 C10 148.64(13) . . ? C9 Fe2 C10 38.63(12) . . ? C30 Fe2 C1 133.11(14) . . ? C29 Fe2 C1 97.58(14) . . ? C2 Fe2 C1 36.69(12) . . ? C9 Fe2 C1 81.51(12) . . ? C10 Fe2 C1 119.75(12) . . ? C30 Fe2 Fe3 109.95(12) . . ? C29 Fe2 Fe3 71.93(11) . . ? C2 Fe2 Fe3 146.23(10) . . ? C9 Fe2 Fe3 70.17(9) . . ? C10 Fe2 Fe3 49.64(9) . . ? C1 Fe2 Fe3 116.86(8) . . ? C30 Fe2 Fe4 169.07(12) . . ? C29 Fe2 Fe4 93.00(12) . . ? C2 Fe2 Fe4 89.65(10) . . ? C9 Fe2 Fe4 51.60(9) . . ? C10 Fe2 Fe4 77.00(9) . . ? C1 Fe2 Fe4 53.76(8) . . ? Fe3 Fe2 Fe4 64.59(2) . . ? C30 Fe2 Fe1 97.91(12) . . ? C29 Fe2 Fe1 139.85(12) . . ? C2 Fe2 Fe1 51.35(9) . . ? C9 Fe2 Fe1 67.42(9) . . ? C10 Fe2 Fe1 98.21(9) . . ? C1 Fe2 Fe1 47.94(8) . . ? Fe3 Fe2 Fe1 136.57(2) . . ? Fe4 Fe2 Fe1 81.86(2) . . ? C31 Fe3 C33 95.5(2) . . ? C31 Fe3 C32 95.0(2) . . ? C33 Fe3 C32 96.5(2) . . ? C31 Fe3 C10 91.9(2) . . ? C33 Fe3 C10 93.79(14) . . ? C32 Fe3 C10 167.05(15) . . ? C31 Fe3 Fe2 89.78(11) . . ? C33 Fe3 Fe2 147.96(11) . . ? C32 Fe3 Fe2 114.56(11) . . ? C10 Fe3 Fe2 54.39(9) . . ? C31 Fe3 Fe4 148.07(11) . . ? C33 Fe3 Fe4 114.33(11) . . ? C32 Fe3 Fe4 92.82(12) . . ? C10 Fe3 Fe4 75.72(10) . . ? Fe2 Fe3 Fe4 58.96(2) . . ? C35 Fe4 C34 90.8(2) . . ? C35 Fe4 C9 154.0(2) . . ? C34 Fe4 C9 98.57(15) . . ? C35 Fe4 C1 85.44(14) . . ? C34 Fe4 C1 172.87(14) . . ? C9 Fe4 C1 82.47(12) . . ? C35 Fe4 S2 102.55(13) . . ? C34 Fe4 S2 87.41(11) . . ? C9 Fe4 S2 102.12(9) . . ? C1 Fe4 S2 99.29(9) . . ? C35 Fe4 Fe2 103.08(13) . . ? C34 Fe4 Fe2 119.91(12) . . ? C9 Fe4 Fe2 51.31(9) . . ? C1 Fe4 Fe2 55.46(9) . . ? S2 Fe4 Fe2 141.84(3) . . ? C35 Fe4 Fe3 97.65(13) . . ? C34 Fe4 Fe3 63.92(11) . . ? C9 Fe4 Fe3 65.64(9) . . ? C1 Fe4 Fe3 110.58(9) . . ? S2 Fe4 Fe3 145.04(3) . . ? Fe2 Fe4 Fe3 56.45(2) . . ? C35 Fe4 Mo1 153.85(13) . . ? C34 Fe4 Mo1 100.64(11) . . ? C9 Fe4 Mo1 47.40(9) . . ? C1 Fe4 Mo1 85.29(8) . . ? S2 Fe4 Mo1 55.14(3) . . ? Fe2 Fe4 Mo1 91.59(2) . . ? Fe3 Fe4 Mo1 108.50(2) . . ? C35 Fe4 Mo2 94.62(12) . . ? C34 Fe4 Mo2 141.20(11) . . ? C9 Fe4 Mo2 93.17(9) . . ? C1 Fe4 Mo2 45.39(9) . . ? S2 Fe4 Mo2 53.91(2) . . ? Fe2 Fe4 Mo2 96.19(2) . . ? Fe3 Fe4 Mo2 151.92(2) . . ? Mo1 Fe4 Mo2 61.944(13) . . ? Fe1 S1 Mo1 80.68(3) . . ? Fe1 S1 Mo2 72.25(3) . . ? Mo1 S1 Mo2 74.61(3) . . ? Fe4 S2 Mo2 75.18(3) . . ? Fe4 S2 Mo1 73.67(3) . . ? Mo2 S2 Mo1 74.99(3) . . ? C2 C1 Mo2 146.8(3) . . ? C2 C1 Fe1 73.2(2) . . ? Mo2 C1 Fe1 85.13(12) . . ? C2 C1 Fe4 128.0(2) . . ? Mo2 C1 Fe4 82.17(12) . . ? Fe1 C1 Fe4 107.98(14) . . ? C2 C1 Fe2 58.9(2) . . ? Mo2 C1 Fe2 139.7(2) . . ? Fe1 C1 Fe2 75.88(11) . . ? Fe4 C1 Fe2 70.78(9) . . ? C1 C2 C3 137.4(3) . . ? C1 C2 Fe2 84.4(2) . . ? C3 C2 Fe2 130.6(2) . . ? C1 C2 Fe1 68.2(2) . . ? C3 C2 Fe1 130.9(2) . . ? Fe2 C2 Fe1 81.79(12) . . ? C4 C3 C8 117.6(3) . . ? C4 C3 C2 119.9(3) . . ? C8 C3 C2 122.5(3) . . ? C3 C4 C5 120.6(4) . . ? C6 C5 C4 120.5(4) . . ? C5 C6 C7 120.3(4) . . ? C6 C7 C8 119.7(4) . . ? C7 C8 C3 121.3(4) . . ? C10 C9 Mo1 150.0(2) . . ? C10 C9 Fe2 72.1(2) . . ? Mo1 C9 Fe2 137.2(2) . . ? C10 C9 Fe4 115.1(2) . . ? Mo1 C9 Fe4 83.42(13) . . ? Fe2 C9 Fe4 77.09(11) . . ? C9 C10 C11 125.5(3) . . ? C9 C10 Fe3 103.4(2) . . ? C11 C10 Fe3 129.8(2) . . ? C9 C10 Fe2 69.2(2) . . ? C11 C10 Fe2 128.0(2) . . ? Fe3 C10 Fe2 75.97(11) . . ? C12 C11 C16 117.0(3) . . ? C12 C11 C10 120.7(3) . . ? C16 C11 C10 122.2(3) . . ? C11 C12 C13 121.6(3) . . ? C14 C13 C12 120.4(4) . . ? C15 C14 C13 118.6(4) . . ? C14 C15 C16 120.9(4) . . ? C15 C16 C11 121.4(4) . . ? C21 C17 C18 108.0(4) . . ? C21 C17 Mo1 73.5(2) . . ? C18 C17 Mo1 72.0(2) . . ? C19 C18 C17 107.6(4) . . ? C19 C18 Mo1 73.9(2) . . ? C17 C18 Mo1 73.2(2) . . ? C20 C19 C18 109.0(4) . . ? C20 C19 Mo1 74.1(2) . . ? C18 C19 Mo1 71.9(2) . . ? C19 C20 C21 108.4(4) . . ? C19 C20 Mo1 72.3(2) . . ? C21 C20 Mo1 72.2(2) . . ? C17 C21 C20 107.0(4) . . ? C17 C21 Mo1 72.1(2) . . ? C20 C21 Mo1 73.4(2) . . ? C26 C22 C23 108.3(5) . . ? C26 C22 Mo2 73.5(3) . . ? C23 C22 Mo2 73.6(3) . . ? C22 C23 C24 107.2(4) . . ? C22 C23 Mo2 71.8(3) . . ? C24 C23 Mo2 73.1(3) . . ? C25 C24 C23 107.2(5) . . ? C25 C24 Mo2 72.8(3) . . ? C23 C24 Mo2 72.2(3) . . ? C26 C25 C24 108.8(5) . . ? C26 C25 Mo2 72.4(2) . . ? C24 C25 Mo2 73.1(2) . . ? C25 C26 C22 108.5(5) . . ? C25 C26 Mo2 73.6(2) . . ? C22 C26 Mo2 72.2(2) . . ? O27 C27 Fe1 173.9(3) . . ? O28 C28 Fe1 179.1(4) . . ? O29 C29 Fe2 169.0(3) . . ? O30 C30 Fe2 177.3(3) . . ? O31 C31 Fe3 177.5(3) . . ? O32 C32 Fe3 178.9(3) . . ? O33 C33 Fe3 176.8(3) . . ? O34 C34 Fe4 162.5(3) . . ? O35 C35 Fe4 178.1(4) . . ? _refine_diff_density_max 0.345 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.078 #===END data_5 _database_code_CSD 168673 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H20 Fe3 Mo2 O7 S2' _chemical_formula_weight 952.04 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Mo' 'Mo' -1.6832 0.6857 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7776(11) _cell_length_b 10.9285(13) _cell_length_c 16.850(2) _cell_angle_alpha 89.301(2) _cell_angle_beta 85.743(2) _cell_angle_gamma 80.224(2) _cell_volume 1588.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 15220 _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max .22 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_method ? _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 2.286 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.576991 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15220 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15220 _reflns_number_observed 11288 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXTL-V.5.03 Sheldrick, 1994' _computing_structure_refinement 'SHELXL-V.5.03 Sheldrick, 1994' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 40 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15180 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_obs 0.0473 _refine_ls_wR_factor_all 0.1300 _refine_ls_wR_factor_obs 0.1195 _refine_ls_goodness_of_fit_all 0.978 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 0.983 _refine_ls_restrained_S_obs 1.053 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.20566(5) 0.78154(4) 0.16010(2) 0.02623(12) Uani 1 d . . Mo2 Mo 0.05960(5) 0.71083(4) 0.31462(2) 0.02550(12) Uani 1 d . . Fe1 Fe -0.04415(8) 0.77068(6) 0.07037(4) 0.0274(2) Uani 1 d . . Fe2 Fe -0.07503(7) 0.85807(6) 0.21274(4) 0.0246(2) Uani 1 d . . Fe3 Fe -0.22498(8) 0.87689(7) 0.35184(4) 0.0344(2) Uani 1 d . . S1 S 0.12355(14) 0.90537(12) 0.27577(7) 0.0316(3) Uani 1 d . . S2 S 0.03597(14) 0.94435(12) 0.10580(7) 0.0314(3) Uani 1 d . . C1 C 0.0371(5) 0.6827(4) 0.1769(2) 0.0204(10) Uani 1 d . . C2 C -0.0046(5) 0.5773(4) 0.2209(2) 0.0223(11) Uani 1 d . . C3 C 0.0805(5) 0.4486(4) 0.2074(2) 0.0244(11) Uani 1 d . . C4 C 0.0749(6) 0.3506(5) 0.2616(3) 0.0356(13) Uani 1 d . . H4A H 0.0104(6) 0.3638(5) 0.3081(3) 0.043 Uiso 1 calc R . C5 C 0.1634(6) 0.2348(5) 0.2470(3) 0.0453(14) Uani 1 d . . H5A H 0.1560(6) 0.1704(5) 0.2830(3) 0.054 Uiso 1 calc R . C6 C 0.2627(6) 0.2144(5) 0.1792(3) 0.053(2) Uani 1 d . . H6A H 0.3254(6) 0.1375(5) 0.1703(3) 0.064 Uiso 1 calc R . C7 C 0.2678(6) 0.3083(5) 0.1252(3) 0.0447(14) Uani 1 d . . H7A H 0.3326(6) 0.2940(5) 0.0788(3) 0.054 Uiso 1 calc R . C8 C 0.1785(5) 0.4239(4) 0.1382(3) 0.0310(12) Uani 1 d . . H8A H 0.1835(5) 0.4862(4) 0.1005(3) 0.037 Uiso 1 calc R . C9 C -0.1828(5) 0.7439(4) 0.2823(2) 0.0242(11) Uani 1 d . . C10 C -0.1453(5) 0.6143(4) 0.2724(2) 0.0234(11) Uani 1 d . . C11 C -0.2399(5) 0.5222(4) 0.3067(3) 0.0274(11) Uani 1 d . . C12 C -0.2879(5) 0.5116(5) 0.3872(3) 0.0340(12) Uani 1 d . . H12A H -0.2614(5) 0.5655(5) 0.4241(3) 0.041 Uiso 1 calc R . C13 C -0.3751(6) 0.4212(5) 0.4126(3) 0.0428(14) Uani 1 d . . H13A H -0.4052(6) 0.4147(5) 0.4663(3) 0.051 Uiso 1 calc R . C14 C -0.4167(6) 0.3420(5) 0.3591(3) 0.047(2) Uani 1 d . . H14A H -0.4734(6) 0.2811(5) 0.3769(3) 0.056 Uiso 1 calc R . C15 C -0.3751(6) 0.3517(5) 0.2790(3) 0.0429(14) Uani 1 d . . H15A H -0.4058(6) 0.2993(5) 0.2425(3) 0.051 Uiso 1 calc R . C16 C -0.2871(5) 0.4406(4) 0.2538(3) 0.0340(12) Uani 1 d . . H16A H -0.2582(5) 0.4463(4) 0.1999(3) 0.041 Uiso 1 calc R . C17 C 0.4507(5) 0.8338(5) 0.1259(3) 0.0440(14) Uani 1 d . . H17A H 0.4781(5) 0.9167(5) 0.1296(3) 0.053 Uiso 1 calc R . C18 C 0.4027(5) 0.7819(5) 0.0573(3) 0.0397(14) Uani 1 d . . H18A H 0.3908(5) 0.8226(5) 0.0055(3) 0.048 Uiso 1 calc R . C19 C 0.3938(5) 0.6559(5) 0.0742(3) 0.0421(14) Uani 1 d . . H19A H 0.3727(5) 0.5949(5) 0.0361(3) 0.050 Uiso 1 calc R . C20 C 0.4340(5) 0.6306(5) 0.1526(3) 0.0433(14) Uani 1 d . . H20A H 0.4471(5) 0.5491(5) 0.1785(3) 0.052 Uiso 1 calc R . C21 C 0.4686(5) 0.7416(5) 0.1843(3) 0.0435(15) Uani 1 d . . H21A H 0.5107(5) 0.7493(5) 0.2359(3) 0.052 Uiso 1 calc R . C22 C 0.0869(7) 0.6815(6) 0.4509(3) 0.054(2) Uani 1 d . . H22A H 0.0126(7) 0.7180(6) 0.4940(3) 0.065 Uiso 1 calc R . C23 C 0.2148(7) 0.7301(6) 0.4196(3) 0.051(2) Uani 1 d . . H23A H 0.2450(7) 0.8075(6) 0.4366(3) 0.061 Uiso 1 calc R . C24 C 0.3025(6) 0.6439(6) 0.3662(3) 0.051(2) Uani 1 d . . H24A H 0.4040(6) 0.6502(6) 0.3396(3) 0.061 Uiso 1 calc R . C25 C 0.2251(6) 0.5427(5) 0.3631(3) 0.0450(15) Uani 1 d . . H25A H 0.2643(6) 0.4648(5) 0.3345(3) 0.054 Uiso 1 calc R . C26 C 0.0910(6) 0.5654(5) 0.4150(3) 0.0439(15) Uani 1 d . . H26A H 0.0218(6) 0.5059(5) 0.4297(3) 0.053 Uiso 1 calc R . O27 O -0.3109(4) 0.9345(3) 0.0094(2) 0.0451(10) Uani 1 d . . C27 C -0.2096(6) 0.8695(5) 0.0339(3) 0.0317(12) Uani 1 d . . O28 O 0.1483(4) 0.7352(4) -0.0805(2) 0.0568(11) Uani 1 d . . C28 C 0.0731(5) 0.7463(4) -0.0217(3) 0.0315(12) Uani 1 d . . O29 O -0.1909(4) 0.5497(3) 0.0613(2) 0.0476(10) Uani 1 d . . C29 C -0.1308(6) 0.6344(5) 0.0654(2) 0.0348(13) Uani 1 d . . O30 O -0.3341(4) 1.0615(3) 0.1909(2) 0.0541(11) Uani 1 d . . C30 C -0.2375(6) 0.9812(5) 0.2057(3) 0.0360(13) Uani 1 d . . O31 O -0.5513(5) 0.9920(5) 0.3456(3) 0.089(2) Uani 1 d . . C31 C -0.4219(7) 0.9499(6) 0.3459(3) 0.053(2) Uani 1 d . . O32 O -0.1033(5) 1.0865(4) 0.4193(3) 0.089(2) Uani 1 d . . C32 C -0.1519(7) 1.0072(6) 0.3930(3) 0.052(2) Uani 1 d . . O33 O -0.2932(6) 0.7699(4) 0.5068(2) 0.088(2) Uani 1 d . . C33 C -0.2643(7) 0.8101(6) 0.4443(3) 0.054(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0216(2) 0.0249(3) 0.0319(2) 0.0020(2) 0.0011(2) -0.0045(2) Mo2 0.0264(2) 0.0262(3) 0.0237(2) -0.0004(2) -0.0028(2) -0.0034(2) Fe1 0.0294(4) 0.0270(4) 0.0255(4) 0.0034(3) -0.0004(3) -0.0047(4) Fe2 0.0245(4) 0.0200(4) 0.0287(4) -0.0006(3) -0.0006(3) -0.0027(3) Fe3 0.0342(4) 0.0314(5) 0.0358(4) -0.0091(3) 0.0052(3) -0.0030(4) S1 0.0308(7) 0.0262(7) 0.0387(7) -0.0042(6) -0.0040(5) -0.0069(7) S2 0.0319(7) 0.0256(7) 0.0375(7) 0.0068(6) -0.0016(5) -0.0076(7) C1 0.022(3) 0.020(3) 0.020(2) 0.001(2) -0.004(2) -0.005(2) C2 0.021(3) 0.022(3) 0.025(2) 0.001(2) -0.004(2) -0.005(2) C3 0.022(3) 0.019(3) 0.031(3) 0.001(2) -0.003(2) 0.000(2) C4 0.037(3) 0.027(3) 0.043(3) 0.003(3) -0.003(2) -0.005(3) C5 0.053(4) 0.023(3) 0.059(4) 0.013(3) -0.010(3) -0.003(3) C6 0.057(4) 0.028(3) 0.069(4) -0.007(3) -0.008(3) 0.009(3) C7 0.039(3) 0.040(4) 0.050(3) -0.018(3) 0.000(3) 0.006(3) C8 0.039(3) 0.024(3) 0.030(3) -0.003(2) 0.000(2) -0.005(3) C9 0.019(3) 0.029(3) 0.024(2) 0.001(2) 0.000(2) -0.004(2) C10 0.023(3) 0.023(3) 0.024(2) 0.001(2) -0.004(2) 0.000(2) C11 0.022(3) 0.029(3) 0.030(3) 0.007(2) 0.001(2) -0.004(2) C12 0.031(3) 0.035(3) 0.035(3) 0.005(2) -0.001(2) -0.003(3) C13 0.034(3) 0.050(4) 0.041(3) 0.018(3) 0.004(2) 0.000(3) C14 0.032(3) 0.041(4) 0.067(4) 0.023(3) 0.006(3) -0.013(3) C15 0.035(3) 0.031(3) 0.066(4) 0.002(3) -0.007(3) -0.013(3) C16 0.037(3) 0.031(3) 0.035(3) 0.003(2) -0.003(2) -0.009(3) C17 0.025(3) 0.037(4) 0.070(4) -0.001(3) 0.013(3) -0.014(3) C18 0.033(3) 0.034(3) 0.048(3) 0.003(3) 0.014(2) -0.003(3) C19 0.023(3) 0.044(4) 0.056(4) -0.010(3) 0.012(2) -0.003(3) C20 0.025(3) 0.040(4) 0.060(4) 0.008(3) 0.002(2) 0.003(3) C21 0.018(3) 0.061(4) 0.052(3) 0.001(3) -0.006(2) -0.008(3) C22 0.053(4) 0.079(5) 0.027(3) 0.003(3) -0.010(3) -0.002(4) C23 0.068(4) 0.045(4) 0.046(4) 0.001(3) -0.032(3) -0.016(4) C24 0.036(3) 0.073(5) 0.045(3) 0.019(3) -0.020(3) -0.006(4) C25 