Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Peter Taylor' 'Alan Bassindale' 'Peter N. Horton' 'Michael B. Hursthouse' 'Mark E. Light' 'Zhihua Liu' 'Iain A. MacKinnon' 'Yuxing Yang' _publ_contact_author_name 'Dr Peter Taylor' _publ_contact_author_address ; Department of Chemistry Open University Walton Hall Milton Keynes Bucks MK7 6AA UNITED KINGDOM ; _publ_contact_author_email P.G.TAYLOR@OPEN.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A higher yielding route for T8 silsesquioxane cages and X-ray crystal structures of some novel spherosilicates ; data_s92 _database_code_CSD 206049 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dr. P. G. Taylor ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H72 O12 Si8' _chemical_formula_weight 969.70 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9936(6) _cell_length_b 10.1401(8) _cell_length_c 12.1205(8) _cell_angle_alpha 98.333(6) _cell_angle_beta 92.328(5) _cell_angle_gamma 95.545(2) _cell_volume 1207.73(14) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4918 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9209 _exptl_absorpt_correction_T_max 0.9411 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree phi range. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15579 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4219 _reflns_number_gt 2726 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' DENZO (Otwinowski and Minor, 1997)' _computing_cell_refinement ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_data_reduction ' DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _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^)+(0.0742P)^2^+0.8818P] 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 4219 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.12242(11) 0.19330(10) 0.65859(8) 0.0221(3) Uani 1 1 d . . . Si2 Si 0.24696(10) -0.06838(10) 0.55281(8) 0.0223(3) Uani 1 1 d . . . Si3 Si 0.15038(11) -0.02231(11) 0.31984(8) 0.0225(3) Uani 1 1 d . . . Si4 Si 0.02568(10) 0.23985(10) 0.42560(8) 0.0220(3) Uani 1 1 d . . . O1 O 0.2087(3) 0.0675(2) 0.6265(2) 0.0279(7) Uani 1 1 d . . . O2 O 0.2501(3) -0.0472(3) 0.4223(2) 0.0267(6) Uani 1 1 d . . . O3 O 0.0951(3) 0.1225(3) 0.3497(2) 0.0286(7) Uani 1 1 d . . . O4 O 0.0999(3) 0.2672(3) 0.5494(2) 0.0276(6) Uani 1 1 d . . . O5 O -0.0237(3) 0.1381(3) 0.6971(2) 0.0269(6) Uani 1 1 d . . . O6 O 0.1310(3) -0.1895(3) 0.5639(2) 0.0273(6) Uani 1 1 d . . . C11 C 0.2409(4) -0.0291(4) 0.1905(3) 0.0285(10) Uani 1 1 d . . . H11 H 0.3184 0.0426 0.2029 0.034 Uiso 1 1 calc R . . C6 C 0.4096(4) -0.1126(4) 0.6054(3) 0.0252(9) Uani 1 1 d . . . H6 H 0.4799 -0.0357 0.6043 0.030 Uiso 1 1 calc R . . C2 C 0.3657(4) 0.3404(4) 0.7591(3) 0.0311(10) Uani 1 1 d . . . H2A H 0.4068 0.2585 0.7292 0.037 Uiso 1 1 calc R . . H2B H 0.3813 0.4078 0.7083 0.037 Uiso 1 1 calc R . . C1 C 0.2139(4) 0.3087(4) 0.7744(3) 0.0269(9) Uani 1 1 d . . . H1 H 0.1717 0.3948 0.7832 0.032 Uiso 1 1 calc R . . C7 C 0.4006(4) -0.1438(4) 0.7274(3) 0.0316(10) Uani 1 1 d . . . H7A H 0.4503 -0.0706 0.7809 0.038 Uiso 1 1 calc R . . H7B H 0.3056 -0.1544 0.7477 0.038 Uiso 1 1 calc R . . C3 C 0.4221(4) 0.3961(4) 0.8784(3) 0.0354(10) Uani 1 1 d . . . H3A H 0.5202 0.3897 0.8858 0.042 Uiso 1 1 calc R . . H3B H 0.4052 0.4910 0.8986 0.042 Uiso 1 1 calc R . . C5 C 0.2125(4) 0.2554(5) 0.8870(3) 0.0402(11) Uani 1 1 d . . . H5A H 0.1365 0.2870 0.9298 0.048 Uiso 1 1 calc R . . H5B H 0.2020 0.1562 0.8746 0.048 Uiso 1 1 calc R . . C16 C 0.0414(4) 0.3933(4) 0.3609(3) 0.0300(10) Uani 1 1 d . . . H16 H -0.0173 0.4575 0.4000 0.036 Uiso 1 1 calc R . . C10 