# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Cristian Vicent' _publ_contact_author_email BARRERA@SG.UJI.ES loop_ _publ_author_name C.Vicent A.G.Algarra M.Basallote M.J.Fernandez-Trujillo ; R.Llusar ; J.A.Pino-Chamorro I.Sorribes data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 755398' #TrackingRef 'compound_1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H50 Cl6 Fe Mo3 P6 S4' _chemical_formula_weight 1149.02 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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 Hexagonal _symmetry_space_group_name_H-M R3c _symmetry_space_group_name_Hall 'R 3 -2"c' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 15.7226(15) _cell_length_b 15.7226(15) _cell_length_c 29.224(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6256.3(11) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 971 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 23.63 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 2.052 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.779045 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16378 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 30.51 _reflns_number_total 4121 _reflns_number_gt 2980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.3504P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(4) _refine_ls_number_reflns 4121 _refine_ls_number_parameters 122 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.55145(3) 0.24929(3) 0.301848(13) 0.02887(11) Uani 1 1 d . . . Fe1 Fe 0.6667 0.3333 0.22648(5) 0.0342(3) Uani 1 3 d S . . Cl1 Cl 0.43393(10) 0.25616(12) 0.35872(5) 0.0444(4) Uani 1 1 d . . . Cl2 Cl 0.6667 0.3333 0.15083(10) 0.0835(11) Uani 1 3 d S . . S1 S 0.6667 0.3333 0.36045(8) 0.0336(5) Uani 1 3 d S . . S2 S 0.62388(10) 0.18337(10) 0.25362(4) 0.0338(3) Uani 1 1 d . . . P1 P 0.39197(11) 0.14625(11) 0.25888(5) 0.0364(3) Uani 1 1 d . . . P2 P 0.47892(12) 0.08275(12) 0.34276(5) 0.0387(4) Uani 1 1 d . . . C1 C 0.2980(5) 0.1809(6) 0.2659(2) 0.0558(18) Uani 1 1 d . . . H1A H 0.2889 0.1880 0.2978 0.084 Uiso 1 1 calc R . . H1B H 0.2373 0.1308 0.2530 0.084 Uiso 1 1 calc R . . H1C H 0.3183 0.2420 0.2505 0.084 Uiso 1 1 calc R . . C2 C 0.3975(5) 0.1346(5) 0.1972(2) 0.0550(18) Uani 1 1 d . . . H2A H 0.4291 0.1986 0.1835 0.083 Uiso 1 1 calc R . . H2B H 0.3321 0.0965 0.1853 0.083 Uiso 1 1 calc R . . H2C H 0.4342 0.1024 0.1903 0.083 Uiso 1 1 calc R . . C3 C 0.3305(5) 0.0192(4) 0.2789(2) 0.0513(17) Uani 1 1 d . . . H3A H 0.2606 -0.0113 0.2729 0.062 Uiso 1 1 calc R . . H3B H 0.3554 -0.0170 0.2622 0.062 Uiso 1 1 calc R . . C4 C 0.3470(5) 0.0140(5) 0.3300(2) 0.0500(16) Uani 1 1 d . . . H4A H 0.3199 -0.0540 0.3391 0.060 Uiso 1 1 calc R . . H4B H 0.3136 0.0416 0.3471 0.060 Uiso 1 1 calc R . . C5 C 0.4868(5) 0.0811(6) 0.4044(2) 0.0574(18) Uani 1 1 d . . . H5A H 0.4690 0.1261 0.4173 0.086 Uiso 1 1 calc R . . H5B H 0.5528 0.1002 0.4132 0.086 Uiso 1 1 calc R . . H5C H 0.4429 0.0160 0.4155 0.086 Uiso 1 1 calc R . . C6 C 0.5133(5) -0.0056(5) 0.3243(3) 0.0566(18) Uani 1 1 d . . . H6A H 0.5111 -0.0096 0.2915 0.085 Uiso 1 1 calc R . . H6B H 0.4685 -0.0688 0.3370 0.085 Uiso 1 1 calc R . . H6C H 0.5787 0.0147 0.3347 0.085 Uiso 1 1 calc R . . C200 C 0.283(3) 0.6340(17) 0.3218(10) 0.148(17) Uiso 0.33 1 d PD A -1 H20A H 0.3244 0.6482 0.2950 0.178 Uiso 0.33 1 calc PR A -1 H20B H 0.2167 0.5851 0.3131 0.178 Uiso 0.33 1 calc PR A -1 Cl20 Cl 0.321(2) 0.5893(18) 0.3612(9) 0.356(16) Uiso 0.33 1 d PD A -1 Cl21 Cl 0.2838(7) 0.7328(7) 0.3372(3) 0.110(3) Uiso 0.33 1 d PD A -1 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 0.0286(2) 0.0294(2) 0.0286(2) -0.00162(19) 0.00237(18) 0.0145(2) Fe1 0.0364(5) 0.0364(5) 0.0297(7) 0.000 0.000 0.0182(2) Cl1 0.0421(8) 0.0493(9) 0.0433(8) -0.0044(7) 0.0101(6) 0.0240(7) Cl2 0.1112(19) 0.1112(19) 0.0282(14) 0.000 0.000 0.0556(9) S1 0.0364(8) 0.0364(8) 0.0279(11) 0.000 0.000 0.0182(4) S2 0.0342(8) 0.0345(7) 0.0327(8) -0.0027(6) 0.0034(6) 0.0171(6) P1 0.0350(8) 0.0355(8) 0.0381(8) -0.0070(6) 0.0001(6) 0.0172(7) P2 0.0380(9) 0.0348(8) 0.0418(8) 0.0046(7) 0.0079(7) 0.0171(7) C1 0.056(4) 0.069(5) 0.057(4) -0.014(3) -0.006(3) 0.042(4) C2 0.057(4) 0.066(5) 0.043(4) -0.013(3) -0.003(3) 0.031(4) C3 0.046(4) 0.034(3) 0.065(5) -0.004(3) 0.000(3) 0.013(3) C4 0.048(4) 0.038(4) 0.058(4) 0.005(3) 0.013(3) 0.017(3) C5 0.056(4) 0.067(5) 0.051(4) 0.014(3) 0.006(3) 0.031(4) C6 0.060(4) 0.045(4) 0.068(5) 0.010(3) 0.018(4) 0.029(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 Mo1 S2 2.3533(14) . ? Mo1 S1 2.3595(17) . ? Mo1 S2 2.3931(14) 3_665 ? Mo1 Cl1 2.5272(14) . ? Mo1 P1 2.5350(16) . ? Mo1 P2 2.5691(16) . ? Mo1 Fe1 2.7358(12) . ? Mo1 Mo1 2.8111(8) 3_665 ? Mo1 Mo1 2.8111(8) 2_655 ? Fe1 Cl2 2.211(3) . ? Fe1 S2 2.2483(15) 2_655 ? Fe1 S2 2.2483(15) . ? Fe1 S2 2.2483(15) 3_665 ? Fe1 Mo1 2.7358(12) 2_655 ? Fe1 Mo1 2.7358(12) 3_665 ? S1 Mo1 2.3595(17) 2_655 ? S1 Mo1 2.3595(17) 3_665 ? S2 Mo1 2.3931(14) 2_655 ? P1 C2 1.817(6) . ? P1 C1 1.824(7) . ? P1 C3 1.826(6) . ? P2 C6 1.806(6) . ? P2 C5 1.808(7) . ? P2 C4 1.836(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.522(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C200 Cl21 1.612(10) . ? C200 Cl20 1.611(10) . ? C200 H20A 0.9700 . ? C200 H20B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Mo1 S1 106.04(5) . . ? S2 Mo1 S2 100.29(7) . 3_665 ? S1 Mo1 S2 104.77(4) . 3_665 ? S2 Mo1 Cl1 159.69(5) . . ? S1 Mo1 Cl1 82.63(5) . . ? S2 Mo1 Cl1 94.98(5) 3_665 . ? S2 Mo1 P1 87.92(5) . . ? S1 Mo1 P1 162.66(5) . . ? S2 Mo1 P1 82.18(5) 3_665 . ? Cl1 Mo1 P1 80.93(5) . . ? S2 Mo1 P2 84.02(5) . . ? S1 Mo1 P2 93.34(5) . . ? S2 Mo1 P2 159.23(5) 3_665 . ? Cl1 Mo1 P2 77.06(5) . . ? P1 Mo1 P2 77.65(5) . . ? S2 Mo1 Fe1 51.77(4) . . ? S1 Mo1 Fe1 100.15(4) . . ? S2 Mo1 Fe1 51.47(4) 3_665 . ? Cl1 Mo1 Fe1 146.14(4) . . ? P1 Mo1 Fe1 96.57(4) . . ? P2 Mo1 Fe1 135.74(4) . . ? S2 Mo1 Mo1 100.60(4) . 3_665 ? S1 Mo1 Mo1 53.44(3) . 3_665 ? S2 Mo1 Mo1 53.03(4) 3_665 3_665 ? Cl1 Mo1 Mo1 99.27(4) . 3_665 ? P1 Mo1 Mo1 135.18(4) . 3_665 ? P2 Mo1 Mo1 146.59(4) . 3_665 ? Fe1 Mo1 Mo1 59.086(16) . 3_665 ? S2 Mo1 Mo1 54.34(4) . 2_655 ? S1 Mo1 Mo1 53.44(3) . 2_655 ? S2 Mo1 Mo1 99.61(4) 3_665 2_655 ? Cl1 Mo1 Mo1 135.88(4) . 2_655 ? P1 Mo1 Mo1 142.09(4) . 