data_b2 # start Validation Reply Form _vrf_THETM01_b2 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Data was collected on a Bruker GADDS instrument with Cu-source and MWPC (multiwire proportional counter) detector. Under these experimental conditions the maximum angle that can be collected is 120 degrees two-theta. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H38 O5 Si' _chemical_formula_weight 422.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.6924(6) _cell_length_b 8.9976(6) _cell_length_c 29.0972(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2275.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8454 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 62.65 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8641 _exptl_absorpt_correction_T_max 0.9661 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18633 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 59.95 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 3357 _reflns_number_gt 3140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Olex2 _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^)+(0.0428P)^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 0.00(2) _refine_ls_number_reflns 3357 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Si20 Si 0.46731(6) 0.43551(6) 0.576867(17) 0.01200(13) Uani 1 1 d . . . O16 O 0.95667(16) -0.06151(15) 0.64673(4) 0.0172(3) Uani 1 1 d . . . O19 O 0.57293(14) 0.44345(15) 0.62476(4) 0.0144(3) Uani 1 1 d . . . O5 O 0.93653(15) 0.40998(14) 0.74411(5) 0.0181(3) Uani 1 1 d . . . O15 O 0.74457(17) 0.01047(16) 0.60839(5) 0.0242(4) Uani 1 1 d . . . O6 O 1.08988(16) 0.44716(17) 0.68351(5) 0.0250(3) Uani 1 1 d . . . C14 C 0.8607(2) 0.0404(2) 0.62850(6) 0.0154(4) Uani 1 1 d . . . C1 C 0.9985(2) 0.3702(2) 0.70326(7) 0.0169(5) Uani 1 1 d . . . C10 C 0.6605(2) 0.3117(2) 0.68934(7) 0.0132(4) Uani 1 1 d . . . C7 C 0.9199(2) 0.1964(2) 0.63716(7) 0.0143(4) Uani 1 1 d . . . H7 H 1.0243 0.2060 0.6230 0.017 Uiso 1 1 calc R . . C9 C 0.6780(2) 0.3508(2) 0.64535(7) 0.0123(4) Uani 1 1 d . . . C27 C 0.3109(2) 0.5732(2) 0.59012(7) 0.0161(4) Uani 1 1 d . . . H27 H 0.2741 0.5493 0.6218 0.019 Uiso 1 1 calc R . . C2 C 0.9344(2) 0.2199(2) 0.68913(7) 0.0139(4) Uani 1 1 d . . . H2 H 1.0010 0.1399 0.7023 0.017 Uiso 1 1 calc R . . C22 C 0.7020(3) 0.6156(2) 0.53505(7) 0.0212(5) Uani 1 1 d . . . H22A H 0.6427 0.7065 0.5405 0.032 Uiso 1 1 calc R . . H22B H 0.7689 0.6295 0.5083 0.032 Uiso 1 1 calc R . . H22C H 0.7650 0.5935 0.5621 0.032 Uiso 1 1 calc R . . C3 C 0.7806(2) 0.2194(2) 0.71407(6) 0.0132(4) Uani 1 1 d . . . H3 H 0.7433 0.1157 0.7193 0.016 Uiso 1 1 calc R . . C4 C 0.8292(2) 