C 0.4556(5) -0.2404(4) 0.5372(4) 0.0377(11) Uani 1 1 d . . . H10A H 0.3983 -0.2679 0.4675 0.045 Uiso 1 1 calc R . . H10B H 0.5504 -0.2242 0.5176 0.045 Uiso 1 1 calc R . . C15 C 0.1534(5) -0.0057(5) 0.0876(3) 0.0367(11) Uani 1 1 d . . . H15A H 0.0572 -0.0340 0.0958 0.044 Uiso 1 1 calc R . . H15B H 0.1634 0.0899 0.0780 0.044 Uiso 1 1 calc R . . C12 C 0.2975(5) -0.1648(5) 0.1528(4) 0.0443(12) Uani 1 1 d . . . H12A H 0.3944 -0.1595 0.1754 0.053 Uiso 1 1 calc R . . H12B H 0.2485 -0.2377 0.1860 0.053 Uiso 1 1 calc R . . C8 C 0.4642(6) -0.2738(5) 0.7287(4) 0.0501(13) Uani 1 1 d . . . H8A H 0.5617 -0.2555 0.7497 0.060 Uiso 1 1 calc R . . H8B H 0.4209 -0.3268 0.7825 0.060 Uiso 1 1 calc R . . C17 C -0.0010(6) 0.3703(4) 0.2350(4) 0.0515(14) Uani 1 1 d . . . H17A H 0.0113 0.2779 0.2007 0.062 Uiso 1 1 calc R . . H17B H -0.0964 0.3858 0.2229 0.062 Uiso 1 1 calc R . . C4 C 0.3464(5) 0.3081(5) 0.9512(4) 0.0507(13) Uani 1 1 d . . . H4A H 0.3308 0.3607 1.0241 0.061 Uiso 1 1 calc R . . H4B H 0.3982 0.2330 0.9646 0.061 Uiso 1 1 calc R . . C20 C 0.1871(5) 0.4633(5) 0.3687(4) 0.0522(14) Uani 1 1 d . . . H20A H 0.1935 0.5499 0.4192 0.063 Uiso 1 1 calc R . . H20B H 0.2508 0.4061 0.3980 0.063 Uiso 1 1 calc R . . C14 C 0.2066(7) -0.0912(6) -0.0102(4) 0.0707(18) Uani 1 1 d . . . H14A H 0.1310 -0.1342 -0.0624 0.085 Uiso 1 1 calc R . . H14B H 0.2673 -0.0346 -0.0509 0.085 Uiso 1 1 calc R . . C9 C 0.4410(7) -0.3469(6) 0.6122(5) 0.0705(17) Uani 1 1 d . . . H9A H 0.3498 -0.3960 0.6013 0.085 Uiso 1 1 calc R . . H9B H 0.5082 -0.4117 0.5961 0.085 Uiso 1 1 calc R . . C18 C 0.0927(6) 0.4732(6) 0.1859(5) 0.0669(18) Uani 1 1 d . . . H18A H 0.1076 0.4412 0.1067 0.080 Uiso 1 1 calc R . . H18B H 0.0548 0.5604 0.1911 0.080 Uiso 1 1 calc R . . C13 C 0.2762(9) -0.1886(9) 0.0288(5) 0.131(4) Uani 1 1 d . . . H13A H 0.3647 -0.1894 -0.0051 0.157 Uiso 1 1 calc R . . H13B H 0.2252 -0.2775 0.0051 0.157 Uiso 1 1 calc R . . C19 C 0.2189(7) 0.4850(10) 0.2555(7) 0.126(4) Uani 1 1 d . . . H19A H 0.2775 0.4176 0.2234 0.151 Uiso 1 1 calc R . . H19B H 0.2676 0.5751 0.2574 0.151 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 0.0237(6) 0.0192(6) 0.0222(6) 0.0006(4) -0.0011(4) 0.0014(5) Si2 0.0224(6) 0.0194(6) 0.0244(6) 0.0016(4) -0.0007(4) 0.0019(5) Si3 0.0232(6) 0.0226(6) 0.0216(6) 0.0022(4) 0.0013(4) 0.0025(5) Si4 0.0230(6) 0.0190(6) 0.0230(6) 0.0022(4) -0.0017(4) 0.0005(5) O1 0.0310(16) 0.0180(15) 0.0330(16) -0.0030(11) -0.0010(12) 0.0053(12) O2 0.0251(15) 0.0302(16) 0.0247(15) 0.0037(11) 0.0001(11) 0.0031(12) O3 0.0327(17) 0.0262(16) 0.0281(15) 0.0044(12) 0.0027(12) 0.0088(13) O4 0.0293(16) 0.0241(16) 0.0286(15) 0.0062(11) -0.0055(11) -0.0019(12) O5 0.0237(15) 0.0299(16) 0.0254(15) 0.0010(11) 0.0011(11) -0.0015(12) O6 0.0252(16) 0.0237(15) 0.0323(16) 0.0039(12) -0.0028(11) 0.0010(12) C11 0.025(2) 0.029(2) 0.030(2) 0.0020(18) 0.0020(17) 0.0010(18) C6 0.023(2) 0.023(2) 0.029(2) 0.0026(17) 0.0024(16) 0.0023(18) C2 0.026(2) 0.032(2) 0.033(2) 0.0022(18) -0.0010(17) -0.0011(19) C1 0.028(2) 0.023(2) 0.029(2) -0.0012(17) 0.0004(17) 0.0037(18) C7 0.029(2) 0.037(3) 0.029(2) 0.0032(18) -0.0013(17) 0.003(2) C3 0.031(3) 0.034(3) 0.036(2) -0.0060(19) -0.0069(18) -0.003(2) C5 0.037(3) 0.051(3) 0.028(2) 0.001(2) -0.0028(19) -0.007(2) C16 0.038(3) 0.025(2) 0.025(2) 0.0019(17) 0.0003(17) -0.0004(19) C10 0.034(3) 0.043(3) 0.039(3) 0.007(2) 0.0059(19) 0.014(2) C15 0.043(3) 0.045(3) 0.023(2) 0.0081(19) 0.0041(18) 0.005(2) C12 0.048(3) 0.050(3) 0.037(3) 0.001(2) 0.004(2) 0.024(2) C8 0.066(4) 0.042(3) 0.045(3) 0.015(2) -0.006(2) 0.011(3) C17 0.093(4) 0.024(3) 0.037(3) 0.002(2) -0.011(3) 