data_[(tBuO)2MoOSi(OtBu)3]2_compound2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C40 H90 Mo2 O12 Si2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H90 Mo2 O12 Si2' _chemical_formula_weight 1011.18 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7732(5) _cell_length_b 12.4173(5) _cell_length_c 17.3864(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.30 _cell_angle_gamma 90.00 _cell_volume 2694.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4842 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 24.7 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.54422 _exptl_absorpt_correction_T_max 0.94427 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 154(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 'Bruker SMART CCD' _diffrn_measurement_method \w-scans _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11663 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 24.69 _reflns_number_total 4418 _reflns_number_observed 3143 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL-XS (Bruker, 1995)' _computing_structure_refinement 'SHELXTL-XL (Bruker, 1995)' _computing_molecular_graphics 'SHELXTL-XP (Bruker, 1995)' _computing_publication_material ? _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. High thermal motion in the some t-Bu groups leads to large thermal parameters in the associated atoms. SADABS was used for data correction,hence Tmax/Tmin may differ slightly from expected values. SAINT was used for cell determination, hence su's may be deflated. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^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 'fixed' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4418 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_obs 0.0333 _refine_ls_wR_factor_all 0.0828 _refine_ls_wR_factor_obs 0.0785 _refine_ls_goodness_of_fit_all 0.931 _refine_ls_goodness_of_fit_obs 1.060 _refine_ls_restrained_S_all 0.931 _refine_ls_restrained_S_obs 1.060 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.43195(2) 0.49566(3) 0.03152(4) 0.0177(2) Uani 0.916(2) d P . Mo2 Mo 0.4164(3) 0.4705(3) -0.0188(6) 0.035(2) Uani 0.084(2) d P . Si1 Si 0.33083(6) 0.27105(6) 0.07520(5) 0.0240(2) Uani 1 d . . O1 O 0.3982(2) 0.3439(2) 0.02519(12) 0.0279(5) Uani 1 d . . O2 O 0.3965(2) 0.16284(15) 0.10764(12) 0.0291(5) Uani 1 d . . O3 O 0.21484(15) 0.2332(2) 0.02540(12) 0.0296(5) Uani 1 d . . O4 O 0.3077(2) 0.35022(15) 0.14399(12) 0.0275(5) Uani 1 d . . O5 O 0.4810(2) 0.5502(2) 0.13259(12) 0.0319(5) Uani 1 d . . O6 O 0.3367(2) 0.5896(2) -0.03447(12) 0.0306(5) Uani 1 d . . C1 C 0.5088(3) 0.1454(2) 0.1414(2) 0.0397(9) Uani 1 d . . C2 C 0.5555(3) 0.2402(3) 0.1926(2) 0.0516(11) Uani 