0.046(4) 0.040(4) 0.043(3) 0.003(3) -0.023(3) 0.015(3) C26 0.053(4) 0.045(4) 0.037(3) 0.023(3) -0.016(3) -0.014(3) O27 0.034(2) 0.043(3) 0.056(2) 0.017(2) -0.007(2) 0.001(2) C27 0.038(3) 0.028(3) 0.033(3) 0.001(2) -0.001(2) -0.017(3) O28 0.064(3) 0.057(3) 0.043(2) -0.004(2) 0.019(2) -0.001(2) C28 0.036(3) 0.022(3) 0.036(3) 0.010(2) -0.002(2) -0.007(3) O29 0.063(3) 0.038(2) 0.048(2) 0.003(2) -0.010(2) -0.026(2) C29 0.043(3) 0.041(4) 0.020(3) 0.004(2) -0.007(2) -0.003(3) O30 0.044(2) 0.041(3) 0.070(3) 0.006(2) -0.006(2) 0.013(2) C30 0.038(3) 0.031(3) 0.039(3) -0.001(3) -0.003(2) -0.003(3) O31 0.041(3) 0.106(4) 0.114(4) -0.027(3) -0.001(3) 0.011(3) C31 0.046(4) 0.049(4) 0.063(4) -0.020(3) 0.005(3) -0.007(4) O32 0.097(4) 0.080(4) 0.095(4) -0.052(3) 0.005(3) -0.034(3) C32 0.048(4) 0.051(4) 0.054(4) -0.022(3) 0.003(3) -0.002(4) O33 0.127(4) 0.085(4) 0.045(3) 0.002(3) 0.032(3) -0.016(3) C33 0.059(4) 0.048(4) 0.052(4) -0.014(3) 0.015(3) -0.006(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 Mo1 C1 1.977(4) . ? Mo1 C21 2.340(5) . ? Mo1 S2 2.3418(13) . ? Mo1 C17 2.348(5) . ? Mo1 C18 2.356(4) . ? Mo1 C20 2.366(5) . ? Mo1 C19 2.373(5) . ? Mo1 S1 2.3820(13) . ? Mo1 Fe2 2.5594(8) . ? Mo1 Fe1 2.7736(8) . ? Mo1 Mo2 2.9683(6) . ? Mo2 C9 2.205(4) . ? Mo2 C26 2.307(5) . ? Mo2 C25 2.321(5) . ? Mo2 C2 2.325(4) . ? Mo2 C22 2.339(5) . ? Mo2 C23 2.344(5) . ? Mo2 C24 2.359(5) . ? Mo2 S1 2.3623(13) . ? Mo2 C1 2.371(4) . ? Mo2 C10 2.389(4) . ? Mo2 Fe2 2.5535(7) . ? Mo2 Fe3 2.8605(8) . ? Fe1 C29 1.789(6) . ? Fe1 C28 1.793(5) . ? Fe1 C27 1.799(5) . ? Fe1 C1 2.138(4) . ? Fe1 S2 2.2352(15) . ? Fe1 Fe2 2.5713(9) . ? Fe2 C30 1.797(5) . ? Fe2 C9 2.006(4) . ? Fe2 C1 2.075(4) . ? Fe2 S1 2.2421(14) . ? Fe2 S2 2.2573(13) . ? Fe2 Fe3 2.5942(9) . ? Fe3 C33 1.748(6) . ? Fe3 C31 1.786(6) . ? Fe3 C32 1.822(6) . ? Fe3 C9 1.849(4) . ? C1 C2 1.447(6) . ? C2 C10 1.456(5) . ? C2 C3 1.488(6) . ? C3 C8 1.397(6) . ? C3 C4 1.403(6) . ? C4 C5 1.383(6) . ? C5 C6 1.382(7) . ? C6 C7 1.368(7) . ? C7 C8 1.381(6) . ? C9 C10 1.407(6) . ? C10 C11 1.496(6) . ? C11 C12 1.398(6) . ? C11 C16 1.400(6) . ? C12 C13 1.394(6) . ? C13 C14 1.367(7) . ? C14 C15 1.380(7) . ? C15 C16 1.385(6) . ? C17 C21 1.398(7) . ? C17 C18 1.415(7) . ? C18 C19 1.417(7) . ? C19 C20 1.404(7) . ? C20 C21 1.419(7) . ? C22 C23 1.389(7) . ? C22 C26 1.406(7) . ? C23 C24 1.400(7) . ? C24 C25 1.396(7) . ? C25 C26 1.403(7) . ? O27 C27 1.139(5) . ? O28 C28 1.145(5) . ? O29 C29 1.145(5) . ? O30 C30 1.150(5) . ? O31 C31 1.151(6) . ? O32 C32 1.137(6) . ? O33 C33 1.163(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 C1 Mo1 C21 132.8(2) . . ? C1 Mo1 S2 90.80(13) . . ? C21 Mo1 S2 136.39(14) . . ? C1 Mo1 C17 160.8(2) . . ? C21 Mo1 C17 34.7(2) . . ? S2 Mo1 C17 103.20(14) . . ? C1 Mo1 C18 132.1(2) . . ? C21 Mo1 C18 58.0(2) . . ? S2 Mo1 C18 94.43(13) . . ? C17 Mo1 C18 35.0(2) . . ? C1 Mo1 C20 103.9(2) . . ? C21 Mo1 C20 35.1(2) . . ? S2 Mo1 C20 151.89(13) . . ? C17 Mo1 C20 58.0(2) . . ? C18 Mo1 C20 57.9(2) . . ? C1 Mo1 C19 103.8(2) . . ? C21 Mo1 C19 57.7(2) . . ? S2 Mo1 C19 119.07(14) . . ? C17 Mo1 C19 57.9(2) . . ? C18 Mo1 C19 34.9(2) . . ? C20 Mo1 C19 34.5(2) . . ? C1 Mo1 S1 93.67(12) . . ? C21 Mo1 S1 95.85(14) . . ? S2 Mo1 S1 79.69(4) . . ? C17 Mo1 S1 101.68(14) . . ? C18 Mo1 S1 134.11(14) . . ? C20 Mo1 S1 122.24(14) . . ? C19 Mo1 S1 153.58(13) . . ? C1 Mo1 Fe2 52.56(13) . . ? C21 Mo1 Fe2 148.42(13) . . ? S2 Mo1 Fe2 54.63(3) . . ? C17 Mo1 Fe2 146.67(13) . . ? C18 Mo1 Fe2 148.45(13) . . ? C20 Mo1 Fe2 151.45(13) . . ? C19 Mo1 Fe2 151.72(13) . . ? S1 Mo1 Fe2 53.82(3) . . ? C1 Mo1 Fe1 50.14(11) . . ? C21 Mo1 Fe1 153.86(13) . . ? S2 Mo1 Fe1 50.97(4) . . ? C17 Mo1 Fe1 131.62(14) . . ? C18 Mo1 Fe1 99.88(13) . . ? C20 Mo1 Fe1 123.34(14) . . ? C19 Mo1 Fe1 96.23(13) . . ? S1 Mo1 Fe1 110.19(4) . . ? Fe2 Mo1 Fe1 57.48(2) . . ? C1 Mo1 Mo2 52.79(11) . . ? C21 Mo1 Mo2 101.44(13) . . ? S2 Mo1 Mo2 108.23(3) . . ? C17 Mo1 Mo2 131.46(14) . . ? C18 Mo1 Mo2 157.12(13) . . ? C20 Mo1 Mo2 99.68(13) . . ? C19 Mo1 Mo2 127.79(13) . . ? S1 Mo1 Mo2 50.97(3) . . ? Fe2 Mo1 Mo2 54.42(2) . . ? Fe1 Mo1 Mo2 96.90(2) . . ? C9 Mo2 C26 110.2(2) . . ? C9 Mo2 C25 135.0(2) . . ? C26 Mo2 C25 35.3(2) . . ? C9 Mo2 C2 63.3(2) . . ? C26 Mo2 C2 95.6(2) . . ? C25 Mo2 C2 87.8(2) . . ? C9 Mo2 C22 114.1(2) . . ? C26 Mo2 C22 35.2(2) . . ? C25 Mo2 C22 58.1(2) . . ? C2 Mo2 C22 129.8(2) . . ? C9 Mo2 C23 142.7(2) . . ? C26 Mo2 C23 58.1(2) . . ? C25 Mo2 C23 57.8(2) . . ? C2 Mo2 C23 145.6(2) . . ? C22 Mo2 C23 34.5(2) . . ? C9 Mo2 C24 168.3(2) . . ? C26 Mo2 C24 58.2(2) . . ? C25 Mo2 C24 34.7(2) . . ? C2 Mo2 C24 114.2(2) . . ? C22 Mo2 C24 57.7(2) . . ? C23 Mo2 C24 34.6(2) . . ? C9 Mo2 S1 98.16(12) . . ? C26 Mo2 S1 141.60(14) . . ? C25 Mo2 S1 126.7(2) . . ? C2 Mo2 S1 120.60(11) . . ? C22 Mo2 S1 109.5(2) . . ? C23 Mo2 S1 83.60(15) . . ? C24 Mo2 S1 92.7(2) . . ? C9 Mo2 C1 67.05(14) . . ? C26 Mo2 C1 129.6(2) . . ? C25 Mo2 C1 109.6(2) . . ? C2 Mo2 C1 35.87(14) . . ? C22 Mo2 C1 164.8(2) . . ? C23 Mo2 C1 149.5(2) . . ? C24 Mo2 C1 118.4(2) . . ? S1 Mo2 C1 84.79(11) . . ? C9 Mo2 C10 35.38(15) . . ? C26 Mo2 C10 88.3(2) . . ? C25 Mo2 C10 101.8(2) . . ? C2 Mo2 C10 35.95(13) . . ? C22 Mo2 C10 111.2(2) . . ? C23 Mo2 C10 144.7(2) . . ? C24 Mo2 C10 136.3(2) . . ? S1 Mo2 C10 128.18(11) . . ? C1 Mo2 C10 60.24(14) . . ? C9 Mo2 Fe2 49.21(11) . . ? C26 Mo2 Fe2 159.33(14) . . ? C25 Mo2 Fe2 158.44(13) . . ? C2 Mo2 Fe2 76.60(11) . . ? C22 Mo2 Fe2 143.3(2) . . ? C23 Mo2 Fe2 135.60(15) . . ? C24 Mo2 Fe2 142.43(14) . . ? S1 Mo2 Fe2 54.10(3) . . ? C1 Mo2 Fe2 49.68(11) . . ? C10 Mo2 Fe2 74.11(10) . . ? C9 Mo2 Fe3 40.27(12) . . ? C26 Mo2 Fe3 107.90(14) . . ? C25 Mo2 Fe3 143.03(14) . . ? C2 Mo2 Fe3 103.60(11) . . ? C22 Mo2 Fe3 89.12(15) . . ? C23 Mo2 Fe3 105.6(2) . . ? C24 Mo2 Fe3 140.3(2) . . ? S1 Mo2 Fe3 77.47(4) . . ? C1 Mo2 Fe3 99.20(10) . . ? C10 Mo2 Fe3 72.54(11) . . ? Fe2 Mo2 Fe3 56.92(2) . . ? C29 Fe1 C28 96.7(2) . . ? C29 Fe1 C27 93.1(2) . . ? C28 Fe1 C27 98.5(2) . . ? C29 Fe1 C1 81.8(2) . . ? C28 Fe1 C1 120.2(2) . . ? C27 Fe1 C1 141.4(2) . . ? C29 Fe1 S2 166.31(15) . . ? C28 Fe1 S2 96.9(2) . . ? C27 Fe1 S2 86.9(2) . . ? C1 Fe1 S2 89.72(12) . . ? C29 Fe1 Fe2 111.02(14) . . ? C28 Fe1 Fe2 147.4(2) . . ? C27 Fe1 Fe2 96.89(15) . . ? C1 Fe1 Fe2 51.29(12) . . ? S2 Fe1 Fe2 55.49(4) . . ? C29 Fe1 Mo1 122.51(15) . . ? C28 Fe1 Mo1 93.94(15) . . ? C27 Fe1 Mo1 140.6(2) . . ? C1 Fe1 Mo1 45.21(11) . . ? S2 Fe1 Mo1 54.47(4) . . ? Fe2 Fe1 Mo1 57.07(2) . . ? C30 Fe2 C9 97.6(2) . . ? C30 Fe2 C1 148.4(2) . . ? C9 Fe2 C1 76.6(2) . . ? C30 Fe2 S1 115.8(2) . . ? C9 Fe2 S1 108.60(12) . . ? C1 Fe2 S1 95.24(12) . . ? C30 Fe2 S2 86.6(2) . . ? C9 Fe2 S2 162.32(13) . . ? C1 Fe2 S2 90.73(12) . . ? S1 Fe2 S2 84.54(5) . . ? C30 Fe2 Mo2 140.85(15) . . ? C9 Fe2 Mo2 56.31(12) . . ? C1 Fe2 Mo2 60.59(11) . . ? S1 Fe2 Mo2 58.59(4) . . ? S2 Fe2 Mo2 127.57(4) . . ? C30 Fe2 Mo1 143.7(2) . . ? C9 Fe2 Mo1 118.32(13) . . ? C1 Fe2 Mo1 49.14(12) . . ? S1 Fe2 Mo1 59.04(4) . . ? S2 Fe2 Mo1 57.77(4) . . ? Mo2 Fe2 Mo1 70.98(2) . . ? C30 Fe2 Fe1 100.97(15) . . ? C9 Fe2 Fe1 107.64(13) . . ? C1 Fe2 Fe1 53.51(11) . . ? S1 Fe2 Fe1 123.05(4) . . ? S2 Fe2 Fe1 54.68(4) . . ? Mo2 Fe2 Fe1 114.04(3) . . ? Mo1 Fe2 Fe1 65.45(2) . . ? C30 Fe2 Fe3 73.49(15) . . ? C9 Fe2 Fe3 45.20(13) . . ? C1 Fe2 Fe3 117.29(11) . . ? S1 Fe2 Fe3 85.43(4) . . ? S2 Fe2 Fe3 150.98(5) . . ? Mo2 Fe2 Fe3 67.51(2) . . ? Mo1 Fe2 Fe3 135.45(3) . . ? Fe1 Fe2 Fe3 148.78(3) . . ? C33 Fe3 C31 92.9(3) . . ? C33 Fe3 C32 94.8(3) . . ? C31 Fe3 C32 98.2(3) . . ? C33 Fe3 C9 104.3(2) . . ? C31 Fe3 C9 108.8(2) . . ? C32 Fe3 C9 145.7(2) . . ? C33 Fe3 Fe2 148.7(2) . . ? C31 Fe3 Fe2 111.5(2) . . ? C32 Fe3 Fe2 100.5(2) . . ? C9 Fe3 Fe2 50.33(13) . . ? C33 Fe3 Mo2 95.1(2) . . ? C31 Fe3 Mo2 159.1(2) . . ? C32 Fe3 Mo2 100.4(2) . . ? C9 Fe3 Mo2 50.43(13) . . ? Fe2 Fe3 Mo2 55.57(2) . . ? Fe2 S1 Mo2 67.30(4) . . ? Fe2 S1 Mo1 67.13(4) . . ? Mo2 S1 Mo1 77.46(4) . . ? Fe1 S2 Fe2 69.83(4) . . ? Fe1 S2 Mo1 74.56(4) . . ? Fe2 S2 Mo1 67.60(4) . . ? C2 C1 Mo1 141.9(3) . . ? C2 C1 Fe2 117.5(3) . . ? Mo1 C1 Fe2 78.3(2) . . ? C2 C1 Fe1 131.6(3) . . ? Mo1 C1 Fe1 84.7(2) . . ? Fe2 C1 Fe1 75.20(14) . . ? C2 C1 Mo2 70.3(2) . . ? Mo1 C1 Mo2 85.60(15) . . ? Fe2 C1 Mo2 69.74(12) . . ? Fe1 C1 Mo2 144.8(2) . . ? C1 C2 C10 110.7(4) . . ? C1 C2 C3 122.5(4) . . ? C10 C2 C3 126.5(4) . . ? C1 C2 Mo2 73.8(2) . . ? C10 C2 Mo2 74.4(2) . . ? C3 C2 Mo2 123.2(3) . . ? C8 C3 C4 117.3(4) . . ? C8 C3 C2 118.4(4) . . ? C4 C3 C2 124.3(4) . . ? C5 C4 C3 121.2(5) . . ? C6 C5 C4 120.1(5) . . ? C7 C6 C5 119.4(5) . . ? C6 C7 C8 121.1(5) . . ? C7 C8 C3 120.8(5) . . ? C10 C9 Fe3 147.5(3) . . ? C10 C9 Fe2 120.7(3) . . ? Fe3 C9 Fe2 84.5(2) . . ? C10 C9 Mo2 79.5(3) . . ? Fe3 C9 Mo2 89.3(2) . . ? Fe2 C9 Mo2 74.48(14) . . ? C9 C10 C2 112.5(4) . . ? C9 C10 C11 125.3(4) . . ? C2 C10 C11 122.2(4) . . ? C9 C10 Mo2 65.2(3) . . ? C2 C10 Mo2 69.6(2) . . ? C11 C10 Mo2 135.9(3) . . ? C12 C11 C16 116.9(4) . . ? C12 C11 C10 125.7(4) . . ? C16 C11 C10 117.4(4) . . ? C13 C12 C11 120.7(5) . . ? C14 C13 C12 120.6(4) . . ? C13 C14 C15 120.5(5) . . ? C14 C15 C16 119.0(5) . . ? C15 C16 C11 122.3(4) . . ? C21 C17 C18 108.0(5) . . ? C21 C17 Mo1 72.4(3) . . ? C18 C17 Mo1 72.8(3) . . ? C17 C18 C19 107.6(5) . . ? C17 C18 Mo1 72.2(3) . . ? C19 C18 Mo1 73.2(3) . . ? C20 C19 C18 108.3(5) . . ? C20 C19 Mo1 72.5(3) . . ? C18 C19 Mo1 71.9(3) . . ? C19 C20 C21 107.5(5) . . ? C19 C20 Mo1 73.1(3) . . ? C21 C20 Mo1 71.5(3) . . ? C17 C21 C20 108.6(5) . . ? C17 C21 Mo1 72.9(3) . . ? C20 C21 Mo1 73.5(3) . . ? C23 C22 C26 107.9(5) . . ? C23 C22 Mo2 72.9(3) . . ? C26 C22 Mo2 71.1(3) . . ? C22 C23 C24 108.7(6) . . ? C22 C23 Mo2 72.6(3) . . ? C24 C23 Mo2 73.3(3) . . ? C25 C24 C23 107.4(5) . . ? C25 C24 Mo2 71.2(3) . . ? C23 C24 Mo2 72.1(3) . . ? C24 C25 C26 108.4(5) . . ? C24 C25 Mo2 74.1(3) . . ? C26 C25 Mo2 71.8(3) . . ? C25 C26 C22 107.5(5) . . ? C25 C26 Mo2 72.9(3) . . ? C22 C26 Mo2 73.7(3) . . ? O27 C27 Fe1 177.6(4) . . ? O28 C28 Fe1 177.5(4) . . ? O29 C29 Fe1 177.5(5) . . ? O30 C30 Fe2 171.0(4) . . ? O31 C31 Fe3 175.9(6) . . ? O32 C32 Fe3 178.3(5) . . ? O33 C33 Fe3 177.5(5) . . ? _refine_diff_density_max 0.614 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.135 #===END data_6 _database_code_CSD 168674 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H20 Fe3 Mo2 O7 Se2' _chemical_formula_weight 1045.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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 8.871(3) _cell_length_b 10.901(3) _cell_length_c 17.446(5) _cell_angle_alpha 92.066(5) _cell_angle_beta 98.906(6) _cell_angle_gamma 105.792(6) _cell_volume 1598.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 5604 _cell_measurement_theta_min 0.719161 _cell_measurement_theta_max 1.000000 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max .30 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.173 _exptl_crystal_density_method ? _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 4.418 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick, 1996)' _exptl_absorpt_correction_T_min 1.19 _exptl_absorpt_correction_T_max 25.