0.2929(2) 0.75949(7) 0.0169(5) Uani 1 1 d . . . H4 H 0.8867 0.2189 0.7785 0.020 Uiso 1 1 calc R . . C29 C 0.1694(2) 0.5606(2) 0.55858(8) 0.0225(5) Uani 1 1 d . . . H29A H 0.2011 0.5741 0.5265 0.034 Uiso 1 1 calc R . . H29B H 0.0944 0.6375 0.5668 0.034 Uiso 1 1 calc R . . H29C H 0.1224 0.4623 0.5623 0.034 Uiso 1 1 calc R . . C8 C 0.8143(2) 0.3128(2) 0.61578(7) 0.0154(4) Uani 1 1 d . . . H8A H 0.8744 0.4044 0.6100 0.019 Uiso 1 1 calc R . . H8B H 0.7771 0.2755 0.5858 0.019 Uiso 1 1 calc R . . C11 C 0.5281(2) 0.3646(2) 0.71859(7) 0.0169(4) Uani 1 1 d . . . H11A H 0.4676 0.2782 0.7294 0.020 Uiso 1 1 calc R . . H11B H 0.4596 0.4290 0.7001 0.020 Uiso 1 1 calc R . . C25 C 0.3485(3) 0.1700(2) 0.61506(8) 0.0234(5) Uani 1 1 d . . . H25A H 0.4458 0.1369 0.6286 0.035 Uiso 1 1 calc R . . H25B H 0.2811 0.0841 0.6103 0.035 Uiso 1 1 calc R . . H25C H 0.2984 0.2408 0.6358 0.035 Uiso 1 1 calc R . . C18 C 0.7855(3) -0.2535(2) 0.67735(8) 0.0266(5) Uani 1 1 d . . . H18A H 0.8238 -0.2299 0.7082 0.040 Uiso 1 1 calc R . . H18B H 0.7617 -0.3598 0.6755 0.040 Uiso 1 1 calc R . . H18C H 0.6922 -0.1957 0.6712 0.040 Uiso 1 1 calc R . . C17 C 0.9061(3) -0.2154(2) 0.64239(7) 0.0214(5) Uani 1 1 d . . . H17A H 0.9955 -0.2823 0.6464 0.026 Uiso 1 1 calc R . . H17B H 0.8640 -0.2316 0.6112 0.026 Uiso 1 1 calc R . . C21 C 0.5919(2) 0.4863(2) 0.52608(6) 0.0163(5) Uani 1 1 d . . . H21 H 0.6580 0.3976 0.5199 0.020 Uiso 1 1 calc R . . C12 C 0.5896(2) 0.4514(2) 0.75983(7) 0.0223(5) Uani 1 1 d . . . H12A H 0.6416 0.5426 0.7489 0.027 Uiso 1 1 calc R . . H12B H 0.5025 0.4818 0.7796 0.027 Uiso 1 1 calc R . . C26 C 0.4707(3) 0.1402(2) 0.53677(8) 0.0234(5) Uani 1 1 d . . . H26A H 0.4800 0.1853 0.5062 0.035 Uiso 1 1 calc R . . H26B H 0.4160 0.0453 0.5343 0.035 Uiso 1 1 calc R . . H26C H 0.5735 0.1231 0.5495 0.035 Uiso 1 1 calc R . . C24 C 0.3803(2) 0.2455(2) 0.56865(7) 0.0177(5) Uani 1 1 d . . . H24 H 0.2778 0.2614 0.5538 0.021 Uiso 1 1 calc R . . C28 C 0.3667(3) 0.7343(2) 0.59165(7) 0.0207(5) Uani 1 1 d . . . H28A H 0.4568 0.7415 0.6118 0.031 Uiso 1 1 calc R . . H28B H 0.2844 0.7980 0.6036 0.031 Uiso 1 1 calc R . . H28C H 0.3945 0.7667 0.5606 0.031 Uiso 1 1 calc R . . C13 C 0.7021(3) 0.3593(2) 0.78784(7) 0.0222(5) Uani 1 1 d . . . H13A H 0.7479 0.4229 0.8120 0.027 Uiso 1 1 calc R . . H13B H 0.6452 0.2782 0.8033 0.027 Uiso 1 1 calc R . . C23 C 0.4979(3) 0.5129(3) 0.48196(7) 0.0243(5) Uani 1 1 d . . . H23A H 0.4249 0.4310 0.4777 0.036 Uiso 1 1 calc R . . H23B H 0.5675 0.5177 0.4555 0.036 Uiso 1 1 calc R . . H23C H 0.4414 0.6067 0.4846 0.036 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 Si20 0.0137(3) 0.0107(3) 0.0115(3) 0.0007(2) -0.0012(2) 