Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Pierpont, Cortlandt' 'Liu, Cai Ming' 'Nordlander, Ebbe' 'Restorp, Per' _publ_contact_author_name 'Prof Cortlandt Pierpont' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Colorado Campus Box 215 Boulder Colorado 80309-0215 UNITED STATES OF AMERICA ; _publ_contact_author_email 'PIERPONT@COLORADO.EDU' _publ_section_title ; Oxo-deficient dioxylene complexes of Mo(VI) containing 3,6-di-tert-butylcatechol ; data_[MoO(3,6-DBCat)2]4 _database_code_CSD 173929 _audit_creation_method SHELXL _chemical_name_systematic ; [MoO(3,6-DBCat)2]4 ; _chemical_formula_sum 'C14 H20 Mo0.50 O2.50' _chemical_formula_weight 276.27 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 Tetragonal _symmetry_space_group_name_H-M P4/nnc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 22.5679(15) _cell_length_b 22.5679(15) _cell_length_c 13.0099(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6626.1(9) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.108 _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type 'Semi-empirical from psi-scans' _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.955 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 45323 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3824 _reflns_number_observed 2713 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+13.3000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_number_reflns 3808 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_obs 0.0584 _refine_ls_wR_factor_all 0.2116 _refine_ls_wR_factor_obs 0.1878 _refine_ls_goodness_of_fit_all 1.261 _refine_ls_goodness_of_fit_obs 1.373 _refine_ls_restrained_S_all 1.297 _refine_ls_restrained_S_obs 1.373 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.166909(15) 0.333091(15) 0.2500 0.0246(2) Uani 1 d S . O1 O 0.1643(2) 0.2500 0.2500 0.0244(9) Uani 1 d S . O3 O 0.17242(12) 0.36019(15) 0.1097(2) 0.0271(6) Uani 1 d . . O2 O 0.08237(13) 0.34070(14) 0.2077(2) 0.0312(7) Uani 1 d . . C3 C 0.1236(2) 0.4099(2) -0.0330(3) 0.0290(9) Uani 1 d . . C1 C 0.0712(2) 0.3682(2) 0.1182(3) 0.0279(9) Uani 1 d . . C6 C 0.0147(2) 0.3856(2) 0.0822(4) 0.0311(10) Uani 1 d . . C7 C -0.0414(2) 0.3753(2) 0.1456(4) 0.0381(11) Uani 1 d . . C11 C 0.1809(2) 0.4253(2) -0.0883(3) 0.0346(11) Uani 1 d . . C5 C 0.0155(2) 0.4142(2) -0.0118(4) 0.0344(11) Uani 1 d . . H5A H -0.0204(2) 0.4263(2) -0.0399(4) 0.041 Uiso 1 calc R . C14 C 0.1687(2) 0.4560(3) -0.1908(4) 0.0475(14) Uani 1 d . . H14A H 0.2056(2) 0.4652(3) -0.2240(4) 0.071 Uiso 1 calc R . H14B H 0.1470(2) 0.4919(3) -0.1789(4) 0.071 Uiso 1 calc R . H14C H 0.1459(2) 0.4302(3) -0.2341(4) 0.071 Uiso 1 calc R . C2 C 0.1233(2) 0.3798(2) 0.0618(3) 0.0263(8) Uani 1 d . . C13 C 0.2174(2) 0.3687(2) -0.1105(4) 0.0409(12) Uani 1 d . . H13A H 0.2533(2) 0.3793(2) -0.1454(4) 0.061 Uiso 1 calc R . H13B H 0.1946(2) 0.3424(2) -0.1530(4) 0.061 Uiso 1 calc R . H13C H 0.2268(2) 0.3493(2) -0.0469(4) 0.061 Uiso 1 calc R . C4 C 0.0675(2) 0.4259(2) -0.0672(4) 0.0348(10) Uani 1 d . . H4A H 0.0643(2) 0.4454(2) -0.1299(4) 0.042 Uiso 1 calc R . C12 C 0.2179(2) 0.4669(2) -0.0193(4) 0.0455(13) Uani 1 d . . H12A H 0.2542(2) 0.4768(2) -0.0537(4) 0.068 Uiso 1 calc R . H12B H 0.2267(2) 0.4472(2) 0.0444(4) 0.068 Uiso 1 calc R . H12C H 0.1958(2) 0.5024(2) -0.0057(4) 0.068 Uiso 1 calc R . C10 C -0.0966(2) 0.3954(3) 0.0856(5) 0.0476(13) Uani 1 d . . H10A H -0.0930(2) 0.4367(3) 0.0688(5) 0.071 Uiso 1 calc R . H10B H -0.1313(2) 0.3895(3) 0.1271(5) 0.071 Uiso 1 calc R . H10C H -0.1000(2) 0.3727(3) 0.0235(5) 0.071 Uiso 1 calc R . C9 C -0.0483(2) 0.3102(3) 0.1709(6) 0.060(2) Uani 1 d . . H9A H -0.0504(2) 0.2878(3) 0.1084(6) 0.091 Uiso 1 calc R . H9B H -0.0839(2) 0.3045(3) 0.2100(6) 0.091 Uiso 1 calc R . H9C H -0.0148(2) 0.2972(3) 0.2106(6) 0.091 Uiso 1 calc R . C8 C -0.0379(2) 0.4116(3) 0.2443(4) 0.0531(15) Uani 1 d . . H8A H -0.0335(2) 0.4528(3) 0.2274(4) 0.080 Uiso 1 calc R . H8B H -0.0044(2) 0.3989(3) 0.2841(4) 0.080 Uiso 1 calc R . H8C H -0.0735(2) 0.4061(3) 0.2835(4) 0.080 Uiso 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 Mo 0.0282(2) 0.0282(2) 0.0176(3) 0.00208(15) 0.00208(15) 0.0042(2) O1 0.026(2) 0.026(2) 0.021(2) -0.001(2) 0.000 0.000 O3 0.025(2) 0.038(2) 0.0189(14) -0.0002(13) 0.0015(11) 0.0056(12) O2 0.026(2) 0.039(2) 0.029(2) 0.0064(14) 0.0055(13) 0.0050(13) C3 0.031(2) 0.030(2) 0.026(2) 0.003(2) 0.000(2) 0.006(2) C1 0.030(2) 0.030(2) 0.024(2) 0.004(2) 0.002(2) 0.003(2) C6 0.029(2) 0.031(2) 0.034(2) 0.000(2) -0.001(2) 0.006(2) C7 0.026(2) 0.043(3) 0.045(3) 0.009(2) 0.008(2) 0.007(2) C11 0.034(2) 0.043(3) 0.026(2) 0.011(2) 