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12038 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.1444 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5604 _reflns_number_observed 3116 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXTL-V.5.03 Sheldrick, 1994' _computing_structure_refinement 'SHELXL-V.5.03 Sheldrick, 1994' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 41 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00062(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5563 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_obs 0.0477 _refine_ls_wR_factor_all 0.1178 _refine_ls_wR_factor_obs 0.0830 _refine_ls_goodness_of_fit_all 0.835 _refine_ls_goodness_of_fit_obs 1.054 _refine_ls_restrained_S_all 1.103 _refine_ls_restrained_S_obs 1.054 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.81601(7) 0.78489(7) 0.17803(5) 0.0236(2) Uani 1 d . . Mo2 Mo 0.97218(8) 0.70213(7) 0.32321(4) 0.0244(2) Uani 1 d . . Fe1 Fe 1.05415(12) 0.78339(11) 0.09008(7) 0.0231(3) Uani 1 d . . Fe2 Fe 1.11544(12) 0.86254(11) 0.23521(7) 0.0212(3) Uani 1 d . . Fe3 Fe 1.28355(13) 0.87257(12) 0.37273(7) 0.0300(3) Uani 1 d . . Se1 Se 0.93129(9) 0.91695(8) 0.30464(5) 0.0298(2) Uani 1 d . . Se2 Se 1.00086(9) 0.97120(8) 0.13515(5) 0.0270(2) Uani 1 d . . C1 C 0.9737(8) 0.6864(7) 0.1873(5) 0.022(2) Uani 1 d . . C2 C 1.0060(8) 0.5734(7) 0.2218(5) 0.020(2) Uani 1 d . . C3 C 0.9062(8) 0.4437(7) 0.1929(5) 0.017(2) Uani 1 d . . C4 C 0.8094(8) 0.4251(8) 0.1204(5) 0.027(2) Uani 1 d . . H4 H 0.8095(8) 0.4942(8) 0.0907(5) 0.032 Uiso 1 calc R . C5 C 0.7116(9) 0.3029(8) 0.0916(5) 0.033(2) Uani 1 d . . H5 H 0.6488(9) 0.2918(8) 0.0426(5) 0.040 Uiso 1 calc R . C6 C 0.7071(10) 0.1997(8) 0.1346(5) 0.035(2) Uani 1 d . . H6 H 0.6395(10) 0.1194(8) 0.1161(5) 0.041 Uiso 1 calc R . C7 C 0.8041(10) 0.2176(8) 0.2052(6) 0.036(2) Uani 1 d . . H7 H 0.8031(10) 0.1474(8) 0.2340(6) 0.043 Uiso 1 calc R . C8 C 0.9043(9) 0.3361(8) 0.2357(5) 0.029(2) Uani 1 d . . H8 H 0.9696(9) 0.3446(8) 0.2838(5) 0.034 Uiso 1 calc R . C9 C 1.2115(8) 0.7435(8) 0.2940(5) 0.022(2) Uani 1 d . . C10 C 1.1556(8) 0.6088(7) 0.2751(4) 0.018(2) Uani 1 d . . C11 C 1.2433(8) 0.5134(8) 0.3026(5) 0.023(2) Uani 1 d . . C12 C 1.2975(8) 0.4985(8) 0.3811(5) 0.025(2) Uani 1 d . . H12 H 1.2823(8) 0.5504(8) 0.4209(5) 0.030 Uiso 1 calc R . C13 C 1.3728(9) 0.4063(8) 0.3974(6) 0.038(3) Uani 1 d . . H13 H 1.4079(9) 0.3959(8) 0.4492(6) 0.045 Uiso 1 calc R . C14 C 1.3989(9) 0.3276(8) 0.3396(6) 0.035(2) Uani 1 d . . H14 H 1.4504(9) 0.2656(8) 0.3527(6) 0.042 Uiso 1 calc R . C15 C 1.3478(8) 0.3421(8) 0.2628(5) 0.030(2) Uani 1 d . . H15 H 1.3634(8) 0.2896(8) 0.2233(5) 0.036 Uiso 1 calc R . C16 C 1.2719(8) 0.4371(7) 0.2449(5) 0.027(2) Uani 1 d . . H16 H 1.2401(8) 0.4490(7) 0.1930(5) 0.032 Uiso 1 calc R . C17 C 0.6063(8) 0.6616(9) 0.0844(6) 0.036(2) Uani 1 d . . H17 H 0.6164(8) 0.6068(9) 0.0408(6) 0.044 Uiso 1 calc R . C18 C 0.6028(9) 0.7912(9) 0.0816(6) 0.040(3) Uani 1 d . . H18 H 0.6087(9) 0.8413(9) 0.0361(6) 0.048 Uiso 1 calc R . C19 C 0.5680(9) 0.8264(9) 0.1523(7) 0.046(3) Uani 1 d . . H19 H 0.5492(9) 0.9085(9) 0.1654(7) 0.056 Uiso 1 calc R . C20 C 0.5531(8) 0.7242(9) 0.2015(6) 0.039(3) Uani 1 d . . H20 H 0.5188(8) 0.7216(9) 0.2523(6) 0.047 Uiso 1 calc R . C21 C 0.5752(8) 0.6218(9) 0.1577(6) 0.037(3) Uani 1 d . . H21 H 0.5612(8) 0.5347(9) 0.1737(6) 0.044 Uiso 1 calc R . C22 C 0.9485(17) 0.6693(18) 0.4516(7) 0.095(5) Uani 1 d . . H22 H 1.0250(17) 0.7129(18) 0.4977(7) 0.113 Uiso 1 calc R . C23 C 0.8130(21) 0.7028(12) 0.4182(9) 0.078(5) Uani 1 d . . H23 H 0.7804(21) 0.7765(12) 0.4359(9) 0.094 Uiso 1 calc R . C24 C 0.7257(14) 0.6092(14) 0.3618(8) 0.075(4) Uani 1 d . . H24 H 0.6199(14) 0.6028(14) 0.3324(8) 0.090 Uiso 1 calc R . C25 C 0.8056(15) 0.5207(10) 0.3613(7) 0.064(4) Uani 1 d . . H25 H 0.7660(15) 0.4383(10) 0.3301(7) 0.076 Uiso 1 calc R . C26 C 0.9446(14) 0.5570(14) 0.4133(8) 0.068(4) Uani 1 d . . H26 H 1.0157(14) 0.5039(14) 0.4281(8) 0.082 Uiso 1 calc R . C27 C 1.1259(9) 0.6459(8) 0.0785(4) 0.021(2) Uani 1 d . . O27 O 1.1787(6) 0.5632(6) 0.0698(4) 0.039(2) Uani 1 d . . C28 C 0.9162(10) 0.7518(8) 0.0014(6) 0.038(3) Uani 1 d . . O28 O 0.8277(8) 0.7323(6) -0.0586(4) 0.051(2) Uani 1 d . . C29 C 1.2238(10) 0.8913(9) 0.0603(5) 0.031(2) Uani 1 d . . O29 O 1.3312(7) 0.9611(6) 0.0422(4) 0.040(2) Uani 1 d . . C30 C 1.2998(9) 0.9847(8) 0.2370(5) 0.024(2) Uani 1 d . . O30 O 1.4109(7) 1.0625(6) 0.2276(4) 0.045(2) Uani 1 d . . C31 C 1.3144(11) 0.7950(9) 0.4569(6) 0.049(3) Uani 1 d . . O31 O 1.3428(10) 0.7495(7) 0.5159(4) 0.084(3) Uani 1 d . . C32 C 1.2465(10) 1.0074(10) 0.4220(6) 0.043(3) Uani 1 d . . O32 O 1.2259(9) 1.0903(7) 0.4568(4) 0.069(2) Uani 1 d . . C33 C 1.4910(12) 0.9438(10) 0.3714(6) 0.047(3) Uani 1 d . . O33 O 1.6221(8) 0.9829(7) 0.3722(4) 0.066(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0201(4) 0.0229(5) 0.0287(5) 0.0067(4) 0.0035(3) 0.0075(3) Mo2 0.0302(4) 0.0265(5) 0.0203(5) 0.0062(4) 0.0071(4) 0.0120(4) Fe1 0.0259(6) 0.0218(7) 0.0204(8) 0.0053(6) 0.0030(6) 0.0049(5) Fe2 0.0231(6) 0.0180(7) 0.0231(8) 0.0024(6) 0.0030(6) 0.0073(5) Fe3 0.0356(7) 0.0261(8) 0.0255(8) -0.0048(7) -0.0054(6) 0.0105(6) Se1 0.0339(5) 0.0286(6) 0.0317(6) 0.0031(5) 0.0086(4) 0.0150(4) Se2 0.0294(5) 0.0222(5) 0.0317(6) 0.0099(5) 0.0058(4) 0.0098(4) C1 0.029(4) 0.015(5) 0.021(5) 0.002(4) 0.004(4) 0.006(4) C2 0.019(4) 0.025(5) 0.019(5) 0.005(4) 0.006(4) 0.010(4) C3 0.015(4) 0.017(5) 0.019(5) 0.006(4) 0.009(4) -0.001(4) C4 0.012(4) 0.035(6) 0.026(6) 0.011(5) -0.002(4) -0.002(4) C5 0.028(5) 0.032(6) 0.030(6) -0.006(5) -0.002(4) -0.002(4) C6 0.044(5) 0.017(5) 0.028(6) -0.011(5) -0.004(5) -0.009(4) C7 0.035(5) 0.022(6) 0.045(7) 0.001(5) 0.008(5) 0.001(5) C8 0.025(5) 0.033(6) 0.029(6) 0.012(5) 0.004(4) 0.008(4) C9 0.016(4) 0.031(5) 0.017(5) 0.006(4) -0.001(4) 0.007(4) C10 0.027(4) 0.017(5) 0.011(5) -0.001(4) 0.001(4) 0.011(4) C11 0.010(4) 0.027(5) 0.029(6) 0.003(5) 0.004(4) 0.000(4) C12 0.031(5) 0.030(5) 0.015(5) 0.000(4) 0.000(4) 0.015(4) C13 0.043(5) 0.032(6) 0.041(7) 0.021(5) 0.004(5) 0.015(5) C14 0.034(5) 0.032(6) 0.039(7) 0.006(5) -0.005(5) 0.015(4) C15 0.029(5) 0.028(5) 0.035(6) -0.002(5) 0.014(5) 0.006(4) C16 0.022(4) 0.025(5) 0.030(6) 0.007(5) 0.003(4) 0.002(4) C17 0.015(4) 0.053(7) 0.038(7) 0.009(6) 0.002(4) 0.005(4) C18 0.023(5) 0.045(7) 0.046(7) 0.014(6) -0.011(5) 0.006(5) C19 0.019(5) 0.032(6) 0.090(10) 0.012(7) -0.001(5) 0.015(4) C20 0.016(4) 0.049(7) 0.060(8) 0.013(6) 0.020(5) 0.014(4) C21 0.007(4) 0.034(6) 0.058(8) 0.004(6) -0.006(5) -0.005(4) C22 0.091(11) 0.142(15) 0.003(6) 0.019(8) 0.001(7) -0.043(10) C23 0.161(15) 0.043(9) 0.056(10) 0.014(7) 0.080(11) 0.035(9) C24 0.071(8) 0.107(12) 0.085(11) 0.052(10) 0.057(8) 0.058(9) C25 0.110(10) 0.037(7) 0.052(9) 0.006(6) 0.062(8) 0.007(7) C26 0.053(7) 0.092(11) 0.080(11) 0.071(9) 0.019(7) 0.042(8) C27 0.030(5) 0.022(5) 0.004(5) -0.002(4) 0.000(4) -0.003(4) O27 0.048(4) 0.034(4) 0.045(5) 0.014(4) 0.019(3) 0.021(3) C28 0.037(5) 0.031(6) 0.049(7) 0.020(6) 0.011(5) 0.010(5) O28 0.060(4) 0.052(5) 0.034(5) 0.013(4) -0.006(4) 0.008(4) C29 0.039(5) 0.030(6) 0.024(6) -0.009(5) 0.001(5) 0.016(5) O29 0.034(4) 0.035(4) 0.051(5) 0.013(4) 0.014(3) 0.006(3) C30 0.024(5) 0.021(5) 0.025(6) -0.004(4) -0.005(4) 0.008(4) O30 0.035(4) 0.036(4) 0.061(5) 0.013(4) 0.015(4) -0.003(3) C31 0.072(7) 0.032(6) 0.038(7) -0.003(6) -0.014(6) 0.019(6) O31 0.136(7) 0.072(6) 0.038(5) -0.008(5) -0.037(5) 0.049(6) C32 0.050(6) 0.054(7) 0.025(6) -0.002(6) 0.001(5) 0.020(5) O32 0.102(6) 0.067(6) 0.046(5) -0.024(4) 0.002(4) 0.045(5) C33 0.042(6) 0.063(8) 0.032(7) -0.012(6) -0.015(5) 0.024(6) O33 0.032(4) 0.099(6) 0.051(5) -0.025(5) -0.009(4) 0.004(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 Mo1 C1 1.974(6) . ? Mo1 C17 2.340(9) . ? Mo1 C19 2.344(7) . ? Mo1 C21 2.345(8) . ? Mo1 C18 2.347(8) . ? Mo1 C20 2.349(7) . ? Mo1 Se2 2.4596(12) . ? Mo1 Se1 2.5035(14) . ? Mo1 Fe2 2.5811(14) . ? Mo1 Fe1 2.7996(14) . ? Mo1 Mo2 2.9844(12) . ? Mo2 C9 2.191(7) . ? Mo2 C26 2.263(10) . ? Mo2 C25 2.312(10) . ? Mo2 C22 2.314(11) . ? Mo2 C2 2.325(8) . ? Mo2 C23 2.338(10) . ? Mo2 C24 2.359(11) . ? Mo2 C1 2.373(8) . ? Mo2 C10 2.377(6) . ? Mo2 Se1 2.4901(12) . ? Mo2 Fe2 2.5724(14) . ? Mo2 Fe3 2.860(2) . ? Fe1 C28 1.776(10) . ? Fe1 C27 1.797(8) . ? Fe1 C29 1.800(10) . ? Fe1 C1 2.144(8) . ? Fe1 Se2 2.3577(15) . ? Fe1 Fe2 2.571(2) . ? Fe2 C30 1.802(9) . ? Fe2 C9 1.972(7) . ? Fe2 C1 2.052(8) . ? Fe2 Se1 2.3613(14) . ? Fe2 Se2 2.3956(14) . ? Fe2 Fe3 2.603(2) . ? Fe3 C31 1.743(10) . ? Fe3 C33 1.797(11) . ? Fe3 C32 1.808(10) . ? Fe3 C9 1.837(9) . ? C1 C2 1.467(10) . ? C2 C10 1.445(10) . ? C2 C3 1.472(10) . ? C3 C4 1.388(11) . ? C3 C8 1.410(10) . ? C4 C5 1.402(11) . ? C5 C6 1.369(11) . ? C6 C7 1.363(12) . ? C7 C8 1.386(11) . ? C9 C10 1.424(10) . ? C10 C11 1.509(9) . ? C11 C16 1.381(10) . ? C11 C12 1.409(11) . ? C12 C13 1.365(9) . ? C13 C14 1.387(11) . ? C14 C15 1.377(11) . ? C15 C16 1.400(9) . ? C17 C21 1.409(11) . ? C17 C18 1.423(11) . ? C18 C19 1.383(12) . ? C19 C20 1.420(11) . ? C20 C21 1.403(11) . ? C22 C26 1.36(2) . ? C22 C23 1.40(2) . ? C23 C24 1.37(2) . ? C24 C25 1.345(13) . ? C25 C26 1.36(2) . ? C27 O27 1.139(8) . ? C28 O28 1.181(10) . ? C29 O29 1.141(9) . ? C30 O30 1.150(9) . ? C31 O31 1.180(11) . ? C32 O32 1.141(9) . ? C33 O33 1.122(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 C1 Mo1 C17 103.9(3) . . ? C1 Mo1 C19 159.0(3) . . ? C17 Mo1 C19 57.3(3) . . ? C1 Mo1 C21 101.9(3) . . ? C17 Mo1 C21 35.0(3) . . ? C19 Mo1 C21 57.4(3) . . ? C1 Mo1 C18 134.1(4) . . ? C17 Mo1 C18 35.4(3) . . ? C19 Mo1 C18 34.3(3) . . ? C21 Mo1 C18 58.5(3) . . ? C1 Mo1 C20 129.1(3) . . ? C17 Mo1 C20 58.4(3) . . ? C19 Mo1 C20 35.2(3) . . ? C21 Mo1 C20 34.8(3) . . ? C18 Mo1 C20 58.8(3) . . ? C1 Mo1 Se2 92.6(2) . . ? C17 Mo1 Se2 117.4(2) . . ? C19 Mo1 Se2 104.4(2) . . ? C21 Mo1 Se2 151.1(2) . . ? C18 Mo1 Se2 93.5(2) . . ? C20 Mo1 Se2 138.3(2) . . ? C1 Mo1 Se1 95.0(2) . . ? C17 Mo1 Se1 153.8(2) . . ? C19 Mo1 Se1 100.2(3) . . ? C21 Mo1 Se1 123.6(2) . . ? C18 Mo1 Se1 130.8(3) . . ? C20 Mo1 Se1 95.6(3) . . ? Se2 Mo1 Se1 79.00(4) . . ? C1 Mo1 Fe2 51.5(2) . . ? C17 Mo1 Fe2 150.4(2) . . ? C19 Mo1 Fe2 149.4(3) . . ? C21 Mo1 Fe2 149.3(2) . . ? C18 Mo1 Fe2 149.6(2) . . ? C20 Mo1 Fe2 147.8(3) . . ? Se2 Mo1 Fe2 56.69(4) . . ? Se1 Mo1 Fe2 55.32(3) . . ? C1 Mo1 Fe1 49.8(2) . . ? C17 Mo1 Fe1 95.4(2) . . ? C19 Mo1 Fe1 134.4(3) . . ? C21 Mo1 Fe1 121.4(2) . . ? C18 Mo1 Fe1 101.9(3) . . ? C20 Mo1 Fe1 153.7(3) . . ? Se2 Mo1 Fe1 52.79(3) . . ? Se1 Mo1 Fe1 110.67(4) . . ? Fe2 Mo1 Fe1 56.92(4) . . ? C1 Mo1 Mo2 52.5(2) . . ? C17 Mo1 Mo2 128.0(2) . . ? C19 Mo1 Mo2 129.0(3) . . ? C21 Mo1 Mo2 98.6(2) . . ? C18 Mo1 Mo2 155.9(2) . . ? C20 Mo1 Mo2 98.4(2) . . ? Se2 Mo1 Mo2 110.00(4) . . ? Se1 Mo1 Mo2 53.09(3) . . ? Fe2 Mo1 Mo2 54.48(3) . . ? Fe1 Mo1 Mo2 96.65(4) . . ? C9 Mo2 C26 109.8(3) . . ? C9 Mo2 C25 132.5(4) . . ? C26 Mo2 C25 34.7(4) . . ? C9 Mo2 C22 117.1(4) . . ? C26 Mo2 C22 34.6(4) . . ? C25 Mo2 C22 56.5(4) . . ? C9 Mo2 C2 63.3(3) . . ? C26 Mo2 C2 98.3(4) . . ? C25 Mo2 C2 87.6(3) . . ? C22 Mo2 C2 132.7(5) . . ? C9 Mo2 C23 148.2(5) . . ? C26 Mo2 C23 57.6(4) . . ? C25 Mo2 C23 55.5(4) . . ? C22 Mo2 C23 35.0(4) . . ? C2 Mo2 C23 142.0(4) . . ? C9 Mo2 C24 165.9(4) . . ? C26 Mo2 C24 57.8(4) . . ? C25 Mo2 C24 33.5(3) . . ? C22 Mo2 C24 57.5(5) . . ? C2 Mo2 C24 109.6(5) . . ? C23 Mo2 C24 33.8(4) . . ? C9 Mo2 C1 66.5(3) . . ? C26 Mo2 C1 133.3(5) . . ? C25 Mo2 C1 111.7(3) . . ? C22 Mo2 C1 167.4(5) . . ? C2 Mo2 C1 36.4(2) . . ? C23 Mo2 C1 144.6(5) . . ? C24 Mo2 C1 115.8(4) . . ? C9 Mo2 C10 36.0(3) . . ? C26 Mo2 C10 88.9(3) . . ? C25 Mo2 C10 99.2(3) . . ? C22 Mo2 C10 114.5(5) . . ? C2 Mo2 C10 35.8(2) . . ? C23 Mo2 C10 146.4(4) . . ? C24 Mo2 C10 131.4(4) . . ? C1 Mo2 C10 60.6(2) . . ? C9 Mo2 Se1 97.7(2) . . ? C26 Mo2 Se1 138.2(4) . . ? C25 Mo2 Se1 129.7(3) . . ? C22 Mo2 Se1 104.7(5) . . ? C2 Mo2 Se1 122.4(2) . . ? C23 Mo2 Se1 82.3(3) . . ? C24 Mo2 Se1 96.3(3) . . ? C1 Mo2 Se1 86.1(2) . . ? C10 Mo2 Se1 129.3(2) . . ? C9 Mo2 Fe2 48.1(2) . . ? C26 Mo2 Fe2 157.6(3) . . ? C25 Mo2 Fe2 160.4(3) . . ? C22 Mo2 Fe2 143.1(4) . . ? C2 Mo2 Fe2 76.1(2) . . ? C23 Mo2 Fe2 137.3(3) . . ? C24 Mo2 Fe2 144.6(3) . . ? C1 Mo2 Fe2 48.8(2) . . ? C10 Mo2 Fe2 73.8(2) . . ? Se1 Mo2 Fe2 55.58(4) . . ? C9 Mo2 Fe3 40.0(2) . . ? C26 Mo2 Fe3 104.7(4) . . ? C25 Mo2 Fe3 139.4(4) . . ? C22 Mo2 Fe3 90.0(3) . . ? C2 Mo2 Fe3 103.3(2) . . ? C23 Mo2 Fe3 110.8(5) . . ? C24 Mo2 Fe3 144.4(4) . . ? C1 Mo2 Fe3 98.7(2) . . ? C10 Mo2 Fe3 72.5(2) . . ? Se1 Mo2 Fe3 76.79(4) . . ? Fe2 Mo2 Fe3 56.97(4) . . ? C28 Fe1 C27 96.5(4) . . ? C28 Fe1 C29 100.6(4) . . ? C27 Fe1 C29 93.8(3) . . ? C28 Fe1 C1 116.4(3) . . ? C27 Fe1 C1 81.4(3) . . ? C29 Fe1 C1 143.0(4) . . ? C28 Fe1 Se2 97.5(3) . . ? C27 Fe1 Se2 166.0(3) . . ? C29 Fe1 Se2 84.8(2) . . ? C1 Fe1 Se2 91.3(2) . . ? C28 Fe1 Fe2 147.5(3) . . ? C27 Fe1 Fe2 108.6(2) . . ? C29 Fe1 Fe2 98.0(3) . . ? C1 Fe1 Fe2 50.6(2) . . ? Se2 Fe1 Fe2 57.96(4) . . ? C28 Fe1 Mo1 92.1(3) . . ? C27 Fe1 Mo1 122.1(2) . . ? C29 Fe1 Mo1 