0.0002(2) O16 0.0202(7) 0.0131(7) 0.0183(7) -0.0011(6) -0.0042(6) 0.0030(7) O19 0.0174(7) 0.0121(7) 0.0137(7) 0.0010(6) -0.0038(5) 0.0033(6) O5 0.0220(8) 0.0147(8) 0.0175(8) -0.0028(6) -0.0022(6) -0.0027(6) O15 0.0245(8) 0.0195(8) 0.0287(8) -0.0026(6) -0.0131(7) 0.0011(6) O6 0.0237(8) 0.0204(8) 0.0310(8) 0.0000(7) 0.0037(7) -0.0081(7) C14 0.0196(11) 0.0169(11) 0.0097(10) -0.0019(8) 0.0035(9) 0.0038(9) C1 0.0150(12) 0.0165(11) 0.0191(11) 0.0003(8) -0.0028(9) 0.0036(9) C10 0.0141(11) 0.0106(10) 0.0150(11) -0.0008(8) -0.0008(8) -0.0028(8) C7 0.0155(11) 0.0140(10) 0.0133(10) 0.0018(8) -0.0001(8) 0.0018(8) C9 0.0135(11) 0.0101(10) 0.0131(11) -0.0003(8) -0.0033(8) -0.0010(8) C27 0.0210(11) 0.0149(10) 0.0125(10) 0.0009(8) 0.0003(8) 0.0048(9) C2 0.0146(11) 0.0129(10) 0.0142(10) 0.0015(8) -0.0020(8) 0.0007(8) C22 0.0259(12) 0.0184(12) 0.0192(12) 0.0018(8) 0.0019(9) -0.0024(9) C3 0.0173(11) 0.0090(11) 0.0132(10) 0.0016(8) -0.0003(8) -0.0006(8) C4 0.0198(12) 0.0168(11) 0.0142(10) 0.0027(8) -0.0021(8) -0.0010(9) C29 0.0180(11) 0.0205(11) 0.0292(12) 0.0013(10) -0.0001(9) 0.0039(10) C8 0.0206(12) 0.0122(10) 0.0134(10) 0.0021(8) 0.0013(8) 0.0004(8) C11 0.0145(10) 0.0173(10) 0.0189(11) 0.0038(8) 0.0028(9) 0.0019(9) C25 0.0204(12) 0.0187(12) 0.0311(13) 0.0040(10) 0.0003(10) -0.0064(9) C18 0.0316(13) 0.0176(12) 0.0304(13) 0.0009(9) -0.0038(11) -0.0063(10) C17 0.0331(13) 0.0078(11) 0.0233(11) -0.0039(8) -0.0059(10) 0.0035(9) C21 0.0204(11) 0.0157(11) 0.0126(10) 0.0011(8) 0.0006(8) 0.0013(9) C12 0.0236(11) 0.0234(12) 0.0198(11) -0.0008(9) 0.0066(9) 0.0019(10) C26 0.0297(13) 0.0157(11) 0.0248(12) -0.0052(8) -0.0054(10) 0.0010(10) C24 0.0148(11) 0.0167(11) 0.0217(11) 0.0001(8) -0.0051(9) -0.0007(9) C28 0.0244(12) 0.0174(11) 0.0204(11) -0.0024(9) -0.0034(9) 0.0065(9) C13 0.0302(13) 0.0241(12) 0.0122(11) -0.0015(9) 0.0012(10) -0.0019(10) C23 0.0277(13) 0.0291(12) 0.0161(11) 0.0012(9) -0.0003(9) 0.0018(10) _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 Si20 O19 1.6704(13) . ? Si20 C27 1.880(2) . ? Si20 C24 1.885(2) . ? Si20 C21 1.888(2) . ? O16 C14 1.348(2) . ? O16 C17 1.459(2) . ? O19 C9 1.375(2) . ? O5 C1 1.353(2) . ? O5 C4 1.476(2) . ? O15 C14 1.198(2) . ? O6 C1 1.201(2) . ? C14 C7 1.516(3) . ? C1 C2 1.519(3) . ? C10 C9 1.336(3) . ? C10 C11 1.509(3) . ? C10 C3 1.515(3) . ? C7 C8 1.525(3) . ? C7 C2 1.532(3) . ? C7 H7 1.0000 . ? C9 C8 1.504(3) . ? C27 C28 1.529(3) . ? C27 C29 1.539(3) . ? C27 H27 1.0000 . ? C2 C3 1.521(3) . ? C2 H2 1.0000 . ? C22 C21 1.529(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C3 C4 1.537(3) . ? C3 H3 1.0000 . ? C4 C13 1.503(3) . ? C4 H4 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C11 