0.004(2) 0.006(2) C5 0.029(2) 0.039(3) 0.035(3) 0.004(2) -0.006(2) 0.007(2) C14 0.039(3) 0.063(4) 0.041(3) 0.024(3) 0.009(2) 0.012(2) C2 0.027(2) 0.029(2) 0.022(2) -0.001(2) -0.003(2) 0.004(2) C13 0.037(3) 0.054(3) 0.031(2) 0.009(2) 0.009(2) 0.011(2) C4 0.038(3) 0.038(3) 0.029(2) 0.007(2) -0.001(2) 0.008(2) C12 0.038(3) 0.048(3) 0.051(3) 0.011(3) 0.007(2) -0.003(2) C10 0.026(2) 0.055(3) 0.062(3) 0.009(3) 0.005(2) 0.007(2) C9 0.036(3) 0.053(3) 0.092(5) 0.024(3) 0.019(3) 0.007(3) C8 0.038(3) 0.078(4) 0.043(3) 0.005(3) 0.011(2) 0.016(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 Mo O1 1.8761(4) 4 ? Mo O1 1.8761(4) . ? Mo O3 1.929(3) . ? Mo O3 1.929(3) 8 ? Mo O2 1.993(3) 8 ? Mo O2 1.993(3) . ? O1 Mo 1.8761(4) 3 ? O3 C2 1.347(5) . ? O2 C1 1.344(5) . ? C3 C4 1.391(6) . ? C3 C2 1.408(6) . ? C3 C11 1.520(6) . ? C1 C2 1.410(6) . ? C1 C6 1.413(6) . ? C6 C5 1.383(6) . ? C6 C7 1.530(6) . ? C7 C9 1.512(8) . ? C7 C8 1.526(8) . ? C7 C10 1.539(7) . ? C11 C14 1.528(7) . ? C11 C12 1.544(8) . ? C11 C13 1.547(7) . ? C5 C4 1.401(7) . ? 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 O1 Mo O1 93.5(2) 4 . ? O1 Mo O3 85.75(9) 4 . ? O1 Mo O3 108.59(10) . . ? O1 Mo O3 108.59(10) 4 8 ? O1 Mo O3 85.75(9) . 8 ? O3 Mo O3 159.4(2) . 8 ? O1 Mo O2 93.25(14) 4 8 ? O1 Mo O2 162.58(10) . 8 ? O3 Mo O2 87.90(13) . 8 ? O3 Mo O2 76.88(12) 8 8 ? O1 Mo O2 162.58(10) 4 . ? O1 Mo O2 93.25(14) . . ? O3 Mo O2 76.88(12) . . ? O3 Mo O2 87.90(13) 8 . ? O2 Mo O2 84.9(2) 8 . ? Mo O1 Mo 176.5(2) . 3 ? C2 O3 Mo 119.3(3) . . ? C1 O2 Mo 117.3(3) . . ? C4 C3 C2 113.6(4) . . ? C4 C3 C11 124.3(4) . . ? C2 C3 C11 122.0(4) . . ? O2 C1 C2 112.3(4) . . ? O2 C1 C6 125.8(4) . . ? C2 C1 C6 121.9(4) . . ? C5 C6 C1 114.2(4) . . ? C5 C6 C7 124.0(4) . . ? C1 C6 C7 121.7(4) . . ? C9 C7 C8 110.1(5) . . ? C9 C7 C6 110.5(4) . . ? C8 C7 C6 109.2(4) . . ? C9 C7 C10 108.3(4) . . ? C8 C7 C10 108.0(4) . . ? C6 C7 C10 110.6(4) . . ? C3 C11 C14 111.3(4) . . ? C3 C11 C12 108.9(4) . . ? C14 C11 C12 109.2(4) . . ? C3 C11 C13 110.6(4) . . ? C14 C11 C13 107.9(4) . . ? C12 C11 C13 108.8(4) . . ? C6 C5 C4 123.6(4) . . ? O3 C2 C3 124.0(4) . . ? O3 C2 C1 112.7(4) . . ? C3 C2 C1 123.4(4) . . ? C3 C4 C5 123.2(4) . . ? _refine_diff_density_max 1.020 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.127 data_MoO(DMSO)(3,6-DBCat)2 _database_code_CSD 173930 _audit_creation_method SHELXL _chemical_name ; MoO(DMSO)(3,6-DBCat)2 ; _chemical_formula_sum 'C30 H46 Mo O6 S' _chemical_formula_weight 630.67 _chemical_compound_source toluene 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2701(5) _cell_length_b 16.7146(7) _cell_length_c 18.4327(6) _cell_angle_alpha 92.2170(10) _cell_angle_beta 90.0720(10) _cell_angle_gamma 93.1140(10) _cell_volume 3771.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 578 _cell_measurement_theta_min 10.11 _cell_measurement_theta_max 42.34 _exptl_crystal_description 'rhombic needle' _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.111 _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.936 _diffrn_ambient_temperature 295(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 'CCD detector' _diffrn_measurement_method 'SMART CCD' _diffrn_reflns_number 17741 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.1073 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 23.31 _reflns_number_total 10391 _reflns_number_observed 6159 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART CCD' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1165P)^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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 10391 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1240 _refine_ls_R_factor_obs 0.0656 _refine_ls_wR_factor_all 0.2190 _refine_ls_wR_factor_obs 0.1879 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.159 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.159 _refine_ls_shift/esd_max 0.111 _refine_ls_shift/esd_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.50860(6) 0.06726(4) 0.33021(4) 0.0547(3) Uani 1 d . . Mo2 Mo 0.96952(6) -0.14992(4) 0.38157(4) 0.0517(3) Uani 1 d . . O12 O 0.8243(5) -0.1091(3) 0.4264(3) 0.069(2) Uani 1 d . . O9 O 0.9757(4) -0.2128(3) 0.4693(2) 0.0535(14) Uani 1 d . . O10 O 1.0945(4) -0.2125(3) 0.3609(3) 0.0607(15) Uani 1 d . . O7 O 0.8682(4) -0.2448(3) 0.3422(3) 0.0591(15) Uani 1 d . . O8 O 0.9545(4) -0.1305(3) 0.2785(2) 0.0482(13) Uani 1 d . . O4 O 0.5005(4) 0.1750(3) 0.3742(3) 0.0559(14) Uani 1 d . . O1 O 0.5295(4) -0.0127(3) 0.2528(3) 0.0573(14) Uani 1 d . . O6 O 0.6513(4) 0.0623(3) 0.3908(3) 0.065(2) Uani 1 d . . O2 O 0.6107(4) 0.1254(3) 0.2557(3) 