data_xyl1_f _publ_contact_author_name 'Takayuki Kawashima' _publ_contact_author_email 'takayuki@chem.s.u-tokyo.ac.jp' _publ_contact_author_fax '+81-5800-6899' _publ_contact_author_phone '+81-5841-4338' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, The University of Tokyo 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan ; _publ_contact_letter ; ; _publ_requested_journal 'Organometallics' _publ_requested_coeditor_name 'Dietmar Seyferth' _publ_section_title ; Disilane Containing Two High Coordinate Silicon Atoms Bridged by Carboxylate Ligands: Synthesis and Structure ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Naokazu Kano' ; ; ; Department of Chemistry, Graduate School of Science, The University of Tokyo 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan ; 'Norikiyo Nakagawa' ; ; ; Department of Chemistry, Graduate School of Science, The University of Tokyo 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan ; 'Yasuhiro Shinozaki' ; ; ; Department of Chemistry, Graduate School of Science, The University of Tokyo 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan ; 'Takayuki Kawashima' ; ; ; Department of Chemistry, Graduate School of Science, The University of Tokyo 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan ; 'Yuki Sato' ; ; ; Department of Chemistry, Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan ; 'Yuji Naruse' ; ; ; Department of Chemistry, Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan ; 'Satoshi Inagaki' ; ; ; Department of Chemistry, Faculty of Engineering, Gifu University, 1-1 Yanagido, Gifu 501-1193, Japan ; _publ_section_synopsis ; ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,2-dimethyl-1,1,2,2-tetrakis[(2,6-dimethylbenzoyl)oxy]disilane ; _chemical_name_common ? _chemical_melting_point 127-128 _chemical_formula_moiety 'C38 H42 O8 Si2, C6 H6' _chemical_formula_sum 'C44 H48 O8 Si2' _chemical_formula_weight 761.00 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21/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 13.236(5) _cell_length_b 10.745(5) _cell_length_c 14.515(5) _cell_angle_alpha 90 _cell_angle_beta 104.961(5) _cell_angle_gamma 90 _cell_volume 1994.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8217 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.1254 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2392 _reflns_number_gt 1700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalStructure' _computing_cell_refinement 'CrystalStructure' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2392 