0.014(3) C4 0.043(3) 0.071(4) 0.036(3) 0.011(2) -0.007(2) -0.007(3) C20 0.056(3) 0.039(3) 0.059(3) 0.007(2) 0.013(3) -0.015(3) C14 0.114(5) 0.073(4) 0.029(3) -0.001(3) 0.002(3) 0.044(4) C9 0.105(5) 0.054(4) 0.059(4) 0.011(3) 0.006(3) 0.038(3) C18 0.085(4) 0.086(4) 0.048(3) 0.038(3) 0.033(3) 0.050(4) C13 0.193(9) 0.171(8) 0.040(4) -0.026(4) -0.018(4) 0.147(8) C19 0.069(5) 0.218(10) 0.128(7) 0.135(7) 0.030(4) 0.030(5) _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 O1 1.618(3) . ? Si1 O5 1.624(3) . ? Si1 O4 1.630(3) . ? Si1 C1 1.841(4) . ? Si2 O1 1.617(3) . ? Si2 O2 1.628(3) . ? Si2 O6 1.629(3) . ? Si2 C6 1.841(4) . ? Si3 O3 1.615(3) . ? Si3 O2 1.624(3) . ? Si3 O5 1.626(3) 2_556 ? Si3 C11 1.838(4) . ? Si4 O6 1.615(3) 2_556 ? Si4 O4 1.622(3) . ? Si4 O3 1.625(3) . ? Si4 C16 1.838(4) . ? O5 Si3 1.626(3) 2_556 ? O6 Si4 1.615(3) 2_556 ? C11 C15 1.553(6) . ? C11 C12 1.553(6) . ? C11 H11 1.0000 . ? C6 C10 1.553(6) . ? C6 C7 1.560(5) . ? C6 H6 1.0000 . ? C2 C3 1.537(6) . ? C2 C1 1.544(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C1 C5 1.538(6) . ? C1 H1 1.0000 . ? C7 C8 1.519(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C3 C4 1.516(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 C4 1.529(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C16 C17 1.545(6) . ? C16 C20 1.550(6) . ? C16 H16 1.0000 . ? C10 C9 1.509(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C15 C14 1.510(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C12 C13 1.491(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C8 C9 1.495(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C17 C18 1.535(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C20 C19 1.463(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C14 C13 1.387(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C18 C19 1.473(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? 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 Si1 O5 108.76(14) . . ? O1 Si1 O4 109.59(14) . . ? O5 Si1 O4 108.65(14) . . ? O1 Si1 C1 108.48(17) . . ? O5 Si1 C1 109.95(16) . . ? O4 Si1 C1 111.37(16) . . ? O1 Si2 O2 109.12(14) . . ? O1 Si2 O6 108.67(14) . . ? O2 Si2 O6 108.61(14) . . ? O1 Si2 C6 110.06(16) . . ? O2 Si2 C6 111.64(16) . . ? O6 Si2 C6 108.68(16) . . ? O3 Si3 O2 109.23(14) . . ? O3 Si3 O5 109.17(15) . 2_556 ? O2 Si3 O5 109.05(14) . 2_556 ? O3 Si3 C11 109.90(16) . . ? O2 Si3 C11 110.11(16) . . ? O5 Si3 C11 109.36(16) 2_556 . ? O6 Si4 O4 108.63(14) 2_556 . ? O6 Si4 O3 108.88(14) 2_556 . ? O4 Si4 O3 108.77(14) . . ? O6 Si4 C16 110.41(17) 2_556 . ? O4 Si4 C16 110.39(16) . . ? O3 Si4 C16 109.72(17) . . ? Si2 O1 Si1 156.06(18) . . ? Si3 O2 Si2 140.51(18) . . ? Si3 O3 Si4 156.05(18) . . ? Si4 O4 Si1 140.81(18) . . ? Si1 O5 Si3 148.45(18) . 2_556 ? Si4 O6 Si2 149.31(19) 2_556 . ? C15 C11 C12 104.4(3) . . ? C15 C11 Si3 113.8(3) . . ? C12 C11 Si3 114.4(3) . . ? C15 C11 H11 108.0 . . ? C12 C11 H11 108.0 . . ? Si3 C11 H11 108.0 . . ? C10 C6 C7 105.3(3) . . ? C10 C6 Si2 113.4(3) . . ? C7 C6 Si2 110.7(3) . . ? C10 C6 H6 109.1 . . ? C7 C6 H6 109.1 . . ? Si2 C6 H6 109.1 . . ? C3 C2 C1 102.9(3) . . ? C3 C2 H2A 111.2 . . ? C1 C2 H2A 111.2 . . ? C3 C2 H2B 111.2 . . ? C1 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? C5 C1 C2 103.0(3) . . ? C5 C1 Si1 113.9(3) . . ? C2 C1 Si1 114.7(3) . . ? C5 C1 H1 108.3 . . ? C2 C1 H1 108.3 . . ? Si1 C1 H1 108.3 . . ? C8 C7 C6 105.6(3) . . ? C8 C7 H7A 110.6 . . ? C6 C7 H7A 110.6 . . ? C8 C7 H7B 110.6 . . ? C6 C7 H7B 110.6 . . ? H7A C7 H7B 108.8 . . ? C4 C3 C2 104.3(3) . . ? C4 C3 H3A 110.9 . . ? C2 C3 H3A 110.9 . . ? C4 C3 H3B 110.9 . . ? C2 