2_655 ? P2 Mo1 Mo1 99.35(4) . 2_655 ? Fe1 Mo1 Mo1 59.086(16) . 2_655 ? Mo1 Mo1 Mo1 60.0 3_665 2_655 ? Cl2 Fe1 S2 110.65(5) . 2_655 ? Cl2 Fe1 S2 110.65(5) . . ? S2 Fe1 S2 108.26(5) 2_655 . ? Cl2 Fe1 S2 110.65(5) . 3_665 ? S2 Fe1 S2 108.26(5) 2_655 3_665 ? S2 Fe1 S2 108.26(5) . 3_665 ? Cl2 Fe1 Mo1 143.61(2) . 2_655 ? S2 Fe1 Mo1 55.31(4) 2_655 2_655 ? S2 Fe1 Mo1 56.37(4) . 2_655 ? S2 Fe1 Mo1 105.73(6) 3_665 2_655 ? Cl2 Fe1 Mo1 143.61(2) . . ? S2 Fe1 Mo1 105.73(6) 2_655 . ? S2 Fe1 Mo1 55.31(4) . . ? S2 Fe1 Mo1 56.37(4) 3_665 . ? Mo1 Fe1 Mo1 61.83(3) 2_655 . ? Cl2 Fe1 Mo1 143.61(2) . 3_665 ? S2 Fe1 Mo1 56.37(4) 2_655 3_665 ? S2 Fe1 Mo1 105.73(6) . 3_665 ? S2 Fe1 Mo1 55.31(4) 3_665 3_665 ? Mo1 Fe1 Mo1 61.83(3) 2_655 3_665 ? Mo1 Fe1 Mo1 61.83(3) . 3_665 ? Mo1 S1 Mo1 73.13(6) 2_655 . ? Mo1 S1 Mo1 73.13(6) 2_655 3_665 ? Mo1 S1 Mo1 73.13(6) . 3_665 ? Fe1 S2 Mo1 72.92(5) . . ? Fe1 S2 Mo1 72.16(5) . 2_655 ? Mo1 S2 Mo1 72.63(4) . 2_655 ? C2 P1 C1 103.2(3) . . ? C2 P1 C3 103.5(3) . . ? C1 P1 C3 103.0(3) . . ? C2 P1 Mo1 118.3(2) . . ? C1 P1 Mo1 116.4(2) . . ? C3 P1 Mo1 110.7(2) . . ? C6 P2 C5 103.7(4) . . ? C6 P2 C4 99.9(3) . . ? C5 P2 C4 105.1(3) . . ? C6 P2 Mo1 119.6(2) . . ? C5 P2 Mo1 118.7(3) . . ? C4 P2 Mo1 107.5(2) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 111.2(4) . . ? C4 C3 H3A 109.4 . . ? P1 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? P1 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 P2 109.9(4) . . ? C3 C4 H4A 109.7 . . ? P2 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? P2 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Cl21 C200 Cl20 113.2(15) . . ? Cl21 C200 H20A 108.9 . . ? Cl20 C200 H20A 108.9 . . ? Cl21 C200 H20B 108.9 . . ? Cl20 C200 H20B 108.9 . . ? H20A C200 H20B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.661 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.120 # Attachment 'compound_2.CIF' data_str956m _database_code_depnum_ccdc_archive 'CCDC 755399' #TrackingRef 'compound_2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H53 Cl3 Fe Mo3 P6 S5' _chemical_formula_weight 1137.80 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 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' _cell_length_a 20.695(4) _cell_length_b 15.641(3) _cell_length_c 13.224(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.978(4) _cell_angle_gamma 90.00 _cell_volume 4202.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1007 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 20.62 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 1.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.737745 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11460 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.1934 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6554 _reflns_number_gt 3567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Carbon atoms of the thiophenolate group had to be refined isotropically (non-positive definite alerts for some of them were observed after anisotropically refinement). The following bond distances C(100)-C(101), C(100)-C(105) and C(104)-C(105) were contrained to reasonable aromatic C-C bond distances (typically 1.42 with standar deviations of 0.02 A). ; _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^)+(0.0735P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.19(9) _refine_ls_number_reflns 6554 _refine_ls_number_parameters 350 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1614 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.1861 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.51128(8) 0.65090(12) 0.40295(12) 0.0270(4) Uani 1 1 d . . . Mo2 Mo 0.43471(8) 0.77730(12) 0.28483(12) 0.0276(5) Uani 1 1 d . . . Mo3 Mo 0.53722(8) 0.82389(12) 0.44587(12) 0.0289(5) Uani 1 1 d . . . Fe1 Fe 0.56220(14) 0.7507(2) 0.2691(2) 0.0328(8) Uani 1 1 d . . . S1 S 0.4405(2) 0.7503(4) 0.4619(4) 0.0308(13) Uani 1 1 d . . . S2 S 0.4819(3) 0.6533(4) 0.2225(4) 0.0347(14) Uani 1 1 d . . . S3 S 0.6165(2) 0.7191(4) 0.4281(4) 0.0337(14) Uani 1 1 d . . . S4 S 0.5171(2) 0.8798(4) 0.2732(4) 0.0381(16) Uani 1 1 d . . . S100 S 0.6088(4) 0.7235(7) 0.1303(5) 0.092(3) Uani 1 1 d . . . Cl1 Cl 0.5239(3) 0.5960(4) 0.5839(4) 0.0428(15) Uani 1 1 d . . . Cl2 Cl 0.3224(2) 0.7081(4) 0.2685(4) 0.0420(15) Uani 1 1 d . . . Cl3 Cl 0.4805(3) 0.9459(4) 0.5200(4) 0.0472(15) Uani 1 1 d . . . P1 P 0.5822(3) 0.5214(4) 0.3880(4) 0.0374(15) Uani 1 1 d . . . P2 P 0.4274(3) 0.5288(4) 0.3869(5) 0.0405(16) Uani 1 1 d . . . P3 P 0.3927(3) 0.8026(4) 0.0935(4) 0.0394(16) Uani 1 1 d . . . P4 P 0.3592(3) 0.9080(4) 0.2846(5) 0.0451(18) Uani 1 1 d . . . P5 P 0.6300(3) 0.9313(4) 0.4714(5) 0.0412(16) Uani 1 1 d . . . P6 P 0.5828(3) 0.8122(4) 0.6414(5) 0.0442(17) Uani 1 1 d . . . C1 C 0.6453(11) 0.4939(18) 0.4965(17) 0.062(8) Uani 1 1 d . . . H1A H 0.6268 0.4930 0.5579 0.093 Uiso 1 1 calc R . . H1B H 0.6799 0.5356 0.5039 0.093 Uiso 1 1 calc R . . H1C H 0.6627 0.4385 0.4857 0.093 Uiso 1 1 calc R . . C2 C 0.6274(10) 0.5181(15) 0.2858(16) 0.045(6) Uani 1 1 d . . . H2A H 0.5984 0.5305 0.2218 0.068 Uiso 1 1 calc R . . H2B H 0.6461 0.4622 0.2826 0.068 Uiso 1 1 calc R . . H2C H 0.6620 0.5598 0.2982 0.068 Uiso 1 1 calc R . . C3 C 0.5316(12) 0.4247(15) 0.368(2) 0.054(7) Uani 1 1 d . . . H3A H 0.5147 0.4169 0.2952 0.064 Uiso 1 1 calc R . . H3B H 0.5584 0.3754 0.3929 0.064 Uiso 1 1 calc R . . C4 C 0.4738(10) 0.4310(15) 0.4258(13) 0.036(6) Uani 1 1 d . . . H4A H 0.4904 0.4318 0.4995 0.044 Uiso 1 1 calc R . . H4B H 0.4453 0.3817 0.4098 0.044 Uiso 1 1 calc R . . C5 C 0.3645(10) 0.5330(19) 0.4722(19) 0.065(8) Uani 1 1 d . . . H5A H 0.3380 0.5834 0.4568 0.097 Uiso 1 1 calc R . . H5B H 0.3865 0.5344 0.5430 0.097 Uiso 1 1 calc R . . H5C H 0.3369 0.4832 0.4604 0.097 Uiso 1 1 calc R . . C6 C 0.3814(11) 0.4989(18) 0.2622(19) 0.066(9) Uani 1 1 d . . . H6A H 0.3544 0.5460 0.2330 0.100 Uiso 1 1 calc R . . H6B H 0.3540 0.4506 0.2693 0.100 Uiso 1 1 calc R . . H6C H 0.4113 0.4842 0.2177 0.100 Uiso 1 1 calc R . . C7 C 0.3390(13) 0.7200(16) 0.0272(18) 0.057(7) Uani 1 1 d . . . H7A H 0.3050 0.7075 0.0653 0.086 Uiso 1 1 calc R . . H7B H 0.3641 0.6692 0.0218 0.086 Uiso 1 1 calc R . . H7C H 0.3194 0.7396 -0.0405 0.086 Uiso 1 1 calc R . . C8 C 0.4515(12) 0.8183(16) 0.013(2) 0.061(8) Uani 1 1 d . . . H8A H 0.4824 0.8614 0.0428 0.091 Uiso 1 1 calc R . . H8B H 0.4295 0.8362 -0.0539 0.091 Uiso 1 1 calc R . . H8C H 0.4745 0.7657 0.0076 0.091 Uiso 1 1 calc R . . C9 C 0.3406(12) 0.8994(17) 0.0735(18) 0.062(8) Uani 1 1 d . . . H9A H 0.3681 0.9492 0.0702 0.075 Uiso 1 1 calc R . . H9B H 0.3098 0.8949 0.0086 0.075 Uiso 1 1 calc R . . C10 C 0.3031(10) 0.9102(16) 0.1605(16) 0.046(6) Uani 1 1 d . . . H10A H 0.2710 0.8645 0.1578 0.055 Uiso 1 1 calc R . . H10B H 0.2795 0.9641 0.1526 0.055 Uiso 1 1 calc R . . C11 C 0.3057(12) 0.9117(18) 0.378(2) 0.065(8) Uani 1 1 d . . . H11A H 0.3317 0.9094 0.4459 0.098 Uiso 1 1 calc R . . H11B H 0.2762 0.8638 0.3671 0.098 Uiso 1 1 calc R . . H11C H 0.2808 0.9638 0.3691 0.098 Uiso 1 1 calc R . . C12 C 0.3956(12) 1.0137(15) 0.283(2) 0.067(9) Uani 1 1 d . . . H12A H 0.4277 1.0221 0.3446 0.101 Uiso 1 1 calc R . . H12B H 0.3619 1.0563 0.2782 0.101 Uiso 1 1 calc R . . H12C H 0.4166 1.0184 0.2240 0.101 Uiso 1 1 calc R . . C13 C 0.6084(13) 1.0400(16) 0.4537(19) 0.065(8) Uani 1 1 d . . . H13A H 0.5746 1.0535 0.4917 0.098 Uiso 1 1 calc R . . H13B H 0.5926 1.0510 0.3818 0.098 Uiso 1 1 calc R . . H13C H 0.6464 1.0749 0.4779 0.098 Uiso 1 1 calc R . . C14 C 0.6938(11) 0.917(2) 0.395(2) 0.072(9) Uani 1 1 d . . . H14A H 0.7089 0.8584 0.4007 0.107 Uiso 1 1 calc R . . H14B H 0.7300 0.9542 0.4195 0.107 Uiso 1 1 calc R . . H14C H 0.6761 0.9292 0.3239 0.107 Uiso 1 1 calc R . . C15 C 0.6756(11) 0.9291(17) 0.6055(15) 0.056(8) Uani 1 1 d . . . H15A H 0.7091 0.8849 0.6126 0.067 Uiso 1 1 calc R . . H15B H 0.6975 0.9835 0.6221 0.067 Uiso 1 1 calc R . . C16 C 0.6309(10) 0.9120(17) 0.6786(18) 0.052(7) Uani 1 1 d . . . H16A H 0.6010 0.9598 0.6783 0.062 Uiso 1 1 calc R . . H16B H 0.6565 0.9061 0.7478 0.062 Uiso 1 1 calc R . . C17 C 0.6427(11) 0.7326(15) 0.6897(19) 0.052(7) Uani 1 1 d . . . H17A H 0.6767 0.7328 0.6496 0.078 Uiso 1 1 calc R . . H17B H 0.6220 0.6775 0.6852 0.078 Uiso 1 1 calc R . . H17C H 0.6614 0.7449 0.7603 0.078 Uiso 1 1 calc R . . C18 C 0.5237(12) 0.8017(16) 0.7242(19) 0.058(8) Uani 1 1 d . . . H18A H 0.4887 0.8421 0.7038 0.087 Uiso 1 1 calc R . . H18B H 0.5447 0.8127 0.7941 0.087 Uiso 1 1 calc R . . H18C H 0.5060 0.7448 0.7188 0.087 Uiso 1 1 calc R . . C100 C 0.6923(10) 0.7413(17) 0.1441(16) 0.056(7) Uiso 1 1 d D . . C101 C 0.7386(12) 0.7400(18) 0.2343(19) 0.072(8) Uiso 1 1 d D . . H101 H 0.7249 0.7356 0.2971 0.086 Uiso 1 1 calc R . . C102 C 0.8073(16) 0.745(2) 0.233(3) 0.089(10) Uiso 1 1 d . . . H102 H 0.8384 0.7369 0.2927 0.107 Uiso 1 1 calc R . . C103 C 0.826(2) 0.763(3) 0.144(3) 0.129(15) Uiso 1 1 d . . . H103 H 0.8702 0.7748 0.1452 0.155 Uiso 1 1 calc R . . C104 C 0.7849(12) 0.763(2) 0.055(3) 0.091(10) Uiso 1 1 d D . . H104 H 0.8009 0.7671 -0.0061 0.109 Uiso 1 1 calc R . . C105 C 0.7174(11) 0.7571(16) 0.0516(17) 0.054(7) Uiso 1 1 d D . . H105 H 0.6883 0.7635 -0.0108 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0245(9) 0.0371(11) 0.0194(9) 0.0019(9) 0.0040(7) 0.0010(9) Mo2 0.0221(9) 0.0370(12) 0.0230(10) 0.0032(9) 0.0026(7) -0.0009(9) Mo3 0.0222(9) 0.0365(11) 0.0270(10) -0.0007(9) 0.0025(7) -0.0005(9) Fe1 0.0265(16) 0.049(2) 0.0249(16) 0.0054(15) 0.0098(13) -0.0016(14) S1 0.018(3) 0.044(4) 0.031(3) 0.002(3) 0.004(2) 0.000(3) S2 0.040(3) 0.042(4) 0.021(3) -0.002(3) 0.005(2) 0.002(3) S3 0.026(3) 0.051(4) 0.025(3) -0.002(3) 0.006(2) 0.002(3) S4 0.027(3) 0.056(4) 0.030(3) 0.006(3) 0.000(3) -0.012(3) S100 0.062(5) 0.177(10) 0.043(4) -0.020(5) 0.026(3) -0.021(5) Cl1 0.054(4) 0.051(4) 0.024(3) 0.006(3) 0.009(3) 0.000(3) Cl2 0.024(3) 0.057(4) 0.047(3) 0.002(3) 0.012(2) -0.006(3) Cl3 0.046(3) 0.052(4) 0.044(4) -0.005(3) 0.008(3) 0.012(3) P1 0.031(3) 0.053(4) 0.028(3) -0.004(3) 0.004(3) 0.009(3) P2 0.046(4) 0.044(4) 0.032(4) 0.005(3) 0.006(3) -0.006(3) P3 0.042(3) 0.052(4) 0.022(3) 0.005(3) -0.002(3) -0.012(3) P4 0.036(3) 0.048(4) 0.046(4) -0.001(3) -0.007(3) 0.000(3) P5 0.035(3) 0.041(4) 0.046(4) -0.001(3) 0.001(3) -0.007(3) P6 0.043(4) 0.045(4) 0.044(4) -0.004(3) 0.009(3) -0.001(3) C1 0.071(17) 0.07(2) 0.036(15) -0.023(14) -0.007(13) 0.032(16) C2 0.050(13) 0.056(17) 0.028(12) -0.016(12) 0.000(11) 0.020(12) C3 0.072(16) 0.020(13) 0.067(18) 0.012(12) 0.008(14) 0.014(12) C4 0.062(15) 0.045(15) 0.004(10) 0.003(10) 0.012(10) -0.005(12) C5 0.036(13) 0.11(3) 0.051(17) -0.010(16) 0.018(12) 0.008(14) C6 0.052(16) 0.07(2) 0.069(19) -0.006(16) -0.021(14) -0.008(14) C7 0.083(19) 0.048(17) 0.040(15) 0.005(13) 0.010(13) -0.001(15) C8 0.067(17) 0.042(16) 0.08(2) -0.001(15) 0.021(15) -0.009(14) C9 0.073(18) 0.061(19) 0.046(16) 0.024(14) -0.006(14) 0.038(15) C10 0.036(12) 0.066(18) 0.037(13) 0.012(13) 0.013(10) -0.002(12) C11 0.054(15) 0.07(2) 0.08(2) -0.008(17) 0.051(15) 0.014(14) C12 0.065(17) 0.040(16) 0.08(2) -0.029(15) -0.028(15) -0.019(14) C13 0.09(2) 0.051(18) 0.043(16) 0.024(14) -0.007(15) -0.006(16) C14 0.046(15) 0.10(2) 0.08(2) 0.025(18) 0.019(14) -0.005(16) C15 0.060(16) 0.08(2) 0.020(12) -0.013(13) -0.022(12) -0.024(15) C16 0.036(12) 0.09(2) 0.043(14) -0.024(14) 0.031(11) -0.001(13) C17 0.048(14) 0.056(17) 0.054(16) 0.021(14) 0.014(12) 0.013(13) C18 0.067(16) 0.065(19) 0.043(15) -0.028(14) 0.012(13) 0.004(15) _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 S2 2.347(6) . ? Mo1 S1 2.368(6) . ? Mo1 S3 2.391(6) . ? Mo1 Cl1 2.509(6) . ? Mo1 P1 2.531(6) . ? Mo1 P2 2.562(7) . ? Mo1 Fe1 2.719(3) . ? Mo1 Mo3 2.796(3) . ? Mo1 Mo2 2.814(2) . ? Mo2 S1 2.360(6) . ? Mo2 S4 2.366(6) . ? Mo2 S2 2.388(6) . ? Mo2 Cl2 2.536(5) . ? Mo2 P3 2.545(6) . ? Mo2 P4 2.573(7) . ? Mo2 Fe1 2.718(3) . ? Mo2 Mo3 2.801(2) . ? Mo3 S1 2.353(5) . ? Mo3 S3 2.363(6) . ? Mo3 S4 2.406(6) . ? Mo3 P5 2.526(6) . ? Mo3 Cl3 2.533(6) . ? Mo3 P6 2.585(7) . ? Mo3 Fe1 2.739(4) . ? Fe1 S4 2.229(7) . ? Fe1 S3 2.243(6) . ? Fe1 S2 2.252(6) . ? Fe1 S100 2.270(8) . ? S100 C100 1.73(2) . ? P1 C2 1.78(2) . ? P1 C1 1.80(2) . ? P1 C3 1.83(2) . ? P2 C6 1.80(2) . ? P2 C4 1.83(2) . ? P2 C5 1.88(2) . ? P3 C8 1.78(3) . ? P3 C7 1.82(2) . ? P3 C9 1.85(2) . ? P4 C11 1.81(2) . ? P4 C12 1.82(2) . ? P4 C10 1.82(2) . ? P5 C13 1.76(2) . ? P5 C14 1.83(3) . ? P5 C15 1.844(19) . ? P6 C17 1.79(2) . ? P6 C18 1.80(3) . ? P6 C16 1.87(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.54(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.52(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.48(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C100 C101 1.381(17) . ? C100 C105 1.439(17) . ? C101 C102 1.43(4) . ? C101 H101 0.9300 . ? C102 C103 1.33(4) . ? C102 H102 0.9300 . ? C103 C104 1.32(4) . ? C103 H103 0.9300 . ? C104 C105 1.392(17) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? 