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _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 Si1 Si -0.04754(7) 0.05362(9) 0.43331(7) 0.0255(3) Uani 1 1 d . . . C1 C -0.1794(2) 0.1244(3) 0.4056(2) 0.0300(10) Uani 1 1 d . . . H1 H -0.1976 0.1539 0.3409 0.045 Uiso 1 1 calc R . . H2 H -0.1795 0.1928 0.4480 0.045 Uiso 1 1 calc R . . H3 H -0.2294 0.0632 0.4133 0.045 Uiso 1 1 calc R . . O1 O 0.01897(16) 0.20347(18) 0.48509(16) 0.0256(6) Uani 1 1 d . . . O2 O 0.10381(15) 0.10524(18) 0.61938(16) 0.0240(6) Uani 1 1 d . . . C2 C 0.0807(2) 0.2013(3) 0.5682(3) 0.0244(9) Uani 1 1 d . . . C3 C 0.1315(3) 0.3235(3) 0.6072(2) 0.0234(9) Uani 1 1 d . . . C4 C 0.0687(3) 0.4208(3) 0.6247(2) 0.0285(9) Uani 1 1 d . . . C5 C 0.1172(3) 0.5329(3) 0.6592(3) 0.0355(10) Uani 1 1 d . . . H4 H 0.0776 0.5983 0.6732 0.043 Uiso 1 1 calc R . . C6 C 0.2237(3) 0.5472(3) 0.6728(3) 0.0371(10) Uani 1 1 d . . . H5 H 0.2552 0.6226 0.6948 0.045 Uiso 1 1 calc R . . C7 C 0.2840(3) 0.4499(3) 0.6538(2) 0.0320(9) Uani 1 1 d . . . H6 H 0.3556 0.4609 0.6633 0.038 Uiso 1 1 calc R . . C8 C 0.2392(3) 0.3363(3) 0.6209(2) 0.0267(9) Uani 1 1 d . . . C9 C -0.0479(2) 0.4072(3) 0.6093(3) 0.0379(10) Uani 1 1 d . . . H7 H -0.0728 0.4697 0.6453 0.057 Uiso 1 1 calc R . . H8 H -0.0633 0.3262 0.6300 0.057 Uiso 1 1 calc R . . H9 H -0.0818 0.4171 0.5427 0.057 Uiso 1 1 calc R . . C10 C 0.3076(2) 0.2316(3) 0.6023(3) 0.0367(10) Uani 1 1 d . . . H10 H 0.3772 0.2622 0.6085 0.055 Uiso 1 1 calc R . . H11 H 0.2797 0.2000 0.5390 0.055 Uiso 1 1 calc R . . H12 H 0.3095 0.1661 0.6477 0.055 Uiso 1 1 calc R . . O3 O 0.00147(16) 0.07543(18) 0.33674(15) 0.0237(6) Uani 1 1 d . . . O4 O 0.12235(17) -0.0730(2) 0.37534(18) 0.0394(7) Uani 1 1 d . . . C11 C 0.0807(3) 0.0089(3) 0.3216(3) 0.0278(9) Uani 1 1 d . . . C12 C 0.1109(2) 0.0439(3) 0.2328(3) 0.0252(9) Uani 1 1 d . . . C13 C 0.0919(2) -0.0390(3) 0.1567(3) 0.0288(9) Uani 1 1 d . . . C14 C 0.1249(3) -0.0082(3) 0.0764(3) 0.0376(10) Uani 1 1 d . . . H13 H 0.1126 -0.0626 0.0249 0.045 Uiso 1 1 calc R . . C15 C 0.1760(3) 0.1028(4) 0.0725(3) 0.0432(11) Uani 1 1 d . . . H14 H 0.1985 0.1222 0.0187 0.052 Uiso 1 1 calc R . . C16 C 0.1939(3) 0.1851(3) 0.1478(3) 0.0393(11) Uani 1 1 d . . . H15 H 0.2288 0.2594 0.1444 0.047 Uiso 1 1 calc R . . C17 C 0.1605(3) 0.1582(3) 0.2286(3) 0.0326(10) Uani 1 1 d . . . C18 C 0.0372(3) -0.1629(3) 0.1612(3) 0.0423(11) Uani 1 1 d . . . H16 H 0.0842 -0.2183 0.2035 0.063 Uiso 1 1 calc R . . H17 H 0.0168 -0.1989 0.0986 0.063 Uiso 1 1 calc R . . H18 H -0.0236 -0.1493 0.1842 0.063 Uiso 1 1 calc R . . C19 C 0.1808(3) 0.2488(3) 0.3109(3) 0.0503(12) Uani 1 1 d . . . H19 H 0.1167 