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? C4 C5 C1 107.4(4) . . ? C4 C5 H5A 110.2 . . ? C1 C5 H5A 110.2 . . ? C4 C5 H5B 110.2 . . ? C1 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? C17 C16 C20 104.9(4) . . ? C17 C16 Si4 113.8(3) . . ? C20 C16 Si4 113.5(3) . . ? C17 C16 H16 108.1 . . ? C20 C16 H16 108.1 . . ? Si4 C16 H16 108.1 . . ? C9 C10 C6 105.6(4) . . ? C9 C10 H10A 110.6 . . ? C6 C10 H10A 110.6 . . ? C9 C10 H10B 110.6 . . ? C6 C10 H10B 110.6 . . ? H10A C10 H10B 108.8 . . ? C14 C15 C11 104.6(4) . . ? C14 C15 H15A 110.8 . . ? C11 C15 H15A 110.8 . . ? C14 C15 H15B 110.8 . . ? C11 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? C13 C12 C11 105.0(4) . . ? C13 C12 H12A 110.8 . . ? C11 C12 H12A 110.8 . . ? C13 C12 H12B 110.8 . . ? C11 C12 H12B 110.8 . . ? H12A C12 H12B 108.8 . . ? C9 C8 C7 105.1(4) . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8A 110.7 . . ? C9 C8 H8B 110.7 . . ? C7 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? C18 C17 C16 104.4(4) . . ? C18 C17 H17A 110.9 . . ? C16 C17 H17A 110.9 . . ? C18 C17 H17B 110.9 . . ? C16 C17 H17B 110.9 . . ? H17A C17 H17B 108.9 . . ? C3 C4 C5 106.0(4) . . ? C3 C4 H4A 110.5 . . ? C5 C4 H4A 110.5 . . ? C3 C4 H4B 110.5 . . ? C5 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? C19 C20 C16 106.7(5) . . ? C19 C20 H20A 110.4 . . ? C16 C20 H20A 110.4 . . ? C19 C20 H20B 110.4 . . ? C16 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? C13 C14 C15 109.2(5) . . ? C13 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? C13 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C8 C9 C10 105.6(4) . . ? C8 C9 H9A 110.6 . . ? C10 C9 H9A 110.6 . . ? C8 C9 H9B 110.6 . . ? C10 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? C19 C18 C17 104.0(5) . . ? C19 C18 H18A 111.0 . . ? C17 C18 H18A 111.0 . . ? C19 C18 H18B 111.0 . . ? C17 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? C14 C13 C12 112.0(5) . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C20 C19 C18 109.1(5) . . ? C20 C19 H19A 109.9 . . ? C18 C19 H19A 109.9 . . ? C20 C19 H19B 109.9 . . ? C18 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.797 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.079 data_s92_b _database_code_CSD 206050 _audit_creation_method SHELXL-97 _chemical_name_systematic ; PG Taylor ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H36 O6 Si4' _chemical_formula_weight 436.81 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9881(13) _cell_length_b 10.8183(14) _cell_length_c 10.9540(18) _cell_angle_alpha 96.541(8) _cell_angle_beta 91.269(7) _cell_angle_gamma 99.439(7) _cell_volume 1159.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9722 _exptl_absorpt_correction_T_max 0.9722 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10942 _diffrn_reflns_av_R_equivalents 0.2177 _diffrn_reflns_av_sigmaI/netI 0.2690 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3921 _reflns_number_gt 1619 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0533P)^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 3921 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2189 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1572 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 C1 C 0.0886(7) 0.7969(6) 0.7397(6) 0.0324(19) Uani 1 1 d . . . H1A H 0.1878 0.8096 0.7286 0.039 Uiso 1 1 calc R . . H1B H 0.0439 0.7605 0.6591 0.039 Uiso 1 1 calc R . . C2 C 0.0486(8) 0.9261(7) 0.7727(6) 0.041(2) Uani 1 1 d . . . H2 H -0.0477 0.9114 0.7981 0.049 Uiso 1 1 calc R . . C3 C 0.0517(8) 0.9966(7) 0.6616(7) 0.056(2) Uani 1 1 d . . . H3A H 0.1446 