0.0626(15) Uani 1 d . . O11 O 1.0258(5) -0.0563(3) 0.3961(3) 0.069(2) Uani 1 d . . O5 O 0.4502(5) -0.0027(3) 0.3839(3) 0.068(2) Uani 1 d . . C15 C 0.3726(7) 0.1856(5) 0.2818(4) 0.055(2) Uani 1 d . . C33 C 0.9099(6) -0.1882(5) 0.2338(4) 0.051(2) Uani 1 d . . C34 C 0.9127(7) -0.1847(5) 0.1571(4) 0.059(2) Uani 1 d . . C47 C 1.1057(6) -0.2782(5) 0.4028(4) 0.052(2) Uani 1 d . . C17 C 0.4469(7) 0.3094(5) 0.3455(4) 0.056(2) Uani 1 d . . C37 C 0.8023(7) -0.3170(5) 0.2331(5) 0.064(2) Uani 1 d . . C51 C 1.0386(7) -0.3393(5) 0.5130(4) 0.058(2) Uani 1 d . . C16 C 0.4411(7) 0.2264(5) 0.3343(4) 0.055(2) Uani 1 d . . C11 C 0.5216(8) -0.1283(6) 0.1273(5) 0.070(3) Uani 1 d . . C48 C 1.1786(7) -0.3355(5) 0.3867(5) 0.063(2) Uani 1 d . . C49 C 1.1789(7) -0.3948(6) 0.4354(5) 0.075(3) Uani 1 d . . H49A H 1.2259(7) -0.4360(6) 0.4274(5) 0.091 Uiso 1 calc R . C19 C 0.3068(8) 0.3058(7) 0.2488(4) 0.076(3) Uani 1 d . . H19A H 0.2607(8) 0.3344(7) 0.2207(4) 0.091 Uiso 1 calc R . C38 C 0.9704(8) -0.1154(6) 0.1195(4) 0.072(3) Uani 1 d . . C8 C 0.6316(10) 0.2641(7) 0.1474(6) 0.106(4) Uani 1 d . . H8A H 0.5766(10) 0.2565(7) 0.1102(6) 0.159 Uiso 1 calc R . H8B H 0.6618(10) 0.3183(7) 0.1476(6) 0.159 Uiso 1 calc R . H8C H 0.5995(10) 0.2537(7) 0.1938(6) 0.159 Uiso 1 calc R . C2 C 0.6209(6) 0.0875(6) 0.1920(4) 0.057(2) Uani 1 d . . C1 C 0.5747(7) 0.0081(5) 0.1896(4) 0.056(2) Uani 1 d . . C6 C 0.5751(7) -0.0453(6) 0.1287(5) 0.067(2) Uani 1 d . . C12 C 0.4006(8) -0.1226(6) 0.1405(5) 0.089(3) Uani 1 d . . H12A H 0.3659(8) -0.1755(6) 0.1397(5) 0.134 Uiso 1 calc R . H12B H 0.3697(8) -0.0923(6) 0.1032(5) 0.134 Uiso 1 calc R . H12C H 0.3894(8) -0.0965(6) 0.1870(5) 0.134 Uiso 1 calc R . C23 C 0.6442(8) 0.3413(6) 0.3760(6) 0.094(3) Uani 1 d . . H23A H 0.6545(8) 0.3614(6) 0.3283(6) 0.140 Uiso 1 calc R . H23B H 0.6572(8) 0.2851(6) 0.3751(6) 0.140 Uiso 1 calc R . H23C H 0.6943(8) 0.3696(6) 0.4092(6) 0.140 Uiso 1 calc R . C3 C 0.6740(7) 0.1210(6) 0.1321(5) 0.072(3) Uani 1 d . . C32 C 0.8586(6) -0.2520(5) 0.2714(4) 0.053(2) Uani 1 d . . C42 C 0.7439(9) -0.3843(6) 0.2730(6) 0.086(3) Uani 1 d . . C21 C 0.5281(8) 0.3536(5) 0.4005(5) 0.067(2) Uani 1 d . . C36 C 0.8060(8) -0.3142(6) 0.1580(6) 0.081(3) Uani 1 d . . H36A H 0.7723(8) -0.3566(6) 0.1307(6) 0.098 Uiso 1 calc R . C50 C 1.1120(7) -0.3968(5) 0.4968(5) 0.069(3) Uani 1 d . . H50A H 1.1173(7) -0.4388(5) 0.5281(5) 0.083 Uiso 1 calc R . C7 C 0.7197(8) 0.2078(7) 0.1326(5) 0.079(3) Uani 1 d . . C20 C 0.3043(7) 0.2255(6) 0.2390(4) 0.061(2) Uani 1 d . . C5 C 0.6281(8) -0.0105(7) 0.0699(5) 0.078(3) Uani 1 d . . H5B H 0.6320(8) -0.0408(7) 0.0267(5) 0.094 Uiso 1 calc R . C46 C 1.0378(6) -0.2793(5) 0.4629(4) 0.053(2) Uani 1 d . . C35 C 0.8580(8) -0.2508(6) 0.1206(5) 0.078(3) Uani 1 d . . H35A H 0.8561(8) -0.2527(6) 0.0701(5) 0.094 Uiso 1 calc R . C4 C 0.6757(8) 0.0673(8) 0.0726(5) 0.082(3) Uani 1 d . . H4A H 0.7115(8) 0.0847(8) 0.0312(5) 0.099 Uiso 1 calc R . C40 C 1.0937(7) -0.1139(6) 0.1377(5) 0.091(3) Uani 1 d . . H40A H 1.1224(7) -0.1641(6) 0.1222(5) 0.136 Uiso 1 calc R . H40B H 1.1040(7) -0.1056(6) 0.1891(5) 0.136 Uiso 1 calc R . H40C H 1.1313(7) -0.0711(6) 0.1130(5) 0.136 Uiso 1 calc R . C61 C 0.6172(9) -0.1279(8) 0.4434(9) 0.162(7) Uani 1 d . . H61A H 0.5999(9) -0.1488(8) 0.3952(9) 0.242 Uiso 1 calc R . H61B H 0.6206(9) -0.0703(8) 0.4438(9) 0.242 Uiso 1 calc R . H61C H 0.5619(9) -0.1464(8) 0.4764(9) 0.242 Uiso 1 calc R . C39 C 0.9239(8) -0.0365(6) 0.1436(5) 0.082(3) Uani 1 d . . H39A H 0.9615(8) 0.0066(6) 0.1192(5) 0.123 Uiso 1 calc R . H39B H 0.9331(8) -0.0282(6) 0.1951(5) 0.123 Uiso 1 calc R . H39C H 0.8476(8) -0.0379(6) 0.1317(5) 0.123 Uiso 1 calc R . C43 C 0.8284(11) -0.4268(6) 0.3161(7) 0.128(5) Uani 1 d . . H43A H 0.8666(11) -0.3887(6) 0.3486(7) 0.192 Uiso 1 calc R . H43B H 0.8795(11) -0.4502(6) 0.2832(7) 0.192 Uiso 1 calc R . H43C H 0.7923(11) -0.4681(6) 0.3434(7) 0.192 Uiso 1 calc R . C18 C 0.3746(8) 0.3477(6) 0.2984(5) 0.077(3) Uani 1 d . . H18A H 0.3732(8) 0.4033(6) 0.3014(5) 0.092 Uiso 1 calc R . O3 O 0.3829(4) 0.1053(3) 0.2792(3) 0.0591(14) Uani 1 d . . C56 C 0.9622(8) -0.3406(5) 0.5795(5) 0.068(2) Uani 1 d . . C25 C 0.2322(9) 0.1801(7) 0.1844(6) 0.091(3) Uani 1 d . . C52 C 1.2518(9) -0.3332(7) 0.3232(6) 0.092(3) Uani 1 d . . C14 C 0.5722(9) -0.1753(6) 0.1859(5) 0.091(3) Uani 1 d . . H14A H 0.5385(9) -0.2285(6) 0.1854(5) 0.136 Uiso 1 calc R . H14B H 0.5612(9) -0.1491(6) 0.2323(5) 0.136 Uiso 1 calc R . H14C H 0.6490(9) -0.1782(6) 0.1770(5) 0.136 Uiso 1 calc R . C57 C 0.9744(10) -0.2630(6) 0.6264(5) 0.096(3) Uani 1 d . . H57A H 0.9256(10) -0.2664(6) 0.6669(5) 0.144 Uiso 1 calc R . H57B H 