1 d . . H2A H 0.5187(3) 0.2482(3) 0.2349(2) 0.077 Uiso 1 calc R . H2B H 0.5472(3) 0.3047(3) 0.1614(2) 0.077 Uiso 1 calc R . H2C H 0.6303(3) 0.2276(3) 0.2137(2) 0.077 Uiso 1 calc R . C3 C 0.5663(3) 0.1318(3) 0.0741(3) 0.0590(12) Uani 1 d . . H3A H 0.5362(3) 0.0717(3) 0.0422(3) 0.089 Uiso 1 calc R . H3B H 0.6411(3) 0.1189(3) 0.0950(3) 0.089 Uiso 1 calc R . H3C H 0.5580(3) 0.1960(3) 0.0427(3) 0.089 Uiso 1 calc R . C4 C 0.5130(3) 0.0423(3) 0.1892(3) 0.077(2) Uani 1 d . . H4A H 0.4762(3) 0.0531(3) 0.2313(3) 0.115 Uiso 1 calc R . H4B H 0.5863(3) 0.0237(3) 0.2107(3) 0.115 Uiso 1 calc R . H4C H 0.4791(3) -0.0148(3) 0.1558(3) 0.115 Uiso 1 calc R . C5 C 0.1774(3) 0.1457(3) -0.0283(2) 0.0342(8) Uani 1 d . . C6 C 0.2480(3) 0.1359(3) -0.0880(2) 0.0535(11) Uani 1 d . . H6A H 0.2464(3) 0.2023(3) -0.1165(2) 0.080 Uiso 1 calc R . H6B H 0.2222(3) 0.0785(3) -0.1240(2) 0.080 Uiso 1 calc R . H6C H 0.3203(3) 0.1207(3) -0.0611(2) 0.080 Uiso 1 calc R . C7 C 0.1771(4) 0.0430(3) 0.0183(2) 0.0649(13) Uani 1 d . . H7A H 0.2493(4) 0.0246(3) 0.0435(2) 0.097 Uiso 1 calc R . H7B H 0.1465(4) -0.0142(3) -0.0164(2) 0.097 Uiso 1 calc R . H7C H 0.1354(4) 0.0533(3) 0.0576(2) 0.097 Uiso 1 calc R . C8 C 0.0646(3) 0.1774(3) -0.0689(2) 0.0592(12) Uani 1 d . . H8A H 0.0668(3) 0.2427(3) -0.0981(2) 0.089 Uiso 1 calc R . H8B H 0.0222(3) 0.1886(3) -0.0302(2) 0.089 Uiso 1 calc R . H8C H 0.0333(3) 0.1210(3) -0.1042(2) 0.089 Uiso 1 calc R . C9 C 0.2405(2) 0.3359(3) 0.2006(2) 0.0321(8) Uani 1 d . . C10 C 0.2464(3) 0.2207(3) 0.2301(2) 0.0537(11) Uani 1 d . . H10A H 0.2193(3) 0.1730(3) 0.1870(2) 0.081 Uiso 1 calc R . H10B H 0.2042(3) 0.2135(3) 0.2694(2) 0.081 Uiso 1 calc R . H10C H 0.3196(3) 0.2026(3) 0.2527(2) 0.081 Uiso 1 calc R . C11 C 0.1260(3) 0.3647(3) 0.1612(2) 0.0484(10) Uani 1 d . . H11A H 0.1003(3) 0.3152(3) 0.1190(2) 0.073 Uiso 1 calc R . H11B H 0.1240(3) 0.4366(3) 0.1407(2) 0.073 Uiso 1 calc R . H11C H 0.0814(3) 0.3605(3) 0.1991(2) 0.073 Uiso 1 calc R . C12 C 0.2827(3) 0.4128(3) 0.2672(2) 0.0558(11) Uani 1 d . . H12A H 0.2783(3) 0.4852(3) 0.2474(2) 0.084 Uiso 1 calc R . H12B H 0.3560(3) 0.3955(3) 0.2899(2) 0.084 Uiso 1 calc R . H12C H 0.2406(3) 0.4064(3) 0.3066(2) 0.084 Uiso 1 calc R . C13 C 0.5602(2) 0.6097(2) 0.1877(2) 0.0282(7) Uani 1 d . . C14 C 0.5422(3) 0.5786(3) 0.2685(2) 0.0497(10) Uani 1 d . . H14A H 0.4713(3) 0.5996(3) 0.2728(2) 0.074 Uiso 1 calc R . H14B H 0.5940(3) 0.6145(3) 0.3084(2) 0.074 Uiso 1 calc R . H14C H 0.5500(3) 0.5021(3) 0.2754(2) 0.074 Uiso 1 calc R . C15 C 0.5388(3) 0.7284(2) 0.1707(2) 0.0420(9) Uani 1 d . . H15A H 0.4676(3) 0.7458(2) 0.1765(2) 0.063 Uiso 1 calc R . H15B H 0.5454(3) 0.7440(2) 0.1179(2) 0.063 Uiso 1 calc R . H15C H 0.5897(3) 0.7706(2) 0.2070(2) 