1.0121 0.6333 0.085 Uiso 1 1 calc R . . H3B H 0.0208 1.0774 0.6835 0.085 Uiso 1 1 calc R . . H3C H -0.0084 0.9463 0.5958 0.085 Uiso 1 1 calc R . . C4 C 0.1322(9) 1.0044(7) 0.8793(7) 0.061(3) Uani 1 1 d . . . H4A H 0.2275 1.0218 0.8574 0.091 Uiso 1 1 calc R . . H4B H 0.1249 0.9581 0.9514 0.091 Uiso 1 1 calc R . . H4C H 0.0985 1.0842 0.8984 0.091 Uiso 1 1 calc R . . C5 C 0.2424(7) 0.3568(6) 0.6863(6) 0.0330(18) Uani 1 1 d . . . H5A H 0.3307 0.4148 0.6938 0.040 Uiso 1 1 calc R . . H5B H 0.2610 0.2731 0.7030 0.040 Uiso 1 1 calc R . . C6 C 0.1894(8) 0.3441(7) 0.5504(6) 0.042(2) Uani 1 1 d . . . H6 H 0.0926 0.3010 0.5460 0.051 Uiso 1 1 calc R . . C7 C 0.2683(8) 0.2634(7) 0.4675(6) 0.053(2) Uani 1 1 d . . . H7A H 0.2328 0.2570 0.3825 0.080 Uiso 1 1 calc R . . H7B H 0.2588 0.1789 0.4938 0.080 Uiso 1 1 calc R . . H7C H 0.3644 0.3019 0.4725 0.080 Uiso 1 1 calc R . . C8 C 0.1928(10) 0.4707(7) 0.5055(7) 0.066(3) Uani 1 1 d . . . H8A H 0.2870 0.5145 0.5075 0.098 Uiso 1 1 calc R . . H8B H 0.1392 0.5210 0.5588 0.098 Uiso 1 1 calc R . . H8C H 0.1544 0.4591 0.4211 0.098 Uiso 1 1 calc R . . C9 C 0.3974(7) 0.4117(6) 1.1478(6) 0.039(2) Uani 1 1 d . . . H9A H 0.4712 0.4644 1.1091 0.046 Uiso 1 1 calc R . . H9B H 0.4042 0.4415 1.2369 0.046 Uiso 1 1 calc R . . C10 C 0.4251(7) 0.2770(6) 1.1319(7) 0.038(2) Uani 1 1 d . . . H10 H 0.3449 0.2212 1.1606 0.046 Uiso 1 1 calc R . . C11 C 0.5486(8) 0.2656(8) 1.2094(8) 0.062(3) Uani 1 1 d . . . H11A H 0.5619 0.1773 1.2015 0.093 Uiso 1 1 calc R . . H11B H 0.5352 0.2942 1.2957 0.093 Uiso 1 1 calc R . . H11C H 0.6289 0.3180 1.1813 0.093 Uiso 1 1 calc R . . C12 C 0.4452(9) 0.2309(8) 0.9985(7) 0.063(3) Uani 1 1 d . . . H12A H 0.3645 0.2368 0.9484 0.095 Uiso 1 1 calc R . . H12B H 0.4593 0.1429 0.9918 0.095 Uiso 1 1 calc R . . H12C H 0.5248 0.2832 0.9692 0.095 Uiso 1 1 calc R . . C13 C 0.2621(7) 0.8507(6) 1.1965(6) 0.0376(19) Uani 1 1 d . . . H13A H 0.3199 0.8864 1.1325 0.045 Uiso 1 1 calc R . . H13B H 0.2061 0.9143 1.2271 0.045 Uiso 1 1 calc R . . C14 C 0.3565(9) 0.8296(7) 1.3055(7) 0.052(2) Uani 1 1 d . . . H14 H 0.3970 0.7526 1.2796 0.063 Uiso 1 1 calc R . . C15 C 0.4714(9) 0.9393(9) 1.3325(7) 0.075(3) Uani 1 1 d . . . H15A H 0.4350 1.0148 1.3646 0.112 Uiso 1 1 calc R . . H15B H 0.5185 0.9546 1.2568 0.112 Uiso 1 1 calc R . . H15C H 0.5354 0.9199 1.3938 0.112 Uiso 1 1 calc R . . C16 C 0.2755(9) 0.8056(8) 1.4166(7) 0.066(3) Uani 1 1 d . . . H16A H 0.3371 0.8005 1.4862 0.099 Uiso 1 1 calc R . . H16B H 0.2121 0.7258 1.3992 0.099 Uiso 1 1 calc R . . H16C H 0.2245 0.8746 1.4372 0.099 Uiso 1 1 calc R . . O1 O -0.1132(4) 0.6501(4) 0.8592(4) 0.0350(13) Uani 1 1 d . . . O2 O 0.1187(5) 0.7260(4) 0.9824(4) 0.0357(13) Uani 1 1 d . . . O3 O 0.2212(4) 0.5873(4) 1.1308(4) 0.0336(12) Uani 1 1 d . . . O4 O 0.2207(5) 0.4193(4) 0.9376(4) 0.0353(13) Uani 1 1 d . . . O5 O -0.0046(5) 0.3156(4) 0.8090(4) 0.0373(13) Uani 1 1 d . . . O6 O 0.1032(4) 0.5511(4) 0.7942(4) 0.0324(12) Uani 1 1 d . . . Si1 Si 0.0494(2) 0.67926(18) 0.84734(18) 0.0308(6) Uani 1 1 d . . . Si2 Si 0.1373(2) 0.41232(18) 0.80820(17) 0.0305(6) Uani 1 1 d . . . Si3 Si 0.2349(2) 0.44238(18) 1.08624(17) 0.0320(6) Uani 1 1 d . . . Si4 Si 0.1486(2) 0.70958(18) 1.12495(17) 0.0324(6) Uani 1 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 C1 0.027(5) 0.032(4) 0.039(4) 0.009(4) 0.001(4) 0.002(4) C2 0.045(5) 0.045(5) 0.039(5) 0.019(4) 0.013(4) 0.014(4) C3 0.074(7) 0.040(5) 0.060(6) 0.014(4) 0.015(5) 0.014(5) C4 0.079(7) 0.042(5) 0.058(6) 0.002(5) -0.018(5) 0.005(5) C5 0.032(5) 0.039(4) 0.029(4) 0.007(4) 0.003(3) 0.008(4) C6 0.048(5) 0.046(5) 0.034(5) 0.004(4) 0.012(4) 