0.9570(10) -0.2185(6) 0.5978(5) 0.144 Uiso 1 calc R . H57C H 1.0482(10) -0.2553(6) 0.6437(5) 0.144 Uiso 1 calc R . C22 C 0.5121(9) 0.4441(5) 0.4046(6) 0.097(3) Uani 1 d . . H22A H 0.4390(9) 0.4534(5) 0.4201(6) 0.146 Uiso 1 calc R . H22B H 0.5242(9) 0.4657(5) 0.3576(6) 0.146 Uiso 1 calc R . H22C H 0.5630(9) 0.4699(5) 0.4388(6) 0.146 Uiso 1 calc R . C45 C 0.6871(11) -0.4468(7) 0.2231(7) 0.141(6) Uani 1 d . . H45A H 0.7388(11) -0.4680(7) 0.1895(7) 0.212 Uiso 1 calc R . H45B H 0.6304(11) -0.4229(7) 0.1969(7) 0.212 Uiso 1 calc R . H45C H 0.6557(11) -0.4893(7) 0.2513(7) 0.212 Uiso 1 calc R . C55 C 1.3257(10) -0.4056(8) 0.3157(6) 0.129(5) Uani 1 d . . H55A H 1.3708(10) -0.4002(8) 0.2735(6) 0.193 Uiso 1 calc R . H55B H 1.2809(10) -0.4544(8) 0.3110(6) 0.193 Uiso 1 calc R . H55C H 1.3711(10) -0.4068(8) 0.3581(6) 0.193 Uiso 1 calc R . C41 C 0.9565(10) -0.1266(7) 0.0354(5) 0.109(4) Uani 1 d . . H41A H 0.9857(10) -0.1764(7) 0.0193(5) 0.163 Uiso 1 calc R . H41B H 0.9949(10) -0.0831(7) 0.0121(5) 0.163 Uiso 1 calc R . H41C H 0.8804(10) -0.1272(7) 0.0230(5) 0.163 Uiso 1 calc R . C58 C 0.8452(8) -0.3554(6) 0.5482(6) 0.089(3) Uani 1 d . . H58A H 0.8410(8) -0.4044(6) 0.5193(6) 0.134 Uiso 1 calc R . H58B H 0.8283(8) -0.3116(6) 0.5186(6) 0.134 Uiso 1 calc R . H58C H 0.7939(8) -0.3592(6) 0.5874(6) 0.134 Uiso 1 calc R . C26 C 0.3057(10) 0.1351(8) 0.1275(5) 0.131(5) Uani 1 d . . H26A H 0.2599(10) 0.1059(8) 0.0922(5) 0.197 Uiso 1 calc R . H26B H 0.3493(10) 0.0986(8) 0.1521(5) 0.197 Uiso 1 calc R . H26C H 0.3525(10) 0.1736(8) 0.1035(5) 0.197 Uiso 1 calc R . C24 C 0.5102(10) 0.3220(6) 0.4763(5) 0.104(4) Uani 1 d . . H24A H 0.4366(10) 0.3301(6) 0.4913(5) 0.155 Uiso 1 calc R . H24B H 0.5600(10) 0.3502(6) 0.5098(5) 0.155 Uiso 1 calc R . H24C H 0.5229(10) 0.2658(6) 0.4756(5) 0.155 Uiso 1 calc R . C9 C 0.7735(10) 0.2314(8) 0.0625(6) 0.138(5) Uani 1 d . . H9A H 0.7216(10) 0.2241(8) 0.0235(6) 0.207 Uiso 1 calc R . H9B H 0.8340(10) 0.1985(8) 0.0528(6) 0.207 Uiso 1 calc R . H9C H 0.7993(10) 0.2867(8) 0.0665(6) 0.207 Uiso 1 calc R . C13 C 0.5452(10) -0.1737(6) 0.0557(5) 0.104(4) Uani 1 d . . H13A H 0.5103(10) -0.2265(6) 0.0560(5) 0.156 Uiso 1 calc R . H13B H 0.6225(10) -0.1776(6) 0.0503(5) 0.156 Uiso 1 calc R . H13C H 0.5174(10) -0.1453(6) 0.0160(5) 0.156 Uiso 1 calc R . C53 C 1.1827(10) -0.3295(9) 0.2542(6) 0.143(6) Uani 1 d . . H53A H 1.2297(10) -0.3280(9) 0.2127(6) 0.214 Uiso 1 calc R . H53B H 1.1418(10) -0.2821(9) 0.2568(6) 0.214 Uiso 1 calc R . H53C H 1.1334(10) -0.3760(9) 0.2500(6) 0.214 Uiso 1 calc R . C59 C 0.9815(9) -0.4138(6) 0.6277(6) 0.104(4) Uani 1 d . . H59A H 0.9739(9) -0.4625(6) 0.5983(6) 0.156 Uiso 1 calc R . H59B H 0.9287(9) -0.4154(6) 0.6661(6) 0.156 Uiso 1 calc R . H59C H 1.0536(9) -0.4082(6) 0.6481(6) 0.156 Uiso 1 calc R . C10 C 0.8039(9) 0.2205(7) 0.1907(6) 0.118(4) Uani 1 d . . H10A H 0.8613(9) 0.1845(7) 0.1818(6) 0.177 Uiso 1 calc R . H10B H 0.7713(9) 0.2102(7) 0.2370(6) 0.177 Uiso 1 calc R . H10C H 0.8336(9) 0.2748(7) 0.1908(6) 0.177 Uiso 1 calc R . C44 C 0.6595(9) -0.3530(7) 0.3244(6) 0.106(4) Uani 1 d . . H44A H 0.6932(9) -0.3129(7) 0.3571(6) 0.160 Uiso 1 calc R . H44B H 0.6283(9) -0.3964(7) 0.3517(6) 0.160 Uiso 1 calc R . H44C H 0.6030(9) -0.3299(7) 0.2973(6) 0.160 Uiso 1 calc R . C28 C 0.1571(11) 0.2387(9) 0.1462(6) 0.152(6) Uani 1 d . . H28A H 0.1112(11) 0.2090(9) 0.1113(6) 0.228 Uiso 1 calc R . H28B H 0.2015(11) 0.2785(9) 0.1220(6) 0.228 Uiso 1 calc R . H28C H 0.1125(11) 0.2645(9) 0.1819(6) 0.228 Uiso 1 calc R . C54 C 1.3276(10) -0.2592(8) 0.3268(7) 0.132(5) Uani 1 d . . H54A H 1.3741(10) -0.2591(8) 0.2850(7) 0.198 Uiso 1 calc R . H54B H 1.3713(10) -0.2590(8) 0.3700(7) 0.198 Uiso 1 calc R . H54C H 1.2855(10) -0.2124(8) 0.3277(7) 0.198 Uiso 1 calc R . C27 C 0.1576(9) 0.1194(8) 0.2239(7) 0.123(5) Uani 1 d . . H27A H 0.1109(9) 0.0899(8) 0.1893(7) 0.185 Uiso 1 calc R . H27B H 0.1138(9) 0.1474(8) 0.2586(7) 0.185 Uiso 1 calc R . H27C H 0.2013(9) 0.0830(8) 0.2485(7) 0.185 Uiso 1 calc R . C31 C 0.8383(9) 0.0620(8) 0.3225(7) 0.131(5) Uani 1 d . . H31A H 0.8110(9) 0.0648(8) 0.2739(7) 0.197 Uiso 1 calc R . H31B H 0.8369(9) 0.0070(8) 0.3359(7) 0.197 Uiso 1 calc R . H31C H 0.9119(9) 0.0845(8) 0.3249(7) 0.197 Uiso 1 calc R . C62 C 0.7567(12) -0.1137(8) 0.5608(7) 0.154(6) Uani 1 d . . H62A H 0.8244(12) -0.1275(8) 0.5818(7) 0.232 Uiso 1 calc R . H62B H 0.6972(12) -0.1326(8) 0.5905(7) 0.232 Uiso 1 calc R . H62C H 0.7559(12) -0.0565(8) 0.5579(7) 0.232 Uiso 1 calc R . C30 C 0.8181(13) 0.1034(7) 0.4629(7) 0.178(8) Uani 1 d . . H30A H 0.7824(13) 0.1301(7) 0.5025(7) 0.267 Uiso 1 calc R . H30B H 0.8923(13) 0.1245(7) 0.4598(7) 0.267 