# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2058 data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H20 Cl Fe3 O6 S2 W2' _chemical_formula_weight 1141.30 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' 'Cl' 'Cl' 0.1484 0.1585 '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 21.561(2) _cell_length_b 8.1880(8) _cell_length_c 21.932(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.668(2) _cell_angle_gamma 90.00 _cell_volume 3460.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.696 _cell_measurement_theta_max 31.267 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.391 _exptl_crystal_size_mid 0.165 _exptl_crystal_size_min 0.024 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 8.092 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1917 _exptl_absorpt_correction_T_max 0.8251 _exptl_absorpt_process_details ? _exptl_special_details ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.0120 -1.00 0.00 0.00 0.0120 1.00 0.00 -1.00 0.0750 -1.00 0.00 1.00 0.0800 0.00 1.00 -1.00 0.1880 -1.00 1.00 1.00 0.2030 1.00 -1.00 -1.00 0.1700 1.00 -1.00 0.00 0.1700 ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47103 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 34.06 _reflns_number_total 13421 _reflns_number_gt 8679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13421 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.26134(3) 0.18334(6) 0.81292(3) 0.02605(11) Uani 1 d . A 3 Fe2 Fe 0.21703(3) 0.08165(7) 0.92098(3) 0.03426(13) Uani 1 d . A 3 Fe3 Fe 0.29800(3) -0.07863(6) 0.88202(3) 0.02730(11) Uani 1 d . A 3 W1 W 0.355615(8) 0.175947(18) 0.950746(8) 0.02800(4) Uani 1 d . A 3 W2 W 0.164257(8) -0.065469(18) 0.789818(8) 0.02968(4) Uani 1 d . A 3 S1 S 0.21025(6) -0.18164(13) 0.89885(5) 0.0380(2) Uani 1 d . A 3 S2 S 0.25195(5) 0.31910(12) 0.89836(5) 0.0340(2) Uani 1 d . A 3 C1 C 0.25121(18) -0.0475(4) 0.78100(18) 0.0270(7) Uani 1 d . A 3 C2 C 0.2890(2) 0.0291(4) 0.75025(19) 0.0292(8) Uani 1 d . A 3 C3 C 0.34999(19) 0.1124(4) 0.79974(18) 0.0276(7) Uani 1 d . A 3 C4 C 0.35700(18) 0.0900(4) 0.86725(18) 0.0272(7) Uani 1 d . A 3 C5 C 0.2645(2) 0.0230(5) 0.67536(19) 0.0334(9) Uani 1 d . A 3 C6 C 0.2055(3) 0.1004(6) 0.6293(2) 0.0505(12) Uani 1 d . A 3 H6 H 0.1815 0.1670 0.6459 0.061 Uiso 1 calc R A 3 C7 C 0.1802(3) 0.0834(7) 0.5595(2) 0.0618(14) Uani 1 d . A 3 H7 H 0.1395 0.1352 0.5295 0.074 Uiso 1 calc R A 3 C8 C 0.2171(4) -0.0125(8) 0.5359(3) 0.0722(18) Uani 1 d . A 3 H8 H 0.2016 -0.0235 0.4892 0.087 Uiso 1 calc R A 3 C9 C 0.2758(3) -0.0920(7) 0.5797(3) 0.0642(15) Uani 1 d . A 3 H9 H 0.2994 -0.1582 0.5626 0.077 Uiso 1 calc R A 3 C10 C 0.3009(3) -0.0742(6) 0.6506(2) 0.0509(12) Uani 1 d . A 3 H10 H 0.3413 -0.1271 0.6805 0.061 Uiso 1 calc R A 3 C11 C 0.3971(2) 0.2213(5) 0.78562(19) 0.0304(8) Uani 1 d . A 3 C12 C 0.3747(2) 0.3153(5) 0.7263(2) 0.0408(10) Uani 1 d . A 3 H12 H 0.3289 0.3075 0.6931 0.049 Uiso 1 calc R A 3 C13 C 0.4197(3) 0.4196(6) 0.7164(2) 0.0506(12) Uani 1 d . A 3 H13 H 0.4045 0.4812 0.6766 0.061 Uiso 1 calc R A 3 C14 C 0.4888(3) 0.4316(6) 0.7669(3) 0.0555(13) Uani 1 d . A 3 H14 H 0.5192 0.5036 0.7613 0.067 Uiso 1 calc R A 3 C15 C 0.5113(2) 0.3370(6) 0.8247(2) 0.0453(11) Uani 1 d . A 3 H15 H 0.5574 0.3426 0.8575 0.054 Uiso 1 calc R A 3 C16 C 0.4661(2) 0.2342(5) 0.8343(2) 0.0342(9) Uani 1 d . A 3 H16 H 0.4819 0.1721 0.8739 0.041 Uiso 1 calc R A 3 C17 C 0.4420(2) 0.3711(5) 0.9739(2) 0.0429(10) Uani 1 d . A 3 H17 H 0.4471 0.4189 0.9379 0.052 Uiso 1 calc R A 3 C18 C 0.4739(2) 0.2262(6) 1.0083(2) 0.0472(11) Uani 1 d . A 3 H18 H 0.5045 0.1619 0.9995 0.057 Uiso 1 calc R A 3 C19 C 0.4517(3) 0.1955(6) 1.0582(2) 0.0516(12) Uani 1 d . A 3 H19 H 0.4645 0.1074 1.0882 0.062 Uiso 1 calc R A 3 C20 C 0.4057(3) 0.3241(6) 1.0547(2) 0.0504(12) Uani 1 d . A 3 H20 H 0.3829 0.3346 1.0817 0.060 Uiso 1 calc R A 3 C21 C 0.4010(2) 0.4299(5) 1.0041(2) 0.0435(10) Uani 1 d . A 3 H21 H 0.3748 0.5253 0.9918 0.052 Uiso 1 calc R A 3 C22 C 0.1099(3) -0.3114(6) 0.7419(3) 0.0582(14) Uani 1 d . A 3 H22 H 0.1310 -0.4104 0.7607 0.070 Uiso 1 calc R A 3 C23 C 0.0651(3) -0.2274(7) 0.7593(3) 0.0657(16) Uani 1 d . A 3 H23 H 0.0512 -0.2589 0.7920 0.079 Uiso 1 calc R A 3 C24 C 0.0442(3) -0.0873(7) 0.7196(4) 0.0745(19) Uani 1 d . A 3 H24 H 0.0134 -0.0088 0.7203 0.089 Uiso 1 calc R A 3 C25 C 0.0784(3) -0.0864(7) 0.6784(3) 0.0683(17) Uani 1 d . A 3 H25 H 0.0747 -0.0056 0.6471 0.082 Uiso 1 calc R A 3 C26 C 0.1185(3) -0.2253(7) 0.6919(3) 0.0602(14) Uani 1 d . A 3 H26 H 0.1462 -0.2556 0.6713 0.072 Uiso 1 calc R A 3 C27 C 0.3526(2) -0.0630(5) 0.9832(2) 0.0354(9) Uani 1 d . A 3 O27 O 0.37471(16) -0.1524(4) 1.03087(15) 0.0453(7) Uani 1 d . A 3 C28 C 0.1387(2) 0.1682(5) 0.7850(2) 0.0371(9) Uani 1 d . A 3 O28 O 0.10382(16) 0.2864(4) 0.76923(16) 0.0474(8) Uani 1 d . A 3 C29 C 0.3440(2) -0.2480(5) 0.8718(2) 0.0393(10) Uani 1 d . A 3 O29 O 0.3744(2) -0.3486(4) 0.8621(2) 0.0694(11) Uani 1 d . A 3 C30 C 0.2433(2) 0.3641(5) 0.7628(2) 0.0393(10) Uani 1 d . A 3 O30 O 0.2332(2) 0.4789(4) 0.7311(2) 0.0696(11) Uani 1 d . A 3 C31 C 0.2486(2) 0.0638(6) 1.0105(2) 0.0476(11) Uani 1 d . A 3 O31 O 0.2641(2) 0.0475(5) 1.06757(18) 0.0742(12) Uani 1 d . A 3 C32 C 0.1361(3) 0.1549(6) 0.9108(2) 0.0492(12) Uani 1 d . A 3 O32 O 0.08417(19) 0.2093(6) 