0.063 Uiso 1 calc R . C16 C 0.6716(3) 0.5773(3) 0.1795(2) 0.0495(10) Uani 1 d . . H16A H 0.6821(3) 0.5019(3) 0.1907(2) 0.074 Uiso 1 calc R . H16B H 0.7238(3) 0.6181(3) 0.2159(2) 0.074 Uiso 1 calc R . H16C H 0.6795(3) 0.5915(3) 0.1268(2) 0.074 Uiso 1 calc R . C17 C 0.2276(2) 0.6158(3) -0.0269(2) 0.0381(9) Uani 1 d . . C18 C 0.1607(3) 0.5150(3) -0.0334(3) 0.075(2) Uani 1 d . . H18A H 0.1894(3) 0.4678(3) 0.0096(3) 0.113 Uiso 1 calc R . H18B H 0.1618(3) 0.4795(3) -0.0823(3) 0.113 Uiso 1 calc R . H18C H 0.0882(3) 0.5336(3) -0.0317(3) 0.113 Uiso 1 calc R . C19 C 0.1836(3) 0.6900(3) -0.0936(3) 0.078(2) Uani 1 d . . H19A H 0.2266(3) 0.7540(3) -0.0891(3) 0.117 Uiso 1 calc R . H19B H 0.1112(3) 0.7088(3) -0.0921(3) 0.117 Uiso 1 calc R . H19C H 0.1847(3) 0.6547(3) -0.1426(3) 0.117 Uiso 1 calc R . C20 C 0.2353(4) 0.6699(6) 0.0517(3) 0.137(3) Uani 1 d . . H20A H 0.2638(4) 0.6200(6) 0.0930(3) 0.205 Uiso 1 calc R . H20B H 0.1653(4) 0.6928(6) 0.0568(3) 0.205 Uiso 1 calc R . H20C H 0.2817(4) 0.7313(6) 0.0552(3) 0.205 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 Mo1 0.0146(2) 0.0201(2) 0.0169(3) 0.0004(2) -0.00021(13) 0.00032(14) Mo2 0.030(2) 0.025(2) 0.050(6) 0.003(2) 0.006(2) 0.000(2) Si1 0.0201(4) 0.0216(4) 0.0286(5) 0.0015(4) 0.0015(4) -0.0026(4) O1 0.0226(11) 0.0267(12) 0.0342(13) 0.0053(9) 0.0055(9) -0.0017(9) O2 0.0222(11) 0.0206(11) 0.0416(13) 0.0040(10) 0.0005(10) 0.0005(9) O3 0.0216(11) 0.0335(12) 0.0310(12) -0.0046(10) -0.0003(9) -0.0048(10) O4 0.0258(12) 0.0243(12) 0.0322(12) -0.0023(10) 0.0061(10) -0.0022(9) O5 0.0300(12) 0.0357(12) 0.0272(12) -0.0027(10) 0.0003(10) -0.0041(10) O6 0.0206(11) 0.0352(13) 0.0353(13) 0.0076(10) 0.0044(10) 0.0082(10) C1 0.025(2) 0.025(2) 0.065(3) 0.009(2) -0.001(2) 0.0026(14) C2 0.032(2) 0.053(2) 0.058(3) -0.003(2) -0.018(2) 0.005(2) C3 0.033(2) 0.049(2) 0.096(3) -0.013(2) 0.017(2) 0.004(2) C4 0.042(2) 0.053(2) 0.125(4) 0.048(3) -0.002(3) 0.006(2) C5 0.030(2) 0.035(2) 0.035(2) -0.009(2) -0.0002(15) -0.0127(15) C6 0.044(2) 0.063(3) 0.053(3) -0.022(2) 0.010(2) -0.010(2) C7 0.077(3) 0.046(2) 0.063(3) 0.000(2) -0.003(2) -0.033(2) C8 0.033(2) 0.080(3) 0.057(3) -0.026(2) -0.009(2) -0.008(2) C9 0.031(2) 0.034(2) 0.032(2) -0.004(2) 0.0090(15) -0.0038(15) C10 0.072(3) 0.048(2) 0.050(3) 0.011(2) 0.034(2) 0.001(2) C11 0.031(2) 0.071(3) 0.044(2) 0.002(2) 0.010(2) 0.002(2) C12 0.052(2) 0.066(3) 0.049(2) -0.022(2) 0.011(2) -0.009(2) C13 0.027(2) 0.030(2) 0.025(2) -0.0051(14) 0.0003(14) -0.0056(14) C14 0.061(3) 0.053(2) 0.032(2) -0.003(2) 0.001(2) -0.011(2) C15 0.051(2) 0.032(2) 0.046(2) -0.004(2) 0.016(2) -0.006(2) C16 0.034(2) 0.051(2) 0.057(3) -0.017(2) -0.005(2) -0.004(2) C17 0.022(2) 0.046(2) 0.046(2) 0.005(2) 0.007(2) 