0.2653 0.3280 0.075 Uiso 1 1 calc R . . H20 H 0.2080 0.3251 0.2926 0.075 Uiso 1 1 calc R . . H21 H 0.2308 0.2136 0.3646 0.075 Uiso 1 1 calc R . . C20 C 0.3949(3) -0.0291(3) 0.4808(4) 0.0551(14) Uani 1 1 d . . . H22 H 0.3240 -0.0480 0.4676 0.066 Uiso 1 1 calc R . . C21 C 0.4554(3) -0.0320(3) 0.5731(4) 0.0521(13) Uani 1 1 d . . . H23 H 0.4261 -0.0540 0.6225 0.062 Uiso 1 1 calc R . . C22 C 0.5608(3) -0.0017(3) 0.5921(3) 0.0547(13) Uani 1 1 d . . . H24 H 0.6019 -0.0023 0.6547 0.066 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 Si1 0.0238(6) 0.0267(6) 0.0268(7) 0.0015(5) 0.0079(5) -0.0002(5) C1 0.026(2) 0.030(2) 0.035(3) 0.0026(19) 0.0087(19) 0.0023(17) O1 0.0254(14) 0.0229(14) 0.0271(17) 0.0024(12) 0.0044(12) -0.0002(11) O2 0.0257(14) 0.0218(13) 0.0235(16) 0.0048(12) 0.0042(12) 0.0007(11) C2 0.018(2) 0.031(2) 0.028(3) 0.002(2) 0.0117(19) 0.0060(18) C3 0.032(2) 0.020(2) 0.018(2) 0.0038(17) 0.0065(18) -0.0039(18) C4 0.027(2) 0.032(2) 0.025(2) 0.0030(18) 0.0045(18) -0.0010(19) C5 0.041(3) 0.030(2) 0.035(3) -0.001(2) 0.008(2) 0.0023(19) C6 0.047(3) 0.024(2) 0.035(3) -0.002(2) 0.002(2) -0.009(2) C7 0.032(2) 0.039(2) 0.022(2) 0.006(2) 0.0019(19) -0.010(2) C8 0.028(2) 0.029(2) 0.021(2) 0.0070(18) 0.0033(18) -0.0013(19) C9 0.040(3) 0.034(2) 0.043(3) 0.000(2) 0.016(2) 0.0071(19) C10 0.030(2) 0.041(2) 0.038(3) 0.001(2) 0.007(2) -0.0052(19) O3 0.0252(13) 0.0240(13) 0.0238(15) 0.0016(11) 0.0097(12) 0.0035(11) O4 0.0370(16) 0.0468(17) 0.0373(19) 0.0157(14) 0.0149(14) 0.0165(13) C11 0.021(2) 0.033(2) 0.029(3) -0.004(2) 0.0063(19) -0.0023(18) C12 0.019(2) 0.030(2) 0.028(2) 0.003(2) 0.0078(18) 0.0017(17) C13 0.026(2) 0.031(2) 0.030(3) 0.004(2) 0.0077(19) 0.0042(17) C14 0.039(3) 0.046(3) 0.028(3) -0.005(2) 0.009(2) 0.009(2) C15 0.039(3) 0.058(3) 0.037(3) 0.014(2) 0.018(2) 0.010(2) C16 0.037(3) 0.038(3) 0.044(3) 0.011(2) 0.013(2) 0.000(2) C17 0.026(2) 0.039(2) 0.036(3) 0.004(2) 0.013(2) 0.0036(19) C18 0.046(3) 0.036(2) 0.043(3) -0.001(2) 0.008(2) 0.003(2) C19 0.060(3) 0.044(3) 0.052(3) -0.008(2) 0.022(3) -0.018(2) C20 0.036(3) 0.047(3) 0.088(4) -0.007(3) 0.027(3) 0.000(2) C21 0.043(3) 0.036(3) 0.084(4) 0.004(3) 0.028(3) 0.004(2) C22 0.042(3) 0.046(3) 0.074(4) -0.007(3) 0.013(3) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O3 1.706(2) . ? Si1 C1 1.850(3) . ? Si1 O1 1.895(2) . ? Si1 O2 1.939(2) 3_556 ? Si1 Si1 2.324(2) 3_556 ? C1 H1 0.9600 . ? C1 H2 0.9600 . ? C1 H3 0.9600 . ? O1 C2 1.271(4) . ? O2 C2 1.262(4) . ? O2 Si1 1.939(2) 3_556 ? C2 C3 1.517(4) . ? C3 C8 1.394(4) . ? C3 C4 1.400(4) . ? C4 C5 1.395(4) . ? C4 C9 1.509(4) . ? C5 C6 