0.9051(2) 0.0805(13) Uani 1 d . A 3 C50 C 0.0559(7) 0.7574(17) 0.9487(7) 0.083(4) Uiso 0.50 d P B 3 Cl1 Cl -0.0078(3) 0.8458(7) 0.8907(3) 0.156(2) Uiso 0.50 d P B 3 Cl2 Cl 0.0237(6) 0.6919(12) 1.0017(5) 0.136(3) Uiso 0.25 d P B 3 Cl2A Cl 0.0944(11) 0.861(2) 1.0224(10) 0.259(8) Uiso 0.25 d P B 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0250(3) 0.0238(2) 0.0288(3) 0.0001(2) 0.0116(2) 0.0004(2) Fe2 0.0306(3) 0.0396(3) 0.0356(3) -0.0045(2) 0.0175(3) -0.0038(2) Fe3 0.0257(3) 0.0240(3) 0.0309(3) 0.0013(2) 0.0116(2) -0.0013(2) W1 0.02625(8) 0.02737(8) 0.02800(7) -0.00162(6) 0.01005(6) -0.00318(6) W2 0.02346(7) 0.02730(8) 0.03635(8) -0.00304(6) 0.01171(6) -0.00321(6) S1 0.0368(6) 0.0366(5) 0.0428(6) 0.0043(5) 0.0197(5) -0.0072(5) S2 0.0316(5) 0.0322(5) 0.0375(5) -0.0056(4) 0.0150(4) 0.0013(4) C1 0.0239(17) 0.0243(17) 0.0301(18) -0.0039(14) 0.0096(15) -0.0001(14) C2 0.029(2) 0.0280(19) 0.0320(19) -0.0021(15) 0.0151(17) 0.0032(15) C3 0.0242(18) 0.0271(18) 0.0319(19) 0.0006(15) 0.0130(16) 0.0027(14) C4 0.0234(18) 0.0234(17) 0.0335(19) 0.0008(14) 0.0116(16) 0.0018(14) C5 0.035(2) 0.036(2) 0.032(2) -0.0077(16) 0.0179(18) -0.0064(17) C6 0.062(3) 0.054(3) 0.035(2) -0.002(2) 0.021(2) 0.010(2) C7 0.066(4) 0.071(4) 0.037(3) 0.001(2) 0.012(3) -0.005(3) C8 0.101(5) 0.086(4) 0.041(3) -0.019(3) 0.041(3) -0.039(4) C9 0.076(4) 0.078(4) 0.055(3) -0.023(3) 0.044(3) -0.013(3) C10 0.044(3) 0.065(3) 0.049(3) -0.013(2) 0.025(2) -0.003(2) C11 0.030(2) 0.0290(19) 0.035(2) 0.0007(16) 0.0179(17) 0.0001(15) C12 0.034(2) 0.048(3) 0.040(2) 0.006(2) 0.0170(19) -0.002(2) C13 0.052(3) 0.056(3) 0.044(3) 0.013(2) 0.022(2) -0.010(2) C14 0.053(3) 0.060(3) 0.059(3) 0.007(3) 0.031(3) -0.021(3) C15 0.032(2) 0.055(3) 0.047(3) 0.004(2) 0.017(2) -0.007(2) C16 0.030(2) 0.039(2) 0.037(2) 0.0035(17) 0.0174(18) -0.0017(17) C17 0.042(3) 0.039(2) 0.045(2) -0.0098(19) 0.016(2) -0.016(2) C18 0.027(2) 0.052(3) 0.049(3) -0.014(2) 0.005(2) -0.007(2) C19 0.048(3) 0.050(3) 0.034(2) 0.000(2) -0.003(2) -0.005(2) C20 0.054(3) 0.055(3) 0.038(2) -0.018(2) 0.018(2) -0.016(2) C21 0.042(3) 0.034(2) 0.048(3) -0.013(2) 0.014(2) -0.0077(19) C22 0.058(3) 0.031(2) 0.069(3) -0.011(2) 0.014(3) -0.012(2) C23 0.047(3) 0.071(4) 0.084(4) -0.027(3) 0.033(3) -0.034(3) C24 0.024(2) 0.063(4) 0.109(5) -0.035(4) 0.005(3) 0.001(2) C25 0.053(3) 0.056(3) 0.054(3) 0.005(3) -0.013(3) -0.019(3) C26 0.046(3) 0.069(4) 0.057(3) -0.031(3) 0.016(3) -0.016(3) C27 0.032(2) 0.035(2) 0.039(2) 0.0047(18) 0.0155(18) -0.0026(17) O27 0.0431(18) 0.0442(18) 0.0400(16) 0.0142(14) 0.0109(14) 0.0007(14) C28 0.031(2) 0.036(2) 0.040(2) -0.0037(18) 0.0123(18) -0.0027(18) O28 0.0371(17) 0.0387(17) 0.062(2) 0.0047(15) 0.0180(16) 0.0088(14) C29 0.036(2) 0.036(2) 0.039(2) 0.0030(18) 0.0103(19) 0.0016(18) O29 0.070(3) 0.051(2) 0.080(3) -0.0024(19) 0.029(2) 0.0273(19) C30 0.039(2) 0.036(2) 0.045(2) 0.0049(19) 0.020(2) 0.0066(18) O30 0.092(3) 0.045(2) 0.082(3) 0.0261(19) 0.048(2) 0.021(2) C31 0.041(3) 0.056(3) 0.047(3) -0.005(2) 0.020(2) 0.000(2) O31 0.078(3) 0.102(3) 0.043(2) 0.000(2) 0.027(2) 0.015(2) C32 0.044(3) 0.067(3) 0.039(2) -0.004(2) 0.020(2) -0.003(2) O32 0.043(2) 0.129(4) 0.072(3) -0.002(3) 0.029(2) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C30 1.780(4) . ? Fe1 C1 1.993(3) . ? Fe1 C4 2.013(4) . ? Fe1 C3 2.138(4) . ? Fe1 C2 2.140(4) . ? Fe1 S2 2.2645(11) . ? Fe1 C28 2.435(4) . ? Fe1 Fe3 2.5391(7) . ? Fe1 W1 2.7852(6) . ? Fe1 W2 2.7993(6) . ? Fe2 C32 1.762(5) . ? Fe2 C31 1.773(5) . ? Fe2 S1 2.2002(12) . ? Fe2 S2 2.2201(12) . ? Fe2 Fe3 2.6151(8) . ? Fe2 W2 2.8430(6) . ? Fe2 W1 2.8636(6) . ? Fe3 C29 1.777(5) . ? Fe3 C27 1.995(4) . ? Fe3 C1 1.996(4) . ? Fe3 C4 2.000(4) . ? Fe3 S1 2.2481(11) . ? Fe3 W1 2.5454(6) . ? Fe3 W2 2.6798(6) . ? W1 C4 1.975(4) . ? W1 C27 2.093(4) . ? W1 C18 2.319(4) . ? W1 S2 2.3204(10) . ? W1 C17 2.331(4) . ? W1 C19 2.343(4) . ? W1 C20 2.371(4) . ? W1 C21 2.371(4) . ? W2 C1 1.975(4) . ? W2 C28 1.981(4) . ? W2 C25 2.317(5) . ? W2 C26 2.322(5) . ? W2 C22 2.330(4) . ? W2 S1 2.3406(11) . ? W2 C23 2.343(5) . ? W2 C24 2.350(5) . ? C1 C2 1.416(5) . ? C2 C3 1.446(5) . ? C2 C5 1.483(5) . ? C3 C4 1.431(5) . ? C3 C11 1.485(5) . ? C5 C6 1.374(6) . ? C5 C10 1.388(6) . ? C6 C7 1.383(6) . ? C7 C8 1.373(8) . ? C8 C9 1.363(8) . ? C9 C10 1.406(7) . ? C11 C16 1.392(5) . ? C11 C12 1.398(5) . ? C12 C13 1.381(6) . ? C13 C14 1.405(7) . ? C14 C15 1.375(6) . ? C15 C16 1.373(6) . ? C17 C21 1.408(6) . ? C17 C18 1.409(6) . ? C18 C19 1.401(7) . ? C19 C20 1.424(7) . ? C20 C21 1.374(6) . ? C22 C23 1.371(7) . ? C22 C26 1.384(7) . ? C23 C24 1.387(8) . ? C24 C25 1.401(8) . ? C25 C26 1.377(8) . ? C27 O27 1.187(4) . ? C28 O28 1.178(5) . ? C29 O29 1.131(5) . ? C30 O30 1.130(5) . ? C31 O31 1.149(5) . ? C32 O32 1.159(6) . ? C50 Cl1 1.570(14) . ? C50 Cl2A 1.68(2) . ? C50 Cl2 1.688(16) . ? Cl2 Cl2A 1.96(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 Fe1 C1 127.77(18) . . ? C30 Fe1 C4 124.27(18) . . ? C1 Fe1 C4 76.66(14) . . ? C30 Fe1 C3 95.90(17) . . ? C1 Fe1 C3 70.03(14) . . ? C4 Fe1 C3 40.19(14) . . ? C30 Fe1 C2 98.08(17) . . ? C1 Fe1 C2 39.88(14) . . ? C4 Fe1 C2 69.45(14) . . ? C3 Fe1 C2 39.52(14) . . ? C30 Fe1 S2 91.56(14) . . ? C1 Fe1 S2 136.03(11) . . ? C4 Fe1 S2 98.34(11) . . ? C3 Fe1 S2 131.50(10) . . ? C2 Fe1 