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 S2 Mo1 S1 105.5(2) . . ? S2 Mo1 S3 100.8(2) . . ? S1 Mo1 S3 105.4(2) . . ? S2 Mo1 Cl1 159.2(2) . . ? S1 Mo1 Cl1 82.49(19) . . ? S3 Mo1 Cl1 95.36(19) . . ? S2 Mo1 P1 88.6(2) . . ? S1 Mo1 P1 162.9(2) . . ? S3 Mo1 P1 80.9(2) . . ? Cl1 Mo1 P1 81.0(2) . . ? S2 Mo1 P2 83.6(2) . . ? S1 Mo1 P2 93.7(2) . . ? S3 Mo1 P2 158.3(2) . . ? Cl1 Mo1 P2 76.68(19) . . ? P1 Mo1 P2 77.9(2) . . ? S2 Mo1 Fe1 52.15(16) . . ? S1 Mo1 Fe1 100.25(16) . . ? S3 Mo1 Fe1 51.59(14) . . ? Cl1 Mo1 Fe1 146.59(16) . . ? P1 Mo1 Fe1 96.11(17) . . ? P2 Mo1 Fe1 135.61(17) . . ? S2 Mo1 Mo3 101.15(17) . . ? S1 Mo1 Mo3 53.44(14) . . ? S3 Mo1 Mo3 53.52(15) . . ? Cl1 Mo1 Mo3 99.00(15) . . ? P1 Mo1 Mo3 134.34(15) . . ? P2 Mo1 Mo3 147.02(17) . . ? Fe1 Mo1 Mo3 59.55(9) . . ? S2 Mo1 Mo2 54.20(15) . . ? S1 Mo1 Mo2 53.34(14) . . ? S3 Mo1 Mo2 99.53(16) . . ? Cl1 Mo1 Mo2 135.67(15) . . ? P1 Mo1 Mo2 142.43(16) . . ? P2 Mo1 Mo2 100.16(15) . . ? Fe1 Mo1 Mo2 58.82(8) . . ? Mo3 Mo1 Mo2 59.91(6) . . ? S1 Mo2 S4 106.53(19) . . ? S1 Mo2 S2 104.5(2) . . ? S4 Mo2 S2 100.4(2) . . ? S1 Mo2 Cl2 83.14(18) . . ? S4 Mo2 Cl2 160.7(2) . . ? S2 Mo2 Cl2 93.0(2) . . ? S1 Mo2 P3 163.23(19) . . ? S4 Mo2 P3 86.8(2) . . ? S2 Mo2 P3 82.4(2) . . ? Cl2 Mo2 P3 81.23(19) . . ? S1 Mo2 P4 93.4(2) . . ? S4 Mo2 P4 84.6(2) . . ? S2 Mo2 P4 159.0(2) . . ? Cl2 Mo2 P4 78.0(2) . . ? P3 Mo2 P4 77.5(2) . . ? S1 Mo2 Fe1 100.48(14) . . ? S4 Mo2 Fe1 51.45(17) . . ? S2 Mo2 Fe1 51.85(15) . . ? Cl2 Mo2 Fe1 144.64(18) . . ? P3 Mo2 Fe1 95.78(16) . . ? P4 Mo2 Fe1 136.03(18) . . ? S1 Mo2 Mo3 53.42(13) . . ? S4 Mo2 Mo3 54.73(14) . . ? S2 Mo2 Mo3 99.97(14) . . ? Cl2 Mo2 Mo3 136.46(15) . . ? P3 Mo2 Mo3 141.40(16) . . ? P4 Mo2 Mo3 99.54(15) . . ? Fe1 Mo2 Mo3 59.49(8) . . ? S1 Mo2 Mo1 53.61(14) . . ? S4 Mo2 Mo1 100.11(15) . . ? S2 Mo2 Mo1 52.88(14) . . ? Cl2 Mo2 Mo1 99.05(15) . . ? P3 Mo2 Mo1 135.31(17) . . ? P4 Mo2 Mo1 146.78(17) . . ? Fe1 Mo2 Mo1 58.84(8) . . ? Mo3 Mo2 Mo1 59.72(6) . . ? S1 Mo3 S3 106.8(2) . . ? S1 Mo3 S4 105.46(18) . . ? S3 Mo3 S4 99.0(2) . . ? S1 Mo3 P5 162.1(2) . . ? S3 Mo3 P5 87.1(2) . . ? S4 Mo3 P5 82.8(2) . . ? S1 Mo3 Cl3 82.4(2) . . ? S3 Mo3 Cl3 160.54(18) . . ? S4 Mo3 Cl3 94.8(2) . . ? P5 Mo3 Cl3 81.0(2) . . ? S1 Mo3 P6 91.7(2) . . ? S3 Mo3 P6 85.5(2) . . ? S4 Mo3 P6 159.9(2) . . ? P5 Mo3 P6 77.9(2) . . ? Cl3 Mo3 P6 76.9(2) . . ? S1 Mo3 Fe1 100.05(16) . . ? S3 Mo3 Fe1 51.51(14) . . ? S4 Mo3 Fe1 50.85(17) . . ? P5 Mo3 Fe1 97.46(18) . . ? Cl3 Mo3 Fe1 145.25(16) . . ? P6 Mo3 Fe1 137.06(18) . . ? S1 Mo3 Mo1 53.93(15) . . ? S3 Mo3 Mo1 54.44(15) . . ? S4 Mo3 Mo1 99.61(17) . . ? P5 Mo3 Mo1 141.52(17) . . ? Cl3 Mo3 Mo1 136.24(15) . . ? P6 Mo3 Mo1 98.87(17) . . ? Fe1 Mo3 Mo1 58.83(8) . . ? S1 Mo3 Mo2 53.64(14) . . ? S3 Mo3 Mo2 100.59(14) . . ? S4 Mo3 Mo2 53.40(13) . . ? P5 Mo3 Mo2 136.15(17) . . ? Cl3 Mo3 Mo2 98.64(14) . . ? P6 Mo3 Mo2 145.24(17) . . ? Fe1 Mo3 Mo2 58.74(8) . . ? Mo1 Mo3 Mo2 60.37(6) . . ? S4 Fe1 S3 108.3(2) . . ? S4 Fe1 S2 109.2(2) . . ? S3 Fe1 S2 108.6(2) . . ? S4 Fe1 S100 115.7(3) . . ? S3 Fe1 S100 120.2(3) . . ? S2 Fe1 S100 93.3(3) . . ? S4 Fe1 Mo2 56.10(16) . . ? S3 Fe1 Mo2 106.41(18) . . ? S2 Fe1 Mo2 56.50(17) . . ? S100 Fe1 Mo2 131.2(2) . . ? S4 Fe1 Mo1 106.7(2) . . ? S3 Fe1 Mo1 56.64(16) . . ? S2 Fe1 Mo1 55.41(16) . . ? S100 Fe1 Mo1 134.1(3) . . ? Mo2 Fe1 Mo1 62.34(8) . . ? S4 Fe1 Mo3 56.82(17) . . ? S3 Fe1 Mo3 55.55(16) . . ? S2 Fe1 Mo3 105.47(19) . . ? S100 Fe1 Mo3 161.2(3) . . ? Mo2 Fe1 Mo3 61.76(8) . . ? Mo1 Fe1 Mo3 61.62(9) . . ? Mo3 S1 Mo2 72.94(17) . . ? Mo3 S1 Mo1 72.63(16) . . ? Mo2 S1 Mo1 73.05(17) . . ? Fe1 S2 Mo1 72.44(18) . . ? Fe1 S2 Mo2 71.65(19) . . ? Mo1 S2 Mo2 72.91(17) . . ? Fe1 S3 Mo3 72.94(18) . . ? Fe1 S3 Mo1 71.77(16) . . ? Mo3 S3 Mo1 72.04(15) . . ? Fe1 S4 Mo2 72.4(2) . . ? Fe1 S4 Mo3 72.33(19) . . ? Mo2 S4 Mo3 71.88(18) . . ? C100 S100 Fe1 117.1(8) . . ? C2 P1 C1 101.0(11) . . ? C2 P1 C3 103.7(12) . . ? C1 P1 C3 103.0(12) . . ? C2 P1 Mo1 118.5(8) . . ? C1 P1 Mo1 118.2(8) . . ? C3 P1 Mo1 110.4(8) . . ? C6 P2 C4 101.4(11) . . ? C6 P2 C5 104.7(12) . . ? C4 P2 C5 104.3(11) . . ? C6 P2 Mo1 120.0(9) . . ? C4 P2 Mo1 106.8(7) . . ? C5 P2 Mo1 117.4(9) . . ? C8 P3 C7 103.6(12) . . ? C8 P3 C9 104.4(12) . . ? C7 P3 C9 103.1(12) . . ? C8 P3 Mo2 118.1(9) . . ? C7 P3 Mo2 115.5(8) . . ? C9 P3 Mo2 110.4(8) . . ? C11 P4 C12 106.9(13) . . ? C11 P4 C10 104.1(12) . . ? C12 P4 C10 99.5(11) . . ? C11 P4 Mo2 118.4(10) . . ? C12 P4 Mo2 118.0(9) . . ? C10 P4 Mo2 107.4(9) . . ? C13 P5 C14 103.9(14) . . ? C13 P5 C15 102.5(12) . . ? C14 P5 C15 103.8(12) . . ? C13 P5 Mo3 117.2(9) . . ? C14 P5 Mo3 117.0(10) . . ? C15 P5 Mo3 110.6(8) . . ? C17 P6 C18 103.0(12) . . ? C17 P6 C16 100.9(11) . . ? C18 P6 C16 107.9(11) . . ? C17 P6 Mo3 120.2(9) . . ? C18 P6 Mo3 117.0(8) . . ? C16 P6 Mo3 106.2(8) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 110.7(18) . . ? C4 C3 H3A 109.5 . . ? P1 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 P2 109.4(15) . . ? C3 C4 H4A 109.8 . . ? P2 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? P2 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P3 110.6(17) . . ? C10 C9 H9A 109.5 . . ? P3 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? P3 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 C10 P4 110.5(15) . . ? C9 C10 H10A 109.6 . . ? P4 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? P4 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P5 C13 H13A 109.5 . . ? P5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P5 C14 H14A 109.5 . . ? P5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 P5 111.2(16) . . ? C16 C15 H15A 109.4 . . ? P5 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? P5 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 P6 110.2(16) . . ? C15 C16 H16A 109.6 . . ? P6 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? P6 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? P6 C17 H17A 109.5 . . ? P6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P6 C18 H18A 109.5 . . ? P6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C101 C100 C105 116(2) . . ? C101 C100 S100 127.3(19) . . ? C105 C100 S100 117.0(16) . . ? C100 C101 C102 121(3) . . ? C100 C101 H101 119.5 . . ? C102 C101 H101 119.5 . . ? C103 C102 C101 119(3) . . ? C103 C102 H102 120.6 . . ? C101 C102 H102 120.6 . . ? C104 C103 C102 123(4) . . ? C104 C103 H103 118.6 . . ? C102 C103 H103 118.6 . . ? C103 C104 C105 120(3) . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C104 C105 C100 121(2) . . ? C104 C105 H105 119.7 . . ? C100 C105 H105 119.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.714 _refine_diff_density_min -1.459 _refine_diff_density_rms 0.213 # Attachment 'compound_3.CIF' data_str1066m _database_code_depnum_ccdc_archive 'CCDC 755400' #TrackingRef 'compound_3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H68 Fe Mo3 P6 S8' _chemical_formula_weight 1358.93 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' P P 0.1023 0.0942 '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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' _symmetry_Int_Tables_number 15 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 24.24(2) _cell_length_b 12.065(11) _cell_length_c 39.59(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.68(2) _cell_angle_gamma 90.00 _cell_volume 11577(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 709 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 20.55 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5520 _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783017 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31783 _diffrn_reflns_av_R_equivalents 0.1646 _diffrn_reflns_av_sigmaI/netI 0.2056 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10184 _reflns_number_gt 4868 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Single-crystals of compound 3 were all weakly diffracting, so that a large proportion of essentially "unobserved" reflections are being used in the refinement. This fact results in poor quality of the data and consequently high R(int) values. The following bond distance C(41)-C(42), was constrained to fixed values (typically 1.42 (2) characteristic of aromatic C-C bond distances). ; _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^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10184 _refine_ls_number_parameters 541 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1689 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1254 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.13578(4) 0.36638(8) 0.16602(2) 0.0243(3) Uani 1 1 d . . . Mo2 Mo 0.17009(4) 0.19333(8) 0.12206(2) 0.0238(3) Uani 1 1 d . . . Mo3 Mo 0.22400(4) 0.40330(8) 0.12006(2) 0.0231(3) Uani 1 1 d . . . Fe1 Fe 0.23636(6) 0.26261(13) 0.17459(4) 0.0286(4) Uani 1 1 d . . . S1 S 0.13009(11) 0.3653(2) 0.10553(7) 0.0258(7) Uani 1 1 d . . . S2 S 0.26781(11) 0.2271(2) 0.12260(8) 0.0317(7) Uani 1 1 d . . . S3 S 0.15452(12) 0.1782(2) 0.18094(7) 0.0313(7) Uani 1 1 d . . . S4 S 0.22322(11) 0.4453(2) 0.17940(7) 0.0290(7) Uani 1 1 d . . . S5 S 0.03016(12) 0.3260(3) 0.16658(8) 0.0397(8) Uani 1 1 d . . . S6 S 0.17556(13) 0.1403(3) 0.05901(8) 0.0388(8) Uani 1 1 d . . . S7 S 0.20367(13) 0.6091(2) 0.10636(8) 0.0374(8) Uani 1 1 d . . . S8 S 0.29019(16) 0.1852(3) 0.21628(9) 0.0578(10) Uani 1 1 d . . . P1 P 0.11644(13) 0.3754(3) 0.22971(8) 0.0345(8) Uani 1 1 d . . . P2 P 0.10106(13) 0.5682(3) 0.17503(8) 0.0346(8) Uani 1 1 d . . . P3 P 0.20357(13) -0.0068(3) 0.12575(9) 0.0375(8) Uani 1 1 d . . . P4 P 0.07810(13) 0.0785(3) 0.11791(8) 0.0364(8) Uani 1 1 d . . . P5 P 0.32027(13) 0.4919(3) 0.12458(9) 0.0433(9) Uani 1 1 d . . . P6 P 0.26002(13) 0.4049(3) 0.05812(8) 0.0346(8) Uani 1 1 d . . . C1 C 0.0737(5) 0.2666(11) 0.2471(3) 0.060(4) Uani 1 1 d . . . H1A H 0.0895 0.1957 0.2420 0.090 Uiso 1 1 calc R . . H1B H 0.0373 0.2711 0.2374 0.090 Uiso 1 1 calc R . . H1C H 0.0716 0.2753 0.2711 0.090 Uiso 1 1 calc R . . C2 C 0.1742(5) 0.3747(11) 0.2595(3) 0.060(4) Uani 1 1 d . . . H2A H 0.1963 0.3097 0.2559 0.090 Uiso 1 1 calc R . . H2B H 0.1606 0.3742 0.2821 0.090 Uiso 1 1 calc R . . H2C H 0.1963 0.4397 0.2561 0.090 Uiso 1 1 calc R . . C3 C 0.0814(5) 0.5042(10) 0.2411(3) 0.051(4) Uani 1 1 d . . . H3A H 0.0536 0.4876 0.2578 0.061 Uiso 1 1 calc R . . H3B H 0.1081 0.5537 0.2516 0.061 Uiso 1 1 calc R . . C4 C 0.0540(5) 0.5641(10) 0.2115(3) 0.045(4) Uani 1 1 d . . . H4A H 0.0446 0.6391 0.2181 0.054 Uiso 1 1 calc R . . H4B H 0.0202 0.5260 0.2051 0.054 Uiso 1 1 calc R . . C5 C 0.1519(5) 0.6706(9) 0.1892(3) 0.046(3) Uani 1 1 d . . . H5A H 0.1758 0.6380 0.2059 0.069 Uiso 1 1 calc R . . H5B H 0.1332 0.7332 0.1987 0.069 Uiso 1 1 calc R . . H5C H 0.1734 0.6945 0.1703 0.069 Uiso 1 1 calc R . . C6 C 0.0612(5) 0.6476(10) 0.1439(3) 0.055(4) Uani 1 1 d . . . H6A H 0.0327 0.6016 0.1344 0.083 Uiso 1 1 calc R . . H6B H 0.0852 0.6722 0.1262 0.083 Uiso 1 1 calc R . . H6C H 0.0449 0.7107 0.1546 0.083 Uiso 1 1 calc R . . C7 C 0.2354(6) -0.0532(10) 0.1656(3) 0.061(4) Uani 1 1 d . . . H7A H 0.2123 -0.0327 0.1841 0.091 Uiso 1 1 calc R . . H7B H 0.2709 -0.0189 0.1684 0.091 Uiso 1 1 calc R . . H7C H 0.2397 -0.1323 0.1652 0.091 Uiso 1 1 calc R . . C8 C 0.2536(5) -0.0520(10) 0.0947(3) 0.053(4) Uani 1 1 d . . . H8A H 0.2852 -0.0040 0.0955 0.080 Uiso 1 1 calc R . . H8B H 0.2372 -0.0495 0.0725 0.080 Uiso 1 1 calc R . . H8C H 0.2650 -0.1266 0.0997 0.080 Uiso 1 1 calc R . . C9 C 0.1455(5) -0.1051(10) 0.1198(4) 0.053(4) Uani 1 1 d . . . H9A H 0.1589 -0.1705 0.1082 0.064 Uiso 1 1 calc R . . H9B H 0.1325 -0.1282 0.1418 0.064 Uiso 1 1 calc R . . C10 C 0.0972(5) -0.0569(9) 0.0997(3) 0.043(3) Uani 1 1 d . . . H10A H 0.0660 -0.1071 0.1005 0.052 Uiso 1 1 calc R . . H10B H 0.1075 -0.0476 0.0763 0.052 Uiso 1 1 calc R . . C11 C 0.0180(5) 0.1173(10) 0.0924(3) 0.054(4) Uani 1 1 d . . . H11A H 0.0299 0.1434 0.0708 0.081 Uiso 1 1 calc R . . H11B H -0.0019 0.1751 0.1037 0.081 Uiso 1 1 calc R . . H11C H -0.0055 0.0540 0.0895 0.081 Uiso 1 1 calc R . . C12 C 