140.3(3) . . ? C1 Fe1 Mo1 44.7(2) . . ? Se2 Fe1 Mo1 56.18(3) . . ? Fe2 Fe1 Mo1 57.25(4) . . ? C30 Fe2 C9 95.6(3) . . ? C30 Fe2 C1 146.1(3) . . ? C9 Fe2 C1 77.0(3) . . ? C30 Fe2 Se1 116.1(2) . . ? C9 Fe2 Se1 108.8(2) . . ? C1 Fe2 Se1 97.4(2) . . ? C30 Fe2 Se2 86.9(2) . . ? C9 Fe2 Se2 164.9(2) . . ? C1 Fe2 Se2 92.6(2) . . ? Se1 Fe2 Se2 83.16(5) . . ? C30 Fe2 Fe1 99.6(3) . . ? C9 Fe2 Fe1 108.4(2) . . ? C1 Fe2 Fe1 53.9(2) . . ? Se1 Fe2 Fe1 124.43(5) . . ? Se2 Fe2 Fe1 56.54(4) . . ? C30 Fe2 Mo2 140.5(3) . . ? C9 Fe2 Mo2 55.8(2) . . ? C1 Fe2 Mo2 60.5(2) . . ? Se1 Fe2 Mo2 60.44(4) . . ? Se2 Fe2 Mo2 128.20(5) . . ? Fe1 Fe2 Mo2 114.33(6) . . ? C30 Fe2 Mo1 145.9(2) . . ? C9 Fe2 Mo1 118.0(2) . . ? C1 Fe2 Mo1 48.8(2) . . ? Se1 Fe2 Mo1 60.67(4) . . ? Se2 Fe2 Mo1 59.10(4) . . ? Fe1 Fe2 Mo1 65.82(4) . . ? Mo2 Fe2 Mo1 70.78(4) . . ? C30 Fe2 Fe3 73.4(3) . . ? C9 Fe2 Fe3 44.8(2) . . ? C1 Fe2 Fe3 117.2(2) . . ? Se1 Fe2 Fe3 84.27(5) . . ? Se2 Fe2 Fe3 148.91(6) . . ? Fe1 Fe2 Fe3 149.08(5) . . ? Mo2 Fe2 Fe3 67.09(5) . . ? Mo1 Fe2 Fe3 134.76(6) . . ? C31 Fe3 C33 95.2(5) . . ? C31 Fe3 C32 94.9(4) . . ? C33 Fe3 C32 97.4(4) . . ? C31 Fe3 C9 104.6(4) . . ? C33 Fe3 C9 107.1(4) . . ? C32 Fe3 C9 146.8(3) . . ? C31 Fe3 Fe2 146.9(3) . . ? C33 Fe3 Fe2 110.7(3) . . ? C32 Fe3 Fe2 101.5(3) . . ? C9 Fe3 Fe2 49.1(2) . . ? C31 Fe3 Mo2 92.5(3) . . ? C33 Fe3 Mo2 157.1(3) . . ? C32 Fe3 Mo2 103.4(3) . . ? C9 Fe3 Mo2 50.0(2) . . ? Fe2 Fe3 Mo2 55.94(4) . . ? Fe2 Se1 Mo2 63.98(4) . . ? Fe2 Se1 Mo1 64.01(4) . . ? Mo2 Se1 Mo1 73.40(4) . . ? Fe1 Se2 Fe2 65.49(5) . . ? Fe1 Se2 Mo1 71.03(4) . . ? Fe2 Se2 Mo1 64.21(4) . . ? C2 C1 Mo1 141.5(5) . . ? C2 C1 Fe2 117.5(5) . . ? Mo1 C1 Fe2 79.7(3) . . ? C2 C1 Fe1 130.6(5) . . ? Mo1 C1 Fe1 85.6(3) . . ? Fe2 C1 Fe1 75.6(3) . . ? C2 C1 Mo2 70.0(4) . . ? Mo1 C1 Mo2 86.2(3) . . ? Fe2 C1 Mo2 70.7(3) . . ? Fe1 C1 Mo2 146.1(4) . . ? C10 C2 C1 110.7(7) . . ? C10 C2 C3 127.7(6) . . ? C1 C2 C3 121.0(7) . . ? C10 C2 Mo2 74.1(4) . . ? C1 C2 Mo2 73.6(4) . . ? C3 C2 Mo2 126.8(5) . . ? C4 C3 C8 118.0(8) . . ? C4 C3 C2 119.2(7) . . ? C8 C3 C2 122.8(7) . . ? C3 C4 C5 120.6(8) . . ? C6 C5 C4 121.0(8) . . ? C7 C6 C5 118.4(8) . . ? C6 C7 C8 122.7(8) . . ? C7 C8 C3 119.3(8) . . ? C10 C9 Fe3 145.8(6) . . ? C10 C9 Fe2 121.6(6) . . ? Fe3 C9 Fe2 86.1(3) . . ? C10 C9 Mo2 79.1(4) . . ? Fe3 C9 Mo2 90.0(3) . . ? Fe2 C9 Mo2 76.1(2) . . ? C9 C10 C2 111.5(6) . . ? C9 C10 C11 125.3(7) . . ? C2 C10 C11 123.1(7) . . ? C9 C10 Mo2 64.8(4) . . ? C2 C10 Mo2 70.1(4) . . ? C11 C10 Mo2 135.6(5) . . ? C16 C11 C12 119.1(7) . . ? C16 C11 C10 115.7(7) . . ? C12 C11 C10 125.2(7) . . ? C13 C12 C11 118.7(8) . . ? C12 C13 C14 122.4(8) . . ? C15 C14 C13 119.4(7) . . ? C14 C15 C16 119.0(8) . . ? C11 C16 C15 121.4(8) . . ? C21 C17 C18 108.2(8) . . ? C21 C17 Mo1 72.7(5) . . ? C18 C17 Mo1 72.6(5) . . ? C19 C18 C17 106.3(9) . . ? C19 C18 Mo1 72.7(5) . . ? C17 C18 Mo1 72.1(5) . . ? C18 C19 C20 110.7(8) . . ? C18 C19 Mo1 73.0(4) . . ? C20 C19 Mo1 72.6(4) . . ? C21 C20 C19 105.8(9) . . ? C21 C20 Mo1 72.4(4) . . ? C19 C20 Mo1 72.2(4) . . ? C20 C21 C17 108.8(8) . . ? C20 C21 Mo1 72.8(5) . . ? C17 C21 Mo1 72.3(5) . . ? C26 C22 C23 107.0(12) . . ? C26 C22 Mo2 70.7(6) . . ? C23 C22 Mo2 73.5(6) . . ? C24 C23 C22 108.7(12) . . ? C24 C23 Mo2 73.9(6) . . ? C22 C23 Mo2 71.5(7) . . ? C25 C24 C23 106.1(12) . . ? C25 C24 Mo2 71.4(6) . . ? C23 C24 Mo2 72.3(7) . . ? C24 C25 C26 111.2(12) . . ? C24 C25 Mo2 75.2(7) . . ? C26 C25 Mo2 70.7(6) . . ? C22 C26 C25 106.8(10) . . ? C22 C26 Mo2 74.7(6) . . ? C25 C26 Mo2 74.6(6) . . ? O27 C27 Fe1 176.1(7) . . ? O28 C28 Fe1 178.2(8) . . ? O29 C29 Fe1 179.0(7) . . ? O30 C30 Fe2 170.8(8) . . ? O31 C31 Fe3 175.7(10) . . ? O32 C32 Fe3 176.4(8) . . ? O33 C33 Fe3 176.4(9) . . ? _refine_diff_density_max 0.892 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.167 #===END data_7 _database_code_CSD 168675 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H22 Fe3 O7 S2 W2' _chemical_formula_weight 1129.88 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'W' 'W' -0.8490 6.8722 '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 10.8005(8) _cell_length_b 16.9398(9) _cell_length_c 18.5162(12) _cell_angle_alpha 90.00 _cell_angle_beta 92.877(3) _cell_angle_gamma 90.00 _cell_volume 3383.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5948 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max .25 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.218 _exptl_crystal_density_method ? _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 8.199 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.240722 _exptl_absorpt_correction_T_max 0.338091 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25413 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5948 _reflns_number_observed 4604 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXTL-V.5.03 Sheldrick, 1994' _computing_structure_refinement 'SHELXL-V.5.03 Sheldrick, 1994' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+10.6950P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00041(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5946 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_obs 0.0453 _refine_ls_wR_factor_all 0.0729 _refine_ls_wR_factor_obs 0.0694 _refine_ls_goodness_of_fit_all 1.097 _refine_ls_goodness_of_fit_obs 1.201 _refine_ls_restrained_S_all 1.098 _refine_ls_restrained_S_obs 1.201 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.37278(3) 0.15644(2) 0.18274(2) 0.02499(10) Uani 1 d . . W2 W 0.53465(4) 0.20649(2) 0.07656(2) 0.03056(11) Uani 1 d . . Fe1 Fe 0.28974(12) 0.30759(6) 0.17765(6) 0.0302(3) Uani 1 d . . Fe2 Fe 0.29055(12) 0.22480(6) 0.05939(6) 0.0273(3) Uani 1 d . . Fe3 Fe 0.3875(23) 0.2261(17) -0.0611(16) 0.032(2) Uani 0.37(2) d P 1 Fe3' Fe 0.4153(15) 0.2336(10) -0.0566(9) 0.032(2) Uani 0.63(2) d P 2 S1 S 0.3850(2) 0.10496(11) 0.06632(11) 0.0333(6) Uani 1 d . . S2 S 0.4953(2) 0.26764(12) 0.19123(11) 0.0311(5) Uani 1 d . . C1 C 0.2079(8) 0.1985(4) 0.1545(5) 0.033(2) Uani 1 d . . C2 C 0.0717(9) 0.1796(5) 0.1672(6) 0.050(3) Uani 1 d . . H2A H 0.0532(9) 0.1983(5) 0.2150(6) 0.061 Uiso 1 calc R . H2B H 0.0201(9) 0.2093(5) 0.1324(6) 0.061 Uiso 1 calc R . C3 C 0.0349(9) 0.0930(6) 0.1614(6) 0.050(3) Uani 1 d . . C4 C -0.0356(10) 0.0601(6) 0.2160(6) 0.065(3) Uani 1 d . . H4 H -0.0557(10) 0.0894(6) 0.2562(6) 0.078 Uiso 1 calc R . C5 C -0.0745(13) -0.0194(8) 0.2069(7) 0.086(4) Uiso 1 d . . H5 H -0.1235(13) -0.0422(8) 0.2411(7) 0.103 Uiso 1 calc R . C6 C -0.0430(13) -0.0613(8) 0.1515(7) 0.086(4) Uiso 1 d . . H6 H -0.0687(13) -0.1137(8) 0.1489(7) 0.104 Uiso 1 calc R . C7 C 0.0268(12) -0.0322(7) 0.0964(7) 0.076(4) Uani 1 d . . H7 H 0.0462(12) -0.0630(7) 0.0569(7) 0.091 Uiso 1 calc R . C8 C 0.0665(10) 0.0473(6) 0.1040(6) 0.056(3) Uani 1 d . . H8 H 0.1154(10) 0.0690(6) 0.0691(6) 0.068 Uiso 1 calc R . C9 C 0.4390(8) 0.2928(4) 0.0335(4) 0.028(2) Uani 1 d . . C10 C 0.3362(8) 0.3232(4) 0.0021(4) 0.030(2) Uani 1 d . . C11 C 0.2833(8) 0.3972(4) -0.0264(4) 0.027(2) Uani 1 d . . C12 C 0.3661(9) 0.4549(5) -0.0485(5) 0.050(3) Uani 1 d . . H12 H 0.4511(9) 0.4457(5) -0.0445(5) 0.060 Uiso 1 calc R . C13 C 0.3214(11) 0.5251(6) -0.0760(6) 0.062(3) Uani 1 d . . H13 H 0.3773(11) 0.5638(6) -0.0887(6) 0.074 Uiso 1 calc R . C14 C 0.1990(10) 0.5399(5) -0.0851(6) 0.050(3) Uani 1 d . . H14 H 0.1709(10) 0.5876(5) -0.1046(6) 0.060 Uiso 1 calc R . C15 C 0.1162(9) 0.4830(5) -0.0651(5) 0.042(2) Uani 1 d . . H15 H 0.0313(9) 0.4921(5) -0.0707(5) 0.050 Uiso 1 calc R . C16 C 0.1600(9) 0.4123(5) -0.0366(5) 0.037(2) Uani 1 d . . H16 H 0.1034(9) 0.3739(5) -0.0241(5) 0.045 Uiso 1 calc R . C17 C 0.4879(10) 0.1032(6) 0.2831(5) 0.051(3) Uani 1 d . . H17 H 0.5706(10) 0.1204(6) 0.3008(5) 0.061 Uiso 1 calc R . C18 C 0.3753(11) 0.1309(5) 0.3078(5) 0.046(3) Uani 1 d . . H18 H 0.3662(11) 0.1705(5) 0.3457(5) 0.055 Uiso 1 calc R . C19 C 0.2802(10) 0.0860(6) 0.2760(5) 0.048(3) Uani 1 d . . H19 H 0.1927(10) 0.0887(6) 0.2875(5) 0.058 Uiso 1 calc R . C20 C 0.3318(13) 0.0316(5) 0.2290(5) 0.058(3) Uani 1 d . . H20 H 0.2874(13) -0.0111(5) 0.2031(5) 0.069 Uiso 1 calc R . C21 C 0.4627(12) 0.0423(6) 0.2345(5) 0.057(3) Uani 1 d . . H21 H 0.5242(12) 0.0086(6) 0.2126(5) 0.068 Uiso 1 calc R . C22 C 0.7367(10) 0.2266(9) 0.1194(8) 0.076(4) Uani 1 d . . H22 H 0.7631(10) 0.2653(9) 0.1563(8) 0.091 Uiso 1 calc R . C23 C 0.7123(10) 0.1475(9) 0.1325(8) 0.078(4) Uani 1 d . . H23 H 0.7173(10) 0.1212(9) 0.1797(8) 0.093 Uiso 1 calc R . C24 C 0.6925(11) 0.1110(6) 0.0656(9) 0.076(4) Uani 1 d . . H24 H 0.6800(11) 0.0544(6) 0.0573(9) 0.091 Uiso 1 calc R . C25 C 0.7069(11) 0.1680(9) 0.0128(7) 0.077(4) Uani 1 d . . H25 H 0.7070(11) 0.1582(9) -0.0394(7) 0.092 Uiso 1 calc R . C26 C 0.7347(10) 0.2392(7) 0.0467(8) 0.072(4) Uani 1 d . . H26 H 0.7595(10) 0.2880(7) 0.0229(8) 0.086 Uiso 1 calc R . C27 C 0.3508(8) 0.4019(5) 0.1507(4) 0.033(2) Uani 1 d . . O27 O 0.3877(7) 0.4618(3) 0.1362(3) 0.051(2) Uani 1 d . . C28 C 0.1392(10) 0.3397(5) 0.1505(6) 0.053(3) Uani 1 d . . O28 O 0.0404(8) 0.3614(5) 0.1338(5) 0.093(3) Uani 1 d . . C29 C 0.2739(11) 0.3240(5) 0.2726(6) 0.054(3) Uani 1 d . . O29 O 0.2591(9) 0.3347(4) 0.3321(4) 0.085(3) Uani 1 d . . C30 C 0.1424(10) 0.2177(5) 0.0165(5) 0.044(2) Uani 1 d . . O30 O 0.0453(7) 0.2139(4) -0.0127(5) 0.075(2) Uani 1 d . . C31 C 0.2662(130) 0.2536(66) -0.1167(66) 0.050(9) Uani 0.37(2) d P 1 O31 O 0.1705(48) 0.2620(39) -0.1571(34) 0.079(8) Uani 0.37(2) d P 1 C31' C 0.2941(70) 0.2432(36) -0.1280(36) 0.050(9) Uani 0.63(2) d P 2 O31' O 0.2253(27) 0.2590(21) -0.1725(19) 0.079(8) Uani 0.63(2) d P 2 C32 C 0.4952(48) 0.2769(39) -0.1157(29) 0.039(6) Uani 0.37(2) d P 1 O32 O 0.5697(58) 0.3085(43) -0.1480(30) 0.082(9) Uani 0.37(2) d P 1 C32' C 0.5389(27) 0.2809(20) -0.0982(16) 0.039(6) Uani 0.63(2) d P 2 O32' O 0.6168(32) 0.3146(23) -0.1233(17) 0.082(9) Uani 0.63(2) d P 2 C33 C 0.4048(45) 0.1273(36) -0.0826(35) 0.046(7) Uani 0.37(2) d P 1 O33 O 0.4211(38) 0.0663(25) -0.1103(22) 0.068(7) Uani 0.37(2) d P 1 C33' C 0.4584(26) 0.1330(18) -0.0858(18) 0.046(7) Uani 0.63(2) d P 2 O33' O 0.4901(23) 0.0715(13) -0.0994(12) 0.068(7) Uani 0.63(2) d P 2 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 W1 0.0275(2) 0.0239(2) 0.0233(2) 0.00200(13) -0.00177(15) 0.0032(2) W2 0.0307(2) 0.0284(2) 0.0329(2) 0.00665(15) 0.0057(2) 0.0091(2) Fe1 0.0335(8) 0.0230(6) 0.0344(7) -0.0006(5) 0.0047(6) 0.0042(6) Fe2 0.0311(8) 0.0226(6) 0.0274(7) 0.0026(5) -0.0056(6) -0.0007(5) Fe3 0.049(6) 0.024(3) 0.023(2) -0.001(2) -0.003(4) 0.001(3) Fe3' 0.049(6) 0.024(3) 0.023(2) -0.001(2) -0.003(4) 0.001(3) S1 0.050(2) 0.0236(11) 0.0260(12) 0.0006(8) -0.0016(11) 0.0027(10) S2 0.0291(14) 0.0310(11) 0.0324(13) 0.0015(9) -0.0051(10) 0.0016(10) C1 0.026(5) 0.028(5) 0.044(6) 0.008(4) 0.004(4) 0.003(4) C2 0.027(6) 0.042(6) 0.083(8) 0.016(5) 0.007(6) -0.005(5) C3 0.014(6) 0.051(6) 0.084(9) 0.029(6) -0.011(5) -0.005(5) C4 0.050(8) 0.060(7) 0.084(9) 0.033(6) -0.019(7) -0.012(6) C7 0.071(10) 0.065(8) 0.087(9) 0.016(6) -0.035(7) -0.021(7) C8 0.043(7) 0.042(6) 0.082(9) 0.024(6) -0.021(6) -0.019(5) C9 0.030(5) 0.029(4) 0.024(5) 0.000(3) 0.001(4) -0.004(4) C10 0.030(6) 0.027(4) 0.032(5) -0.003(3) -0.004(4) 0.005(4) C11 0.033(6) 0.026(4) 0.021(5) 0.003(3) -0.009(4) 0.005(4) C12 0.030(6) 0.041(6) 0.079(8) 0.019(5) 0.009(6) 0.009(5) C13 0.044(8) 0.040(6) 0.101(9) 0.028(6) 0.005(7) -0.001(5) C14 0.050(8) 0.025(5) 0.075(8) 0.017(5) -0.003(6) 0.006(5) C15 0.033(7) 0.042(5) 0.048(6) 0.001(4) -0.015(5) 0.016(5) C16 0.033(6) 0.036(5) 0.041(6) 0.007(4) -0.013(5) -0.001(4) C17 0.049(7) 0.071(7) 0.031(6) 0.021(5) -0.021(5) -0.004(6) C18 0.068(8) 0.043(6) 0.026(5) 0.009(4) 0.002(5) 0.009(6) C19 0.040(7) 0.059(7) 0.046(6) 0.015(5) 0.010(5) 0.000(5) C20 0.112(12) 0.025(5) 0.035(6) 0.010(4) -0.012(7) -0.020(6) C21 0.088(10) 0.039(6) 0.044(7) 0.019(5) 0.018(7) 0.032(6) C22 0.025(7) 0.110(11) 0.092(11) -0.009(8) -0.001(7) 0.016(7) C23 0.033(7) 0.116(11) 0.085(10) 0.051(9) 0.008(7) 0.038(8) C24 0.055(9) 0.047(7) 0.130(13) 0.010(7) 0.047(9) 0.034(6) C25 0.060(9) 0.119(11) 0.055(8) 0.008(8) 0.028(7) 0.041(8) C26 