S2 167.34(11) . . ? C30 Fe1 C28 88.59(17) . . ? C1 Fe1 C28 85.87(15) . . ? C4 Fe1 C28 146.95(14) . . ? C3 Fe1 C28 152.63(14) . . ? C2 Fe1 C28 113.13(14) . . ? S2 Fe1 C28 75.11(10) . . ? C30 Fe1 Fe3 173.98(14) . . ? C1 Fe1 Fe3 50.52(10) . . ? C4 Fe1 Fe3 50.51(10) . . ? C3 Fe1 Fe3 78.09(10) . . ? C2 Fe1 Fe3 77.45(10) . . ? S2 Fe1 Fe3 92.31(3) . . ? C28 Fe1 Fe3 96.85(10) . . ? C30 Fe1 W1 122.64(15) . . ? C1 Fe1 W1 105.79(10) . . ? C4 Fe1 W1 45.13(10) . . ? C3 Fe1 W1 83.08(10) . . ? C2 Fe1 W1 113.97(10) . . ? S2 Fe1 W1 53.51(3) . . ? C28 Fe1 W1 116.95(10) . . ? Fe3 Fe1 W1 56.894(16) . . ? C30 Fe1 W2 123.73(15) . . ? C1 Fe1 W2 44.86(10) . . ? C4 Fe1 W2 108.36(10) . . ? C3 Fe1 W2 114.78(10) . . ? C2 Fe1 W2 81.69(10) . . ? S2 Fe1 W2 99.78(3) . . ? C28 Fe1 W2 43.79(10) . . ? Fe3 Fe1 W2 60.028(17) . . ? W1 Fe1 W2 107.629(18) . . ? C32 Fe2 C31 92.0(2) . . ? C32 Fe2 S1 109.98(17) . . ? C31 Fe2 S1 96.78(16) . . ? C32 Fe2 S2 95.12(17) . . ? C31 Fe2 S2 108.64(16) . . ? S1 Fe2 S2 143.56(5) . . ? C32 Fe2 Fe3 153.85(15) . . ? C31 Fe2 Fe3 109.85(15) . . ? S1 Fe2 Fe3 54.85(3) . . ? S2 Fe2 Fe3 91.34(3) . . ? C32 Fe2 W2 95.27(15) . . ? C31 Fe2 W2 150.05(16) . . ? S1 Fe2 W2 53.48(3) . . ? S2 Fe2 W2 99.60(3) . . ? Fe3 Fe2 W2 58.633(17) . . ? C32 Fe2 W1 144.07(17) . . ? C31 Fe2 W1 85.80(15) . . ? S1 Fe2 W1 105.88(4) . . ? S2 Fe2 W1 52.48(3) . . ? Fe3 Fe2 W1 55.144(17) . . ? W2 Fe2 W1 104.341(18) . . ? C29 Fe3 C27 96.11(18) . . ? C29 Fe3 C1 89.54(17) . . ? C27 Fe3 C1 168.00(16) . . ? C29 Fe3 C4 94.99(18) . . ? C27 Fe3 C4 92.02(16) . . ? C1 Fe3 C4 76.90(15) . . ? C29 Fe3 S1 106.63(15) . . ? C27 Fe3 S1 87.79(12) . . ? C1 Fe3 S1 100.77(11) . . ? C4 Fe3 S1 158.29(11) . . ? C29 Fe3 Fe1 128.75(14) . . ? C27 Fe3 Fe1 118.68(12) . . ? C1 Fe3 Fe1 50.43(10) . . ? C4 Fe3 Fe1 50.98(10) . . ? S1 Fe3 Fe1 110.82(4) . . ? C29 Fe3 W1 124.23(14) . . ? C27 Fe3 W1 53.24(12) . . ? C1 Fe3 W1 114.96(10) . . ? C4 Fe3 W1 49.74(10) . . ? S1 Fe3 W1 115.66(4) . . ? Fe1 Fe3 W1 66.428(18) . . ? C29 Fe3 Fe2 157.69(14) . . ? C27 Fe3 Fe2 75.62(12) . . ? C1 Fe3 Fe2 102.69(10) . . ? C4 Fe3 Fe2 105.84(10) . . ? S1 Fe3 Fe2 53.15(3) . . ? Fe1 Fe3 Fe2 72.33(2) . . ? W1 Fe3 Fe2 67.391(19) . . ? C29 Fe3 W2 114.10(14) . . ? C27 Fe3 W2 137.27(12) . . ? C1 Fe3 W2 47.22(10) . . ? C4 Fe3 W2 113.41(10) . . ? S1 Fe3 W2 55.89(3) . . ? Fe1 Fe3 W2 64.809(18) . . ? W1 Fe3 W2 119.20(2) . . ? Fe2 Fe3 W2 64.936(19) . . ? C4 W1 C27 89.86(15) . . ? C4 W1 C18 95.60(16) . . ? C27 W1 C18 100.09(17) . . ? C4 W1 S2 97.64(10) . . ? C27 W1 S2 118.07(11) . . ? C18 W1 S2 139.43(12) . . ? C4 W1 C17 95.89(15) . . ? C27 W1 C17 135.30(16) . . ? C18 W1 C17 35.28(16) . . ? S2 W1 C17 105.05(12) . . ? C4 W1 C19 125.66(17) . . ? C27 W1 C19 82.55(17) . . ? C18 W1 C19 34.97(16) . . ? S2 W1 C19 133.13(13) . . ? C17 W1 C19 58.34(17) . . ? C4 W1 C20 152.12(16) . . ? C27 W1 C20 102.82(17) . . ? C18 W1 C20 58.06(17) . . ? S2 W1 C20 98.01(13) . . ? C17 W1 C20 57.71(16) . . ? C19 W1 C20 35.17(16) . . ? C4 W1 C21 126.58(15) . . ? C27 W1 C21 136.13(16) . . ? C18 W1 C21 57.76(16) . . ? S2 W1 C21 83.90(12) . . ? C17 W1 C21 34.84(15) . . ? C19 W1 C21 57.38(16) . . ? C20 W1 C21 33.69(15) . . ? C4 W1 Fe3 50.61(10) . . ? C27 W1 Fe3 49.78(11) . . ? C18 W1 Fe3 126.36(12) . . ? S2 W1 Fe3 90.85(3) . . ? C17 W1 Fe3 145.09(11) . . ? C19 W1 Fe3 128.89(12) . . ? C20 W1 Fe3 151.49(12) . . ? C21 W1 Fe3 173.70(11) . . ? C4 W1 Fe1 46.26(10) . . ? C27 W1 Fe1 105.68(11) . . ? C18 W1 Fe1 132.51(12) . . ? S2 W1 Fe1 51.69(3) . . ? C17 W1 Fe1 110.11(11) . . ? C19 W1 Fe1 167.28(13) . . ? C20 W1 Fe1 145.86(13) . . ? C21 W1 Fe1 117.07(11) . . ? Fe3 W1 Fe1 56.677(16) . . ? C4 W1 Fe2 98.10(10) . . ? C27 W1 Fe2 68.71(11) . . ? C18 W1 Fe2 162.18(12) . . ? S2 W1 Fe2 49.36(3) . . ? C17 W1 Fe2 152.23(12) . . ? C19 W1 Fe2 127.48(13) . . ? C20 W1 Fe2 109.59(12) . . ? C21 W1 Fe2 120.40(11) . . ? Fe3 W1 Fe2 57.465(17) . . ? Fe1 W1 Fe2 65.154(16) . . ? C1 W2 C28 100.18(16) . . ? C1 W2 C25 104.2(2) . . ? C28 W2 C25 86.76(19) . . ? C1 W2 C26 88.85(17) . . ? C28 W2 C26 120.14(19) . . ? C25 W2 C26 34.54(19) . . ? C1 W2 C22 109.14(18) . . ? C28 W2 C22 137.65(18) . . ? C25 W2 C22 57.21(19) . . ? C26 W2 C22 34.61(18) . . ? C1 W2 S1 98.32(11) . . ? C28 W2 S1 115.31(12) . . ? C25 W2 S1 145.03(14) . . ? C26 W2 S1 121.66(16) . . ? C22 W2 S1 90.35(14) . . ? C1 W2 C23 142.99(18) . . ? C28 W2 C23 109.6(2) . . ? C25 W2 C23 57.5(2) . . ? C26 W2 C23 57.5(2) . . ? C22 W2 C23 34.12(18) . . ? S1 W2 C23 88.62(16) . . ? C1 W2 C24 139.1(2) . . ? C28 W2 C24 80.79(18) . . ? C25 W2 C24 34.9(2) . . ? C26 W2 C24 57.7(2) . . ? C22 W2 C24 57.02(19) . . ? S1 W2 C24 118.4(2) . . ? C23 W2 C24 34.4(2) . . ? C1 W2 Fe3 47.90(10) . . ? C28 W2 Fe3 105.00(12) . . ? C25 W2 Fe3 150.75(18) . . ? C26 W2 Fe3 122.82(14) . . ? C22 W2 Fe3 117.31(14) . . ? S1 W2 Fe3 52.68(3) . . ? C23 W2 Fe3 136.68(17) . . ? C24 W2 Fe3 170.69(19) . . ? C1 W2 Fe1 45.41(10) . . ? C28 W2 Fe1 58.29(12) . . ? C25 W2 Fe1 115.02(14) . . ? C26 W2 Fe1 123.40(15) . . ? C22 W2 Fe1 153.47(15) . . ? S1 W2 Fe1 99.87(3) . . ? C23 W2 Fe1 167.32(17) . . ? C24 W2 Fe1 133.47(17) . . ? Fe3 W2 Fe1 55.163(16) . . ? C1 W2 Fe2 95.80(10) . . ? C28 W2 Fe2 67.69(12) . . ? C25 W2 Fe2 150.02(17) . . ? C26 W2 Fe2 170.10(16) . . ? C22 W2 Fe2 135.59(14) . . ? S1 