Uiso 1 calc R . H30C H 0.8172(13) 0.0470(7) 0.4708(7) 0.267 Uiso 1 calc R . S1 S 0.7525(2) 0.11881(15) 0.3852(2) 0.0811(8) Uani 1 d . . S2 S 0.7423(2) -0.1605(2) 0.4697(2) 0.0865(8) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0559(5) 0.0590(5) 0.0494(4) 0.0006(4) 0.0046(4) 0.0047(4) Mo2 0.0542(5) 0.0559(5) 0.0460(4) 0.0077(3) 0.0006(3) 0.0087(4) O12 0.074(4) 0.065(4) 0.070(4) 0.012(3) 0.021(3) 0.018(3) O9 0.055(3) 0.062(3) 0.046(3) 0.011(3) 0.007(3) 0.010(3) O10 0.057(4) 0.073(4) 0.055(3) 0.009(3) 0.006(3) 0.018(3) O7 0.066(4) 0.061(4) 0.050(3) 0.010(3) -0.003(3) -0.006(3) O8 0.045(3) 0.057(3) 0.044(3) 0.013(3) -0.005(2) 0.003(3) O4 0.060(4) 0.055(3) 0.053(3) -0.001(3) -0.002(3) 0.003(3) O1 0.055(3) 0.063(4) 0.055(3) 0.000(3) 0.006(3) 0.013(3) O6 0.056(4) 0.073(4) 0.066(4) 0.008(3) -0.010(3) 0.004(3) O2 0.063(4) 0.071(4) 0.053(3) 0.003(3) 0.006(3) 0.000(3) O11 0.085(4) 0.065(4) 0.059(3) 0.010(3) -0.003(3) -0.002(3) O5 0.080(4) 0.066(4) 0.058(3) 0.003(3) 0.010(3) 0.003(3) C15 0.056(5) 0.062(6) 0.046(5) -0.013(4) -0.001(4) -0.003(5) C33 0.038(5) 0.064(6) 0.051(5) 0.002(4) -0.008(4) 0.010(4) C34 0.056(5) 0.073(6) 0.050(5) 0.005(5) -0.002(4) 0.015(5) C47 0.047(5) 0.058(5) 0.053(5) 0.009(4) -0.009(4) 0.009(4) C17 0.067(6) 0.049(5) 0.053(5) 0.001(4) 0.019(4) 0.005(4) C37 0.067(6) 0.055(6) 0.071(6) 0.006(5) -0.003(5) 0.012(5) C51 0.064(6) 0.057(5) 0.054(5) 0.006(4) -0.006(4) 0.003(5) C16 0.055(5) 0.062(6) 0.050(5) 0.006(4) 0.017(4) 0.011(5) C11 0.074(7) 0.078(7) 0.058(6) -0.004(5) -0.011(5) 0.012(5) C48 0.055(6) 0.066(6) 0.072(6) 0.015(5) 0.002(5) 0.018(5) C49 0.063(6) 0.070(7) 0.096(7) 0.001(6) -0.003(6) 0.026(5) C19 0.083(7) 0.099(8) 0.046(5) -0.005(5) -0.026(5) 0.024(6) C38 0.079(7) 0.086(7) 0.051(5) 0.013(5) 0.005(5) 0.001(6) C8 0.118(10) 0.097(9) 0.103(9) 0.014(7) 0.005(7) 0.001(8) C2 0.047(5) 0.080(7) 0.046(5) 0.000(5) 0.001(4) 0.017(5) C1 0.056(5) 0.069(6) 0.045(5) 0.006(5) 0.001(4) 0.019(5) C6 0.058(6) 0.094(7) 0.050(5) 0.001(5) -0.001(4) 0.022(5) C12 0.079(8) 0.102(8) 0.086(7) 0.000(6) -0.001(6) -0.007(6) C23 0.069(7) 0.095(8) 0.115(8) -0.009(7) -0.015(6) -0.006(6) C3 0.061(6) 0.102(8) 0.053(6) 0.020(6) 0.002(5) 0.006(6) C32 0.051(5) 0.051(5) 0.058(5) 0.005(4) -0.006(4) 0.010(4) C42 0.086(8) 0.066(7) 0.107(8) 0.016(6) -0.022(7) -0.010(6) C21 0.076(7) 0.052(5) 0.071(6) -0.011(5) -0.011(5) -0.011(5) C36 0.088(8) 0.070(7) 0.084(7) -0.014(6) -0.007(6) -0.003(6) C50 0.073(7) 0.060(6) 0.079(6) 0.020(5) -0.010(5) 0.017(5) C7 0.070(7) 0.102(8) 0.065(6) 0.018(6) 0.006(5) -0.004(6) C20 0.053(6) 0.076(7) 0.054(5) -0.007(5) -0.010(4) 0.010(5) C5 0.075(7) 0.101(8) 0.058(6) -0.010(6) 0.002(5) 0.014(6) C46 0.051(5) 0.063(6) 0.047(5) 0.007(4) -0.010(4) 0.010(4) C35 0.086(7) 0.094(8) 0.053(6) -0.010(6) -0.004(5) 0.002(6) C4 0.062(6) 0.135(10) 0.051(6) 0.014(7) 0.010(5) 0.019(7) C40 0.066(7) 0.109(9) 0.097(8) 0.018(6) 0.024(6) -0.005(6) C61 0.062(8) 0.139(12) 0.293(19) 0.123(13) 0.007(10) 0.008(8) C39 0.087(7) 0.079(7) 0.082(7) 0.017(6) -0.005(6) 0.003(6) C43 0.169(13) 0.073(8) 0.145(11) 0.052(8) 0.000(10) 0.005(8) C18 0.096(8) 0.061(6) 0.078(7) 0.019(5) 0.017(6) 0.031(6) O3 0.059(4) 0.064(4) 0.054(3) -0.008(3) -0.008(3) 0.006(3) C56 0.072(7) 0.067(6) 0.067(6) 0.014(5) 0.000(5) 0.009(5) C25 0.086(8) 0.111(9) 0.077(7) -0.012(7) -0.024(6) 0.033(7) C52 0.062(7) 0.114(9) 0.101(8) 0.012(7) 0.002(6) 0.029(7) C14 0.098(8) 0.086(7) 0.090(7) -0.001(6) -0.007(6) 0.023(6) C57 0.146(10) 0.082(7) 0.061(6) 0.006(6) 0.015(6) 0.010(7) C22 0.132(10) 0.057(6) 0.100(8) -0.009(6) -0.003(7) -0.005(6) C45 0.188(14) 0.099(9) 0.129(10) 0.007(8) -0.036(10) -0.063(10) C55 0.113(10) 0.154(12) 0.127(10) 0.025(9) 0.036(8) 0.070(9) C41 0.148(11) 0.126(10) 0.050(6) 0.017(6) 0.007(6) -0.021(8) C58 0.081(7) 0.081(7) 0.108(8) 0.029(6) 0.008(6) 0.004(6) C26 0.121(10) 0.193(14) 0.079(7) -0.057(8) -0.024(7) 0.045(10) C24 0.157(11) 0.089(8) 0.062(6) 0.002(6) -0.018(7) -0.022(8) C9 0.148(12) 0.170(13) 0.094(9) 0.043(9) 0.031(8) -0.037(10) C13 0.138(10) 0.097(8) 0.075(7) -0.031(6) -0.003(7) 0.017(7) C53 0.132(11) 0.215(16) 0.089(9) -0.012(9) 0.027(8) 0.083(11) C59 0.117(9) 0.105(9) 0.093(8) 0.045(7) 0.000(7) 0.014(7) C10 0.101(9) 0.134(11) 0.115(9) 0.021(8) -0.006(8) -0.042(8) C44 0.091(8) 0.102(9) 0.126(10) 0.038(8) 0.010(8) -0.027(7) C28 0.156(13) 0.184(14) 0.118(10) -0.044(10) -0.079(9) 0.069(11) C54 0.090(9) 0.154(13) 0.157(12) 0.030(10) 0.050(8) 0.028(9) C27 0.076(8) 0.143(11) 0.145(11) -0.060(9) -0.032(8) 0.001(8) C31 0.095(9) 0.130(11) 0.175(13) 0.038(10) 0.043(9) 0.046(8) C62 0.184(14) 0.161(14) 0.122(10) 0.006(9) 0.092(10) 0.040(11) C30 