0.036(7) 0.064(8) 0.118(12) 0.021(8) 0.025(8) 0.017(6) C27 0.036(6) 0.037(5) 0.025(5) -0.010(4) -0.011(4) 0.002(4) O27 0.078(6) 0.027(3) 0.050(4) 0.002(3) 0.017(4) -0.007(3) C28 0.034(7) 0.032(5) 0.094(9) 0.014(5) 0.008(6) 0.003(5) O28 0.039(5) 0.074(6) 0.163(9) 0.037(5) -0.008(6) 0.029(5) C29 0.085(9) 0.022(5) 0.056(7) -0.004(4) 0.024(7) 0.000(5) O29 0.144(9) 0.068(5) 0.047(5) -0.014(4) 0.031(6) -0.007(5) C30 0.049(7) 0.031(5) 0.051(6) 0.004(4) -0.012(5) -0.011(5) O30 0.053(5) 0.066(5) 0.100(7) 0.021(4) -0.049(5) -0.017(4) C31 0.090(36) 0.030(17) 0.031(22) -0.016(11) 0.005(16) 0.013(16) O31 0.096(25) 0.076(7) 0.060(16) -0.009(9) -0.037(15) 0.015(17) C31' 0.090(36) 0.030(17) 0.031(22) -0.016(11) 0.005(16) 0.013(16) O31' 0.096(25) 0.076(7) 0.060(16) -0.009(9) -0.037(15) 0.015(17) C32 0.046(21) 0.046(7) 0.024(16) -0.008(10) -0.011(10) 0.003(14) O32 0.096(26) 0.087(9) 0.068(21) 0.018(14) 0.041(15) -0.014(16) C32' 0.046(21) 0.046(7) 0.024(16) -0.008(10) -0.011(10) 0.003(14) O32' 0.096(26) 0.087(9) 0.068(21) 0.018(14) 0.041(15) -0.014(16) C33 0.061(23) 0.044(8) 0.036(7) 0.003(6) 0.033(16) 0.003(15) O33 0.117(21) 0.043(6) 0.041(8) -0.010(5) -0.010(13) 0.035(14) C33' 0.061(23) 0.044(8) 0.036(7) 0.003(6) 0.033(16) 0.003(15) O33' 0.117(21) 0.043(6) 0.041(8) -0.010(5) -0.010(13) 0.035(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 W1 C1 1.965(9) . ? W1 S2 2.303(2) . ? W1 C20 2.331(8) . ? W1 S1 2.335(2) . ? W1 C21 2.346(9) . ? W1 C18 2.354(9) . ? W1 C19 2.362(9) . ? W1 C17 2.362(9) . ? W1 Fe2 2.6726(12) . ? W1 Fe1 2.7131(11) . ? W1 W2 2.8259(5) . ? W2 C9 1.938(8) . ? W2 C22 2.310(12) . ? W2 C26 2.324(11) . ? W2 C25 2.346(10) . ? W2 C23 2.357(11) . ? W2 S1 2.362(2) . ? W2 C24 2.366(9) . ? W2 S2 2.419(2) . ? W2 Fe2 2.6577(13) . ? W2 Fe3' 2.76(2) . ? W2 Fe3 2.95(3) . ? Fe1 C28 1.763(11) . ? Fe1 C29 1.796(10) . ? Fe1 C27 1.808(9) . ? Fe1 C1 2.083(8) . ? Fe1 S2 2.323(3) . ? Fe1 Fe2 2.601(2) . ? Fe2 C30 1.755(11) . ? Fe2 C10 2.048(8) . ? Fe2 C9 2.050(8) . ? Fe2 C1 2.063(8) . ? Fe2 S1 2.273(2) . ? Fe2 Fe3 2.51(3) . ? Fe2 Fe3' 2.60(2) . ? Fe3 C31 1.69(15) . ? Fe3 C33 1.73(7) . ? Fe3 C32 1.80(7) . ? Fe3 C10 2.11(3) . ? Fe3 C9 2.14(3) . ? Fe3' C32' 1.77(4) . ? Fe3' C31' 1.82(9) . ? Fe3' C33' 1.85(4) . ? Fe3' C9 1.95(2) . ? Fe3' C10 2.07(2) . ? C1 C2 1.535(12) . ? C2 C3 1.523(13) . ? C3 C8 1.371(14) . ? C3 C4 1.410(13) . ? C4 C5 1.419(15) . ? C5 C6 1.31(2) . ? C6 C7 1.39(2) . ? C7 C8 1.419(13) . ? C9 C10 1.330(12) . ? C10 C11 1.466(11) . ? C11 C16 1.361(12) . ? C11 C12 1.399(11) . ? C12 C13 1.373(12) . ? C13 C14 1.347(14) . ? C14 C15 1.379(12) . ? C15 C16 1.381(11) . ? C17 C21 1.388(14) . ? C17 C18 1.401(13) . ? C18 C19 1.385(14) . ? C19 C20 1.402(13) . ? C20 C21 1.42(2) . ? C22 C26 1.36(2) . ? C22 C23 1.39(2) . ? C23 C24 1.39(2) . ? C24 C25 1.39(2) . ? C25 C26 1.39(2) . ? C27 O27 1.129(9) . ? C28 O28 1.157(12) . ? C29 O29 1.137(11) . ? C30 O30 1.157(11) . ? C31 O31 1.25(16) . ? C31' O31' 1.11(8) . ? C32 O32 1.16(9) . ? C32' O32' 1.14(5) . ? C33 O33 1.17(7) . ? C33' O33' 1.13(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 W1 S2 103.4(2) . . ? C1 W1 C20 103.9(4) . . ? S2 W1 C20 146.7(3) . . ? C1 W1 S1 89.0(3) . . ? S2 W1 S1 108.03(7) . . ? C20 W1 S1 91.2(2) . . ? C1 W1 C21 139.3(4) . . ? S2 W1 C21 114.9(3) . . ? C20 W1 C21 35.4(4) . . ? S1 W1 C21 91.6(3) . . ? C1 W1 C18 107.1(4) . . ? S2 W1 C18 96.0(3) . . ? C20 W1 C18 57.7(3) . . ? S1 W1 C18 147.2(2) . . ? C21 W1 C18 57.5(3) . . ? C1 W1 C19 88.1(3) . . ? S2 W1 C19 128.8(3) . . ? C20 W1 C19 34.8(3) . . ? S1 W1 C19 122.1(3) . . ? C21 W1 C19 57.8(4) . . ? C18 W1 C19 34.2(3) . . ? C1 W1 C17 141.4(4) . . ? S2 W1 C17 88.9(3) . . ? C20 W1 C17 57.8(4) . . ? S1 W1 C17 122.1(3) . . ? C21 W1 C17 34.3(3) . . ? C18 W1 C17 34.6(3) . . ? C19 W1 C17 57.1(4) . . ? C1 W1 Fe2 50.0(2) . . ? S2 W1 Fe2 82.48(6) . . ? C20 W1 Fe2 130.2(3) . . ? S1 W1 Fe2 53.46(6) . . ? C21 W1 Fe2 145.0(3) . . ? C18 W1 Fe2 155.1(2) . . ? C19 W1 Fe2 135.1(3) . . ? C17 W1 Fe2 167.7(3) . . ? C1 W1 Fe1 49.8(2) . . ? S2 W1 Fe1 54.43(6) . . ? C20 W1 Fe1 143.1(3) . . ? S1 W1 Fe1 110.74(6) . . ? C21 W1 Fe1 157.1(3) . . ? C18 W1 Fe1 101.3(2) . . ? C19 W1 Fe1 110.5(2) . . ? C17 W1 Fe1 123.2(3) . . ? Fe2 W1 Fe1 57.74(4) . . ? C1 W1 W2 106.9(2) . . ? S2 W1 W2 55.15(5) . . ? C20 W1 W2 131.5(3) . . ? S1 W1 W2 53.44(6) . . ? C21 W1 W2 105.9(3) . . ? C18 W1 W2 139.7(3) . . ? C19 W1 W2 163.7(2) . . ? C17 W1 W2 110.0(3) . . ? Fe2 W1 W2 57.73(3) . . ? Fe1 W1 W2 84.70(3) . . ? C9 W2 C22 120.3(4) . . ? C9 W2 C26 101.8(4) . . ? C22 W2 C26 34.2(4) . . ? C9 W2 C25 115.0(4) . . ? C22 W2 C25 56.9(5) . . ? C26 W2 C25 34.5(4) . . ? C9 W2 C23 155.0(4) . . ? C22 W2 C23 34.6(4) . . ? C26 W2 C23 57.3(4) . . ? C25 W2 C23 57.0(4) . . ? C9 W2 S1 99.6(2) . . ? C22 W2 S1 140.0(4) . . ? C26 W2 S1 142.7(3) . . ? C25 W2 S1 108.3(4) . . ? C23 W2 S1 105.4(4) . . ? C9 W2 C24 148.4(4) . . ? C22 W2 C24 57.1(5) . . ? C26 W2 C24 57.3(4) . . ? C25 W2 C24 34.3(4) . . ? C23 W2 C24 34.3(4) . . ? S1 W2 C24 89.3(3) . . ? C9 W2 S2 85.7(2) . . ? C22 W2 S2 80.8(3) . . ? C26 W2 S2 108.2(4) . . ? C25 W2 S2 137.7(4) . . ? C23 W2 S2 88.3(4) . . ? S1 W2 S2 103.46(7) . . ? C24 W2 S2 121.8(4) . . ? C9 W2 Fe2 50.0(2) . . ? C22 W2 Fe2 159.8(3) . . ? C26 W2 Fe2 150.7(3) . . ? C25 W2 Fe2 141.2(3) . . ? C23 W2 Fe2 152.0(3) . . ? S1 W2 Fe2 53.45(6) . . ? C24 W2 Fe2 141.6(3) . . ? S2 W2 Fe2 80.69(6) . . ? C9 W2 Fe3' 45.0(4) . . ? C22 W2 Fe3' 132.2(5) . . ? C26 W2 Fe3' 98.4(5) . . ? C25 W2 Fe3' 86.7(5) . . ? C23 W2 Fe3' 142.8(5) . . ? S1 W2 Fe3' 76.3(3) . . ? C24 W2 Fe3' 110.1(5) . . ? S2 W2 Fe3' 128.1(4) . . ? Fe2 W2 Fe3' 57.2(4) . . ? C9 W2 W1 100.2(2) . . ? C22 W2 W1 114.4(4) . . ? C26 W2 W1 148.4(4) . . ? C25 W2 W1 143.2(3) . . ? C23 W2 W1 94.9(3) . . ? S1 W2 W1 52.58(5) . . ? C24 W2 W1 109.2(3) . . ? S2 W2 W1 51.38(5) . . ? Fe2 W2 W1 58.24(3) . . ? Fe3' W2 W1 113.2(3) . . ? C9 W2 Fe3 46.2(6) . . ? C22 W2 Fe3 137.5(6) . . ? C26 W2 Fe3 103.6(7) . . ? C25 W2 Fe3 90.1(7) . . ? C23 W2 Fe3 144.9(7) . . ? S1 W2 Fe3 71.1(5) . . ? C24 W2 Fe3 111.2(7) . . ? S2 W2 Fe3 126.8(6) . . ? Fe2 W2 Fe3 52.9(6) . . ? W1 W2 Fe3 108.0(5) . . ? C28 Fe1 C29 95.7(5) . . ? C28 Fe1 C27 89.6(4) . . ? C29 Fe1 C27 100.8(4) . . ? C28 Fe1 C1 80.8(4) . . ? C29 Fe1 C1 106.1(4) . . ? C27 Fe1 C1 152.1(3) . . ? C28 Fe1 S2 169.5(4) . . ? C29 Fe1 S2 94.4(4) . . ? C27 Fe1 S2 85.8(3) . . ? C1 Fe1 S2 99.1(2) . . ? C28 Fe1 Fe2 88.2(4) . . ? C29 Fe1 Fe2 155.8(3) . . ? C27 Fe1 Fe2 103.1(3) . . ? C1 Fe1 Fe2 50.8(2) . . ? S2 Fe1 Fe2 83.71(7) . . ? C28 Fe1 W1 126.9(3) . . ? C29 Fe1 W1 99.2(3) . . ? C27 Fe1 W1 136.0(3) . . ? C1 Fe1 W1 46.1(2) . . ? S2 Fe1 W1 53.75(6) . . ? Fe2 Fe1 W1 60.35(3) . . ? C30 Fe2 C10 93.4(4) . . ? C30 Fe2 C9 129.7(4) . . ? C10 Fe2 C9 37.9(3) . . ? C30 Fe2 C1 87.0(4) . . ? C10 Fe2 C1 138.0(3) . . ? C9 Fe2 C1 134.2(3) . . ? C30 Fe2 S1 111.1(3) . . ? C10 Fe2 S1 129.5(2) . . ? C9 Fe2 S1 99.3(2) . . ? C1 Fe2 S1 88.4(2) . . ? C30 Fe2 Fe3 90.6(6) . . ? C10 Fe2 Fe3 53.9(7) . . ? C9 Fe2 Fe3 54.7(5) . . ? C1 Fe2 Fe3 167.9(7) . . ? S1 Fe2 Fe3 81.5(7) . . ? C30 Fe2 Fe3' 97.4(5) . . ? C10 Fe2 Fe3' 51.4(4) . . ? C9 Fe2 Fe3' 47.9(4) . . ? C1 Fe2 Fe3' 169.6(4) . . ? S1 Fe2 Fe3' 81.3(4) . . ? C30 Fe2 Fe1 112.1(3) . . ? C10 Fe2 Fe1 90.5(2) . . ? C9 Fe2 Fe1 86.0(2) . . ? C1 Fe2 Fe1 51.5(2) . . ? S1 Fe2 Fe1 117.04(8) . . ? Fe3 Fe2 Fe1 139.7(5) . . ? Fe3' Fe2 Fe1 133.6(3) . . ? C30 Fe2 W2 157.3(3) . . ? C10 Fe2 W2 83.9(3) . . ? C9 Fe2 W2 46.4(2) . . ? C1 Fe2 W2 110.0(3) . . ? S1 Fe2 W2 56.59(7) . . ? Fe3 Fe2 W2 69.7(6) . . ? Fe3' Fe2 W2 63.4(4) . . ? Fe1 Fe2 W2 90.43(5) . . ? C30 Fe2 W1 127.8(3) . . ? C10 Fe2 W1 135.8(3) . . ? C9 Fe2 W1 102.3(2) . . ? C1 Fe2 W1 46.9(2) . . ? S1 Fe2 W1 55.65(6) . . ? Fe3 Fe2 W1 128.9(7) . . ? Fe3' Fe2 W1 124.6(4) . . ? Fe1 Fe2 W1 61.91(4) . . ? W2 Fe2 W1 64.03(3) . . ? C31 Fe3 C33 102.5(42) . . ? C31 Fe3 C32 91.7(48) . . ? C33 Fe3 C32 104.7(28) . . ? C31 Fe3 C10 84.6(28) . . ? C33 Fe3 C10 156.2(24) . . ? C32 Fe3 C10 97.7(23) . . ? C31 Fe3 C9 121.0(30) . . ? C33 Fe3 C9 132.3(28) . . ? C32 Fe3 C9 93.3(17) . . ? C10 Fe3 C9 36.5(6) . . ? C31 Fe3 Fe2 101.4(34) . . ? C33 Fe3 Fe2 104.5(21) . . ? C32 Fe3 Fe2 144.4(20) . . ? C10 Fe3 Fe2 51.7(7) . . ? C9 Fe3 Fe2 51.6(7) . . ? C31 Fe3 W2 157.4(29) . . ? C33 Fe3 W2 91.7(26) . . ? C32 Fe3 W2 101.7(14) . . ? C10 Fe3 W2 75.7(8) . . ? C9 Fe3 W2 40.9(5) . . ? Fe2 Fe3 W2 57.5(6) . . ? C32' Fe3' C31' 100.0(24) . . ? C32' Fe3' C33' 94.8(14) . . ? C31' Fe3' C33' 93.0(19) . . ? C32' Fe3' C9 94.0(10) . . ? C31' Fe3' C9 129.3(13) . . ? C33' Fe3' C9 134.2(15) . . ? C32' Fe3' C10 103.7(13) . . ? C31' Fe3' C10 90.9(12) . . ? C33' Fe3' C10 160.2(12) . . ? C9 Fe3' C10 38.4(5) . . ? C32' Fe3' Fe2 145.2(10) . . ? C31' Fe3' Fe2 102.8(18) . . ? C33' Fe3' Fe2 109.7(10) . . ? C9 Fe3' Fe2 51.2(5) . . ? C10 Fe3' Fe2 50.5(4) . . ? C32' Fe3' W2 97.8(8) . . ? C31' Fe3' W2 161.7(21) . . ? C33' Fe3' W2 89.7(13) . . ? C9 Fe3' W2 44.6(4) . . ? C10 Fe3' W2 80.8(6) . . ? Fe2 Fe3' W2 59.4(4) . . ? Fe2 S1 W1 70.89(6) . . ? Fe2 S1 W2 69.96(6) . . ? W1 S1 W2 73.98(6) . . ? W1 S2 Fe1 71.82(7) . . ? W1 S2 W2 73.47(6) . . ? Fe1 S2 W2 103.81(9) . . ? C2 C1 W1 138.3(6) . . ? C2 C1 Fe2 129.4(7) . . ? W1 C1 Fe2 83.1(3) . . ? C2 C1 Fe1 123.6(6) . . ? W1 C1 Fe1 84.1(3) . . ? Fe2 C1 Fe1 77.7(3) . . ? C3 C2 C1 116.1(8) . . ? C8 C3 C4 119.8(10) . . ? C8 C3 C2 121.6(9) . . ? C4 C3 C2 118.6(10) . . ? C3 C4 C5 117.2(12) . . ? C6 C5 C4 121.5(13) . . ? C5 C6 C7 123.8(14) . . ? C6 C7 C8 115.8(12) . . ? C3 C8 C7 121.8(10) . . ? C10 C9 W2 152.5(7) . . ? C10 C9 Fe3' 75.8(7) . . ? W2 C9 Fe3' 90.5(6) . . ? C10 C9 Fe2 71.0(5) . . ? W2 C9 Fe2 83.5(3) . . ? Fe3' C9 Fe2 80.8(6) . . ? C10 C9 Fe3 70.6(9) . . ? W2 C9 Fe3 92.9(9) . . ? Fe2 C9 Fe3 73.7(8) . . ? C9 C10 C11 142.2(8) . . ? C9 C10 Fe2 71.1(5) . . ? C11 C10 Fe2 141.5(6) . . ? C9 C10 Fe3' 65.8(6) . . ? C11 C10 Fe3' 126.9(8) . . ? Fe2 C10 Fe3' 78.0(5) . . ? C9 C10 Fe3 72.8(8) . . ? C11 C10 Fe3 125.1(10) . . ? Fe2 C10 Fe3 74.3(9) . . ? C16 C11 C12 117.6(8) . . ? C16 C11 C10 124.9(8) . . ? C12 C11 C10 117.4(8) . . ? C13 C12 C11 119.7(9) . . ? C14 C13 C12 122.1(10) . . ? C13 C14 C15 118.8(8) . . ? C14 C15 C16 119.6(9) . . ? C11 C16 C15 122.1(9) . . ? C21 C17 C18 108.4(10) . . ? C21 C17 W1 72.2(6) . . ? C18 C17 W1 72.4(5) . . ? C19 C18 C17 108.4(9) . . ? C19 C18 W1 73.2(5) . . ? C17 C18 W1 73.1(5) . . ? C18 C19 C20 108.3(10) . . ? C18 C19 W1 72.6(5) . . ? C20 C19 W1 71.4(5) . . ? C19 C20 C21 107.2(9) . . ? C19 C20 W1 73.8(5) . . ? C21 C20 W1 72.8(5) . . ? C17 C21 C20 107.6(9) . . ? C17 C21 W1 73.5(5) . . ? C20 C21 W1 71.7(5) . . ? C26 C22 C23 109.4(12) . . ? C26 C22 W2 73.5(8) . . ? C23 C22 W2 74.5(7) . . ? C22 C23 C24 107.1(11) . . ? C22 C23 W2 70.8(7) . . ? C24 C23 W2 73.2(7) . . ? C25 C24 C23 107.5(11) . . ? C25 C24 W2 72.1(6) . . ? C23 C24 W2 72.5(6) . . ? C26 C25 C24 108.3(12) . . ? C26 C25 W2 71.8(6) . . ? C24 C25 W2 73.6(6) . . ? C22 C26 C25 107.7(11) . . ? C22 C26 W2 72.4(7) . . ? C25 C26 W2 73.6(7) . . ? O27 C27 Fe1 177.5(7) . . ? O28 C28 Fe1 178.9(10) . . ? O29 C29 Fe1 177.3(11) . . ? O30 C30 Fe2 178.8(9) . . ? O31 C31 Fe3 170.1(100) . . ? O31' C31' Fe3' 170.8(62) . . ? O32 C32 Fe3 176.2(43) . . ? O32' C32' Fe3' 176.8(33) . . ? O33 C33 Fe3 166.8(51) . . ? O33' C33' Fe3' 175.1(31) . . ? _refine_diff_density_max 1.384 _refine_diff_density_min -1.204 _refine_diff_density_rms 0.160 #===END data_8 _database_code_CSD 168676 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H22 Fe3 O7 Se2 W2' _chemical_formula_weight 1223.