W2 Fe2 49.06(3) . . ? C23 W2 Fe2 115.37(15) . . ? C24 W2 Fe2 121.19(16) . . ? Fe3 W2 Fe2 56.431(17) . . ? Fe1 W2 Fe2 65.249(16) . . ? Fe2 S1 Fe3 72.01(4) . . ? Fe2 S1 W2 77.46(4) . . ? Fe3 S1 W2 71.43(3) . . ? Fe2 S2 Fe1 85.43(4) . . ? Fe2 S2 W1 78.17(4) . . ? Fe1 S2 W1 74.80(3) . . ? C2 C1 W2 148.7(3) . . ? C2 C1 Fe1 75.6(2) . . ? W2 C1 Fe1 89.73(14) . . ? C2 C1 Fe3 118.2(3) . . ? W2 C1 Fe3 84.89(14) . . ? Fe1 C1 Fe3 79.05(13) . . ? C1 C2 C3 112.0(3) . . ? C1 C2 C5 121.2(3) . . ? C3 C2 C5 126.8(3) . . ? C1 C2 Fe1 64.49(19) . . ? C3 C2 Fe1 70.2(2) . . ? C5 C2 Fe1 131.9(3) . . ? C4 C3 C2 110.7(3) . . ? C4 C3 C11 121.9(3) . . ? C2 C3 C11 127.1(3) . . ? C4 C3 Fe1 65.20(19) . . ? C2 C3 Fe1 70.3(2) . . ? C11 C3 Fe1 127.0(3) . . ? C3 C4 W1 151.1(3) . . ? C3 C4 Fe3 118.5(3) . . ? W1 C4 Fe3 79.65(13) . . ? C3 C4 Fe1 74.6(2) . . ? W1 C4 Fe1 88.60(14) . . ? Fe3 C4 Fe1 78.51(13) . . ? C6 C5 C10 118.5(4) . . ? C6 C5 C2 123.4(4) . . ? C10 C5 C2 118.0(4) . . ? C5 C6 C7 122.8(5) . . ? C8 C7 C6 117.9(5) . . ? C9 C8 C7 121.4(5) . . ? C8 C9 C10 120.2(5) . . ? C5 C10 C9 119.2(5) . . ? C16 C11 C12 118.4(4) . . ? C16 C11 C3 118.8(3) . . ? C12 C11 C3 122.8(4) . . ? C13 C12 C11 120.9(4) . . ? C12 C13 C14 119.4(4) . . ? C15 C14 C13 119.9(4) . . ? C16 C15 C14 120.4(4) . . ? C15 C16 C11 121.1(4) . . ? C21 C17 C18 107.1(4) . . ? C21 C17 W1 74.1(2) . . ? C18 C17 W1 71.9(2) . . ? C19 C18 C17 108.3(4) . . ? C19 C18 W1 73.4(3) . . ? C17 C18 W1 72.8(2) . . ? C18 C19 C20 107.4(4) . . ? C18 C19 W1 71.6(2) . . ? C20 C19 W1 73.5(3) . . ? C21 C20 C19 107.9(4) . . ? C21 C20 W1 73.2(2) . . ? C19 C20 W1 71.3(2) . . ? C20 C21 C17 109.3(4) . . ? C20 C21 W1 73.1(2) . . ? C17 C21 W1 71.0(2) . . ? C23 C22 C26 109.0(5) . . ? C23 C22 W2 73.4(3) . . ? C26 C22 W2 72.4(3) . . ? C22 C23 C24 108.2(5) . . ? C22 C23 W2 72.4(3) . . ? C24 C23 W2 73.1(3) . . ? C23 C24 C25 107.0(5) . . ? C23 C24 W2 72.5(3) . . ? C25 C24 W2 71.2(3) . . ? C26 C25 C24 108.5(5) . . ? C26 C25 W2 72.9(3) . . ? C24 C25 W2 73.8(3) . . ? C25 C26 C22 107.4(5) . . ? C25 C26 W2 72.5(3) . . ? C22 C26 W2 73.0(3) . . ? O27 C27 Fe3 138.1(3) . . ? O27 C27 W1 144.5(3) . . ? Fe3 C27 W1 76.99(14) . . ? O28 C28 W2 159.2(3) . . ? O28 C28 Fe1 120.7(3) . . ? W2 C28 Fe1 77.92(14) . . ? O29 C29 Fe3 174.8(4) . . ? O30 C30 Fe1 178.6(4) . . ? O31 C31 Fe2 174.6(5) . . ? O32 C32 Fe2 177.1(5) . . ? Cl1 C50 Cl2A 115.0(11) . . ? Cl1 C50 Cl2 102.9(9) . . ? Cl2A C50 Cl2 71.1(9) . . ? C50 Cl2 Cl2A 54.2(7) . . ? C50 Cl2A Cl2 54.7(8) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 34.06 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 1.791 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.154 data_12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Metal acetylidine complex' ; _chemical_name_common 'Mixed metal cluster' _chemical_formula_moiety 'C31H20Fe2O5S2W2' _chemical_formula_sum 'C15.50 H10 Fe O2.50 S W' _chemical_formula_weight 507.99 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C 2/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 15.0470(3) _cell_length_b 9.50700(10) _cell_length_c 20.4070(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.1950(9) _cell_angle_gamma 90.00 _cell_volume 2907.27(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'hexagonal plates' _exptl_crystal_colour 'Red' _exptl_crystal_size_max '0.217 mm' _exptl_crystal_size_mid '0.217 mm' _exptl_crystal_size_min '0.023 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 9.050 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD Diffractometer' _diffrn_measurement_method 'combination of four set of frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 4%' _diffrn_reflns_number 3555 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 24.74 _reflns_number_total 2484 _reflns_number_gt 2449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO-SMN (Nonius-Denzo Software)' _computing_cell_refinement 'DENZO-SMN (Nonius-Denzo Software)' _computing_data_reduction 'DENZO-SMN (Nonius-Denzo Software)' _computing_structure_solution 'SHELXS-93 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+16.5829P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00042(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2484 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0516 _refine_ls_wR_factor_gt 0.0506 _refine_ls_goodness_of_fit_ref 1.258 _refine_ls_restrained_S_all 1.258 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W -0.006338(11) 0.062734(18) 0.180457(8) 0.02306(9) Uani 1 d . . . Fe Fe 0.10901(4) 0.23942(6) 0.25492(3) 0.02362(15) Uani 1 d . . . S S 0.11809(7) 0.00465(12) 0.25029(5) 0.0285(2) Uani 1 d . . . O1 O 0.0000 0.6182(5) 0.2500 0.0547(15) Uani 1 d S . . O2 O 0.2685(3) 0.2368(5) 0.3496(2) 0.0598(11) Uani 1 d . . . O3 O 0.1898(3) 0.4051(5) 0.1553(2) 0.0575(11) Uani 1 d . . . C1 C -0.0048(3) 0.2698(5) 0.1895(2) 0.0246(9) Uani 1 d . . . C2 C 0.0436(3) 0.4021(5) 0.3049(2) 0.0257(9) Uani 1 d . . . C3 C 0.0000 0.4905(7) 0.2500 0.0308(14) Uani 1 d S . . C4 C 0.0962(3) 0.4695(5) 0.3619(2) 0.0290(10) Uani 1 d . . . C5 C 0.1676(4) 0.5600(5) 0.3543(3) 0.0388(12) Uani 1 d . . . C6 C 0.2173(4) 0.6127(6) 0.4090(3) 0.0498(14) Uani 1 d . . . C7 C 0.1972(5) 0.5778(7) 0.4714(3) 0.0562(16) Uani 1 d . . . C8 C 0.1259(5) 0.4927(7) 