0.0460(5) 0.0334(11) 0.1572(3) 0.054(4) Uani 1 1 d . . . H12A H 0.0741 0.0098 0.1729 0.080 Uiso 1 1 calc R . . H12B H 0.0214 -0.0272 0.1525 0.080 Uiso 1 1 calc R . . H12C H 0.0257 0.0938 0.1667 0.080 Uiso 1 1 calc R . . C13 C 0.3743(5) 0.4063(15) 0.1409(5) 0.107(7) Uani 1 1 d . . . H13A H 0.3648 0.3810 0.1631 0.160 Uiso 1 1 calc R . . H13B H 0.4079 0.4481 0.1421 0.160 Uiso 1 1 calc R . . H13C H 0.3792 0.3436 0.1263 0.160 Uiso 1 1 calc R . . C14 C 0.3273(6) 0.6205(13) 0.1489(4) 0.095(6) Uani 1 1 d . . . H14A H 0.2997 0.6726 0.1415 0.142 Uiso 1 1 calc R . . H14B H 0.3633 0.6514 0.1455 0.142 Uiso 1 1 calc R . . H14C H 0.3224 0.6050 0.1725 0.142 Uiso 1 1 calc R . . C15 C 0.3485(6) 0.5251(12) 0.0829(3) 0.067(5) Uani 1 1 d . . . H15A H 0.3653 0.5980 0.0841 0.081 Uiso 1 1 calc R . . H15B H 0.3775 0.4723 0.0780 0.081 Uiso 1 1 calc R . . C16 C 0.3068(5) 0.5241(10) 0.0539(3) 0.042(3) Uani 1 1 d . . . H16A H 0.3261 0.5194 0.0326 0.051 Uiso 1 1 calc R . . H16B H 0.2857 0.5924 0.0539 0.051 Uiso 1 1 calc R . . C17 C 0.2176(5) 0.4173(11) 0.0197(3) 0.059(4) Uani 1 1 d . . . H17A H 0.1912 0.4757 0.0225 0.088 Uiso 1 1 calc R . . H17B H 0.1987 0.3487 0.0156 0.088 Uiso 1 1 calc R . . H17C H 0.2408 0.4340 0.0009 0.088 Uiso 1 1 calc R . . C18 C 0.3049(5) 0.2906(10) 0.0472(3) 0.057(4) Uani 1 1 d . . . H18A H 0.3297 0.2757 0.0657 0.085 Uiso 1 1 calc R . . H18B H 0.3257 0.3097 0.0275 0.085 Uiso 1 1 calc R . . H18C H 0.2831 0.2259 0.0425 0.085 Uiso 1 1 calc R . . C20 C -0.0145(5) 0.4036(11) 0.1400(3) 0.043(3) Uani 1 1 d . . . C21 C -0.0602(6) 0.4574(13) 0.1547(4) 0.072(5) Uani 1 1 d . . . H21 H -0.0661 0.4497 0.1778 0.086 Uiso 1 1 calc R . . C22 C -0.0955(6) 0.5203(17) 0.1359(5) 0.095(7) Uani 1 1 d . . . H22 H -0.1250 0.5544 0.1464 0.114 Uiso 1 1 calc R . . C23 C -0.0888(6) 0.5357(14) 0.1005(6) 0.094(7) Uani 1 1 d . . . H23 H -0.1119 0.5820 0.0879 0.113 Uiso 1 1 calc R . . C24 C -0.0466(7) 0.4787(15) 0.0859(4) 0.093(6) Uani 1 1 d . . . H24 H -0.0431 0.4819 0.0626 0.111 Uiso 1 1 calc R . . C25 C -0.0081(5) 0.4154(12) 0.1045(4) 0.059(4) Uani 1 1 d . . . H25 H 0.0213 0.3816 0.0937 0.071 Uiso 1 1 calc R . . C26 C 0.1675(6) 0.6391(9) 0.0680(3) 0.038(3) Uani 1 1 d . . . C27 C 0.1169(6) 0.5981(11) 0.0584(3) 0.053(4) Uani 1 1 d . . . H27 H 0.0999 0.5479 0.0727 0.063 Uiso 1 1 calc R . . C28 C 0.0894(7) 0.6264(14) 0.0288(4) 0.085(5) Uani 1 1 d . . . H28 H 0.0547 0.5980 0.0235 0.102 Uiso 1 1 calc R . . C29 C 0.1168(8) 0.7009(16) 0.0069(5) 0.096(6) Uani 1 1 d . . . H29 H 0.0998 0.7207 -0.0134 0.116 Uiso 1 1 calc R . . C30 C 0.1661(9) 0.7433(15) 0.0145(5) 0.094(6) Uani 1 1 d . . . H30 H 0.1825 0.7922 -0.0005 0.113 Uiso 1 1 calc R . . C31 C 0.1945(6) 0.7151(10) 0.0456(4) 0.055(4) Uani 1 1 d . . . H31 H 0.2289 0.7449 0.0508 0.066 Uiso 1 1 calc R . . C32 C 0.1175(5) 0.1615(10) 0.0326(3) 0.037(3) Uani 1 1 d . . . C33 C 0.0914(5) 0.2647(12) 0.0271(3) 0.055(4) Uani 1 1 d . . . H33 H 0.1020 0.3265 0.0396 0.066 Uiso 1 1 calc R . . C34 C 0.0491(6) 0.2730(15) 0.0025(4) 0.077(5) Uani 1 1 d . . . H34 H 0.0325 0.3411 -0.0018 0.093 Uiso 1 1 calc R . . C35 C 0.0324(7) 0.1801(18) -0.0152(4) 0.087(6) Uani 1 1 d . . . H35 H 0.0037 0.1861 -0.0309 0.104 Uiso 1 1 calc R . . C36 C 0.0566(6) 0.0809(15) -0.0103(4) 0.069(5) Uani 1 1 d . . . H36 H 0.0456 0.0195 -0.0229 0.083 Uiso 1 1 calc R . . C37 C 0.0977(5) 0.0720(11) 0.0135(3) 0.045(4) Uani 1 1 d . . . H37 H 0.1134 0.0026 0.0173 0.054 Uiso 1 1 calc R . . C38 C 0.3446(5) 0.2847(10) 0.2242(3) 0.043(3) Uani 1 1 d . . . C39 C 0.3327(6) 0.3812(12) 0.2404(3) 0.062(4) Uani 1 1 d . . . H39 H 0.2964 0.3949 0.2465 0.074 Uiso 1 1 calc R . . C40 C 0.3728(7) 0.4600(14) 0.2481(4) 0.084(6) Uani 1 1 d . . . H40 H 0.3642 0.5248 0.2596 0.101 Uiso 1 1 calc R . . C41 C 0.4246(7) 0.4381(15) 0.2380(5) 0.093(6) Uani 1 1 d D . . H41 H 0.4517 0.4912 0.2423 0.111 Uiso 1 1 calc R . . C42 C 0.4404(6) 0.3399(14) 0.2215(4) 0.076(5) Uani 1 1 d D . . H42 H 0.4768 0.3270 0.2155 0.091 Uiso 1 1 calc R . . C43 C 0.3987(6) 0.2622(12) 0.2144(4) 0.061(4) Uani 1 1 d . . . H43 H 0.4070 0.1964 0.2033 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0278(6) 0.0229(6) 0.0222(6) -0.0005(4) 0.0026(4) 0.0002(4) Mo2 0.0265(6) 0.0203(6) 0.0247(6) -0.0007(4) 0.0013(4) -0.0025(4) Mo3 0.0255(6) 0.0204(6) 0.0234(6) 0.0005(4) 0.0017(4) -0.0023(4) Fe1 0.0325(10) 0.0273(10) 0.0260(10) 0.0025(7) -0.0043(8) -0.0002(7) S1 0.0279(17) 0.0234(16) 0.0263(16) 0.0015(13) 0.0010(13) 0.0004(12) S2 0.0289(18) 0.0257(17) 0.0404(19) 0.0022(14) 0.0015(14) 0.0001(13) S3 0.0383(19) 0.0290(18) 0.0266(17) 0.0049(13) 0.0041(14) -0.0044(13) S4 0.0298(17) 0.0265(17) 0.0305(18) 0.0016(13) -0.0020(14) -0.0029(12) S5 0.0252(18) 0.049(2) 0.045(2) 0.0053(16) 0.0031(15) -0.0009(14) S6 0.044(2) 0.043(2) 0.0300(18) -0.0067(15) 0.0078(15) -0.0015(15) S7 0.056(2) 0.0235(18) 0.0330(18) 0.0031(14) 0.0018(16) -0.0026(14) S8 0.074(3) 0.041(2) 0.058(2) 0.0097(18) -0.033(2) -0.0016(18) P1 0.038(2) 0.038(2) 0.0274(18) 0.0003(15) 0.0057(15) 0.0007(15) P2 0.041(2) 0.033(2) 0.0305(19) 0.0010(15) 0.0056(15) 0.0038(15) P3 0.042(2) 0.0255(19) 0.045(2) -0.0013(15) -0.0021(16) 0.0048(14) P4 0.0331(19) 0.034(2) 0.042(2) 0.0005(16) 0.0016(16) -0.0109(14) P5 0.036(2) 0.050(2) 0.044(2) 0.0049(17) -0.0018(17) -0.0193(16) P6 0.042(2) 0.034(2) 0.0281(18) -0.0005(15) 0.0098(15) -0.0015(15) C1 0.067(10) 0.067(11) 0.047(9) 0.014(7) 0.017(8) -0.021(8) C2 0.049(9) 0.069(11) 0.060(10) 0.004(8) -0.009(7) 0.007(7) C3 0.080(10) 0.034(8) 0.038(9) 0.007(6) 0.018(7) 0.004(7) C4 0.056(9) 0.048(9) 0.031(8) -0.017(6) 0.030(7) 0.006(6) C5 0.075(10) 0.033(8) 0.030(8) -0.014(6) -0.005(7) -0.003(6) C6 0.064(10) 0.040(9) 0.063(10) 0.012(7) 0.006(8) 0.007(7) C7 0.089(11) 0.029(8) 0.065(10) 0.006(7) -0.004(8) 0.012(7) C8 0.053(9) 0.034(8) 0.072(10) -0.029(7) 0.004(7) 0.013(6) C9 0.043(9) 0.031(8) 0.086(11) -0.015(7) 0.013(8) -0.008(6) C10 0.056(9) 0.027(8) 0.047(9) 0.007(6) -0.003(7) -0.001(6) C11 0.057(9) 0.051(10) 0.054(9) 0.007(7) 0.000(7) 0.000(7) C12 0.036(8) 0.074(11) 0.051(9) -0.004(8) 0.003(7) -0.026(7) C13 0.033(10) 0.135(18) 0.152(19) 0.051(14) -0.007(10) -0.011(10) C14 0.082(13) 0.101(15) 0.101(14) -0.052(11) -0.004(10) -0.039(10) C15 0.069(11) 0.079(12) 0.056(11) 0.005(8) 