1.380(4) . ? C5 H4 0.9300 . ? C6 C7 1.385(4) . ? C6 H5 0.9300 . ? C7 C8 1.386(4) . ? C7 H6 0.9300 . ? C8 C10 1.512(4) . ? C9 H7 0.9600 . ? C9 H8 0.9600 . ? C9 H9 0.9600 . ? C10 H10 0.9600 . ? C10 H11 0.9600 . ? C10 H12 0.9600 . ? O3 C11 1.333(4) . ? O4 C11 1.211(4) . ? C11 C12 1.493(5) . ? C12 C13 1.391(4) . ? C12 C17 1.402(4) . ? C13 C14 1.386(4) . ? C13 C18 1.524(4) . ? C14 C15 1.379(4) . ? C14 H13 0.9300 . ? C15 C16 1.378(5) . ? C15 H14 0.9300 . ? C16 C17 1.387(5) . ? C16 H15 0.9300 . ? C17 C19 1.510(4) . ? C18 H16 0.9600 . ? C18 H17 0.9600 . ? C18 H18 0.9600 . ? C19 H19 0.9600 . ? C19 H20 0.9600 . ? C19 H21 0.9600 . ? C20 C21 1.372(5) . ? C20 C22 1.376(5) 3_656 ? C20 H22 0.9300 . ? C21 C22 1.389(5) . ? C21 H23 0.9300 . ? C22 C20 1.376(5) 3_656 ? C22 H24 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 O3 Si1 C1 107.57(14) . . ? O3 Si1 O1 88.45(10) . . ? C1 Si1 O1 93.01(12) . . ? O3 Si1 O2 89.18(10) . 3_556 ? C1 Si1 O2 91.80(12) . 3_556 ? O1 Si1 O2 175.10(10) . 3_556 ? O3 Si1 Si1 120.90(10) . 3_556 ? C1 Si1 Si1 131.51(13) . 3_556 ? O1 Si1 Si1 89.70(9) . 3_556 ? O2 Si1 Si1 87.84(9) 3_556 3_556 ? Si1 C1 H1 109.5 . . ? Si1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? Si1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C2 O1 Si1 118.7(2) . . ? C2 O2 Si1 118.5(2) . 3_556 ? O2 C2 O1 125.0(3) . . ? O2 C2 C3 118.1(3) . . ? O1 C2 C3 116.9(3) . . ? C8 C3 C4 122.2(3) . . ? C8 C3 C2 118.6(3) . . ? C4 C3 C2 119.2(3) . . ? C5 C4 C3 118.1(3) . . ? C5 C4 C9 119.7(3) . . ? C3 C4 C9 122.2(3) . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H4 119.8 . . ? C4 C5 H4 119.8 . . ? C5 C6 C7 120.5(3) . . ? C5 C6 H5 119.8 . . ? C7 C6 H5 119.8 . . ? C6 C7 C8 121.1(3) . . ? C6 C7 H6 119.5 . . ? C8 C7 H6 119.5 . . ? C7 C8 C3 117.8(3) . . ? C7 C8 C10 119.6(3) . . ? C3 C8 C10 122.6(3) . . ? C4 C9 H7 109.5 . . ? C4 C9 H8 109.5 . . ? H7 C9 H8 109.5 . . ? C4 C9 H9 109.5 . . ? H7 C9 H9 109.5 . . ? H8 C9 H9 109.5 . . ? C8 C10 H10 109.5 . . ? C8 C10 H11 109.5 . . ? H10 C10 H11 109.5 . . ? C8 C10 H12 109.5 . . ? H10 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C11 O3 Si1 122.9(2) . . ? O4 C11 O3 122.1(3) . . ? O4 C11 C12 124.1(3) . . ? O3 C11 C12 113.9(3) . . ? C13 C12 C17 121.2(3) . . ? C13 C12 C11 119.4(3) . . ? C17 C12 C11 119.4(3) . . ? C14 C13 C12 118.9(3) . . ? C14 C13 C18 120.1(3) . . ? C12 C13 C18 121.0(3) . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H13 119.8 . . ? C13 C14 H13 119.8 . . ? C16 C15 C14 120.6(4) . . ? C16 C15 H14 119.7 . . ? C14 C15 H14 119.7 . . ? C15 C16 C17 120.7(4) . . ? C15 C16 H15 119.7 . . ? C17 C16 H15 119.7 . . ? C16 C17 C12 118.3(3) . . ? C16 C17 C19 120.3(3) . . ? C12 C17 C19 121.4(3) . . ? C13 C18 H16 109.5 . . ? C13 C18 H17 109.5 . . ? H16 C18 H17 109.5 . . ? C13 C18 H18 109.5 . . ? H16 C18 H18 109.5 . . ? H17 C18 H18 109.5 . . ? C17 C19 H19 109.5 . . ? C17 C19 H20 109.5 . . ? H19 C19 H20 109.5 . . ? C17 C19 H21 109.5 . . ? H19 C19 H21 109.5 . . ? H20 C19 H21 109.5 . . ? C21 C20 C22 119.9(4) . 3_656 ? C21 C20 H22 120.0 . . ? C22 C20 H22 120.0 3_656 . ? C20 C21 C22 119.5(4) . . ? C20 C21 H23 120.3 . . ? C22 C21 H23 120.3 . . ? C20 C22 C21 120.6(4) 3_656 . ? C20 C22 H24 119.7 3_656 . ? C21 C22 H24 119.7 . . ? 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 O3 Si1 O1 C2 -125.4(2) . . . . ? C1 Si1 O1 C2 127.1(2) . . . . ? O2 Si1 O1 C2 -64.4(13) 3_556 . . . ? Si1 Si1 O1 C2 -4.5(2) 3_556 . . . ? Si1 O2 C2 O1 3.2(4) 3_556 . . . ? Si1 O2 C2 C3 -175.5(2) 3_556 . . . ? Si1 O1 C2 O2 1.8(4) . . . . ? Si1 O1 C2 C3 -179.5(2) . . . . ? O2 C2 C3 C8 66.2(4) . . . . ? O1 C2 C3 C8 -112.5(4) . . . . ? O2 C2 C3 C4 -116.2(3) . . . . ? O1 C2 C3 C4 65.1(4) . . . . ? C8 C3 C4 C5 -1.6(5) . . . . ? C2 C3 C4 C5 -179.1(3) . . . . ? C8 C3 C4 C9 179.6(3) . . . . ? C2 C3 C4 C9 2.1(5) . . . . ? C3 C4 C5 C6 1.8(5) . . . . ? C9 C4 C5 C6 -179.3(3) . . . . ? C4 C5 C6 C7 -1.1(6) . . . . ? C5 C6 C7 C8 0.0(6) . . . . ? C6 C7 C8 C3 0.3(5) . . . . ? C6 C7 C8 C10 -179.1(3) . . . . ? C4 C3 C8 C7 0.5(5) . . . . ? C2 C3 C8 C7 178.1(3) . . . . ? C4 C3 C8 C10 179.9(3) . . . . ? C2 C3 C8 C10 -2.6(5) . . . . ? C1 Si1 O3 C11 -161.3(2) . . . . ? O1 Si1 O3 C11 106.0(2) . . . . ? O2 Si1 O3 C11 -69.7(2) 3_556 . . . ? Si1 Si1 O3 C11 17.3(3) 3_556 . . . ? Si1 O3 C11 O4 0.9(4) . . . . ? Si1 O3 C11 C12 -179.9(2) . . . . ? O4 C11 C12 C13 68.0(5) . . . . ? O3 C11 C12 C13 -111.2(3) . . . . ? O4 C11 C12 C17 -110.2(4) . . . . ? O3 C11 C12 C17 70.6(4) . . . . ? C17 C12 C13 C14 1.4(5) . . . . ? C11 C12 C13 C14 -176.9(3) . . . . ? C17 C12 C13 C18 -179.5(3) . . . . ? C11 C12 C13 C18 2.2(5) . . . . ? C12 C13 C14 C15 0.2(5) . . . . ? C18 C13 C14 C15 -178.9(3) . . . . ? C13 C14 C15 C16 -0.7(5) . . . . ? C14 C15 C16 C17 -0.4(6) . . . . ? C15 C16 C17 C12 1.9(5) . . . . ? C15 C16 C17 C19 179.8(3) . . . . ? C13 C12 C17 C16 -2.4(5) . . . . ? C11 C12 C17 C16 175.9(3) . . . . ? C13 C12 C17 C19 179.7(3) . . . . ? C11 C12 C17 C19 -2.0(5) . . . . ? C22 C20 C21 C22 1.0(7) 3_656 . . . ? C20 C21 C22 C20 -1.0(7) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.524 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.524 _refine_diff_density_max 0.356 _refine_diff_density_min -0.223 _refine_diff_density_rms 0.050