0.4797(3) 0.0584(16) Uani 1 d . . . C9 C 0.0751(4) 0.4404(6) 0.4249(3) 0.0433(13) Uani 1 d . . . C10 C 0.2061(3) 0.2392(5) 0.3136(2) 0.0360(11) Uani 1 d . . . C11 C 0.1625(3) 0.3372(5) 0.1955(2) 0.0341(11) Uani 1 d . . . C12 C -0.0088(5) -0.1385(6) 0.1132(3) 0.0503(15) Uani 1 d . . . C13 C 0.0601(4) -0.0492(6) 0.0946(2) 0.0408(12) Uani 1 d . . . C14 C 0.0200(4) 0.0737(6) 0.0683(2) 0.0398(12) Uani 1 d . . . C15 C -0.0726(4) 0.0635(6) 0.0715(3) 0.0450(14) Uani 1 d . . . C16 C -0.0907(4) -0.0664(7) 0.0987(3) 0.0519(16) Uani 1 d . . . H5 H 0.8185 0.5871 0.1919 0.056 Uiso 1 d . . . H6 H 0.7285 0.6749 0.0951 0.063 Uiso 1 d . . . H7 H 0.7650 0.6165 -0.0114 0.070 Uiso 1 d . . . H8 H 0.8906 0.4683 -0.0258 0.078 Uiso 1 d . . . H9 H 0.9778 0.3798 0.0689 0.059 Uiso 1 d . . . H12 H -0.0043 -0.2355 0.1330 0.067 Uiso 1 d . . . H13 H 0.1315 -0.0697 0.1014 0.058 Uiso 1 d . . . H14 H 0.0517 0.1566 0.0486 0.058 Uiso 1 d . . . H15 H -0.1189 0.1368 0.0540 0.058 Uiso 1 d . . . H16 H -0.1502 -0.1014 0.1070 0.066 Uiso 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 W 0.02467(12) 0.02491(13) 0.01904(12) -0.00224(6) -0.00101(7) -0.00044(6) Fe 0.0208(3) 0.0269(3) 0.0228(3) -0.0022(2) 0.0002(2) -0.0004(2) S 0.0263(5) 0.0310(6) 0.0274(6) -0.0038(5) -0.0012(4) 0.0061(4) O1 0.079(4) 0.024(3) 0.057(3) 0.000 -0.019(3) 0.000 O2 0.042(2) 0.061(3) 0.069(3) -0.005(2) -0.030(2) 0.0003(19) O3 0.060(3) 0.063(3) 0.051(2) 0.013(2) 0.017(2) -0.017(2) C1 0.019(2) 0.032(2) 0.023(2) -0.0016(17) 0.0015(16) -0.0032(16) C2 0.030(2) 0.021(2) 0.026(2) -0.0022(17) 0.0017(18) -0.0013(18) C3 0.036(3) 0.027(3) 0.029(3) 0.000 -0.002(3) 0.000 C4 0.031(2) 0.024(2) 0.032(2) -0.0043(18) -0.0018(19) 0.0033(18) C5 0.037(3) 0.034(3) 0.044(3) -0.004(2) 0.000(2) -0.004(2) C6 0.042(3) 0.033(3) 0.072(4) -0.012(3) -0.008(3) -0.008(2) C7 0.067(4) 0.051(4) 0.046(4) -0.015(3) -0.021(3) -0.004(3) C8 0.081(4) 0.062(4) 0.031(3) -0.013(3) -0.005(3) -0.011(4) C9 0.052(3) 0.046(3) 0.031(3) -0.010(2) 0.003(2) -0.011(2) C10 0.035(3) 0.034(3) 0.038(3) -0.002(2) -0.001(2) 0.000(2) C11 0.027(2) 0.040(3) 0.035(3) -0.003(2) 0.0005(19) -0.004(2) C12 0.083(4) 0.033(3) 0.035(3) -0.016(2) 0.006(3) -0.005(3) C13 0.050(3) 0.050(3) 0.023(2) -0.011(2) 0.002(2) 0.012(2) C14 0.055(3) 0.047(3) 0.017(2) -0.007(2) 0.002(2) -0.002(2) C15 0.050(3) 0.060(4) 0.022(3) -0.012(2) -0.013(2) 0.010(3) C16 0.051(3) 0.075(4) 0.029(3) -0.022(3) -0.002(2) -0.026(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 W C1 1.978(5) . ? W S 2.3148(11) . ? W C16 2.350(5) . ? W C13 2.349(5) . ? W C12 2.352(5) . ? W C15 2.354(5) . ? W S 2.3580(11) 2 ? W C14 2.360(5) . ? W Fe 2.7048(6) 2 ? W Fe 2.7686(6) . ? W W 2.8274(3) 2 ? Fe C11 1.778(5) . ? Fe C10 1.803(5) . ? Fe C1 2.038(4) 2 ? Fe C1 2.094(4) . ? Fe C2 2.140(4) . ? Fe S 2.2386(13) . ? Fe W 2.7048(6) 2 ? S W 2.3580(11) 2 ? O1 C3 1.214(9) . ? O2 C10 1.139(6) . ? O3 C11 1.148(6) . ? C1 C2 1.395(6) 2 ? C1 Fe 2.038(4) 2 ? C2 C1 1.395(6) 2 ? C2 C4 1.492(6) . ? C2 C3 1.503(6) . ? C3 C2 1.503(6) 2 ? C4 C9 1.380(7) . ? C4 C5 1.395(7) . ? C5 C6 1.380(8) . ? C6 C7 1.376(9) . ? C7 C8 1.366(10) . ? C8 C9 1.389(8) . ? C12 C13 1.417(8) . ? C12 C16 1.419(9) . ? C12 H12 1.007(6) . ? C13 C14 1.399(8) . ? C13 H13 1.089(6) . ? C14 C15 1.404(8) . ? C14 H14 1.023(5) . ? C15 C16 1.391(9) . ? C15 H15 1.026(5) . ? C16 H16 0.984(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 W S 100.26(12) . . ? C1 W C16 126.0(2) . . ? S W C16 131.89(18) . . ? C1 W C13 121.21(18) . . ? S W C13 88.63(13) . . ? C16 W C13 58.2(2) . . ? C1 W C12 149.69(19) . . ? S W C12 97.70(16) . . ? C16 W C12 35.1(2) . . ? C13 W C12 35.1(2) . . ? C1 W C15 94.88(18) . . ? S W C15 146.35(14) . . ? C16 W C15 34.4(2) . . ? C13 W C15 57.94(19) . . ? C12 W C15 57.9(2) . . ? C1 W S 100.40(12) . 2 ? S W S 98.98(4) . 2 ? C16 W S 86.24(15) . 2 ? C13 W S 135.69(15) . 2 ? C12 W S 100.65(16) . 2 ? C15 W S 107.63(16) . 2 ? C1 W C14 92.56(17) . . ? S W C14 114.21(14) . . ? C16 W C14 57.4(2) . . ? C13 W C14 34.58(18) . . ? C12 W C14 57.69(19) . . ? C15 W C14 34.7(2) . . ? S W C14 141.54(14) 2 . ? C1 W Fe 48.61(11) . 2 ? S W Fe 108.29(3) . 2 ? C16 W Fe 112.01(16) . 2 ? C13 W Fe 160.97(13) . 2 ? C12 W Fe 144.09(17) . 2 ? C15 W Fe 104.29(14) . 2 ? S W Fe 51.93(3) 2 2 ? C14 W Fe 126.79(14) . 2 ? C1 W Fe 48.95(12) . . ? S W Fe 51.31(3) . . ? C16 W Fe 168.08(15) . . ? C13 W Fe 113.35(14) . . ? C12 W Fe 142.12(17) . . ? C15 W Fe 135.04(16) . . ? S W Fe 105.00(3) 2 . ? C14 W Fe 110.70(13) . . ? Fe W Fe 73.32(2) 2 . ? C1 W W 84.69(12) . 2 ? S W W 53.47(3) . 2 ? C16 W W 134.11(15) . 2 ? C13 W W 138.95(13) . 2 ? C12 W W 125.56(14) . 2 ? C15 W W 158.89(15) . 2 ? S W W 52.07(3) 2 2 ? C14 W W 166.28(14) . 2 ? Fe W W 60.011(13) 2 2 ? Fe W W 57.797(13) . 2 ? C11 Fe C10 93.7(2) . . ? C11 Fe C1 136.4(2) . 2 ? C10 Fe C1 104.4(2) . 2 ? C11 Fe C1 83.49(19) . . ? C10 Fe C1 172.0(2) . . ? C1 Fe C1 73.12(18) 2 . ? C11 Fe C2 101.7(2) . . ? C10 Fe C2 93.7(2) . . ? C1 Fe C2 38.91(17) 2 . ? C1 Fe C2 79.59(17) . . ? C11 Fe S 117.35(17) . . ? C10 Fe S 88.74(16) . . ? C1 Fe S 102.59(14) 2 . ? C1 Fe S 99.23(13) . . ? C2 Fe S 140.61(12) . . ? C11 Fe W 166.23(15) . 2 ? C10 Fe W 98.03(16) . 2 ? C1 Fe W 46.72(13) 2 2 ? C1 Fe W 85.80(12) . 2 ? C2 Fe W 84.77(12) . 