0.007(4) C7 0.065(6) 0.058(6) 0.037(5) 0.001(4) 0.013(4) 0.013(5) C8 0.103(8) 0.060(6) 0.042(5) 0.017(5) 0.014(5) 0.027(6) C9 0.034(5) 0.045(5) 0.039(5) 0.011(4) 0.007(4) 0.010(4) C10 0.030(5) 0.032(5) 0.057(5) 0.014(4) 0.005(4) 0.012(4) C11 0.045(6) 0.067(6) 0.083(7) 0.020(5) 0.005(5) 0.026(5) C12 0.064(7) 0.055(6) 0.073(7) 0.001(5) 0.011(5) 0.019(5) C13 0.037(5) 0.045(5) 0.034(4) 0.016(4) 0.004(4) 0.007(4) C14 0.063(6) 0.041(5) 0.042(5) -0.004(4) 0.003(5) -0.013(5) C15 0.072(7) 0.091(7) 0.055(6) 0.007(5) -0.008(5) -0.001(6) C16 0.064(7) 0.089(7) 0.041(5) 0.023(5) -0.010(5) -0.010(5) O1 0.033(3) 0.035(3) 0.039(3) 0.013(2) 0.007(2) 0.007(2) O2 0.045(3) 0.036(3) 0.029(3) 0.013(2) 0.001(2) 0.006(3) O3 0.033(3) 0.029(3) 0.040(3) 0.006(2) 0.000(2) 0.008(2) O4 0.037(3) 0.046(3) 0.026(3) 0.010(2) 0.002(2) 0.012(3) O5 0.041(3) 0.039(3) 0.035(3) 0.004(2) 0.006(2) 0.013(3) O6 0.036(3) 0.028(3) 0.035(3) 0.007(2) 0.012(2) 0.009(2) Si1 0.0336(14) 0.0340(13) 0.0276(12) 0.0112(10) 0.0040(10) 0.0081(11) Si2 0.0315(14) 0.0350(13) 0.0273(12) 0.0097(10) 0.0026(10) 0.0084(11) Si3 0.0329(14) 0.0354(13) 0.0306(13) 0.0111(10) 0.0052(10) 0.0090(11) Si4 0.0333(14) 0.0357(13) 0.0312(13) 0.0086(10) 0.0035(10) 0.0114(11) _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 C1 C2 1.523(9) . ? C1 Si1 1.833(6) . ? C2 C3 1.506(9) . ? C2 C4 1.510(9) . ? C5 C6 1.553(9) . ? C5 Si2 1.825(7) . ? C6 C8 1.502(9) . ? C6 C7 1.511(9) . ? C9 C10 1.519(9) . ? C9 Si3 1.838(7) . ? C10 C11 1.512(9) . ? C10 C12 1.518(9) . ? C13 C14 1.565(9) . ? C13 Si4 1.830(7) . ? C14 C16 1.501(10) . ? C14 C15 1.507(10) . ? O1 Si1 1.614(5) . ? O1 Si3 1.614(5) 2_567 ? O2 Si1 1.611(5) . ? O2 Si4 1.618(4) . ? O3 Si4 1.616(4) . ? O3 Si3 1.617(4) . ? O4 Si2 1.616(4) . ? O4 Si3 1.619(4) . ? O5 Si2 1.618(5) . ? O5 Si4 1.622(5) 2_567 ? O6 Si2 1.615(4) . ? O6 Si1 1.620(4) . ? Si3 O1 1.614(5) 2_567 ? Si4 O5 1.622(5) 2_567 ? 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 C2 C1 Si1 118.0(5) . . ? C3 C2 C4 111.1(6) . . ? C3 C2 C1 110.7(6) . . ? C4 C2 C1 113.6(6) . . ? C6 C5 Si2 119.2(5) . . ? C8 C6 C7 110.5(6) . . ? C8 C6 C5 111.7(6) . . ? C7 C6 C5 111.2(6) . . ? C10 C9 Si3 118.4(5) . . ? C11 C10 C12 109.4(6) . . ? C11 C10 C9 110.7(6) . . ? C12 C10 C9 112.0(6) . . ? C14 C13 Si4 115.4(5) . . ? C16 C14 C15 112.1(7) . . ? C16 C14 C13 110.5(7) . . ? C15 C14 C13 110.7(6) . . ? Si1 O1 Si3 143.7(3) . 2_567 ? Si1 O2 Si4 153.3(3) . . ? Si4 O3 Si3 151.9(3) . . ? Si2 O4 Si3 152.5(3) . . ? Si2 O5 Si4 144.2(3) . 2_567 ? Si2 O6 Si1 152.1(3) . . ? O2 Si1 O1 108.5(2) . . ? O2 Si1 O6 108.3(2) . . ? O1 Si1 O6 109.6(2) . . ? O2 Si1 C1 112.9(3) . . ? O1 Si1 C1 108.5(3) . . ? O6 Si1 C1 109.1(3) . . ? O6 Si2 O4 108.2(2) . . ? O6 Si2 O5 108.4(2) . . ? O4 Si2 O5 109.5(2) . . ? O6 Si2 C5 112.6(3) . . ? O4 Si2 C5 107.6(3) . . ? O5 Si2 C5 110.4(3) . . ? O1 Si3 O3 109.2(2) 2_567 . ? O1 Si3 O4 108.6(3) 2_567 . ? O3 Si3 O4 108.6(2) . . ? O1 Si3 C9 108.5(3) 2_567 . ? O3 Si3 C9 108.8(3) . . ? O4 Si3 C9 113.1(3) . . ? O3 Si4 O2 108.9(2) . . ? O3 Si4 O5 108.1(2) . 2_567 ? O2 Si4 O5 108.4(2) . 2_567 ? O3 Si4 C13 109.6(3) . . ? O2 Si4 C13 108.7(3) . . ? O5 Si4 C13 113.1(3) 2_567 . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.445 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.090 data_s92_c _database_code_CSD 206051 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H120 O28 Si8' _chemical_formula_weight 1562.32 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3683(3) _cell_length_b 18.0913(4) _cell_length_c 18.3397(4) _cell_angle_alpha 106.2590(10) _cell_angle_beta 109.9200(10) _cell_angle_gamma 101.9080(10) _cell_volume 4055.20(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9597 _exptl_absorpt_correction_T_max 0.9597 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30226 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13466 _reflns_number_gt 8566 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0489P)^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 SHELXL _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13466 _refine_ls_number_parameters 926 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_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_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 C1 C 0.1680(2) 0.02460(17) 0.33529(18) 0.0169(7) Uani 1 1 d . . . H1A H 0.1985 -0.0199 0.3317 0.020 Uiso 1 1 calc R . . H1B H 0.1172 0.0137 0.2779 0.020 Uiso 1 1 calc R . . C2 C 0.2558(2) 0.10528(18) 0.36645(19) 0.0195(7) Uani 1 1 d . . . H2A H 0.3036 0.1173 0.4251 0.023 Uiso 1 1 calc R . . H2B H 0.2240 0.1489 0.3675 0.023 Uiso 1 1 calc R . . C3 C 0.3226(2) 0.11108(18) 0.31702(19) 0.0182(7) Uani 1 1 d . . . C4 C 0.2552(3) 0.0999(2) 0.2277(2) 0.0291(8) Uani 1 1 d . . . H4A H 0.2200 0.1409 0.2290 0.044 Uiso 1 1 calc R . . H4B H 0.2024 0.0451 0.1986 0.044 Uiso 1 1 calc R . . H4C H 0.2997 0.1064 0.1981 0.044 Uiso 1 1 calc R . . C5 C 0.4067(2) 0.19566(18) 0.3624(2) 0.0283(8) Uani 1 1 d . . . H5A H 0.3731 0.2376 0.3680 0.042 Uiso 1 1 calc R . . H5B H 0.4476 0.2029 0.3301 0.042 Uiso 1 1 calc R . . H5C H 0.4535 0.2008 0.4182 0.042 Uiso 1 1 calc R . . C6 C 0.3767(2) 0.04495(18) 0.3186(2) 0.0209(8) Uani 1 1 d . . . H6A H 0.4087 0.0479 0.3769 0.025 Uiso 1 1 calc R . . H6B H 0.3227 -0.0097 0.2840 0.025 Uiso 1 1 calc R . . C7 C 0.4599(3) 0.05422(19) 0.2867(2) 0.0223(8) Uani 1 1 d . . . C8 C 0.4942(3) 0.0358(2) 0.1674(2) 0.0405(10) Uani 1 1 d . . . H8A H 0.5257 0.0945 0.1830 0.061 Uiso 1 1 calc R . . H8B H 0.4581 0.0087 0.1062 0.061 Uiso 1 1 calc R . . H8C H 0.5494 0.0133 0.1890 0.061 Uiso 1 1 calc R . . C9 C -0.0742(2) -0.24077(18) 0.29430(19) 0.0201(7) Uani 1 1 d . . . H9A H -0.1348 -0.2842 0.2875 0.024 Uiso 1 1 calc R . . H9B H -0.0926 -0.2324 0.2407 0.024 Uiso 1 1 calc R . . C10 C 0.0198(3) -0.2704(2) 0.3102(2) 0.0288(8) Uani 1 1 d . . . H10A H 0.0193 -0.3007 0.3476 0.035 Uiso 1 1 calc R . . H10B H 0.0845 -0.2219 0.3410 0.035 Uiso 1 1 calc R . . C11 C 0.0270(2) -0.32576(19) 0.2325(2) 0.0248(8) Uani 1 1 d . . . C12 C -0.0698(3) -0.4027(2) 0.1841(2) 0.0388(10) Uani 1 1 d . . . H12A H -0.0606 -0.4405 0.1391 0.058 Uiso 1 1 calc R . . H12B H -0.1320 -0.3881 0.1599 0.058 Uiso 1 1 calc R . . H12C H -0.0790 -0.4291 0.2223 0.058 Uiso 1 1 calc R . . C13 C 0.1252(3) -0.3491(2) 0.2655(2) 0.0394(10) Uani 1 1 d . . . H13A H 0.1187 -0.3774 0.3029 0.059 Uiso 1 1 calc R . . H13B H 0.1873 -0.2996 0.2966 0.059 Uiso 1 1 calc R . . H13C H 0.1324 -0.3853 0.2183 0.059 Uiso 1 1 calc R . . C14 C 0.0396(3) -0.2769(2) 0.1783(2) 0.0393(10) Uani 1 1 d . . . H14A H -0.0303 -0.2757 0.1451 0.047 Uiso 1 1 calc R . . H14B H 0.0845 -0.2199 0.2159 0.047 Uiso 1 1 calc R . . C15 C 0.0854(3) -0.3079(2) 0.1202(2) 0.0387(10) Uani 1 1 d . . . C16 C 0.0609(3) -0.4104(2) -0.0052(2) 0.0483(11) Uani 1 1 d . . . H16A H 0.0803 -0.3703 -0.0286 0.072 Uiso 1 1 calc R . . H16B H 0.0072 -0.4604 -0.0506 0.072 Uiso 1 1 calc R . . H16C H 0.1230 -0.4230 0.0239 0.072 Uiso 1 1 calc R . . C17 C -0.1082(2) 0.17866(17) 0.39096(18) 0.0166(7) Uani 1 1 d . . . H17A H -0.0481 0.2248 0.4014 0.020 Uiso 1 1 calc R . . H17B H -0.1512 0.1517 0.3296 0.020 Uiso 1 1 calc R . . C18 C -0.1751(2) 0.21170(18) 0.43312(18) 0.0182(7) Uani 1 1 d . . . H18A H -0.1348 0.2305 