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 '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 10.7612(2) _cell_length_b 17.0519(3) _cell_length_c 18.832 _cell_angle_alpha 90.00 _cell_angle_beta 92.73 _cell_angle_gamma 90.00 _cell_volume 3451.77(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6084 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max .30 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.355 _exptl_crystal_density_method ? _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 10.025 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.112488 _exptl_absorpt_correction_T_max 0.266840 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26018 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6084 _reflns_number_observed 4460 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXTL-V.5.03 Sheldrick, 1994' _computing_structure_refinement 'SHELXL-V.5.03 Sheldrick, 1994' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 19 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00026(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6065 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_obs 0.0370 _refine_ls_wR_factor_all 0.0808 _refine_ls_wR_factor_obs 0.0727 _refine_ls_goodness_of_fit_all 0.997 _refine_ls_goodness_of_fit_obs 1.067 _refine_ls_restrained_S_all 1.003 _refine_ls_restrained_S_obs 1.067 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.37520(3) 0.15742(2) 0.18221(2) 0.03339(11) Uani 1 d . . W2 W 0.53781(3) 0.20507(2) 0.07338(2) 0.03765(11) Uani 1 d . . Fe1 Fe 0.28577(11) 0.30810(6) 0.17582(6) 0.0383(3) Uani 1 d . . Fe2 Fe 0.29050(11) 0.22498(6) 0.05976(6) 0.0340(3) Uani 1 d . . Fe3 Fe 0.40277(13) 0.22979(6) -0.05795(6) 0.0483(3) Uani 1 d . . Se1 Se 0.50554(8) 0.27384(4) 0.19096(4) 0.0413(2) Uani 1 d . . Se2 Se 0.38254(8) 0.09744(4) 0.06358(4) 0.0409(2) Uani 1 d . . C1 C 0.2101(8) 0.1974(4) 0.1542(5) 0.045(2) Uani 1 d . . C2 C 0.0728(8) 0.1774(5) 0.1672(5) 0.057(3) Uani 1 d . . H2A H 0.0547(8) 0.1952(5) 0.2145(5) 0.068 Uiso 1 calc R . H2B H 0.0205(8) 0.2073(5) 0.1337(5) 0.068 Uiso 1 calc R . C3 C 0.0352(8) 0.0920(5) 0.1607(6) 0.061(3) Uani 1 d . . C4 C 0.0605(10) 0.0469(5) 0.1033(6) 0.069(3) Uani 1 d . . H4 H 0.1055(10) 0.0679(5) 0.0669(6) 0.083 Uiso 1 calc R . C5 C 0.0185(12) -0.0319(6) 0.0988(7) 0.092(4) Uani 1 d . . H5 H 0.0340(12) -0.0622(6) 0.0592(7) 0.110 Uiso 1 calc R . C6 C -0.0448(14) -0.0626(8) 0.1533(9) 0.111(5) Uani 1 d . . H6 H -0.0699(14) -0.1148(8) 0.1514(9) 0.133 Uiso 1 calc R . C7 C -0.0711(12) -0.0185(8) 0.2095(9) 0.104(5) Uani 1 d . . H7 H -0.1167(12) -0.0404(8) 0.2452(9) 0.124 Uiso 1 calc R . C8 C -0.0325(9) 0.0592(6) 0.2161(6) 0.079(3) Uani 1 d . . H8 H -0.0507(9) 0.0887(6) 0.2558(6) 0.095 Uiso 1 calc R . C9 C 0.4405(8) 0.2917(4) 0.0318(4) 0.036(2) Uani 1 d . . C10 C 0.3359(8) 0.3214(4) 0.0024(4) 0.038(2) Uani 1 d . . C11 C 0.2876(8) 0.3966(4) -0.0255(4) 0.040(2) Uani 1 d . . C12 C 0.3692(9) 0.4531(5) -0.0472(5) 0.060(3) Uani 1 d . . H12 H 0.4544(9) 0.4440(5) -0.0426(5) 0.072 Uiso 1 calc R . C13 C 0.3258(10) 0.5228(5) -0.0756(6) 0.077(3) Uani 1 d . . H13 H 0.3823(10) 0.5606(5) -0.0891(6) 0.093 Uiso 1 calc R . C14 C 0.2013(10) 0.5373(5) -0.0843(6) 0.068(3) Uani 1 d . . H14 H 0.1736(10) 0.5848(5) -0.1034(6) 0.082 Uiso 1 calc R . C15 C 0.1168(9) 0.4818(5) -0.0650(5) 0.060(3) Uani 1 d . . H15 H 0.0319(9) 0.4910(5) -0.0715(5) 0.072 Uiso 1 calc R . C16 C 0.1604(9) 0.4113(5) -0.0354(5) 0.052(2) Uani 1 d . . H16 H 0.1036(9) 0.3736(5) -0.0221(5) 0.062 Uiso 1 calc R . C17 C 0.2843(10) 0.0920(6) 0.2759(5) 0.062(3) Uani 1 d . . H17 H 0.1972(10) 0.0966(6) 0.2883(5) 0.074 Uiso 1 calc R . C18 C 0.3810(12) 0.1350(5) 0.3049(5) 0.062(3) Uani 1 d . . H18 H 0.3743(12) 0.1755(5) 0.3414(5) 0.074 Uiso 1 calc R . C19 C 0.4918(10) 0.1052(6) 0.2808(5) 0.067(3) Uani 1 d . . H19 H 0.5761(10) 0.1206(6) 0.2972(5) 0.080 Uiso 1 calc R . C20 C 0.4598(12) 0.0434(6) 0.2355(5) 0.071(3) Uani 1 d . . H20 H 0.5185(12) 0.0078(6) 0.2138(5) 0.085 Uiso 1 calc R . C21 C 0.3314(12) 0.0360(5) 0.2311(5) 0.071(3) Uani 1 d . . H21 H 0.2841(12) -0.0064(5) 0.2074(5) 0.085 Uiso 1 calc R . C22 C 0.7068(11) 0.1674(9) 0.0063(7) 0.093(4) Uani 1 d . . H22 H 0.7065(11) 0.1579(9) -0.0450(7) 0.111 Uiso 1 calc R . C23 C 0.6974(10) 0.1115(6) 0.0605(9) 0.086(4) Uani 1 d . . H23 H 0.6841(10) 0.0552(6) 0.0528(9) 0.103 Uiso 1 calc R . C24 C 0.7196(10) 0.1470(9) 0.1267(7) 0.088(4) Uani 1 d . . H24 H 0.7278(10) 0.1210(9) 0.1731(7) 0.106 Uiso 1 calc R . C25 C 0.7437(9) 0.2247(8) 0.1120(8) 0.085(4) Uani 1 d . . H25 H 0.7710(9) 0.2635(8) 0.1478(8) 0.102 Uiso 1 calc R . C26 C 0.7365(10) 0.2381(7) 0.0428(9) 0.089(4) Uani 1 d . . H26 H 0.7595(10) 0.2873(7) 0.0200(9) 0.107 Uiso 1 calc R . C27 C 0.2688(10) 0.3244(5) 0.2695(5) 0.061(3) Uani 1 d . . O27 O 0.2534(9) 0.3364(4) 0.3271(4) 0.105(3) Uani 1 d . . O28 O 0.3791(7) 0.4624(3) 0.1346(3) 0.066(2) Uani 1 d . . C28 C 0.3453(8) 0.4018(5) 0.1507(4) 0.044(2) Uani 1 d . . O29 O 0.0360(8) 0.3601(4) 0.1326(5) 0.107(3) Uani 1 d . . C29 C 0.1354(10) 0.3388(5) 0.1505(6) 0.066(3) Uani 1 d . . O30 O 0.0433(7) 0.2146(4) -0.0097(4) 0.086(2) Uani 1 d . . C30 C 0.1400(10) 0.2187(5) 0.0184(5) 0.054(2) Uani 1 d . . C31 C 0.2791(13) 0.2464(6) -0.1211(6) 0.079(4) Uani 1 d . . O31 O 0.1973(11) 0.2595(5) -0.1613(5) 0.142(4) Uani 1 d . . O32 O 0.4595(11) 0.0723(4) -0.1097(4) 0.134(4) Uani 1 d . . C32 C 0.4372(12) 0.1332(6) -0.0873(5) 0.078(4) Uani 1 d . . C33 C 0.5216(12) 0.2793(6) -0.1045(6) 0.080(4) Uani 1 d . . O33 O 0.5938(11) 0.3118(5) -0.1339(5) 0.146(5) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0327(2) 0.0330(2) 0.0340(2) 0.00101(13) -0.00298(14) 0.00336(13) W2 0.0307(2) 0.0384(2) 0.0439(2) 0.00618(14) 0.00184(15) 0.00885(14) Fe1 0.0346(8) 0.0336(6) 0.0466(7) -0.0037(5) 0.0015(5) 0.0046(5) Fe2 0.0298(7) 0.0315(5) 0.0397(7) 0.0026(5) -0.0072(5) 0.0025(5) Fe3 0.0700(10) 0.0393(6) 0.0353(7) -0.0002(5) -0.0007(6) 0.0126(6) Se1 0.0353(5) 0.0423(4) 0.0452(5) -0.0028(4) -0.0110(4) -0.0012(4) Se2 0.0523(6) 0.0318(4) 0.0382(5) -0.0014(3) -0.0028(4) 0.0044(4) C1 0.041(6) 0.038(4) 0.059(6) 0.000(4) 0.012(4) 0.003(4) C2 0.036(6) 0.050(5) 0.084(7) 0.018(5) 0.008(5) 0.001(4) C3 0.028(6) 0.051(5) 0.101(8) 0.020(5) -0.020(5) -0.008(4) C4 0.057(8) 0.057(6) 0.091(8) 0.008(6) -0.013(6) -0.011(5) C5 0.090(10) 0.058(7) 0.123(11) 0.009(7) -0.045(8) -0.018(6) C6 0.104(13) 0.068(8) 0.154(15) 0.043(9) -0.060(11) -0.034(8) C7 0.069(10) 0.098(10) 0.142(14) 0.058(9) -0.015(9) -0.037(8) C8 0.041(7) 0.084(7) 0.111(9) 0.048(7) -0.012(6) -0.017(6) C9 0.034(5) 0.033(4) 0.040(5) 0.005(3) -0.001(4) -0.004(4) C10 0.041(6) 0.029(4) 0.044(5) 0.001(3) -0.004(4) 0.001(4) C11 0.044(6) 0.029(4) 0.045(5) 0.001(3) -0.011(4) 0.011(4) C12 0.045(6) 0.044(5) 0.092(8) 0.018(5) 0.002(5) 0.008(4) C13 0.052(8) 0.047(5) 0.132(10) 0.032(6) 0.004(7) -0.003(5) C14 0.055(8) 0.046(5) 0.104(9) 0.026(5) -0.008(6) 0.010(5) C15 0.040(6) 0.057(6) 0.083(7) 0.008(5) -0.015(5) 0.023(5) C16 0.048(6) 0.040(5) 0.066(6) 0.004(4) -0.013(5) 0.008(4) C17 0.060(8) 0.078(7) 0.049(6) 0.020(5) 0.010(5) 0.002(6) C18 0.096(10) 0.053(5) 0.036(6) 0.009(4) -0.005(6) 0.019(6) C19 0.057(8) 0.082(7) 0.059(7) 0.027(6) -0.029(5) -0.012(6) C20 0.104(10) 0.061(6) 0.048(6) 0.017(5) 0.012(6) 0.043(6) C21 0.108(11) 0.046(5) 0.056(7) 0.022(5) -0.020(6) -0.029(6) C22 0.063(9) 0.143(12) 0.075(9) 0.007(9) 0.024(7) 0.053(8) C23 0.043(8) 0.068(7) 0.148(13) -0.008(8) 0.020(8) 0.029(5) C24 0.033(7) 0.135(11) 0.096(10) 0.054(9) 0.000(6) 0.052(7) C25 0.027(7) 0.120(11) 0.106(11) -0.006(9) -0.011(6) 0.009(6) C26 0.037(7) 0.093(9) 0.139(13) 0.033(9) 0.033(8) 0.016(6) C27 0.074(8) 0.048(5) 0.060(7) -0.003(5) 0.015(6) -0.007(5) O27 0.169(10) 0.091(5) 0.060(5) -0.014(4) 0.044(6) -0.021(5) O28 0.091(6) 0.041(3) 0.067(5) 0.000(3) 0.011(4) -0.007(3) C28 0.039(6) 0.044(5) 0.046(5) -0.003(4) -0.005(4) 0.010(4) O29 0.051(6) 0.081(5) 0.188(10) 0.017(5) -0.024(6) 0.019(4) C29 0.042(7) 0.045(5) 0.111(9) 0.008(5) 0.002(6) 0.003(5) O30 0.056(6) 0.079(5) 0.118(7) 0.020(4) -0.046(5) -0.019(4) C30 0.048(7) 0.042(5) 0.069(7) 0.003(4) -0.020(5) -0.004(4) C31 0.126(11) 0.054(6) 0.053(7) -0.016(5) -0.043(7) 0.011(6) O31 0.188(12) 0.108(7) 0.118(8) -0.024(6) -0.108(8) 0.037(7) O32 0.269(14) 0.059(5) 0.076(6) -0.009(4) 0.033(7) 0.068(6) C32 0.139(11) 0.057(6) 0.039(6) 0.008(5) 0.013(6) 0.035(6) C33 0.118(11) 0.060(6) 0.064(7) 0.009(5) 0.029(7) 0.019(6) O33 0.179(11) 0.122(7) 0.144(9) 0.040(6) 0.105(9) 0.002(7) _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 W1 C1 1.951(9) . ? W1 C21 2.323(8) . ? W1 C18 2.339(9) . ? W1 C17 2.340(8) . ? W1 C20 2.351(9) . ? W1 C19 2.365(9) . ? W1 Se1 2.4316(8) . ? W1 Se2 2.4616(8) . ? W1 Fe2 2.6972(11) . ? W1 Fe1 2.7443(10) . ? W1 W2 2.8747(4) . ? W2 C9 1.952(8) . ? W2 C26 2.310(10) . ? W2 C25 2.323(11) . ? W2 C22 2.352(9) . ? W2 C23 2.365(9) . ? W2 C24 2.372(9) . ? W2 Se2 2.4828(9) . ? W2 Se1 2.5441(8) . ? W2 Fe2 2.6831(12) . ? W2 Fe3 2.8397(14) . ? Fe1 C29 1.746(11) . ? Fe1 C28 1.793(8) . ? Fe1 C27 1.804(10) . ? Fe1 C1 2.088(8) . ? Fe1 Se1 2.4396(15) . ? Fe1 Fe2 2.6075(15) . ? Fe2 C30 1.767(11) . ? Fe2 C10 2.039(7) . ? Fe2 C9 2.063(7) . ? Fe2 C1 2.069(8) . ? Fe2 Se2 2.3894(12) . ? Fe2 Fe3 2.5761(15) . ? Fe3 C31 1.765(12) . ? Fe3 C32 1.782(9) . ? Fe3 C33 1.795(11) . ? Fe3 C9 2.017(8) . ? Fe3 C10 2.081(7) . ? C1 C2 1.548(11) . ? C2 C3 1.514(11) . ? C3 C4 1.366(13) . ? C3 C8 1.415(13) . ? C4 C5 1.417(13) . ? C5 C6 1.36(2) . ? C6 C7 1.34(2) . ? C7 C8 1.392(15) . ? C9 C10 1.331(11) . ? C10 C11 1.470(10) . ? C11 C12 1.378(11) . ? C11 C16 1.396(12) . ? C12 C13 1.377(12) . ? C13 C14 1.365(14) . ? C14 C15 1.373(12) . ? C15 C16 1.396(11) . ? C17 C18 1.365(14) . ? C17 C21 1.386(13) . ? C18 C19 1.391(13) . ? C19 C20 1.389(13) . ? C20 C21 1.386(15) . ? C22 C23 1.40(2) . ? C22 C26 1.42(2) . ? C23 C24 1.40(2) . ? C24 C25 1.380(15) . ? C25 C26 1.32(2) . ? C27 O27 1.124(10) . ? O28 C28 1.141(9) . ? O29 C29 1.164(12) . ? O30 C30 1.147(11) . ? C31 O31 1.155(13) . ? O32 C32 1.151(10) . ? C33 O33 1.122(12) . ? 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 W1 C21 102.6(4) . . ? C1 W1 C18 107.8(4) . . ? C21 W1 C18 57.3(3) . . ? C1 W1 C17 87.8(3) . . ? C21 W1 C17 34.6(3) . . ? C18 W1 C17 33.9(3) . . ? C1 W1 C20 137.1(4) . . ? C21 W1 C20 34.5(4) . . ? C18 W1 C20 56.8(3) . . ? C17 W1 C20 56.7(3) . . ? C1 W1 C19 141.8(4) . . ? C21 W1 C19 57.6(4) . . ? C18 W1 C19 34.4(3) . . ? C17 W1 C19 56.9(4) . . ? C20 W1 C19 34.3(3) . . ? C1 W1 Se1 104.4(2) . . ? C21 W1 Se1 145.9(3) . . ? C18 W1 Se1 94.5(3) . . ? C17 W1 Se1 126.7(3) . . ? C20 W1 Se1 115.8(4) . . ? C19 W1 Se1 88.4(2) . . ? C1 W1 Se2 88.2(2) . . ? C21 W1 Se2 90.3(3) . . ? C18 W1 Se2 145.9(2) . . ? C17 W1 Se2 121.3(3) . . ? C20 W1 Se2 90.9(2) . . ? C19 W1 Se2 121.2(3) . . ? Se1 W1 Se2 110.94(3) . . ? C1 W1 Fe2 49.7(2) . . ? C21 W1 Fe2 130.7(3) . . ? C18 W1 Fe2 155.0(2) . . ? C17 W1 Fe2 135.4(3) . . ? C20 W1 Fe2 145.7(3) . . ? C19 W1 Fe2 167.7(3) . . ? Se1 W1 Fe2 83.09(3) . . ? Se2 W1 Fe2 54.96(3) . . ? C1 W1 Fe1 49.3(2) . . ? C21 W1 Fe1 140.7(3) . . ? C18 W1 Fe1 100.9(2) . . ? C17 W1 Fe1 108.7(2) . . ? C20 W1 Fe1 157.0(3) . . ? C19 W1 Fe1 124.0(3) . . ? Se1 W1 Fe1 55.85(3) . . ? Se2 W1 Fe1 112.06(3) . . ? Fe2 W1 Fe1 57.26(3) . . ? C1 W1 W2 106.6(2) . . ? C21 W1 W2 132.5(3) . . ? C18 W1 W2 139.6(3) . . ? C17 W1 W2 164.3(3) . . ? C20 W1 W2 107.5(3) . . ? C19 W1 W2 110.4(3) . . ? Se1 W1 W2 56.56(2) . . ? Se2 W1 W2 54.79(2) . . ? Fe2 W1 W2 57.47(2) . . ? Fe1 W1 W2 85.89(2) . . ? C9 W2 C26 101.6(4) . . ? C9 W2 C25 120.1(4) . . ? C26 W2 C25 33.2(4) . . ? C9 W2 C22 113.9(4) . . ? C26 W2 C22 35.3(4) . . ? C25 W2 C22 57.1(4) . . ? C9 W2 C23 147.9(4) . . ? C26 W2 C23 56.9(4) . . ? C25 W2 C23 56.1(4) . . ? C22 W2 C23 34.6(4) . . ? C9 W2 C24 154.3(4) . . ? C26 W2 C24 56.8(4) . . ? C25 W2 C24 34.2(4) . . ? C22 W2 C24 58.0(4) . . ? C23 W2 C24 34.3(4) . . ? C9 W2 Se2 100.5(2) . . ? C26 W2 Se2 142.1(4) . . ? C25 W2 Se2 139.3(4) . . ? C22 W2 Se2 107.0(4) . . ? C23 W2 Se2 89.0(3) . . ? C24 W2 Se2 105.2(4) . . ? C9 W2 Se1 84.7(2) . . ? C26 W2 Se1 105.7(4) . . ? C25 W2 Se1 80.1(3) . . ? C22 W2 Se1 137.2(4) . . ? C23 W2 Se1 122.0(4) . . ? C24 W2 Se1 88.2(4) . . ? Se2 W2 Se1 106.62(3) . . ? C9 W2 Fe2 49.8(2) . . ? C26 W2 Fe2 150.5(3) . . ? C25 W2 Fe2 159.8(3) . . ? C22 W2 Fe2 140.5(4) . . ? C23 W2 Fe2 142.9(3) . . ? C24 W2 Fe2 152.6(3) . . ? Se2 W2 Fe2 54.94(3) . . ? Se1 W2 Fe2 81.31(3) . . ? C9 W2 Fe3 45.3(2) . . ? C26 W2 Fe3 100.8(4) . . ? C25 W2 Fe3 133.8(4) . . ? C22 W2 Fe3 87.1(3) . . ? C23 W2 Fe3 110.8(4) . . ? C24 W2 Fe3 143.9(3) . . ? Se2 W2 Fe3 74.36(3) . . ? Se1 W2 Fe3 