2 ? S Fe W 56.03(3) . 2 ? C11 Fe W 104.04(15) . . ? C10 Fe W 142.53(16) . . ? C1 Fe W 85.18(12) 2 . ? C1 Fe W 45.41(13) . . ? C2 Fe W 114.03(12) . . ? S Fe W 53.81(3) . . ? W Fe W 62.193(14) 2 . ? Fe S W 74.87(4) . . ? Fe S W 72.04(4) . 2 ? W S W 74.46(3) . 2 ? C2 C1 W 154.6(3) 2 . ? C2 C1 Fe 74.5(2) 2 2 ? W C1 Fe 84.67(16) . 2 ? C2 C1 Fe 113.3(3) 2 . ? W C1 Fe 85.64(17) . . ? Fe C1 Fe 104.55(18) 2 . ? C1 C2 C4 121.3(4) 2 . ? C1 C2 C3 114.1(4) 2 . ? C4 C2 C3 120.4(4) . . ? C1 C2 Fe 66.6(2) 2 . ? C4 C2 Fe 116.6(3) . . ? C3 C2 Fe 103.7(3) . . ? O1 C3 C2 124.0(3) . 2 ? O1 C3 C2 124.0(3) . . ? C2 C3 C2 112.0(5) 2 . ? C9 C4 C5 118.2(5) . . ? C9 C4 C2 119.3(4) . . ? C5 C4 C2 122.5(4) . . ? C6 C5 C4 120.0(5) . . ? C7 C6 C5 120.7(5) . . ? C8 C7 C6 120.0(5) . . ? C7 C8 C9 119.6(6) . . ? C4 C9 C8 121.4(5) . . ? O2 C10 Fe 178.2(5) . . ? O3 C11 Fe 174.0(5) . . ? C13 C12 C16 107.3(5) . . ? C13 C12 W 72.3(3) . . ? C16 C12 W 72.3(3) . . ? C13 C12 H12 129.2(6) . . ? C16 C12 H12 123.5(6) . . ? W C12 H12 120.9(4) . . ? C14 C13 C12 107.6(5) . . ? C14 C13 W 73.1(3) . . ? C12 C13 W 72.6(3) . . ? C14 C13 H13 125.7(5) . . ? C12 C13 H13 126.6(5) . . ? W C13 H13 117.9(3) . . ? C13 C14 C15 108.7(5) . . ? C13 C14 W 72.3(3) . . ? C15 C14 W 72.4(3) . . ? C13 C14 H14 126.5(6) . . ? C15 C14 H14 124.8(5) . . ? W C14 H14 122.7(3) . . ? C16 C15 C14 108.1(5) . . ? C16 C15 W 72.6(3) . . ? C14 C15 W 72.9(3) . . ? C16 C15 H15 126.2(6) . . ? C14 C15 H15 125.6(6) . . ? W C15 H15 123.2(4) . . ? C15 C16 C12 108.3(5) . . ? C15 C16 W 73.0(3) . . ? C12 C16 W 72.5(3) . . ? C15 C16 H16 125.7(7) . . ? C12 C16 H16 125.9(7) . . ? W C16 H16 119.7(4) . . ? _diffrn_measured_fraction_theta_max 0.468 _diffrn_reflns_theta_full 24.74 _diffrn_measured_fraction_theta_full 0.468 _refine_diff_density_max 1.109 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.102 data_15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H21 Mo2 O5.50' _chemical_formula_weight 673.36 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 13.38(5) _cell_length_b 19.69(5) _cell_length_c 20.15(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5312(27) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark brown ' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 221(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4819 _diffrn_reflns_av_R_equivalents 0.0104 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.92 _reflns_number_total 4657 _reflns_number_gt 3868 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+6.0024P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4657 _refine_ls_number_parameters 348 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.21730(2) 0.218405(15) 0.051973(14) 0.02646(10) Uani 1 d . . . Mo2 Mo 0.25785(2) 0.219943(15) 0.196662(14) 0.02788(10) Uani 1 d . . . C1 C 0.3169(3) 0.1197(2) 0.03542(19) 0.0442(10) Uani 1 d . . . H1A H 0.3441 0.0918 0.0700 0.080 Uiso 1 d R . . C2 C 0.2223(3) 0.1108(2) 0.00494(19) 0.0441(10) Uani 1 d . . . H2A H 0.1761 0.0746 0.0138 0.080 Uiso 1 d R . . C3 C 0.2134(3) 0.1592(2) -0.04579(18) 0.0427(9) Uani 1 d . . . H3A H 0.1610 0.1613 -0.0782 0.080 Uiso 1 d R . . C4 C 0.3025(3) 0.1996(2) -0.04602(17) 0.0423(9) Uani 1 d . . . H4A H 0.3198 0.2336 -0.0781 0.080 Uiso 1 d R . . C5 C 0.3655(3) 0.1747(2) 0.00492(18) 0.0437(10) Uani 1 d . . . H5A H 0.4321 0.1901 0.0144 0.080 Uiso 1 d R . . C6 C 0.2631(6) 0.1910(3) 0.3080(2) 0.080(2) Uani 1 d . . . H6A H 0.2912 0.1498 0.3253 0.080 Uiso 1 d R . . C7 C 0.1646(6) 0.2007(4) 0.2935(2) 0.090(2) Uani 1 d . . . H7A H 0.1128 0.1674 0.2982 0.080 Uiso 1 d R . . C8 C 0.1510(4) 0.2681(3) 0.2762(2) 0.0672(16) Uani 1 d . . . H8A H 0.0881 0.2897 0.2676 0.080 Uiso 1 d R . . C9 C 0.2446(4) 0.2998(2) 0.2819(2) 0.0544(12) Uani 1 d . . . H9A H 0.2575 0.3476 0.2784 0.080 Uiso 1 d R . . C10 C 0.3125(3) 0.2503(3) 0.30186(19) 0.0595(13) Uani 1 d . . . H10A H 0.3808 0.2581 0.3142 0.080 Uiso 1 d R . . C11 C 0.3606(3) 0.45062(18) -0.06420(17) 0.0357(8) Uani 1 d . . . C12 C 0.4485(3) 0.4756(2) -0.0913(2) 0.0498(11) Uani 1 d . . . H12A H 0.5110 0.4671 -0.0694 0.080 Uiso 1 d R . . C13 C 0.4459(4) 0.5122(3) -0.1504(2) 0.0630(13) Uani 1 d . . . H13A H 0.5065 0.5307 -0.1683 0.080 Uiso 1 d R . . C14 C 0.3568(4) 0.5228(2) -0.1823(2) 0.0601(12) Uani 1 d . . . H14A H 0.3554 0.5466 -0.2239 0.080 Uiso 1 d R . . C15 C 0.2703(3) 0.4989(2) -0.1547(2) 0.0549(11) Uani 1 d . . . H15A H 0.2080 0.5072 -0.1769 0.080 Uiso 1 d R . . C16 C 0.2701(3) 0.4633(2) -0.0958(2) 0.0461(10) Uani 1 d . . . H16A H 0.2086 0.4473 -0.0768 0.080 Uiso 1 d R . . C17 C 0.3658(3) 0.40893(19) -0.00549(18) 0.0363(8) Uani 1 d . . . C18 C 0.3759(3) 0.37149(19) 0.04082(17) 0.0354(8) Uani 1 d . . . C19 C 0.3925(3) 0.32292(19) 0.09415(17) 0.0344(8) Uani 1 d . . . O19 O 0.47734(19) 0.31561(16) 0.11679(14) 0.0537(8) Uani 1 d . . . C20 C 0.3071(3) 0.28464(18) 0.11626(16) 0.0288(7) Uani 1 d . . . C21 C 0.2062(2) 0.29765(18) 0.12691(16) 0.0273(7) Uani 1 d . . . C22 C 0.1471(2) 0.35952(18) 0.13805(16) 0.0295(7) Uani 1 d . . . C23 C 0.0429(3) 0.3593(2) 0.1310(2) 0.0447(10) Uani 1 d . . . H23A H 0.0096 0.3179 0.1190 0.080 Uiso 1 d R . . C24 C -0.0118(3) 0.4171(2) 0.1411(3) 0.0591(12) Uani 1 d . . . H24A H -0.0828 0.4160 0.1344 0.080 Uiso 1 d R . . C25 C 0.0329(3) 0.4766(2) 0.1610(2) 