0.252(18) 0.116(11) 0.160(12) 0.054(10) -0.136(13) -0.086(11) S1 0.075(2) 0.061(2) 0.108(2) 0.0127(15) -0.0236(15) 0.0045(13) S2 0.072(2) 0.072(2) 0.119(2) 0.038(2) 0.027(2) 0.0210(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O5 1.692(5) . ? Mo1 O1 1.944(5) . ? Mo1 O3 1.953(5) . ? Mo1 O4 1.953(5) . ? Mo1 O6 2.083(5) . ? Mo1 O2 2.092(5) . ? Mo2 O11 1.688(5) . ? Mo2 O10 1.933(5) . ? Mo2 O8 1.951(4) . ? Mo2 O9 1.966(5) . ? Mo2 O7 2.070(5) . ? Mo2 O12 2.101(5) . ? O12 S2 1.532(6) . ? O9 C46 1.384(9) . ? O10 C47 1.380(9) . ? O7 C32 1.310(9) . ? O8 C33 1.336(8) . ? O4 C16 1.389(9) . ? O1 C1 1.341(9) . ? O6 S1 1.525(6) . ? O2 C2 1.322(9) . ? C15 O3 1.354(9) . ? C15 C20 1.368(11) . ? C15 C16 1.411(10) . ? C33 C32 1.414(10) . ? C33 C34 1.419(10) . ? C34 C35 1.408(12) . ? C34 C38 1.517(12) . ? C47 C48 1.370(11) . ? C47 C46 1.387(11) . ? C17 C16 1.393(11) . ? C17 C18 1.433(12) . ? C17 C21 1.557(11) . ? C37 C36 1.388(12) . ? C37 C32 1.419(11) . ? C37 C42 1.515(12) . ? C51 C50 1.377(12) . ? C51 C46 1.388(10) . ? C51 C56 1.545(12) . ? C11 C6 1.502(12) . ? C11 C14 1.511(12) . ? C11 C12 1.513(12) . ? C11 C13 1.532(12) . ? C48 C49 1.362(11) . ? C48 C52 1.477(13) . ? C49 C50 1.400(12) . ? C19 C20 1.346(12) . ? C19 C18 1.379(12) . ? C38 C39 1.516(12) . ? C38 C40 1.548(12) . ? C38 C41 1.563(11) . ? C8 C7 1.489(14) . ? C2 C3 1.403(11) . ? C2 C1 1.413(11) . ? C1 C6 1.407(11) . ? C6 C5 1.394(12) . ? C23 C21 1.517(12) . ? C3 C4 1.390(13) . ? C3 C7 1.527(13) . ? C42 C45 1.506(13) . ? C42 C44 1.507(14) . ? C42 C43 1.527(14) . ? C21 C24 1.525(12) . ? C21 C22 1.536(12) . ? C36 C35 1.410(12) . ? C7 C10 1.488(13) . ? C7 C9 1.509(12) . ? C20 C25 1.497(12) . ? C5 C4 1.396(13) . ? C61 S2 1.732(11) . ? C56 C57 1.531(12) . ? C56 C58 1.550(12) . ? C56 C59 1.567(12) . ? C25 C27 1.535(15) . ? C25 C28 1.566(14) . ? C25 C26 1.579(14) . ? C52 C54 1.506(15) . ? C52 C53 1.531(14) . ? C52 C55 1.553(14) . ? C31 S1 1.837(12) . ? C62 S2 1.829(13) . ? C30 S1 1.677(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O1 91.5(2) . . ? O5 Mo1 O3 102.4(3) . . ? O1 Mo1 O3 90.6(2) . . ? O5 Mo1 O4 111.3(2) . . ? O1 Mo1 O4 156.5(2) . . ? O3 Mo1 O4 78.9(2) . . ? O5 Mo1 O6 88.2(2) . . ? O1 Mo1 O6 102.1(2) . . ? O3 Mo1 O6 163.3(2) . . ? O4 Mo1 O6 85.3(2) . . ? O5 Mo1 O2 162.7(3) . . ? O1 Mo1 O2 75.1(2) . . ? O3 Mo1 O2 88.8(2) . . ? O4 Mo1 O2 83.6(2) . . ? O6 Mo1 O2 84.1(2) . . ? O11 Mo2 O10 103.1(3) . . ? O11 Mo2 O8 90.2(2) . . ? O10 Mo2 O8 90.0(2) . . ? O11 Mo2 O9 111.5(2) . . ? O10 Mo2 O9 78.8(2) . . ? O8 Mo2 O9 157.3(2) . . ? O11 Mo2 O7 161.3(2) . . ? O10 Mo2 O7 89.5(2) . . ? O8 Mo2 O7 75.8(2) . . ? O9 Mo2 O7 84.3(2) . . ? O11 Mo2 O12 87.9(3) . . ? O10 Mo2 O12 162.8(2) . . ? O8 Mo2 O12 103.3(2) . . ? O9 Mo2 O12 84.8(2) . . ? O7 Mo2 O12 83.5(2) . . ? S2 O12 Mo2 124.6(3) . . ? C46 O9 Mo2 115.0(4) . . ? C47 O10 Mo2 116.2(5) . . ? C32 O7 Mo2 115.8(5) . . ? C33 O8 Mo2 119.6(4) . . ? C16 O4 Mo1 114.5(5) . . ? C1 O1 Mo1 120.8(5) . . ? S1 O6 Mo1 125.7(3) . . ? C2 O2 Mo1 115.7(5) . . ? O3 C15 C20 125.3(7) . . ? O3 C15 C16 113.1(7) . . ? C20 C15 C16 121.6(8) . . ? O8 C33 C32 112.7(7) . . ? O8 C33 C34 123.3(7) . . ? C32 C33 C34 124.0(8) . . ? C35 C34 C33 113.9(8) . . ? C35 C34 C38 124.4(8) . . ? C33 C34 C38 121.8(8) . . ? C48 C47 O10 122.7(7) . . ? C48 C47 C46 123.8(8) . . ? O10 C47 C46 113.5(7) . . ? C16 C17 C18 112.0(8) . . ? C16 C17 C21 122.6(8) . . ? C18 C17 C21 125.3(8) . . ? C36 C37 C32 115.4(8) . . ? C36 C37 C42 123.5(9) . . ? C32 C37 C42 121.1(8) . . ? C50 C51 C46 113.7(8) . . ? C50 C51 C56 124.1(8) . . ? C46 C51 C56 122.2(8) . . ? O4 C16 C17 123.7(8) . . ? O4 C16 C15 112.8(7) . . ? C17 C16 C15 123.5(8) . . ? C6 C11 C14 108.9(7) . . ? C6 C11 C12 109.0(8) . . ? C14 C11 C12 110.3(8) . . ? C6 C11 C13 110.8(8) . . ? C14 C11 C13 105.5(8) . . ? C12 C11 C13 112.2(8) . . ? C49 C48 C47 113.9(8) . . ? C49 C48 C52 122.6(9) . . ? C47 C48 C52 123.5(8) . . ? C48 C49 C50 123.3(9) . . ? C20 C19 C18 123.1(9) . . ? C39 C38 C34 110.8(7) . . ? C39 C38 C40 110.1(8) . . ? C34 C38 C40 108.9(7) . . ? C39 C38 C41 108.5(8) . . ? C34 C38 C41 110.2(8) . . ? C40 C38 C41 108.3(8) . . ? O2 C2 C3 124.2(9) . . ? O2 C2 C1 113.7(7) . . ? C3 C2 C1 122.1(8) . . ? O1 C1 C6 122.1(8) . . ? O1 C1 C2 112.8(7) . . ? C6 C1 C2 125.2(8) . . ? C5 C6 C1 111.6(9) . . ? C5 C6 C11 124.8(8) . . ? C1 C6 C11 123.6(8) . . ? C4 C3 C2 112.3(9) . . ? C4 C3 C7 124.9(9) . . ? C2 C3 C7 122.8(9) . . ? O7 C32 C33 114.4(7) . . ? O7 C32 C37 124.9(8) . . ? C33 C32 C37 120.7(7) . . ? C45 C42 C44 107.3(10) . . ? C45 C42 C37 113.4(9) . . ? C44 C42 C37 111.5(9) . . ? C45 C42 C43 107.0(10) . . ? C44 C42 C43 109.1(10) . . ? C37 