127.17(3) . . ? Fe2 W2 Fe3 55.52(3) . . ? C9 W2 W1 99.6(2) . . ? C26 W2 W1 148.1(4) . . ? C25 W2 W1 114.9(4) . . ? C22 W2 W1 144.9(4) . . ? C23 W2 W1 110.6(3) . . ? C24 W2 W1 95.6(3) . . ? Se2 W2 W1 54.11(2) . . ? Se1 W2 W1 52.90(2) . . ? Fe2 W2 W1 57.94(2) . . ? Fe3 W2 W1 111.06(3) . . ? C29 Fe1 C28 90.0(4) . . ? C29 Fe1 C27 94.9(5) . . ? C28 Fe1 C27 100.1(4) . . ? C29 Fe1 C1 82.5(4) . . ? C28 Fe1 C1 153.5(4) . . ? C27 Fe1 C1 105.8(3) . . ? C29 Fe1 Se1 170.0(3) . . ? C28 Fe1 Se1 83.5(3) . . ? C27 Fe1 Se1 93.7(3) . . ? C1 Fe1 Se1 100.0(2) . . ? C29 Fe1 Fe2 89.3(4) . . ? C28 Fe1 Fe2 104.0(3) . . ? C27 Fe1 Fe2 155.5(3) . . ? C1 Fe1 Fe2 50.8(2) . . ? Se1 Fe1 Fe2 84.85(4) . . ? C29 Fe1 W1 127.7(3) . . ? C28 Fe1 W1 135.8(3) . . ? C27 Fe1 W1 98.8(3) . . ? C1 Fe1 W1 45.1(2) . . ? Se1 Fe1 W1 55.57(3) . . ? Fe2 Fe1 W1 60.46(3) . . ? C30 Fe2 C10 93.0(4) . . ? C30 Fe2 C9 129.3(4) . . ? C10 Fe2 C9 37.9(3) . . ? C30 Fe2 C1 87.3(4) . . ? C10 Fe2 C1 139.4(3) . . ? C9 Fe2 C1 135.1(3) . . ? C30 Fe2 Se2 109.2(3) . . ? C10 Fe2 Se2 129.8(2) . . ? C9 Fe2 Se2 100.4(2) . . ? C1 Fe2 Se2 87.5(2) . . ? C30 Fe2 Fe3 94.6(3) . . ? C10 Fe2 Fe3 52.0(2) . . ? C9 Fe2 Fe3 50.1(2) . . ? C1 Fe2 Fe3 168.4(2) . . ? Se2 Fe2 Fe3 81.03(4) . . ? C30 Fe2 Fe1 110.4(3) . . ? C10 Fe2 Fe1 91.2(2) . . ? C9 Fe2 Fe1 87.8(2) . . ? C1 Fe2 Fe1 51.5(2) . . ? Se2 Fe2 Fe1 119.61(5) . . ? Fe3 Fe2 Fe1 137.11(6) . . ? C30 Fe2 W2 156.7(3) . . ? C10 Fe2 W2 83.8(2) . . ? C9 Fe2 W2 46.3(2) . . ? C1 Fe2 W2 110.0(3) . . ? Se2 Fe2 W2 58.27(3) . . ? Fe3 Fe2 W2 65.32(4) . . ? Fe1 Fe2 W2 92.73(5) . . ? C30 Fe2 W1 128.1(3) . . ? C10 Fe2 W1 135.8(3) . . ? C9 Fe2 W1 102.5(2) . . ? C1 Fe2 W1 46.0(3) . . ? Se2 Fe2 W1 57.50(3) . . ? Fe3 Fe2 W1 126.59(5) . . ? Fe1 Fe2 W1 62.28(4) . . ? W2 Fe2 W1 64.59(3) . . ? C31 Fe3 C32 95.8(5) . . ? C31 Fe3 C33 97.3(6) . . ? C32 Fe3 C33 96.9(5) . . ? C31 Fe3 C9 126.6(4) . . ? C32 Fe3 C9 135.0(4) . . ? C33 Fe3 C9 92.5(4) . . ? C31 Fe3 C10 88.8(4) . . ? C32 Fe3 C10 161.0(4) . . ? C33 Fe3 C10 100.8(4) . . ? C9 Fe3 C10 37.9(3) . . ? C31 Fe3 Fe2 102.5(4) . . ? C32 Fe3 Fe2 110.5(3) . . ? C33 Fe3 Fe2 144.0(4) . . ? C9 Fe3 Fe2 51.6(2) . . ? C10 Fe3 Fe2 50.6(2) . . ? C31 Fe3 W2 161.6(4) . . ? C32 Fe3 W2 91.6(4) . . ? C33 Fe3 W2 98.5(4) . . ? C9 Fe3 W2 43.4(2) . . ? C10 Fe3 W2 79.1(2) . . ? Fe2 Fe3 W2 59.16(4) . . ? W1 Se1 Fe1 68.58(3) . . ? W1 Se1 W2 70.54(2) . . ? Fe1 Se1 W2 100.40(4) . . ? Fe2 Se2 W1 67.54(3) . . ? Fe2 Se2 W2 66.80(3) . . ? W1 Se2 W2 71.10(2) . . ? C2 C1 W1 138.1(6) . . ? C2 C1 Fe2 128.8(7) . . ? W1 C1 Fe2 84.2(3) . . ? C2 C1 Fe1 122.3(5) . . ? W1 C1 Fe1 85.5(3) . . ? Fe2 C1 Fe1 77.7(3) . . ? C3 C2 C1 116.9(7) . . ? C4 C3 C8 119.3(9) . . ? C4 C3 C2 122.8(9) . . ? C8 C3 C2 117.8(10) . . ? C3 C4 C5 120.4(10) . . ? C6 C5 C4 119.3(13) . . ? C7 C6 C5 120.7(12) . . ? C6 C7 C8 122.1(12) . . ? C7 C8 C3 118.2(12) . . ? C10 C9 W2 151.9(6) . . ? C10 C9 Fe3 73.7(5) . . ? W2 C9 Fe3 91.3(3) . . ? C10 C9 Fe2 70.1(5) . . ? W2 C9 Fe2 83.8(3) . . ? Fe3 C9 Fe2 78.3(3) . . ? C9 C10 C11 139.3(8) . . ? C9 C10 Fe2 72.0(4) . . ? C11 C10 Fe2 143.4(6) . . ? C9 C10 Fe3 68.5(4) . . ? C11 C10 Fe3 125.8(6) . . ? Fe2 C10 Fe3 77.4(2) . . ? C12 C11 C16 117.9(7) . . ? C12 C11 C10 119.8(8) . . ? C16 C11 C10 122.2(7) . . ? C13 C12 C11 120.7(9) . . ? C14 C13 C12 121.0(9) . . ? C13 C14 C15 120.1(8) . . ? C14 C15 C16 119.0(9) . . ? C15 C16 C11 121.2(8) . . ? C18 C17 C21 108.6(10) . . ? C18 C17 W1 73.0(5) . . ? C21 C17 W1 72.0(5) . . ? C17 C18 C19 108.9(9) . . ? C17 C18 W1 73.1(5) . . ? C19 C18 W1 73.8(5) . . ? C20 C19 C18 106.6(10) . . ? C20 C19 W1 72.3(6) . . ? C18 C19 W1 71.8(6) . . ? C21 C20 C19 108.9(9) . . ? C21 C20 W1 71.6(5) . . ? C19 C20 W1 73.4(5) . . ? C20 C21 C17 107.0(9) . . ? C20 C21 W1 73.9(5) . . ? C17 C21 W1 73.4(5) . . ? C23 C22 C26 104.4(11) . . ? C23 C22 W2 73.2(5) . . ? C26 C22 W2 70.7(5) . . ? C24 C23 C22 109.8(11) . . ? C24 C23 W2 73.1(5) . . ? C22 C23 W2 72.2(5) . . ? C25 C24 C23 105.3(11) . . ? C25 C24 W2 71.0(6) . . ? C23 C24 W2 72.6(6) . . ? C26 C25 C24 111.1(13) . . ? C26 C25 W2 72.9(7) . . ? C24 C25 W2 74.9(7) . . ? C25 C26 C22 109.4(11) . . ? C25 C26 W2 74.0(6) . . ? C22 C26 W2 74.0(6) . . ? O27 C27 Fe1 176.8(10) . . ? O28 C28 Fe1 177.6(8) . . ? O29 C29 Fe1 178.8(9) . . ? O30 C30 Fe2 178.6(10) . . ? O31 C31 Fe3 177.7(9) . . ? O32 C32 Fe3 176.4(8) . . ? O33 C33 Fe3 178.2(11) . . ? _refine_diff_density_max 1.489 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.165 #===END data_9 _database_code_CSD 168677 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H10 Fe2 O8 W' _chemical_formula_weight 685.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 '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 8.0835(2) _cell_length_b 14.3002(2) _cell_length_c 37.4493(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.2130(10) _cell_angle_gamma 90.00 _cell_volume 4325.75(13) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7623 _cell_measurement_theta_min 1.09 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max .42 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.106 _exptl_crystal_density_method ? _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 6.674 _exptl_absorpt_correction_type 'empirical (SADABS Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.112488 _exptl_absorpt_correction_T_max 0.266840 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker Smart CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32487 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7623 _reflns_number_observed 5840 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXTL-V.5.03 Sheldrick, 1994' _computing_structure_refinement 'SHELXL-V.5.03 Sheldrick, 1994' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+4.2615P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00069(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7608 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_obs 0.0306 _refine_ls_wR_factor_all 0.0585 _refine_ls_wR_factor_obs 0.0537 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.021 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 1.77362(3) 1.21668(2) 0.424012(6) 0.03868(8) Uani 1 d . . W1' W 0.70540(3) 1.07270(2) 0.184610(6) 0.04356(8) Uani 1 d . . Fe1 Fe 1.64217(9) 1.14353(6) 0.48735(2) 0.0413(2) Uani 1 d . . Fe1' Fe 0.68237(10) 0.90066(5) 0.22284(2) 0.0438(2) Uani 1 d . . Fe2 Fe 1.63557(10) 1.31732(6) 0.48311(2) 0.0495(2) Uani 1 d . . Fe2' Fe 0.85829(9) 1.02184(6) 0.25294(2) 0.0427(2) Uani 1 d . . C1 C 1.8331(6) 1.2307(3) 0.47595(14) 0.0385(13) Uani 1 d . . C1' C 0.6222(6) 1.0368(4) 0.23178(14) 0.0392(13) Uani 1 d . . C2 C 1.8179(7) 1.2294(4) 0.51023(14) 0.0416(13) Uani 1 d . . C2' C 0.6032(6) 0.9918(4) 0.26150(15) 0.0442(14) Uani 1 d . . C3 C 1.9088(7) 1.2376(4) 0.54464(15) 0.0464(14) Uani 1 d . . C3' C 0.5080(7) 0.9951(4) 0.29382(14) 0.0460(14) Uani 1 d . . C4 C 2.0161(9) 1.3115(5) 0.5523(2) 0.075(2) Uani 1 d . . H4 H 2.0268(9) 1.3585(5) 0.5354(2) 0.090 Uiso 1 calc R . C4' C 0.4033(7) 1.0704(5) 0.2989(2) 0.058(2) Uani 1 d . . H4' H 0.3950(7) 1.1172(5) 0.2817(2) 0.070 Uiso 1 calc R . C5 C 2.1073(9) 1.3175(6) 0.5842(2) 0.087(2) Uani 1 d . . H5 H 2.1794(9) 1.3672(6) 0.5885(2) 0.104 Uiso 1 calc R . C5' C 0.3108(8) 1.0771(6) 0.3292(2) 0.074(2) Uani 1 d . . H5' H 0.2411(8) 1.1281(6) 0.3320(2) 0.089 Uiso 1 calc R . C6 C 2.0899(9) 1.2498(6) 0.6090(2) 0.073(2) Uani 1 d . . H6 H 2.1495(9) 1.2535(6) 0.6307(2) 0.088 Uiso 1 calc R . C6' C 0.3205(9) 1.0107(6) 0.3548(2) 0.074(2) Uani 1 d . . H6' H 0.2575(9) 1.0156(6) 0.3750(2) 0.089 Uiso 1 calc R . C7 C 1.9862(9) 1.1763(5) 0.6024(2) 0.071(2) Uani 1 d . . H7 H 1.9774(9) 1.1297(5) 0.6196(2) 0.085 Uiso 1 calc R . C7' C 0.4236(10) 0.9361(5) 0.3508(2) 0.080(2) Uani 1 d . . H7' H 0.4319(10) 0.8906(5) 0.3686(2) 0.096 Uiso 1 calc R . C8 C 1.8935(8) 1.1699(4) 0.5707(2) 0.060(2) Uani 1 d . . H8 H 1.8209(8) 1.1202(4) 0.5669(2) 0.073 Uiso 1 calc R . C8' C 0.5167(8) 0.9273(4) 0.3204(2) 0.067(2) Uani 1 d . . H8' H 0.5852(8) 0.8757(4) 0.3179(2) 0.080 Uiso 1 calc R . C9 C 1.8118(8) 1.0610(4) 0.4056(2) 0.060(2) Uani 1 d . . H9 H 1.7568(8) 1.0057(4) 0.4151(2) 0.072 Uiso 1 calc R . C9' C 0.5685(16) 1.0030(7) 0.1359(2) 0.097(3) Uani 1 d . . H9' H 0.5592(16) 0.9354(7) 0.1319(2) 0.117 Uiso 1 calc R . C10 C 1.7589(8) 1.1127(4) 0.3753(2) 0.058(2) Uani 1 d . . H10 H 1.6597(8) 1.0998(4) 0.3603(2) 0.069 Uiso 1 calc R . C10' C 0.6835(13) 1.0577(10) 0.1225(2) 0.108(3) Uani 1 d . . H10' H 0.7723(13) 1.0367(10) 0.1074(2) 0.129 Uiso 1 calc R . C11 C 1.8779(8) 1.1821(5) 0.3688(2) 0.059(2) Uani 1 d . . H11 H 1.8787(8) 1.2238(5) 0.3481(2) 0.071 Uiso 1 calc R . C11' C 0.6505(14) 1.1472(8) 0.1305(2) 0.097(3) Uani 1 d . . H11' H 0.7095(14) 1.2019(8) 0.1217(2) 0.116 Uiso 1 calc R . C12 C 2.0066(8) 1.1720(5) 0.3955(2) 0.061(2) Uani 1 d . . H12 H 2.1126(8) 1.2054(5) 0.3963(2) 0.073 Uiso 1 calc R . C12' C 0.5121(14) 1.1497(7) 0.1498(2) 0.104(3) Uani 1 d . . H12' H 0.4511(14) 1.2058(7) 0.1565(2) 0.125 Uiso 1 calc R . C13 C 1.9637(8) 1.0981(4) 0.4180(2) 0.061(2) Uani 1 d . . H13 H 2.0344(8) 1.0720(4) 0.4374(2) 0.073 Uiso 1 calc R . C13' C 0.4584(10) 1.0558(9) 0.1536(2) 0.098(3) Uani 1 d . . H13' H 0.3535(10) 1.0347(9) 0.1631(2) 0.118 Uiso 1 calc R . C14 C 1.5505(8) 1.2527(4) 0.4036(2) 0.054(2) Uani 1 d . . O14 O 1.4277(6) 1.2684(4) 0.38850(12) 0.0808(15) Uani 1 d . . C14' C 0.7597(12) 1.1993(6) 0.2026(2) 0.100(3) Uani 1 d . . O14' O 0.7809(12) 1.2749(5) 0.2113(2) 0.173(4) Uani 1 d . . C15 C 1.8516(9) 1.3457(5) 0.4144(2) 0.070(2) Uani 1 d . . O15 O 1.9016(9) 1.4176(4) 0.4068(2) 0.125(3) Uani 1 d . . C15' C 0.9440(9) 1.0601(6) 0.1751(2) 0.096(3) Uani 1 d . . O15' O 1.0752(7) 1.0570(6) 0.1657(2) 0.176(4) Uani 1 d . . C16 C 1.4346(11) 1.3354(7) 0.4638(2) 0.103(3) Uani 1 d . . O16 O 1.2998(9) 1.3461(7) 0.4535(2) 0.175(4) Uani 1 d . . C16' C 0.8964(8) 0.9657(5) 0.2944(2) 0.066(2) Uani 1 d . . O16' O 0.9224(7) 0.9317(4) 0.32177(14) 0.109(2) Uani 1 d . . C17 C 1.7220(11) 1.4314(6) 0.4791(2) 0.091(3) Uani 1 d . . O17 O 1.7748(10) 1.5051(4) 0.4778(2) 0.163(3) Uani 1 d . . C17' C 0.9088(8) 1.1368(5) 0.2699(2) 0.059(2) Uani 1 d . . O17' O 0.9492(7) 1.2074(4) 0.28132(13) 0.094(2) Uani 1 d . . C18 C 1.5632(8) 1.3391(5) 0.5262(2) 0.070(2) Uani 1 d . . O18 O 1.5144(7) 1.3549(5) 0.55377(13) 0.111(2) Uani 1 d . . C18' C 1.0549(8) 0.9855(5) 0.2377(2) 0.068(2) Uani 1 d . . O18' O 1.1807(6) 0.9607(5) 0.23017(14) 0.114(2) Uani 1 d . . C19 C 1.4759(8) 1.1101(4) 0.45748(15) 0.051(2) Uani 1 d . . O19 O 1.3628(6) 1.0883(4) 0.43978(11) 0.0786(15) Uani 1 d . . C19' C 0.7268(9) 0.8076(5) 0.2536(2) 0.066(2) Uani 1 d . . O19' O 0.7511(8) 0.7478(4) 0.27308(14) 0.097(2) Uani 1 d . . C20 C 1.5326(7) 1.1334(4) 0.5275(2) 0.057(2) Uani 1 d . . O20 O 1.4641(6) 1.1272(4) 0.55371(12) 0.084(2) Uani 1 d . . C20' C 0.4968(9) 0.8517(5) 0.2036(2) 0.065(2) Uani 1 d . . O20' O 0.3836(7) 0.8149(4) 0.1906(2) 0.107(2) Uani 1 d . . C21 C 1.7519(7) 1.0348(5) 0.4896(2) 0.0490(15) Uani 1 d . . O21 O 1.8251(6) 0.9662(3) 0.49173(13) 0.0704(13) Uani 1 d . . C21' C 0.8122(8) 0.8643(4) 0.1883(2) 0.057(2) Uani 1 d . . O21' O 0.8916(6) 0.8367(3) 0.16562(12) 0.086(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.04212(14) 0.04343(14) 0.03066(12) 0.00473(10) 0.00380(9) -0.00471(11) W1' 0.04279(14) 0.0529(2) 0.03483(13) 0.00578(11) -0.00070(9) 0.00292(12) Fe1 0.0424(5) 0.0501(5) 0.0314(4) 0.0052(4) 0.0006(3) -0.0102(4) Fe1' 0.0505(5) 0.0420(5) 0.0393(5) -0.0048(4) 0.0063(4) 0.0032(4) Fe2 0.0574(6) 0.0519(5) 0.0392(5) -0.0011(4) 0.0001(4) 0.0066(4) Fe2' 0.0415(5) 0.0523(5) 0.0341(4) 0.0009(4) -0.0008(3) 0.0003(4) C1 0.039(3) 0.032(3) 0.044(3) 0.007(2) -0.003(2) -0.006(2) C1' 0.035(3) 0.039(3) 0.043(3) -0.007(3) -0.002(2) 0.005(2) C2 0.047(3) 0.041(3) 0.037(3) 0.001(3) -0.005(2) -0.006(3) C2' 0.044(3) 0.040(3) 0.048(4) -0.003(3) 0.009(3) 0.000(3) C3 0.049(4) 0.050(4) 0.040(3) -0.002(3) -0.001(3) -0.007(3) C3' 0.053(4) 0.050(4) 0.035(3) -0.005(3) 0.007(3) -0.006(3) C4 0.088(5) 0.082(5) 0.055(4) 0.017(4) -0.014(4) -0.041(4) C4' 0.059(4) 0.072(5) 0.043(4) -0.007(3) 0.007(3) 0.002(4) C5 