0.0548(11) Uani 1 d . . . H25A H -0.0065 0.5165 0.1689 0.080 Uiso 1 d R . . C26 C 0.1352(3) 0.4781(2) 0.1687(2) 0.0479(10) Uani 1 d . . . H26A H 0.1675 0.5192 0.1828 0.080 Uiso 1 d R . . C27 C 0.1916(3) 0.42041(19) 0.15678(18) 0.0382(8) Uani 1 d . . . H27A H 0.2629 0.4224 0.1614 0.080 Uiso 1 d R . . C28 C 0.1618(3) 0.2959(2) 0.00055(18) 0.0369(9) Uani 1 d . . . O28 O 0.1266(2) 0.33811(16) -0.03045(15) 0.0534(7) Uani 1 d . . . C29 C 0.0746(3) 0.20121(18) 0.07625(17) 0.0325(8) Uani 1 d . . . O29 O -0.00643(19) 0.18957(14) 0.08909(14) 0.0473(7) Uani 1 d . . . C30 C 0.3920(3) 0.1826(2) 0.17675(17) 0.0381(9) Uani 1 d . . . O30 O 0.4703(2) 0.16078(16) 0.16763(15) 0.0543(8) Uani 1 d . . . C31 C 0.1990(3) 0.1332(2) 0.16826(17) 0.0340(8) Uani 1 d . . . O31 O 0.1642(2) 0.07985(14) 0.16089(14) 0.0482(7) Uani 1 d . . . O1 O 0.5000 0.3618(5) 0.2500 0.193(4) Uani 1 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01936(16) 0.04066(19) 0.01937(16) -0.00287(12) 0.00065(10) -0.00175(12) Mo2 0.02395(17) 0.04034(19) 0.01935(16) 0.00023(12) 0.00026(11) -0.00203(12) C1 0.044(2) 0.054(2) 0.034(2) -0.0098(18) 0.0071(18) 0.0162(19) C2 0.043(2) 0.049(2) 0.041(2) -0.0186(19) 0.0079(17) -0.0032(18) C3 0.036(2) 0.064(3) 0.0279(19) -0.0160(18) 0.0002(15) 0.0011(19) C4 0.037(2) 0.068(3) 0.0216(18) -0.0065(17) 0.0084(15) 0.005(2) C5 0.0293(19) 0.070(3) 0.0318(19) -0.0099(19) 0.0056(15) 0.0072(19) C6 0.145(6) 0.066(4) 0.030(2) 0.015(2) 0.017(3) 0.021(4) C7 0.114(5) 0.118(5) 0.039(3) -0.027(3) 0.050(3) -0.071(5) C8 0.040(3) 0.134(5) 0.027(2) -0.021(3) 0.0016(18) 0.031(3) C9 0.088(4) 0.051(2) 0.0241(19) -0.0083(19) 0.010(2) -0.003(2) C10 0.043(2) 0.112(4) 0.024(2) -0.015(2) -0.0103(18) 0.014(3) C11 0.043(2) 0.0342(18) 0.0302(18) -0.0038(15) 0.0042(16) 0.0028(16) C12 0.042(2) 0.059(3) 0.048(2) 0.016(2) 0.0056(19) 0.004(2) C13 0.057(3) 0.071(3) 0.061(3) 0.028(3) 0.018(2) 0.010(2) C14 0.069(3) 0.063(3) 0.048(3) 0.015(2) 0.007(2) 0.018(2) C15 0.054(3) 0.057(3) 0.054(3) 0.002(2) -0.009(2) 0.016(2) C16 0.043(2) 0.049(2) 0.046(2) -0.0020(19) 0.0031(18) 0.0033(18) C17 0.0343(19) 0.041(2) 0.0333(19) -0.0032(17) 0.0070(15) -0.0032(16) C18 0.0282(18) 0.047(2) 0.0313(19) -0.0039(17) 0.0056(15) -0.0062(16) C19 0.0261(18) 0.048(2) 0.0287(18) -0.0027(16) 0.0017(14) -0.0056(15) O19 0.0239(14) 0.080(2) 0.0573(18) 0.0181(16) -0.0071(13) -0.0134(14) C20 0.0239(17) 0.044(2) 0.0182(16) -0.0006(14) -0.0014(13) -0.0041(15) C21 0.0221(16) 0.0380(19) 0.0219(16) 0.0005(14) -0.0022(13) -0.0046(14) C22 0.0284(17) 0.0381(19) 0.0221(16) 0.0004(14) 0.0035(13) -0.0024(15) C23 0.0277(19) 0.045(2) 0.061(3) -0.0115(19) 0.0013(18) -0.0010(17) C24 0.036(2) 0.053(3) 0.088(3) -0.015(2) 0.002(2) 0.007(2) C25 0.052(3) 0.041(2) 0.072(3) -0.006(2) 0.005(2) 0.0111(19) C26 0.056(3) 0.038(2) 0.050(2) -0.0065(19) 0.005(2) -0.0085(19) C27 0.0310(19) 0.046(2) 0.037(2) -0.0022(17) 0.0006(16) -0.0087(17) C28 0.0239(18) 0.058(2) 0.0286(18) -0.0020(18) -0.0013(15) -0.0058(17) O28 0.0397(16) 0.068(2) 0.0523(17) 0.0178(16) -0.0103(14) 0.0017(15) C29 0.031(2) 0.041(2) 0.0250(17) -0.0065(15) -0.0021(15) -0.0013(15) O29 0.0251(14) 0.0605(17) 0.0564(17) -0.0118(14) 0.0063(13) -0.0098(13) C30 0.036(2) 0.052(2) 0.0273(18) 0.0029(17) -0.0053(16) -0.0031(18) O30 0.0307(15) 0.070(2) 0.0623(19) -0.0051(16) -0.0018(14) 0.0108(14) C31 0.0286(18) 0.047(2) 0.0260(18) 0.0037(16) -0.0005(15) 0.0028(17) O31 0.0467(16) 0.0456(16) 0.0524(17) 0.0026(14) -0.0057(14) -0.0107(13) O1 0.252(12) 0.161(8) 0.166(9) 0.000 0.022(9) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C28 1.988(5) . ? Mo1 C29 2.001(8) . ? Mo1 C21 2.177(5) . ? Mo1 C20 2.196(5) . ? Mo1 C3 2.290(6) . ? Mo1 C4 2.311(6) . ? Mo1 C2 2.322(6) . ? Mo1 C5 2.361(7) . ? Mo1 C1 2.381(6) . ? Mo1 Mo2 2.966(7) . ? Mo2 C31 1.967(6) . ? Mo2 C30 1.982(7) . ? Mo2 C20 2.164(5) . ? Mo2 C21 2.190(5) . ? Mo2 C6 2.317(7) . ? Mo2 C10 2.321(6) . ? Mo2 C9 2.335(6) . ? Mo2 C7 2.347(6) . ? Mo2 C8 2.348(6) . ? C1 C5 1.406(6) . ? C1 C2 1.418(7) . ? C1 H1A 0.9599 . ? C2 C3 1.402(6) . ? C2 H2A 0.9599 . ? C3 C4 1.434(7) . ? C3 H3A 0.9600 . ? C4 C5 1.416(6) . ? C4 H4A 0.9600 . ? C5 H5A 0.9600 . ? C6 C10 1.348(9) . ? C6 C7 1.364(10) . ? C6 H6A 0.9601 . ? C7 C8 1.383(9) . ? C7 H7A 0.9600 . ? C8 C9 1.404(8) . ? C8 H8A 0.9600 . ? C9 C10 1.391(7) . ? C9 H9A 0.9601 . ? C10 H10A 0.9599 . ? C11 C12 1.387(6) . ? C11 C16 1.392(7) . ? C11 C17 1.442(6) . ? C12 C13 1.392(6) . ? C12 H12A 0.9600 . ? C13 C14 1.370(8) . ? C13 H13A 0.9600 . ? C14 C15 1.369(7) . ? C14 H14A 0.9600 . ? C15 C16 1.379(7) . ? C15 H15A 0.9600 . ? C16 H16A 0.9599 . ? C17 C18 1.197(5) . ? C18 C19 1.456(6) . ? C19 O19 1.232(6) . ? C19 C20 1.441(6) . ? C20 C21 1.390(7) . ? C21 C22 1.470(6) . ? C22 C27 1.391(6) . ? C22 C23 1.401(7) . ? C23 C24 1.368(6) . ? C23 H23A 0.9601 . ? C24 C25 1.375(7) . ? C24 H24A 0.9599 . ? C25 C26 1.379(8) . ? C25 H25A 0.9601 . ? C26 C27 1.385(6) . ? C26 H26A 0.9600 . ? C27 H27A 0.9600 . ? C28 O28 1.142(5) . ? C29 O29 1.138(6) . ? C30 O30 1.148(6) . ? C31 O31 1.158(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 C28 Mo1 C29 84.3(2) . . ? C28 Mo1 C21 77.7(2) . . ? C29 Mo1 C21 83.49(14) . . ? C28 Mo1 C20 93.2(2) . . ? C29 Mo1 C20 118.59(19) . . ? C21 Mo1 C20 37.07(18) . . ? C28 Mo1 C3 86.2(2) . . ? C29 