C42 C43 108.4(8) . . ? C23 C21 C24 110.1(9) . . ? C23 C21 C22 107.9(8) . . ? C24 C21 C22 107.9(8) . . ? C23 C21 C17 109.4(7) . . ? C24 C21 C17 110.4(7) . . ? C22 C21 C17 111.1(8) . . ? C37 C36 C35 123.7(9) . . ? C51 C50 C49 122.8(8) . . ? C10 C7 C8 108.7(10) . . ? C10 C7 C9 106.9(9) . . ? C8 C7 C9 107.2(9) . . ? C10 C7 C3 109.2(9) . . ? C8 C7 C3 110.7(8) . . ? C9 C7 C3 114.0(9) . . ? C19 C20 C15 116.7(8) . . ? C19 C20 C25 123.2(9) . . ? C15 C20 C25 120.1(9) . . ? C6 C5 C4 123.4(9) . . ? O9 C46 C47 112.9(7) . . ? O9 C46 C51 124.6(7) . . ? C47 C46 C51 122.4(8) . . ? C34 C35 C36 122.3(8) . . ? C3 C4 C5 125.4(9) . . ? C19 C18 C17 123.0(8) . . ? C15 O3 Mo1 116.2(5) . . ? C57 C56 C51 112.3(7) . . ? C57 C56 C58 112.0(8) . . ? C51 C56 C58 105.6(7) . . ? C57 C56 C59 109.4(8) . . ? C51 C56 C59 111.6(8) . . ? C58 C56 C59 105.7(8) . . ? C20 C25 C27 108.8(8) . . ? C20 C25 C28 110.1(9) . . ? C27 C25 C28 107.4(10) . . ? C20 C25 C26 109.0(9) . . ? C27 C25 C26 110.2(10) . . ? C28 C25 C26 111.2(9) . . ? C48 C52 C54 111.1(10) . . ? C48 C52 C53 109.0(8) . . ? C54 C52 C53 107.1(11) . . ? C48 C52 C55 114.0(9) . . ? C54 C52 C55 106.2(9) . . ? C53 C52 C55 109.3(10) . . ? O6 S1 C30 101.9(5) . . ? O6 S1 C31 102.0(5) . . ? C30 S1 C31 98.7(8) . . ? O12 S2 C61 103.4(4) . . ? O12 S2 C62 101.9(5) . . ? C61 S2 C62 101.2(7) . . ? _refine_diff_density_max 0.705 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.098 data_Mo(O-i-Pr)2(3,6-DBCat)2 _database_code_CSD 173931 _audit_creation_method SHELXL _chemical_name ; Mo(O-i-Pr)2(3,6-DBCat)2 ; _chemical_formula_sum 'C34 H54 Mo O6' _chemical_formula_weight 654.71 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.1595(2) _cell_length_b 29.0306(6) _cell_length_c 11.8944(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.7030(10) _cell_angle_gamma 90.00 _cell_volume 3442.42(11) _cell_formula_units_Z 4 _cell_measurement_temperature 144(2) _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 1.263 _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.968 _exptl_absorpt_correction_T_max 0.855 _exptl_special_details ; ? ; _diffrn_ambient_temperature 144(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 'Siemens SMART' _diffrn_reflns_number 15777 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 31.22 _reflns_number_total 5242 _reflns_number_observed 4865 _reflns_observed_criterion >2sigma(I) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+2.9400P] 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 fixed _refine_ls_extinction_method none _refine_ls_number_reflns 5242 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_obs 0.0316 _refine_ls_wR_factor_all 0.0916 _refine_ls_wR_factor_obs 0.0869 _refine_ls_goodness_of_fit_all 1.031 _refine_ls_goodness_of_fit_obs 1.018 _refine_ls_restrained_S_all 1.031 _refine_ls_restrained_S_obs 1.018 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.0000 0.066610(5) 0.2500 0.01702(6) Uani 1 d S . O1 O 0.18851(10) 0.07816(4) 0.36496(9) 0.0183(2) Uani 1 d . . O2 O -0.01004(10) 0.11629(4) 0.35804(10) 0.0200(2) Uani 1 d . . O3 O 0.06668(11) 0.02415(4) 0.17673(10) 0.0233(2) Uani 1 d . . C1 C 0.21894(13) 0.11644(5) 0.43818(12) 0.0168(2) Uani 1 d . . C2 C 0.10440(14) 0.13785(5) 0.43513(13) 0.0178(2) Uani 1 d . . C3 C 0.11162(14) 0.17726(5) 0.50602(13) 0.0192(3) Uani 1 d . . C4 C 0.2412(2) 0.19410(5) 0.57771(14) 0.0222(3) Uani 1 d . . H4A H 0.2526(2) 0.22089(5) 0.62737(14) 0.028(5) Uiso 1 calc R . C5 C 0.35495(15) 0.17313(5) 0.57948(14) 0.0218(3) Uani 1 d . . H5A H 0.44025(15) 0.18641(5) 0.63017(14) 0.021(5) Uiso 1 calc R . C6 C 0.34897(14) 0.13361(5) 0.51023(13) 0.0180(2) Uani 1 d . . C7 C -0.0146(2) 0.19947(5) 0.50221(15) 0.0238(3) Uani 1 d . . C8 C -0.0907(2) 0.16421(6) 0.5427(2) 0.0380(4) Uani 1 d . . H8A H -0.1713(2) 0.17865(6) 0.5401(2) 0.042(6) Uiso 1 calc R . H8B H -0.0326(2) 0.15372(6) 0.6285(2) 0.039(6) Uiso 1 calc R . H8C H -0.1166(2) 0.13782(6) 0.4852(2) 0.054(7) Uiso 1 calc R . C9 C -0.1058(2) 0.21639(6) 0.3676(2) 0.0328(4) Uani 1 d . . H9A H -0.1872(2) 0.23019(6) 0.3650(2) 0.049(7) Uiso 1 calc R . H9B H -0.1304(2) 0.19028(6) 0.3093(2) 0.039(6) Uiso 1 calc R . H9C H -0.0579(2) 0.23944(6) 0.3431(2) 0.033(6) Uiso 1 calc R . C10 C 0.0205(2) 0.24088(6) 0.5924(2) 0.0306(3) Uani 1 d . . H10A H -0.0619(2) 0.25362(6) 0.5902(2) 0.033(6) Uiso 1 calc R . H10B H 0.0654(2) 0.26457(6) 0.5663(2) 0.034(6) Uiso 1 calc R . H10C H 0.0804(2) 0.23080(6) 0.6782(2) 0.031(5) Uiso 1 calc R . C11 C 0.47227(14) 0.11127(5) 0.50854(13) 0.0199(3) Uani 1 d . . C12 C 0.4842(2) 0.06078(5) 0.5518(2) 0.0255(3) Uani 1 d . . H12A H 0.5627(2) 0.04664(5) 