C12 1.528(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C25 C24 1.537(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C18 C17 1.500(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C21 C23 1.540(3) . ? C21 H21 1.0000 . ? C12 C13 1.519(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C26 C24 1.541(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C24 H24 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 O19 Si20 C27 101.44(8) . . ? O19 Si20 C24 111.42(8) . . ? C27 Si20 C24 109.48(10) . . ? O19 Si20 C21 109.11(8) . . ? C27 Si20 C21 114.58(9) . . ? C24 Si20 C21 110.51(9) . . ? C14 O16 C17 115.14(16) . . ? C9 O19 Si20 134.68(12) . . ? C1 O5 C4 109.20(15) . . ? O15 C14 O16 124.13(18) . . ? O15 C14 C7 125.12(18) . . ? O16 C14 C7 110.74(17) . . ? O6 C1 O5 122.08(19) . . ? O6 C1 C2 128.81(19) . . ? O5 C1 C2 109.11(17) . . ? C9 C10 C11 122.97(18) . . ? C9 C10 C3 121.39(18) . . ? C11 C10 C3 115.50(16) . . ? C14 C7 C8 111.33(16) . . ? C14 C7 C2 108.64(15) . . ? C8 C7 C2 110.92(16) . . ? C14 C7 H7 108.6 . . ? C8 C7 H7 108.6 . . ? C2 C7 H7 108.6 . . ? C10 C9 O19 120.11(17) . . ? C10 C9 C8 125.32(18) . . ? O19 C9 C8 114.34(16) . . ? C28 C27 C29 109.90(16) . . ? C28 C27 Si20 113.66(15) . . ? C29 C27 Si20 114.05(14) . . ? C28 C27 H27 106.2 . . ? C29 C27 H27 106.2 . . ? Si20 C27 H27 106.2 . . ? C1 C2 C3 101.30(15) . . ? C1 C2 C7 114.84(16) . . ? C3 C2 C7 113.48(17) . . ? C1 C2 H2 109.0 . . ? C3 C2 H2 109.0 . . ? C7 C2 H2 109.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C3 C2 112.17(16) . . ? C10 C3 C4 111.24(16) . . ? C2 C3 C4 99.62(16) . . ? C10 C3 H3 111.1 . . ? C2 C3 H3 111.1 . . ? C4 C3 H3 111.1 . . ? O5 C4 C13 110.33(16) . . ? O5 C4 C3 102.71(15) . . ? C13 C4 C3 116.15(17) . . ? O5 C4 H4 109.1 . . ? C13 C4 H4 109.1 . . ? C3 C4 H4 109.1 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C9 C8 C7 113.37(16) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C11 C12 109.74(17) . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O16 C17 C18 111.65(17) . . ? O16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? O16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C22 C21 C23 110.88(17) . . ? C22 C21 Si20 114.17(14) . . ? C23 C21 Si20 112.68(14) . . ? C22 C21 H21 106.1 . . ? C23 C21 H21 106.1 . . ? Si20 C21 H21 106.1 . . ? C13 C12 C11 111.56(18) . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C24 C26 110.41(17) . . ? C25 C24 Si20 111.21(14) . . ? C26 C24 Si20 115.43(15) . . ? C25 C24 H24 106.4 . . ? C26 C24 H24 106.4 . . ? Si20 C24 H24 106.