Mo1 C3 95.89(15) . . ? C21 Mo1 C3 163.84(14) . . ? C20 Mo1 C3 145.32(16) . . ? C28 Mo1 C4 82.0(2) . . ? C29 Mo1 C4 130.80(15) . . ? C21 Mo1 C4 137.85(16) . . ? C20 Mo1 C4 109.2(2) . . ? C3 Mo1 C4 36.32(18) . . ? C28 Mo1 C2 119.9(2) . . ? C29 Mo1 C2 88.45(15) . . ? C21 Mo1 C2 159.94(14) . . ? C20 Mo1 C2 140.08(17) . . ? C3 Mo1 C2 35.39(15) . . ? C4 Mo1 C2 59.39(16) . . ? C28 Mo1 C5 112.57(19) . . ? C29 Mo1 C5 147.01(19) . . ? C21 Mo1 C5 126.66(16) . . ? C20 Mo1 C5 89.6(3) . . ? C3 Mo1 C5 59.20(17) . . ? C4 Mo1 C5 35.26(14) . . ? C2 Mo1 C5 58.63(17) . . ? C28 Mo1 C1 139.70(18) . . ? C29 Mo1 C1 115.5(2) . . ? C21 Mo1 C1 136.12(16) . . ? C20 Mo1 C1 105.2(2) . . ? C3 Mo1 C1 58.41(16) . . ? C4 Mo1 C1 58.20(16) . . ? C2 Mo1 C1 35.07(18) . . ? C5 Mo1 C1 34.50(15) . . ? C28 Mo1 Mo2 124.95(13) . . ? C29 Mo1 Mo2 86.33(14) . . ? C21 Mo1 Mo2 47.39(13) . . ? C20 Mo1 Mo2 46.68(11) . . ? C3 Mo1 Mo2 148.77(14) . . ? C4 Mo1 Mo2 138.72(18) . . ? C2 Mo1 Mo2 113.91(13) . . ? C5 Mo1 Mo2 104.17(16) . . ? C1 Mo1 Mo2 92.50(11) . . ? C31 Mo2 C30 88.9(2) . . ? C31 Mo2 C20 114.6(2) . . ? C30 Mo2 C20 77.95(18) . . ? C31 Mo2 C21 107.1(2) . . ? C30 Mo2 C21 114.55(17) . . ? C20 Mo2 C21 37.24(19) . . ? C31 Mo2 C6 94.6(2) . . ? C30 Mo2 C6 94.4(2) . . ? C20 Mo2 C6 149.4(2) . . ? C21 Mo2 C6 143.44(18) . . ? C31 Mo2 C10 128.02(19) . . ? C30 Mo2 C10 89.7(2) . . ? C20 Mo2 C10 115.9(2) . . ? C21 Mo2 C10 120.4(2) . . ? C6 Mo2 C10 33.8(2) . . ? C31 Mo2 C9 140.23(18) . . ? C30 Mo2 C9 117.88(19) . . ? C20 Mo2 C9 100.2(2) . . ? C21 Mo2 C9 88.7(2) . . ? C6 Mo2 C9 57.0(2) . . ? C10 Mo2 C9 34.75(19) . . ? C31 Mo2 C7 83.6(2) . . ? C30 Mo2 C7 126.2(3) . . ? C20 Mo2 C7 151.6(2) . . ? C21 Mo2 C7 118.6(3) . . ? C6 Mo2 C7 34.0(3) . . ? C10 Mo2 C7 56.6(3) . . ? C9 Mo2 C7 57.1(2) . . ? C31 Mo2 C8 107.8(3) . . ? C30 Mo2 C8 147.13(16) . . ? C20 Mo2 C8 117.3(2) . . ? C21 Mo2 C8 87.9(2) . . ? C6 Mo2 C8 57.1(2) . . ? C10 Mo2 C8 57.6(2) . . ? C9 Mo2 C8 34.9(2) . . ? C7 Mo2 C8 34.3(2) . . ? C31 Mo2 Mo1 68.39(11) . . ? C30 Mo2 Mo1 87.88(14) . . ? C20 Mo2 Mo1 47.59(14) . . ? C21 Mo2 Mo1 47.03(13) . . ? C6 Mo2 Mo1 162.84(19) . . ? C10 Mo2 Mo1 163.38(16) . . ? C9 Mo2 Mo1 135.75(16) . . ? C7 Mo2 Mo1 135.9(2) . . ? C8 Mo2 Mo1 124.33(19) . . ? C5 C1 C2 108.6(4) . . ? C5 C1 Mo1 72.0(3) . . ? C2 C1 Mo1 70.2(3) . . ? C5 C1 H1A 125.7 . . ? C2 C1 H1A 125.7 . . ? Mo1 C1 H1A 125.3 . . ? C3 C2 C1 107.9(4) . . ? C3 C2 Mo1 71.1(3) . . ? C1 C2 Mo1 74.7(2) . . ? C3 C2 H2A 125.8 . . ? C1 C2 H2A 125.8 . . ? Mo1 C2 H2A 125.7 . . ? C2 C3 C4 108.0(4) . . ? C2 C3 Mo1 73.5(3) . . ? C4 C3 Mo1 72.6(2) . . ? C2 C3 H3A 126.0 . . ? C4 C3 H3A 125.5 . . ? Mo1 C3 H3A 125.5 . . ? C5 C4 C3 107.5(4) . . ? C5 C4 Mo1 74.3(3) . . ? C3 C4 Mo1 71.1(2) . . ? C5 C4 H4A 126.0 . . ? C3 C4 H4A 126.2 . . ? Mo1 C4 H4A 125.7 . . ? C1 C5 C4 108.0(4) . . ? C1 C5 Mo1 73.5(3) . . ? C4 C5 Mo1 70.4(3) . . ? C1 C5 H5A 125.9 . . ? C4 C5 H5A 125.9 . . ? Mo1 C5 H5A 125.8 . . ? C10 C6 C7 109.4(6) . . ? C10 C6 Mo2 73.3(3) . . ? C7 C6 Mo2 74.2(3) . . ? C10 C6 H6A 125.0 . . ? C7 C6 H6A 125.2 . . ? Mo2 C6 H6A 124.8 . . ? C6 C7 C8 108.4(5) . . ? C6 C7 Mo2 71.8(3) . . ? C8 C7 Mo2 72.9(3) . . ? C6 C7 H7A 125.5 . . ? C8 C7 H7A 125.8 . . ? Mo2 C7 H7A 125.3 . . ? C7 C8 C9 106.7(5) . . ? C7 C8 Mo2 72.8(3) . . ? C9 C8 Mo2 72.1(3) . . ? C7 C8 H8A 125.9 . . ? C9 C8 H8A 126.9 . . ? Mo2 C8 H8A 126.1 . . ? C10 C9 C8 107.2(5) . . ? C10 C9 Mo2 72.1(3) . . ? C8 C9 Mo2 73.1(3) . . ? C10 C9 H9A 126.2 . . ? C8 C9 H9A 126.1 . . ? Mo2 C9 H9A 126.3 . . ? C6 C10 C9 108.2(5) . . ? C6 C10 Mo2 72.9(3) . . ? C9 C10 Mo2 73.2(3) . . ? C6 C10 H10A 125.6 . . ? C9 C10 H10A 125.8 . . ? Mo2 C10 H10A 125.3 . . ? C12 C11 C16 119.7(4) . . ? C12 C11 C17 119.0(4) . . ? C16 C11 C17 121.3(4) . . ? C11 C12 C13 119.9(4) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 120.4 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 119.8 . . ? C15 C14 C13 119.5(5) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 121.8(4) . . ? C14 C15 H15A 119.2 . . ? C16 C15 H15A 119.1 . . ? C15 C16 C11 118.9(4) . . ? C15 C16 H16A 120.8 . . ? C11 C16 H16A 120.3 . . ? C18 C17 C11 174.8(4) . . ? C17 C18 C19 176.0(4) . . ? O19 C19 C20 123.8(4) . . ? O19 C19 C18 119.4(3) . . ? C20 C19 C18 116.8(3) . . ? C21 C20 C19 136.2(4) . . ? C21 C20 Mo2 72.4(2) . . ? C19 C20 Mo2 141.4(3) . . ? C21 C20 Mo1 70.7(3) . . ? C19 C20 Mo1 124.2(3) . . ? Mo2 C20 Mo1 85.7(2) . . ? C20 C21 C22 134.3(3) . . ? C20 C21 Mo1 72.2(2) . . ? C22 C21 Mo1 137.5(2) . . ? C20 C21 Mo2 70.4(2) . . ? C22 C21 Mo2 130.6(3) . . ? Mo1 C21 Mo2 85.6(2) . . ? C27 C22 C23 117.1(4) . . ? C27 C22 C21 121.7(4) . . ? C23 C22 C21 121.2(3) . . ? C24 C23 C22 121.0(4) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.3 . . ? C23 C24 C25 121.3(5) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.3 . . ? C24 C25 C26 118.9(4) . . ? C24 C25 H25A 120.5 . . ? C26 C25 H25A 120.6 . . ? C25 C26 C27 120.3(4) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.8 . . ? C26 C27 C22 121.4(4) . . ? C26 C27 H27A 119.5 . . ? C22 C27 H27A 119.1 . . ? O28 C28 Mo1 176.5(3) . . ? O29 C29 Mo1 177.9(3) . . ? O30 C30 Mo2 177.5(3) . . ? O31 C31 Mo2 170.4(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.619 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.129