0.090(6) 0.099(6) 0.069(5) 0.001(5) -0.018(4) -0.042(5) C5' 0.059(4) 0.108(6) 0.058(4) -0.031(4) 0.014(3) 0.010(4) C6 0.074(5) 0.093(6) 0.051(4) -0.010(4) -0.023(4) -0.006(4) C6' 0.071(5) 0.103(6) 0.051(4) -0.021(4) 0.023(4) -0.020(5) C7 0.085(5) 0.080(5) 0.045(4) 0.012(4) -0.024(3) -0.006(4) C7' 0.110(6) 0.075(5) 0.057(5) 0.000(4) 0.032(4) -0.026(5) C8 0.074(5) 0.059(4) 0.048(4) 0.005(3) -0.016(3) -0.012(4) C8' 0.089(5) 0.049(4) 0.063(4) -0.005(3) 0.026(4) -0.002(4) C9 0.067(5) 0.051(4) 0.063(4) -0.002(3) 0.017(3) 0.002(3) C9' 0.139(9) 0.084(7) 0.064(6) -0.007(5) -0.055(6) 0.006(7) C10 0.061(4) 0.069(4) 0.043(4) -0.019(3) 0.004(3) -0.004(4) C10' 0.110(8) 0.171(11) 0.041(5) -0.010(6) 0.000(4) 0.035(8) C11 0.075(5) 0.072(5) 0.030(3) 0.002(3) 0.017(3) 0.004(4) C11' 0.132(9) 0.109(8) 0.048(5) 0.034(5) -0.027(5) -0.015(7) C12 0.050(4) 0.081(5) 0.053(4) 0.000(4) 0.019(3) 0.003(3) C12' 0.136(9) 0.105(8) 0.068(6) -0.005(5) -0.041(6) 0.074(7) C13 0.061(4) 0.070(5) 0.051(4) 0.004(3) 0.012(3) 0.025(4) C13' 0.051(5) 0.166(10) 0.077(6) 0.040(7) -0.025(4) -0.018(6) C14 0.054(4) 0.069(4) 0.039(4) 0.006(3) 0.007(3) 0.012(3) O14 0.078(4) 0.107(4) 0.057(3) 0.011(3) -0.014(3) 0.027(3) C14' 0.153(8) 0.053(5) 0.090(6) 0.023(5) -0.051(5) -0.022(5) O14' 0.304(11) 0.060(4) 0.146(6) 0.015(4) -0.105(6) -0.036(5) C15 0.104(6) 0.053(4) 0.055(4) 0.005(3) 0.022(4) -0.018(4) O15 0.210(7) 0.062(4) 0.106(5) 0.001(3) 0.064(5) -0.049(4) C15' 0.052(5) 0.151(8) 0.086(6) 0.065(5) 0.002(4) 0.010(5) O15' 0.053(4) 0.330(11) 0.148(6) 0.138(6) 0.037(4) 0.031(5) C16 0.089(6) 0.157(9) 0.061(5) -0.043(5) -0.011(4) 0.056(6) O16 0.103(5) 0.302(11) 0.118(6) -0.084(6) -0.037(4) 0.107(6) C16' 0.060(4) 0.079(5) 0.059(4) 0.017(4) -0.012(3) -0.008(4) O16' 0.119(5) 0.139(5) 0.066(4) 0.045(4) -0.025(3) -0.006(4) C17 0.124(7) 0.061(5) 0.091(6) 0.003(5) 0.042(5) 0.007(5) O17 0.226(8) 0.050(4) 0.219(8) -0.012(5) 0.084(7) -0.022(5) C17' 0.061(4) 0.077(5) 0.041(4) 0.003(4) 0.002(3) -0.009(4) O17' 0.131(5) 0.078(4) 0.072(4) -0.017(3) -0.008(3) -0.039(3) C18 0.076(5) 0.081(5) 0.052(4) -0.009(4) -0.002(4) 0.014(4) O18 0.116(5) 0.166(6) 0.052(3) -0.035(4) 0.013(3) 0.023(4) C18' 0.052(4) 0.105(6) 0.048(4) -0.005(4) -0.010(3) 0.018(4) O18' 0.059(3) 0.208(7) 0.075(4) -0.013(4) 0.004(3) 0.052(4) C19 0.054(4) 0.063(4) 0.036(3) 0.013(3) 0.002(3) -0.010(3) O19 0.068(3) 0.114(4) 0.052(3) 0.014(3) -0.017(2) -0.037(3) C19' 0.092(5) 0.044(4) 0.062(5) -0.003(3) 0.016(4) 0.002(4) O19' 0.156(5) 0.061(3) 0.076(4) 0.021(3) 0.019(3) 0.020(3) C20 0.057(4) 0.068(4) 0.046(4) 0.001(3) -0.002(3) -0.019(3) O20 0.089(4) 0.113(4) 0.052(3) 0.000(3) 0.028(3) -0.026(3) C20' 0.068(5) 0.056(4) 0.071(5) -0.019(4) 0.011(4) -0.009(4) O20' 0.085(4) 0.114(5) 0.123(5) -0.048(4) 0.007(3) -0.026(4) C21 0.046(4) 0.057(4) 0.043(4) 0.010(3) 0.002(3) -0.012(3) O21 0.065(3) 0.061(3) 0.086(4) 0.018(3) 0.002(2) -0.005(3) C21' 0.067(4) 0.055(4) 0.050(4) -0.004(3) 0.004(3) 0.022(3) O21' 0.103(4) 0.097(4) 0.058(3) -0.003(3) 0.024(3) 0.043(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 W1 C15 1.987(7) . ? W1 C1 1.996(5) . ? W1 C14 1.999(7) . ? W1 C12 2.290(5) . ? W1 C13 2.305(6) . ? W1 C11 2.316(5) . ? W1 C10 2.352(6) . ? W1 C9 2.356(6) . ? W1 Fe1 2.8362(7) . ? W1 Fe2 2.8993(8) . ? W1' C14' 1.975(9) . ? W1' C1' 1.982(5) . ? W1' C15' 1.983(7) . ? W1' C12' 2.279(7) . ? W1' C13' 2.284(7) . ? W1' C11' 2.317(7) . ? W1' C9' 2.322(8) . ? W1' C10' 2.334(8) . ? W1' Fe1' 2.8562(8) . ? W1' Fe2' 2.8915(8) . ? Fe1 C20 1.780(6) . ? Fe1 C19 1.781(7) . ? Fe1 C21 1.791(7) . ? Fe1 C2 2.041(5) . ? Fe1 C1 2.042(5) . ? Fe1 Fe2 2.4908(12) . ? Fe1' C21' 1.776(6) . ? Fe1' C20' 1.782(8) . ? Fe1' C19' 1.787(7) . ? Fe1' C1' 2.037(5) . ? Fe1' C2' 2.068(5) . ? Fe1' Fe2' 2.4844(11) . ? Fe2 C18 1.765(7) . ? Fe2 C16 1.771(9) . ? Fe2 C17 1.784(9) . ? Fe2 C1 2.046(5) . ? Fe2 C2 2.161(6) . ? Fe2' C16' 1.765(7) . ? Fe2' C18' 1.786(7) . ? Fe2' C17' 1.804(8) . ? Fe2' C1' 2.049(5) . ? Fe2' C2' 2.143(5) . ? C1 C2 1.294(7) . ? C1' C2' 1.300(7) . ? C2 C3 1.463(7) . ? C2' C3' 1.460(7) . ? C3 C8 1.383(8) . ? C3 C4 1.390(8) . ? C3' C4' 1.386(8) . ? C3' C8' 1.389(8) . ? C4 C5 1.380(9) . ? C4' C5' 1.388(8) . ? C5 C6 1.353(9) . ? C5' C6' 1.349(10) . ? C6 C7 1.360(9) . ? C6' C7' 1.366(10) . ? C7 C8 1.384(8) . ? C7' C8' 1.396(8) . ? C9 C13 1.401(9) . ? C9 C10 1.405(8) . ? C9' C10' 1.327(12) . ? C9' C13' 1.359(11) . ? C10 C11 1.410(8) . ? C10' C11' 1.344(12) . ? C11 C12 1.423(9) . ? C11' C12' 1.355(11) . ? C12 C13 1.404(8) . ? C12' C13' 1.420(12) . ? C14 O14 1.145(7) . ? C14' O14' 1.140(9) . ? C15 O15 1.145(7) . ? C15' O15' 1.131(8) . ? C16 O16 1.152(9) . ? C16' O16' 1.145(7) . ? C17 O17 1.139(8) . ? C17' O17' 1.139(7) . ? C18 O18 1.142(7) . ? C18' O18' 1.124(7) . ? C19 O19 1.151(7) . ? C19' O19' 1.137(7) . ? C20 O20 1.149(6) . ? C20' O20' 1.148(8) . ? C21 O21 1.147(7) . ? C21' O21' 1.153(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 C15 W1 C1 91.0(2) . . ? C15 W1 C14 88.8(3) . . ? C1 W1 C14 121.8(2) . . ? C15 W1 C12 84.4(3) . . ? C1 W1 C12 108.1(2) . . ? C14 W1 C12 129.7(2) . . ? C15 W1 C13 116.6(3) . . ? C1 W1 C13 91.9(2) . . ? C14 W1 C13 138.3(3) . . ? C12 W1 C13 35.6(2) . . ? C15 W1 C11 84.7(2) . . ? C1 W1 C11 144.0(2) . . ? C14 W1 C11 93.9(2) . . ? C12 W1 C11 36.0(2) . . ? C13 W1 C11 59.3(2) . . ? C15 W1 C10 117.0(2) . . ? C1 W1 C10 145.3(2) . . ? C14 W1 C10 81.3(2) . . ? C12 W1 C10 58.7(2) . . ? C13 W1 C10 58.2(2) . . ? C11 W1 C10 35.1(2) . . ? C15 W1 C9 141.1(2) . . ? C1 W1 C9 110.6(2) . . ? C14 W1 C9 104.9(3) . . ? C12 W1 C9 58.7(2) . . ? C13 W1 C9 35.0(2) . . ? C11 W1 C9 58.7(2) . . ? C10 W1 C9 34.7(2) . . ? C15 W1 Fe1 128.7(2) . . ? C1 W1 Fe1 46.05(14) . . ? C14 W1 Fe1 93.1(2) . . ? C12 W1 Fe1 128.9(2) . . ? C13 W1 Fe1 94.74(15) . . ? C11 W1 Fe1 146.0(2) . . ? C10 W1 Fe1 113.9(2) . . ? C9 W1 Fe1 87.38(15) . . ? C15 W1 Fe2 79.1(2) . . ? C1 W1 Fe2 44.87(15) . . ? C14 W1 Fe2 78.2(2) . . ? C12 W1 Fe2 147.3(2) . . ? C13 W1 Fe2 135.8(2) . . ? C11 W1 Fe2 162.1(2) . . ? C10 W1 Fe2 153.7(2) . . ? C9 W1 Fe2 138.76(15) . . ? Fe1 W1 Fe2 51.46(2) . . ? C14' W1' C1' 90.7(3) . . ? C14' W1' C15' 86.5(4) . . ? C1' W1' C15' 120.2(2) . . ? C14' W1' C12' 83.7(4) . . ? C1' W1' C12' 112.7(3) . . ? C15' W1' C12' 126.2(4) . . ? C14' W1' C13' 116.7(4) . . ? C1' W1' C13' 96.1(3) . . ? C15' W1' C13' 137.4(4) . . ? C12' W1' C13' 36.3(3) . . ? C14' W1' C11' 84.8(3) . . ? C1' W1' C11' 147.0(3) . . ? C15' W1' C11' 92.3(4) . . ? C12' W1' C11' 34.3(3) . . ? C13' W1' C11' 58.0(3) . . ? C14' W1' C9' 139.0(3) . . ? C1' W1' C9' 114.9(4) . . ? C15' W1' C9' 104.9(4) . . ? C12' W1' C9' 57.5(3) . . ? C13' W1' C9' 34.3(3) . . ? C11' W1' C9' 56.0(3) . . ? C14' W1' C10' 115.6(4) . . ? C1' W1' C10' 148.0(4) . . ? C15' W1' C10' 81.3(3) . . ? C12' W1' C10' 56.7(3) . . ? C13' W1' C10' 56.8(3) . . ? C11' W1' C10' 33.6(3) . . ? C9' W1' C10' 33.1(3) . . ? C14' W1' Fe1' 129.5(2) . . ? C1' W1' Fe1' 45.50(15) . . ? C15' W1' Fe1' 95.4(2) . . ? C12' W1' Fe1' 130.3(4) . . ? C13' W1' Fe1' 95.2(3) . . ? C11' W1' Fe1' 145.1(3) . . ? C9' W1' Fe1' 89.2(2) . . ? C10' W1' Fe1' 114.6(4) . . ? C14' W1' Fe2' 81.2(2) . . ? C1' W1' Fe2' 45.10(15) . . ? C15' W1' Fe2' 75.6(2) . . ? C12' W1' Fe2' 152.6(2) . . ? C13' W1' Fe2' 139.4(2) . . ? C11' W1' Fe2' 161.9(2) . . ? C9' W1' Fe2' 139.6(2) . . ? C10' W1' Fe2' 150.6(3) . . ? Fe1' W1' Fe2' 51.21(2) . . ? C20 Fe1 C19 96.9(3) . . ? C20 Fe1 C21 98.7(3) . . ? C19 Fe1 C21 99.0(3) . . ? C20 Fe1 C2 93.2(2) . . ? C19 Fe1 C2 157.2(2) . . ? C21 Fe1 C2 99.6(2) . . ? C20 Fe1 C1 129.1(2) . . ? C19 Fe1 C1 126.2(2) . . ? C21 Fe1 C1 99.4(2) . . ? C2 Fe1 C1 37.0(2) . . ? C20 Fe1 Fe2 97.2(2) . . ? C19 Fe1 Fe2 102.4(2) . . ? C21 Fe1 Fe2 151.5(2) . . ? C2 Fe1 Fe2 55.9(2) . . ? C1 Fe1 Fe2 52.54(14) . . ? C20 Fe1 W1 162.0(2) . . ? C19 Fe1 W1 82.6(2) . . ? C21 Fe1 W1 99.1(2) . . ? C2 Fe1 W1 81.50(14) . . ? C1 Fe1 W1 44.72(15) . . ? Fe2 Fe1 W1 65.57(2) . . ? C21' Fe1' C20' 95.9(3) . . ? C21' Fe1' C19' 98.2(3) . . ? C20' Fe1' C19' 96.5(3) . . ? C21' Fe1' C1' 123.4(3) . . ? C20' Fe1' C1' 103.8(3) . . ? C19' Fe1' C1' 130.5(3) . . ? C21' Fe1' C2' 154.5(3) . . ? C20' Fe1' C2' 104.6(3) . . ? C19' Fe1' C2' 94.5(3) . . ? C1' Fe1' C2' 36.9(2) . . ? C21' Fe1' Fe2' 101.0(2) . . ? C20' Fe1' Fe2' 156.3(2) . . ? C19' Fe1' Fe2' 97.5(2) . . ? C1' Fe1' Fe2' 52.77(15) . . ? C2' Fe1' Fe2' 55.2(2) . . ? C21' Fe1' W1' 80.5(2) . . ? C20' Fe1' W1' 101.9(2) . . ? C19' Fe1' W1' 161.6(2) . . ? C1' Fe1' W1' 43.94(15) . . ? C2' Fe1' W1' 80.5(2) . . ? Fe2' Fe1' W1' 65.13(3) . . ? C18 Fe2 C16 90.9(3) . . ? C18 Fe2 C17 93.5(3) . . ? C16 Fe2 C17 100.8(5) . . ? C18 Fe2 C1 121.0(3) . . ? C16 Fe2 C1 138.0(3) . . ? C17 Fe2 C1 103.4(3) . . ? C18 Fe2 C2 85.3(3) . . ? C16 Fe2 C2 151.0(4) . . ? C17 Fe2 C2 108.1(3) . . ? C1 Fe2 C2 35.7(2) . . ? C18 Fe2 Fe1 97.2(2) . . ? C16 Fe2 Fe1 100.9(3) . . ? C17 Fe2 Fe1 155.6(3) . . ? C1 Fe2 Fe1 52.39(14) . . ? C2 Fe2 Fe1 51.45(14) . . ? C18 Fe2 W1 159.4(2) . . ? C16 Fe2 W1 97.8(2) . . ? C17 Fe2 W1 103.1(2) . . ? C1 Fe2 W1 43.48(15) . . ? C2 Fe2 W1 78.13(14) . . ? Fe1 Fe2 W1 62.96(2) . . ? C16' Fe2' C18' 91.2(3) . . ? C16' Fe2' C17' 94.3(3) . . ? C18' Fe2' C17' 100.7(3) . . ? C16' Fe2' C1' 121.1(3) . . ? C18' Fe2' C1' 137.2(2) . . ? C17' Fe2' C1' 103.7(3) . . ? C16' Fe2' C2' 85.1(3) . . ? C18' Fe2' C2' 149.6(3) . . ? C17' Fe2' C2' 109.6(2) . . ? C1' Fe2' C2' 36.0(2) . . ? C16' Fe2' Fe1' 99.2(2) . . ? C18' Fe2' Fe1' 98.8(2) . . ? C17' Fe2' Fe1' 156.0(2) . . ? C1' Fe2' Fe1' 52.34(14) . . ? C2' Fe2' Fe1' 52.47(14) . . ? C16' Fe2' W1' 161.4(2) . . ? C18' Fe2' W1' 98.4(2) . . ? C17' Fe2' W1' 99.5(2) . . ? C1' Fe2' W1' 43.25(15) . . ? C2' Fe2' W1' 78.6(2) . . ? Fe1' Fe2' W1' 63.66(3) . . ? C2 C1 W1 159.5(4) . . ? C2 C1 Fe1 71.5(3) . . ? W1 C1 Fe1 89.2(2) . . ? C2 C1 Fe2 77.0(3) . . ? W1 C1 Fe2 91.7(2) . . ? Fe1 C1 Fe2 75.1(2) . . ? C2' C1' W1' 161.3(4) . . ? C2' C1' Fe1' 72.8(3) . . ? W1' C1' Fe1' 90.6(2) . . ? C2' C1' Fe2' 75.9(3) . . ? W1' C1' Fe2' 91.7(2) . . ? Fe1' C1' Fe2' 74.9(2) . . ? C1 C2 C3 143.9(5) . . ? C1 C2 Fe1 71.6(3) . . ? C3 C2 Fe1 137.4(4) . . ? C1 C2 Fe2 67.3(3) . . ? C3 C2 Fe2 132.6(4) . . ? Fe1 C2 Fe2 72.6(2) . . ? C1' C2' C3' 141.1(5) . . ? C1' C2' Fe1' 70.3(3) . . ? C3' C2' Fe1' 142.0(4) . . ? C1' C2' Fe2' 68.1(3) . . ? C3' C2' Fe2' 131.2(4) . . ? Fe1' C2' Fe2' 72.3(2) . . ? C8 C3 C4 117.3(6) . . ? C8 C3 C2 120.6(5) . . ? C4 C3 C2 122.1(5) . . ? C4' C3' C8' 117.3(5) . . ? C4' C3' C2' 118.9(5) . . ? C8' C3' C2' 123.9(5) . . ? C5 C4 C3 122.3(6) . . ? C3' C4' C5' 121.2(6) . . ? C6 C5 C4 118.9(7) . . ? C6' C5' C4' 120.9(7) . . ? C5 C6 C7 120.6(6) . . ? C5' C6' C7' 119.4(6) . . ? C6 C7 C8 121.0(6) . . ? C6' C7' C8' 120.7(7) . . ? C3 C8 C7 120.0(6) . . ? C3' C8' C7' 120.5(6) . . ? C13 C9 C10 107.7(6) . . ? C13 C9 W1 70.5(4) . . ? C10 C9 W1 72.5(3) . . ? C10' C9' C13' 109.7(9) . . ? C10' C9' W1' 73.9(5) . . ? C13' C9' W1' 71.3(5) . . ? C9 C10 C11 108.8(6) . . ? C9 C10 W1 72.8(3) . . ? C11 C10 W1 71.0(3) . . ? C9' C10' C11' 109.3(9) . . ? C9' C10' W1' 72.9(5) . . ? C11' C10' W1' 72.5(5) . . ? C10 C11 C12 107.0(6) . . ? C10 C11 W1 73.8(3) . . ? C12 C11 W1 71.0(3) . . ? C10' C11' C12' 108.5(9) . . ? C10' C11' W1' 73.9(5) . . ? C12' C11' W1' 71.3(4) . . ? C13 C12 C11 107.9(6) . . ? C13 C12 W1 72.8(3) . . ? C11 C12 W1 73.0(3) . . ? C11' C12' C13' 106.9(8) . . ? C11' C12' W1' 74.4(5) . . ? C13' C12' W1' 72.1(4) . . ? C9 C13 C12 108.6(6) . . ? C9 C13 W1 74.5(4) . . ? C12 C13 W1 71.6(3) . . ? C9' C13' C12' 105.6(8) . . ? C9' C13' W1' 74.4(5) . . ? C12' C13' W1' 71.7(5) . . ? O14 C14 W1 172.4(5) . . ? O14' C14' W1' 174.6(8) . . ? O15 C15 W1 175.2(6) . . ? O15' C15' W1' 171.8(6) . . ? O16 C16 Fe2 175.5(8) . . ? O16' C16' Fe2' 178.1(7) . . ? O17 C17 Fe2 177.3(7) . . ? O17' C17' Fe2' 176.1(6) . . ? O18 C18 Fe2 178.4(7) . . ? O18' C18' Fe2' 175.8(6) . . ? O19 C19 Fe1 176.2(5) . . ? O19' C19' Fe1' 178.3(7) . . ? O20 C20 Fe1 179.0(6) . . ? O20' C20' Fe1' 175.2(6) . . ? O21 C21 Fe1 178.1(5) . . ? O21' C21' Fe1' 176.5(6) . . ? _refine_diff_density_max 0.673 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.097