0.017(2) C18 0.030(2) 0.068(3) 0.133(4) 0.045(3) 0.030(3) 0.013(2) C19 0.030(2) 0.084(3) 0.115(4) 0.065(3) 0.005(2) 0.014(2) C20 0.057(3) 0.268(8) 0.081(4) -0.078(5) 0.005(3) 0.070(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O5 1.863(2) . ? Mo1 O6 1.887(2) . ? Mo1 O1 1.931(2) . ? Mo1 Mo2 2.039(4) 3_665 ? Mo1 Mo1 2.2464(7) 3_665 ? Mo2 O6 1.783(4) . ? Mo2 O1 1.785(4) . ? Mo2 Mo1 2.039(4) 3_665 ? Mo2 Mo2 2.220(10) 3_665 ? Si1 O3 1.618(2) . ? Si1 O2 1.620(2) . ? Si1 O4 1.623(2) . ? Si1 O1 1.623(2) . ? O2 C1 1.446(4) . ? O3 C5 1.446(3) . ? O4 C9 1.448(4) . ? O5 C13 1.440(3) . ? O6 C17 1.465(3) . ? C1 C3 1.518(5) . ? C1 C2 1.518(5) . ? C1 C4 1.521(5) . ? C5 C7 1.513(5) . ? C5 C8 1.514(5) . ? C5 C6 1.518(5) . ? C9 C12 1.509(4) . ? C9 C10 1.517(4) . ? C9 C11 1.518(4) . ? C13 C16 1.514(4) . ? C13 C15 1.517(4) . ? C13 C14 1.521(4) . ? C17 C19 1.494(5) . ? C17 C18 1.506(5) . ? C17 C20 1.506(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O6 113.13(9) . . ? O5 Mo1 O1 115.75(9) . . ? O6 Mo1 O1 117.48(9) . . ? O5 Mo1 Mo2 83.7(3) . 3_665 ? O6 Mo1 Mo2 108.1(2) . 3_665 ? O1 Mo1 Mo2 113.6(2) . 3_665 ? O5 Mo1 Mo1 107.64(7) . 3_665 ? O6 Mo1 Mo1 98.01(7) . 3_665 ? O1 Mo1 Mo1 101.86(7) . 3_665 ? Mo2 Mo1 Mo1 23.9(3) 3_665 3_665 ? O6 Mo2 O1 132.3(3) . . ? O6 Mo2 Mo1 109.7(2) . 3_665 ? O1 Mo2 Mo1 116.2(2) . 3_665 ? O6 Mo2 Mo2 104.6(3) . 3_665 ? O1 Mo2 Mo2 111.7(4) . 3_665 ? Mo1 Mo2 Mo2 24.2(2) 3_665 3_665 ? O3 Si1 O2 106.99(11) . . ? O3 Si1 O4 106.32(11) . . ? O2 Si1 O4 114.06(11) . . ? O3 Si1 O1 113.88(11) . . ? O2 Si1 O1 110.76(11) . . ? O4 Si1 O1 104.92(11) . . ? Si1 O1 Mo2 148.5(2) . . ? Si1 O1 Mo1 130.60(12) . . ? Mo2 O1 Mo1 28.0(3) . . ? C1 O2 Si1 131.3(2) . . ? C5 O3 Si1 134.7(2) . . ? C9 O4 Si1 130.8(2) . . ? C13 O5 Mo1 149.5(2) . . ? C17 O6 Mo2 134.0(2) . . ? C17 O6 Mo1 125.8(2) . . ? Mo2 O6 Mo1 28.5(3) . . ? O2 C1 C3 107.7(3) . . ? O2 C1 C2 110.8(3) . . ? C3 C1 C2 110.1(3) . . ? O2 C1 C4 105.3(3) . . ? C3 C1 C4 111.1(3) . . ? C2 C1 C4 111.7(3) . . ? O3 C5 C7 109.0(3) . . ? O3 C5 C8 104.9(3) . . ? C7 C5 C8 111.0(3) . . ? O3 C5 C6 109.8(3) . . ? C7 C5 C6 111.6(3) . . ? C8 C5 C6 110.4(3) . . ? O4 C9 C12 106.1(3) . . ? O4 C9 C10 110.6(3) . . ? C12 C9 C10 110.6(3) . . ? O4 C9 C11 108.6(3) . . ? C12 C9 C11 110.5(3) . . ? C10 C9 C11 110.4(3) . . ? O5 C13 C16 110.0(2) . . ? O5 C13 C15 107.3(2) . . ? C16 C13 C15 111.9(3) . . ? O5 C13 C14 105.2(2) . . ? C16 C13 C14 110.4(3) . . ? C15 C13 C14 111.7(3) . . ? O6 C17 C19 106.0(3) . . ? O6 C17 C18 110.1(3) . . ? C19 C17 C18 109.9(3) . . ? O6 C17 C20 107.5(3) . . ? C19 C17 C20 111.8(4) . . ? C18 C17 C20 111.4(4) . . ? _refine_diff_density_max 0.655 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.070