0.022(9) -0.028(8) C16 0.051(9) 0.038(8) 0.038(8) 0.006(6) 0.012(7) -0.009(6) C17 0.074(11) 0.063(10) 0.040(9) -0.009(7) 0.009(8) -0.011(8) C18 0.063(10) 0.048(10) 0.059(10) -0.004(7) 0.030(8) 0.004(7) C20 0.030(8) 0.059(9) 0.040(8) 0.008(7) -0.010(6) -0.008(6) C21 0.039(10) 0.081(13) 0.096(13) 0.000(10) 0.011(9) 0.014(8) C22 0.035(11) 0.15(2) 0.097(16) 0.031(14) -0.001(10) 0.015(10) C23 0.037(11) 0.081(13) 0.16(2) 0.009(14) -0.032(12) 0.028(9) C24 0.074(13) 0.116(16) 0.088(14) 0.049(12) -0.026(11) 0.007(11) C25 0.038(9) 0.081(12) 0.057(10) 0.005(8) -0.011(7) 0.001(8) C26 0.078(10) 0.015(7) 0.022(7) -0.005(5) 0.005(7) 0.012(6) C27 0.062(10) 0.056(10) 0.040(9) 0.015(7) 0.005(8) 0.015(8) C28 0.098(14) 0.077(13) 0.079(13) 0.020(11) -0.042(11) 0.002(10) C29 0.101(16) 0.093(16) 0.095(15) 0.043(12) -0.016(13) 0.030(12) C30 0.116(17) 0.088(15) 0.079(14) 0.043(11) 0.018(13) 0.023(13) C31 0.074(10) 0.028(8) 0.062(10) 0.016(7) 0.013(8) 0.007(7) C32 0.044(8) 0.044(9) 0.023(7) 0.002(6) 0.009(6) -0.008(6) C33 0.051(10) 0.072(12) 0.043(9) -0.016(8) 0.005(7) 0.001(8) C34 0.068(12) 0.107(15) 0.056(11) -0.014(10) -0.026(9) 0.022(10) C35 0.064(12) 0.15(2) 0.045(11) -0.022(12) -0.030(9) 0.005(12) C36 0.053(11) 0.097(15) 0.057(11) -0.025(10) 0.004(9) -0.013(9) C37 0.048(9) 0.059(10) 0.029(8) -0.008(7) 0.015(7) -0.010(7) C38 0.036(8) 0.037(9) 0.055(9) 0.005(7) -0.024(7) 0.004(6) C39 0.081(12) 0.052(11) 0.052(10) -0.006(8) -0.020(8) 0.001(9) C40 0.063(12) 0.085(14) 0.105(15) -0.054(11) -0.013(10) 0.010(10) C41 0.073(14) 0.094(16) 0.111(16) -0.023(12) -0.030(12) -0.006(11) C42 0.044(10) 0.087(14) 0.096(14) 0.026(11) -0.037(9) 0.009(9) C43 0.063(11) 0.057(10) 0.062(11) 0.015(8) -0.016(9) 0.014(8) _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 S4 2.378(3) . ? Mo1 S3 2.389(4) . ? Mo1 S1 2.397(4) . ? Mo1 P1 2.572(4) . ? Mo1 P2 2.602(4) . ? Mo1 S5 2.607(4) . ? Mo1 Fe1 2.758(3) . ? Mo1 Mo2 2.848(2) . ? Mo1 Mo3 2.859(2) . ? Mo2 S3 2.372(4) . ? Mo2 S1 2.378(3) . ? Mo2 S2 2.404(4) . ? Mo2 P3 2.551(4) . ? Mo2 S6 2.582(4) . ? Mo2 P4 2.629(4) . ? Mo2 Fe1 2.743(3) . ? Mo2 Mo3 2.852(2) . ? Mo3 S2 2.377(3) . ? Mo3 S1 2.386(3) . ? Mo3 S4 2.403(4) . ? Mo3 P5 2.571(4) . ? Mo3 S7 2.588(4) . ? Mo3 P6 2.612(4) . ? Mo3 Fe1 2.760(3) . ? Fe1 S4 2.235(4) . ? Fe1 S2 2.244(4) . ? Fe1 S3 2.247(4) . ? Fe1 S8 2.291(4) . ? S5 C20 1.769(12) . ? S6 C32 1.762(13) . ? S7 C26 1.780(12) . ? S8 C38 1.807(12) . ? P1 C1 1.813(11) . ? P1 C2 1.819(12) . ? P1 C3 1.831(12) . ? P2 C5 1.829(11) . ? P2 C6 1.829(12) . ? P2 C4 1.851(10) . ? P3 C8 1.822(11) . ? P3 C7 1.835(13) . ? P3 C9 1.854(12) . ? P4 C11 1.822(12) . ? P4 C12 1.829(12) . ? P4 C10 1.848(12) . ? P5 C13 1.783(15) . ? P5 C14 1.834(14) . ? P5 C15 1.837(13) . ? P6 C18 1.812(11) . ? P6 C17 1.832(13) . ? P6 C16 1.841(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.523(16) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.522(16) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.522(17) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C20 C21 1.415(16) . ? C20 C25 1.422(16) . ? C21 C22 1.36(2) . ? C21 H21 0.9300 . ? C22 C23 1.42(2) . ? C22 H22 0.9300 . ? C23 C24 1.37(2) . ? C23 H23 0.9300 . ? C24 C25 1.407(18) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.374(16) . ? C26 C31 1.440(16) . ? C27 C28 1.383(18) . ? C27 H27 0.9300 . ? C28 C29 1.42(2) . ? C28 H28 0.9300 . ? C29 C30 1.33(2) . ? C29 H29 0.9300 . ? C30 C31 1.44(2) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C37 1.399(16) . ? C32 C33 1.411(17) . ? C33 C34 1.411(18) . ? C33 H33 0.9300 . ? C34 C35 1.38(2) . ? C34 H34 0.9300 . ? C35 C36 1.35(2) . ? C35 H35 0.9300 . ? C36 C37 1.368(18) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.362(17) . ? C38 C43 1.400(17) . ? C39 C40 1.391(19) . ? C39 H39 0.9300 . ? C40 C41 1.350(19) . ? C40 H40 0.9300 . ? C41 C42 1.410(12) . ? C41 H41 0.9300 . ? C42 C43 1.404(19) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? 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 S4 Mo1 S3 99.15(11) . . ? S4 Mo1 S1 105.40(10) . . ? S3 Mo1 S1 104.48(10) . . ? S4 Mo1 P1 86.39(11) . . ? S3 Mo1 P1 80.45(10) . . ? S1 Mo1 P1 166.04(10) . . ? S4 Mo1 P2 83.33(11) . . ? S3 Mo1 P2 156.43(11) . . ? S1 Mo1 P2 97.32(10) . . ? P1 Mo1 P2 76.30(10) . . ? S4 Mo1 S5 161.12(11) . . ? S3 Mo1 S5 90.23(10) . . ? S1 Mo1 S5 87.85(10) . . ? P1 Mo1 S5 79.00(10) . . ? P2 Mo1 S5 81.64(11) . . ? S4 Mo1 Fe1 50.94(9) . . ? S3 Mo1 Fe1 51.15(8) . . ? S1 Mo1 Fe1 99.24(8) . . ? P1 Mo1 Fe1 94.00(9) . . ? P2 Mo1 Fe1 134.01(9) . . ? S5 Mo1 Fe1 141.34(10) . . ? S4 Mo1 Mo2 99.41(9) . . ? S3 Mo1 Mo2 52.99(9) . . ? S1 Mo1 Mo2 53.08(8) . . ? P1 Mo1 Mo2 133.44(9) . . ? P2 Mo1 Mo2 150.10(8) . . ? S5 Mo1 Mo2 99.32(9) . . ? Fe1 Mo1 Mo2 58.55(5) . . ? S4 Mo1 Mo3 53.69(9) . . ? S3 Mo1 Mo3 99.43(8) . . ? S1 Mo1 Mo3 53.11(8) . . ? P1 Mo1 Mo3 139.78(9) . . ? P2 Mo1 Mo3 100.78(8) . . ? S5 Mo1 Mo3 140.96(9) . . ? Fe1 Mo1 Mo3 58.81(6) . . ? Mo2 Mo1 Mo3 59.96(5) . . ? S3 Mo2 S1 105.58(10) . . ? S3 Mo2 S2 99.94(11) . . ? S1 Mo2 S2 104.65(11) . . ? S3 Mo2 P3 85.69(11) . . ? S1 Mo2 P3 165.86(11) . . ? S2 Mo2 P3 81.22(11) . . ? S3 Mo2 S6 160.25(11) . . ? S1 Mo2 S6 88.60(11) . . ? S2 Mo2 S6 89.35(11) . . ? P3 Mo2 S6 78.50(11) . . ? S3 Mo2 P4 82.88(11) . . ? S1 Mo2 P4 95.72(12) . . ? S2 Mo2 P4 157.70(11) . . ? P3 Mo2 P4 76.93(12) . . ? S6 Mo2 P4 82.07(10) . . ? S3 Mo2 Fe1 51.49(9) . . ? S1 Mo2 Fe1 100.14(9) . . ? S2 Mo2 Fe1 51.19(9) . . ? P3 Mo2 Fe1 93.55(10) . . ? S6 Mo2 Fe1 140.54(9) . . ? P4 Mo2 Fe1 134.17(9) . . ? S3 Mo2 Mo1 53.52(8) . . ? S1 Mo2 Mo1 53.69(9) . . ? S2 Mo2 Mo1 99.50(8) . . ? P3 Mo2 Mo1 138.93(9) . . ? S6 Mo2 Mo1 142.29(9) . . ? P4 Mo2 Mo1 99.84(9) . . ? Fe1 Mo2 Mo1 59.08(6) . . ? S3 Mo2 Mo3 100.03(8) . . ? S1 Mo2 Mo3 53.35(9) . . ? S2 Mo2 Mo3 52.96(7) . . ? P3 Mo2 Mo3 134.17(10) . . ? S6 Mo2 Mo3 99.47(8) . . ? P4 Mo2 Mo3 148.76(8) . . ? Fe1 Mo2 Mo3 59.07(5) . . ? Mo1 Mo2 Mo3 60.21(6) . . ? S2 Mo3 S1 105.23(11) . . ? S2 Mo3 S4 98.96(11) . . ? S1 Mo3 S4 104.93(10) . . ? S2 Mo3 P5 87.93(12) . . ? S1 Mo3 P5 163.62(11) . . ? S4 Mo3 P5 82.07(11) . . ? S2 Mo3 S7 161.90(10) . . ? S1 Mo3 S7 87.44(10) . . ? S4 Mo3 S7 89.94(10) . . ? P5 Mo3 S7 77.66(12) . . ? S2 Mo3 P6 83.81(11) . . ? S1 Mo3 P6 95.95(11) . . ? S4 