0.5494(2) 0.036(6) Uiso 1 calc R . H12B H 0.4032(2) 0.04391(5) 0.4955(2) 0.028(5) Uiso 1 calc R . H12C H 0.4942(2) 0.05965(5) 0.6379(2) 0.034(6) Uiso 1 calc R . C13 C 0.6022(2) 0.13615(6) 0.5964(2) 0.0274(3) Uani 1 d . . H13A H 0.6789(2) 0.12061(6) 0.5938(2) 0.035(6) Uiso 1 calc R . H13B H 0.6123(2) 0.13556(6) 0.6826(2) 0.022(5) Uiso 1 calc R . H13C H 0.5984(2) 0.16817(6) 0.5689(2) 0.042(6) Uiso 1 calc R . C14 C 0.4583(2) 0.11336(6) 0.3738(2) 0.0286(3) Uani 1 d . . H14A H 0.5376(2) 0.09950(6) 0.3722(2) 0.034(6) Uiso 1 calc R . H14B H 0.4504(2) 0.14556(6) 0.3466(2) 0.032(5) Uiso 1 calc R . H14C H 0.3779(2) 0.09636(6) 0.3168(2) 0.032(5) Uiso 1 calc R . C15 C 0.1880(2) 0.00364(6) 0.1869(2) 0.0290(3) Uani 1 d . . H15A H 0.2618(2) 0.00939(6) 0.2732(2) 0.034(6) Uiso 1 calc R . C16 C 0.2241(2) 0.02577(8) 0.0910(2) 0.0415(4) Uani 1 d . . H16A H 0.3101(2) 0.01349(8) 0.1008(2) 0.057(8) Uiso 1 calc R . H16B H 0.2314(2) 0.05919(8) 0.1039(2) 0.050(8) Uiso 1 calc R . H16C H 0.1541(2) 0.01897(8) 0.0060(2) 0.046(7) Uiso 1 calc R . C17 C 0.1643(2) -0.04785(6) 0.1673(2) 0.0410(5) Uani 1 d . . H17A H 0.2479(2) -0.06313(6) 0.1804(2) 0.058(9) Uiso 1 calc R . H17B H 0.0951(2) -0.05375(6) 0.0814(2) 0.043(6) Uiso 1 calc R . H17C H 0.1346(2) -0.05993(6) 0.2276(2) 0.040(7) Uiso 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 Mo 0.01415(9) 0.01606(9) 0.01754(9) 0.000 0.00418(7) 0.000 O1 0.0143(4) 0.0188(4) 0.0182(4) -0.0038(4) 0.0041(4) -0.0013(3) O2 0.0167(5) 0.0196(5) 0.0228(5) -0.0026(4) 0.0082(4) -0.0006(4) O3 0.0190(5) 0.0223(5) 0.0232(5) -0.0061(4) 0.0045(4) 0.0015(4) C1 0.0169(6) 0.0164(6) 0.0162(5) 0.0000(4) 0.0067(5) -0.0003(4) C2 0.0174(6) 0.0182(6) 0.0176(6) 0.0010(5) 0.0076(5) -0.0007(5) C3 0.0220(6) 0.0178(6) 0.0197(6) 0.0005(5) 0.0111(5) 0.0004(5) C4 0.0243(7) 0.0204(6) 0.0216(6) -0.0039(5) 0.0102(5) -0.0019(5) C5 0.0204(6) 0.0224(6) 0.0204(6) -0.0041(5) 0.0074(5) -0.0038(5) C6 0.0172(6) 0.0188(6) 0.0172(6) 0.0009(5) 0.0072(5) -0.0005(5) C7 0.0242(7) 0.0218(6) 0.0299(7) -0.0020(5) 0.0162(6) 0.0011(5) C8 0.0421(10) 0.0331(9) 0.0566(12) -0.0048(8) 0.0380(10) -0.0038(7) C9 0.0284(8) 0.0299(8) 0.0349(9) -0.0015(7) 0.0096(7) 0.0084(6) C10 0.0347(9) 0.0268(8) 0.0358(8) -0.0052(6) 0.0208(7) 0.0028(6) C11 0.0166(6) 0.0221(6) 0.0200(6) -0.0008(5) 0.0073(5) -0.0006(5) C12 0.0199(7) 0.0237(7) 0.0278(7) 0.0014(5) 0.0061(6) 0.0021(5) C13 0.0179(6) 0.0277(7) 0.0335(8) -0.0029(6) 0.0088(6) -0.0026(5) C14 0.0251(7) 0.0388(9) 0.0251(7) 0.0006(6) 0.0142(6) 0.0026(6) C15 0.0204(7) 0.0298(8) 0.0277(7) -0.0074(6) 0.0027(6) 0.0062(6) C16 0.0336(9) 0.0497(12) 0.0456(11) -0.0128(9) 0.0216(8) -0.0039(8) C17 0.0438(11) 0.0274(9) 0.0392(10) -0.0040(7) 0.0074(8) 0.0128(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 Mo O3 1.8481(11) 2 ? Mo O3 1.8482(11) . ? Mo O1 1.9551(10) . ? Mo O1 1.9551(10) 2 ? Mo O2 1.9680(10) . ? Mo O2 1.9680(10) 2 ? O1 C1 1.358(2) . ? O2 C2 1.346(2) . ? O3 C15 1.434(2) . ? C1 C6 1.404(2) . ? C1 C2 1.407(2) . ? C2 C3 1.402(2) . ? C3 C4 1.396(2) . ? C3 C7 1.531(2) . ? C4 C5 1.400(2) . ? C5 C6 1.396(2) . ? C6 C11 1.529(2) . ? C7 C8 1.538(2) . ? C7 C10 1.540(2) . ? C7 C9 1.541(2) . ? C11 C13 1.534(2) . ? C11 C12 1.539(2) . ? C11 C14 1.540(2) . ? C15 C16 1.513(3) . ? C15 C17 1.518(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mo O3 96.32(7) 2 . ? O3 Mo O1 108.62(4) 2 . ? O3 Mo O1 84.81(4) . . ? O3 Mo O1 84.81(4) 2 2 ? O3 Mo O1 108.62(4) . 2 ? O1 Mo O1 160.25(6) . 2 ? O3 Mo O2 91.59(5) 2 . ? O3 Mo O2 161.77(5) . . ? O1 Mo O2 77.10(4) . . ? O1 Mo O2 88.39(4) 2 . ? O3 Mo O2 161.77(5) 2 2 ? O3 Mo O2 91.59(5) . 2 ? O1 Mo O2 88.39(4) . 2 ? O1 Mo O2 77.10(4) 2 2 ? O2 Mo O2 85.76(6) . 2 ? C1 O1 Mo 118.00(8) . . ? C2 O2 Mo 118.09(8) . . ? C15 O3 Mo 143.35(9) . . ? O1 C1 C6 125.04(12) . . ? O1 C1 C2 112.50(12) . . ? C6 C1 C2 122.46(12) . . ? O2 C2 C3 124.75(13) . . ? O2 C2 C1 112.64(12) . . ? C3 C2 C1 122.61(13) . . ? C4 C3 C2 114.65(13) . . ? C4 C3 C7 123.87(13) . . ? C2 C3 C7 121.48(13) . . ? C3 C4 C5 122.71(13) . . ? C6 C5 C4 123.08(13) . . ? C5 C6 C1 114.46(12) . . ? C5 C6 C11 123.46(12) . . ? C1 C6 C11 122.05(12) . . ? C3 C7 C8 109.90(13) . . ? C3 C7 C10 111.41(13) . . ? C8 C7 C10 107.75(13) . . ? C3 C7 C9 109.53(12) . . ? C8 C7 C9 109.72(15) . . ? C10 C7 C9 108.50(13) . . ? C6 C11 C13 111.84(12) . . ? C6 C11 C12 110.03(12) . . ? C13 C11 C12 107.91(12) . . ? C6 C11 C14 109.01(12) . . ? C13 C11 C14 108.24(12) . . ? C12 C11 C14 109.77(13) . . ? O3 C15 C16 108.74(14) . . ? O3 C15 C17 107.63(15) . . ? C16 C15 C17 112.9(2) . . ? _refine_diff_density_max 0.538 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.081