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C4 C13 C12 113.31(17) . . ? C4 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? C4 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C27 Si20 O19 C9 159.30(17) . . . . ? C24 Si20 O19 C9 42.88(19) . . . . ? C21 Si20 O19 C9 -79.42(18) . . . . ? C17 O16 C14 O15 -2.8(3) . . . . ? C17 O16 C14 C7 176.94(16) . . . . ? C4 O5 C1 O6 -179.92(18) . . . . ? C4 O5 C1 C2 -0.3(2) . . . . ? O15 C14 C7 C8 -1.5(3) . . . . ? O16 C14 C7 C8 178.72(16) . . . . ? O15 C14 C7 C2 120.9(2) . . . . ? O16 C14 C7 C2 -58.8(2) . . . . ? C11 C10 C9 O19 0.1(3) . . . . ? C3 C10 C9 O19 -175.24(16) . . . . ? C11 C10 C9 C8 174.27(18) . . . . ? C3 C10 C9 C8 -1.1(3) . . . . ? Si20 O19 C9 C10 -127.29(17) . . . . ? Si20 O19 C9 C8 57.9(2) . . . . ? O19 Si20 C27 C28 69.21(15) . . . . ? C24 Si20 C27 C28 -172.95(14) . . . . ? C21 Si20 C27 C28 -48.17(17) . . . . ? O19 Si20 C27 C29 -163.74(14) . . . . ? C24 Si20 C27 C29 -45.91(17) . . . . ? C21 Si20 C27 C29 78.87(17) . . . . ? O6 C1 C2 C3 -154.3(2) . . . . ? O5 C1 C2 C3 26.09(19) . . . . ? O6 C1 C2 C7 -31.6(3) . . . . ? O5 C1 C2 C7 148.79(16) . . . . ? C14 C7 C2 C1 177.79(16) . . . . ? C8 C7 C2 C1 -59.5(2) . . . . ? C14 C7 C2 C3 -66.3(2) . . . . ? C8 C7 C2 C3 56.4(2) . . . . ? C9 C10 C3 C2 17.4(3) . . . . ? C11 C10 C3 C2 -158.24(16) . . . . ? C9 C10 C3 C4 128.05(19) . . . . ? C11 C10 C3 C4 -47.6(2) . . . . ? C1 C2 C3 C10 78.57(19) . . . . ? C7 C2 C3 C10 -45.1(2) . . . . ? C1 C2 C3 C4 -39.20(17) . . . . ? C7 C2 C3 C4 -162.83(15) . . . . ? C1 O5 C4 C13 -149.86(16) . . . . ? C1 O5 C4 C3 -25.43(19) . . . . ? C10 C3 C4 O5 -78.63(18) . . . . ? C2 C3 C4 O5 39.82(17) . . . . ? C10 C3 C4 C13 41.9(2) . . . . ? C2 C3 C4 C13 160.32(17) . . . . ? C10 C9 C8 C7 12.1(3) . . . . ? O19 C9 C8 C7 -173.47(16) . . . . ? C14 C7 C8 C9 82.9(2) . . . . ? C2 C7 C8 C9 -38.2(2) . . . . ? C9 C10 C11 C12 -119.9(2) . . . . ? C3 C10 C11 C12 55.7(2) . . . . ? C14 O16 C17 C18 -78.6(2) . . . . ? O19 Si20 C21 C22 -40.72(17) . . . . ? C27 Si20 C21 C22 72.19(17) . . . . ? C24 Si20 C21 C22 -163.56(14) . . . . ? O19 Si20 C21 C23 -168.39(14) . . . . ? C27 Si20 C21 C23 -55.48(18) . . . . ? C24 Si20 C21 C23 68.77(17) . . . . ? C10 C11 C12 C13 -56.4(2) . . . . ? O19 Si20 C24 C25 30.53(17) . . . . ? C27 Si20 C24 C25 -80.86(16) . . . . ? C21 Si20 C24 C25 152.02(14) . . . . ? O19 Si20 C24 C26 -96.24(15) . . . . ? C27 Si20 C24 C26 152.36(15) . . . . ? C21 Si20 C24 C26 25.24(17) . . . . ? O5 C4 C13 C12 70.8(2) . . . . ? C3 C4 C13 C12 -45.5(3) . . . . ? C11 C12 C13 C4 52.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 59.95 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.167 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.052 _chemical_absolute_configuration ad