Mo3 P6 157.27(11) . . ? P5 Mo3 P6 75.47(11) . . ? S7 Mo3 P6 82.02(10) . . ? S2 Mo3 Fe1 51.15(9) . . ? S1 Mo3 Fe1 99.48(8) . . ? S4 Mo3 Fe1 50.73(9) . . ? P5 Mo3 Fe1 96.38(10) . . ? S7 Mo3 Fe1 140.61(9) . . ? P6 Mo3 Fe1 134.77(9) . . ? S2 Mo3 Mo2 53.80(9) . . ? S1 Mo3 Mo2 53.10(7) . . ? S4 Mo3 Mo2 98.68(8) . . ? P5 Mo3 Mo2 141.54(9) . . ? S7 Mo3 Mo2 140.53(9) . . ? P6 Mo3 Mo2 101.01(8) . . ? Fe1 Mo3 Mo2 58.49(6) . . ? S2 Mo3 Mo1 99.84(8) . . ? S1 Mo3 Mo1 53.47(9) . . ? S4 Mo3 Mo1 52.86(8) . . ? P5 Mo3 Mo1 134.88(10) . . ? S7 Mo3 Mo1 98.10(8) . . ? P6 Mo3 Mo1 149.23(8) . . ? Fe1 Mo3 Mo1 58.77(6) . . ? Mo2 Mo3 Mo1 59.83(4) . . ? S4 Fe1 S2 108.45(12) . . ? S4 Fe1 S3 108.10(12) . . ? S2 Fe1 S3 109.03(12) . . ? S4 Fe1 S8 114.91(14) . . ? S2 Fe1 S8 112.71(15) . . ? S3 Fe1 S8 103.33(14) . . ? S4 Fe1 Mo2 106.40(10) . . ? S2 Fe1 Mo2 56.57(10) . . ? S3 Fe1 Mo2 55.71(9) . . ? S8 Fe1 Mo2 138.18(12) . . ? S4 Fe1 Mo1 55.68(8) . . ? S2 Fe1 Mo1 106.45(10) . . ? S3 Fe1 Mo1 55.89(10) . . ? S8 Fe1 Mo1 140.25(13) . . ? Mo2 Fe1 Mo1 62.37(6) . . ? S4 Fe1 Mo3 56.36(9) . . ? S2 Fe1 Mo3 55.59(10) . . ? S3 Fe1 Mo3 106.18(10) . . ? S8 Fe1 Mo3 150.46(12) . . ? Mo2 Fe1 Mo3 62.44(7) . . ? Mo1 Fe1 Mo3 62.42(5) . . ? Mo2 S1 Mo3 73.54(9) . . ? Mo2 S1 Mo1 73.23(9) . . ? Mo3 S1 Mo1 73.42(9) . . ? Fe1 S2 Mo3 73.26(10) . . ? Fe1 S2 Mo2 72.24(10) . . ? Mo3 S2 Mo2 73.24(9) . . ? Fe1 S3 Mo2 72.79(9) . . ? Fe1 S3 Mo1 72.95(10) . . ? Mo2 S3 Mo1 73.49(9) . . ? Fe1 S4 Mo1 73.37(10) . . ? Fe1 S4 Mo3 72.91(10) . . ? Mo1 S4 Mo3 73.45(9) . . ? C20 S5 Mo1 119.4(4) . . ? C32 S6 Mo2 119.2(4) . . ? C26 S7 Mo3 117.7(4) . . ? C38 S8 Fe1 105.2(4) . . ? C1 P1 C2 101.0(6) . . ? C1 P1 C3 104.6(6) . . ? C2 P1 C3 101.5(6) . . ? C1 P1 Mo1 116.9(5) . . ? C2 P1 Mo1 119.1(4) . . ? C3 P1 Mo1 111.6(4) . . ? C5 P2 C6 101.6(6) . . ? C5 P2 C4 101.4(6) . . ? C6 P2 C4 102.4(6) . . ? C5 P2 Mo1 117.2(4) . . ? C6 P2 Mo1 124.5(4) . . ? C4 P2 Mo1 106.6(4) . . ? C8 P3 C7 102.2(6) . . ? C8 P3 C9 103.5(6) . . ? C7 P3 C9 103.0(6) . . ? C8 P3 Mo2 117.3(4) . . ? C7 P3 Mo2 117.9(4) . . ? C9 P3 Mo2 111.0(4) . . ? C11 P4 C12 101.6(6) . . ? C11 P4 C10 102.4(6) . . ? C12 P4 C10 100.3(6) . . ? C11 P4 Mo2 124.8(4) . . ? C12 P4 Mo2 118.2(4) . . ? C10 P4 Mo2 105.9(4) . . ? C13 P5 C14 103.7(8) . . ? C13 P5 C15 99.9(7) . . ? C14 P5 C15 104.7(7) . . ? C13 P5 Mo3 116.5(5) . . ? C14 P5 Mo3 117.8(5) . . ? C15 P5 Mo3 112.1(5) . . ? C18 P6 C17 101.3(6) . . ? C18 P6 C16 101.5(6) . . ? C17 P6 C16 101.6(6) . . ? C18 P6 Mo3 115.3(4) . . ? C17 P6 Mo3 126.1(4) . . ? C16 P6 Mo3 107.8(4) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P1 114.3(9) . . ? C4 C3 H3A 108.7 . . ? P1 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? P1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C3 C4 P2 110.3(8) . . ? C3 C4 H4A 109.6 . . ? P2 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? P2 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? P2 C5 H5A 109.5 . . ? P2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P2 C6 H6A 109.5 . . ? P2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C7 H7A 109.5 . . ? P3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P3 C8 H8A 109.5 . . ? P3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P3 113.6(9) . . ? C10 C9 H9A 108.8 . . ? P3 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? P3 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 P4 109.2(8) . . ? C9 C10 H10A 109.8 . . ? P4 C10 H10A 109.8 . . ? C9 C10 H10B 109.8 . . ? P4 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? P4 C11 H11A 109.5 . . ? P4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P4 C12 H12A 109.5 . . ? P4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P5 C13 H13A 109.5 . . ? P5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P5 C14 H14A 109.5 . . ? P5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 P5 115.2(9) . . ? C16 C15 H15A 108.5 . . ? P5 C15 H15A 108.5 . . ? C16 C15 H15B 108.5 . . ? P5 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C15 C16 P6 109.9(8) . . ? C15 C16 H16A 109.7 . . ? P6 C16 H16A 109.7 . . ? C15 C16 H16B 109.7 . . ? P6 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? P6 C17 H17A 109.5 . . ? P6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P6 C18 H18A 109.5 . . ? P6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C20 C25 117.2(13) . . ? C21 C20 S5 118.3(11) . . ? C25 C20 S5 124.6(10) . . ? C22 C21 C20 121.3(16) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 122.4(16) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C24 C23 C22 116.3(16) . . ? C24 C23 H23 121.9 . . ? C22 C23 H23 121.9 . . ? C23 C24 C25 123.3(17) . . ? C23 C24 H24 118.3 . . ? C25 C24 H24 118.3 . . ? C24 C25 C20 119.4(14) . . ? C24 C25 H25 120.3 . . ? C20 C25 H25 120.3 . . ? C27 C26 C31 117.9(12) . . ? C27 C26 S7 126.4(10) . . ? C31 C26 S7 115.7(11) . . ? C26 C27 C28 124.5(14) . . ? C26 C27 H27 117.8 . . ? C28 C27 H27 117.8 . . ? C27 C28 C29 116.7(16) . . ? C27 C28 H28 121.7 . . ? C29 C28 H28 121.7 . . ? C30 C29 C28 122.0(17) . . ? C30 C29 H29 119.0 . . ? C28 C29 H29 119.0 . . ? C29 C30 C31 121.4(17) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C26 C31 C30 117.4(14) . . ? C26 C31 H31 121.3 . . ? C30 C31 H31 121.3 . . ? C37 C32 C33 116.6(13) . . ? C37 C32 S6 118.3(10) . . ? C33 C32 S6 124.9(10) . . ? C34 C33 C32 119.3(13) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 120.0(16) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 121.6(16) . . ? C36 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C35 C36 C37 118.8(15) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C36 C37 C32 123.6(14) . . ? C36 C37 H37 118.2 . . ? C32 C37 H37 118.2 . . ? C39 C38 C43 120.0(13) . . ? C39 C38 S8 119.4(11) . . ? C43 C38 S8 120.6(11) . . ? C38 C39 C40 122.5(14) . . ? C38 C39 H39 118.8 . . ? C40 C39 H39 118.8 . . ? C41 C40 C39 116.9(15) . . ? C41 C40 H40 121.5 . . ? C39 C40 H40 121.5 . . ? C40 C41 C42 124.1(16) . . ? C40 C41 H41 118.0 . . ? C42 C41 H41 118.0 . . ? C43 C42 C41 117.1(15) . . ? C43 C42 H42 121.4 . . ? C41 C42 H42 121.4 . . ? C38 C43 C42 119.4(14) . . ? C38 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.752 _refine_diff_density_min -1.252 _refine_diff_density_rms 0.184