0.4946 0.022 Uiso 1 1 calc R . . H18B H -0.2389 0.1656 0.4165 0.022 Uiso 1 1 calc R . . C19 C -0.2101(2) 0.28194(18) 0.41432(18) 0.0180(7) Uani 1 1 d . . . C20 C -0.2833(3) 0.2988(2) 0.4562(2) 0.0314(9) Uani 1 1 d . . . H20A H -0.2458 0.3141 0.5168 0.047 Uiso 1 1 calc R . . H20B H -0.3446 0.2495 0.4332 0.047 Uiso 1 1 calc R . . H20C H -0.3064 0.3436 0.4455 0.047 Uiso 1 1 calc R . . C21 C -0.1160(3) 0.35898(18) 0.4485(2) 0.0290(9) Uani 1 1 d . . . H21A H -0.0710 0.3489 0.4196 0.043 Uiso 1 1 calc R . . H21B H -0.0760 0.3740 0.5088 0.043 Uiso 1 1 calc R . . H21C H -0.1405 0.4036 0.4391 0.043 Uiso 1 1 calc R . . C22 C -0.2700(2) 0.25254(18) 0.31867(19) 0.0225(8) Uani 1 1 d . . . H22A H -0.2195 0.2474 0.2935 0.027 Uiso 1 1 calc R . . H22B H -0.3218 0.1974 0.2977 0.027 Uiso 1 1 calc R . . C23 C -0.3269(3) 0.3069(2) 0.2887(2) 0.0272(8) Uani 1 1 d . . . C24 C -0.4921(3) 0.3169(2) 0.2180(2) 0.0431(10) Uani 1 1 d . . . H24A H -0.4848 0.3630 0.2655 0.065 Uiso 1 1 calc R . . H24B H -0.5662 0.2826 0.1858 0.065 Uiso 1 1 calc R . . H24C H -0.4668 0.3377 0.1818 0.065 Uiso 1 1 calc R . . C25 C 0.3528(2) 0.09798(17) 0.65435(18) 0.0163(7) Uani 1 1 d . . . H25A H 0.3693 0.1067 0.7138 0.020 Uiso 1 1 calc R . . H25B H 0.3802 0.0550 0.6325 0.020 Uiso 1 1 calc R . . C26 C 0.4086(2) 0.17730(17) 0.64998(19) 0.0203(7) Uani 1 1 d . . . H26A H 0.3745 0.2177 0.6654 0.024 Uiso 1 1 calc R . . H26B H 0.3969 0.1663 0.5910 0.024 Uiso 1 1 calc R . . C27 C 0.5281(2) 0.21694(18) 0.70570(19) 0.0209(8) Uani 1 1 d . . . C28 C 0.5479(3) 0.2481(2) 0.7974(2) 0.0459(11) Uani 1 1 d . . . H28A H 0.5226 0.2021 0.8118 0.069 Uiso 1 1 calc R . . H28B H 0.5106 0.2868 0.8071 0.069 Uiso 1 1 calc R . . H28C H 0.6234 0.2756 0.8324 0.069 Uiso 1 1 calc R . . C29 C 0.5705(3) 0.2892(2) 0.6844(3) 0.0434(11) Uani 1 1 d . . . H29A H 0.5355 0.3294 0.6956 0.065 Uiso 1 1 calc R . . H29B H 0.5569 0.2697 0.6250 0.065 Uiso 1 1 calc R . . H29C H 0.6464 0.3149 0.7191 0.065 Uiso 1 1 calc R . . C30 C 0.5882(2) 0.15723(19) 0.69327(18) 0.0199(7) Uani 1 1 d . . . H30A H 0.6625 0.1849 0.7346 0.024 Uiso 1 1 calc R . . H30B H 0.5592 0.1103 0.7059 0.024 Uiso 1 1 calc R . . C31 C 0.5855(3) 0.1251(2) 0.6077(2) 0.0251(8) Uani 1 1 d . . . C32 C 0.6829(3) 0.0902(2) 0.5313(2) 0.0375(10) Uani 1 1 d . . . H32A H 0.6402 0.0321 0.5043 0.056 Uiso 1 1 calc R . . H32B H 0.7555 0.0961 0.5396 0.056 Uiso 1 1 calc R . . H32C H 0.6546 0.1189 0.4956 0.056 Uiso 1 1 calc R . . C33 C 0.2935(2) 0.23502(17) -0.11483(18) 0.0197(7) Uani 1 1 d . . . H33A H 0.2188 0.2307 -0.1404 0.024 Uiso 1 1 calc R . . H33B H 0.3095 0.2027 -0.1594 0.024 Uiso 1 1 calc R . . C34 C 0.3101(2) 0.19869(17) -0.04693(18) 0.0182(7) Uani 1 1 d . . . H34A H 0.2860 0.2274 -0.0063 0.022 Uiso 1 1 calc R . . H34B H 0.3865 0.2107 -0.0163 0.022 Uiso 1 1 calc R . . C35 C 0.2550(2) 0.10611(18) -0.07684(19) 0.0211(8) Uani 1 1 d . . . C36 C 0.3003(3) 0.0588(2) -0.1312(2) 0.0337(9) Uani 1 1 d . . . H36A H 0.2673 0.0000 -0.1477 0.050 Uiso 1 1 calc R . . H36B H 0.3763 0.0743 -0.0991 0.050 Uiso 1 1 calc R . . H36C H 0.2863 0.0718 -0.1814 0.050 Uiso 1 1 calc R . . C37 C 0.2754(3) 0.0847(2) 0.0011(2) 0.0326(9) Uani 1 1 d . . . H37A H 0.2447 0.1137 0.0351 0.049 Uiso 1 1 calc R . . H37B H 0.3513 0.1009 0.0342 0.049 Uiso 1 1 calc R . . H37C H 0.2433 0.0256 -0.0162 0.049 Uiso 1 1 calc R . . C38 C 0.1355(2) 0.07862(18) -0.1298(2) 0.0247(8) Uani 1 1 d . . . H38A H 0.1231 0.0929 -0.1799 0.030 Uiso 1 1 calc R . . H38B H 0.1062 0.0184 -0.1497 0.030 Uiso 1 1 calc R . . C39 C 0.0772(3) 0.1156(2) -0.0844(2) 0.0291(8) Uani 1 1 d . . . C40 C -0.0439(4) 0.0908(3) -0.0264(3) 0.0778(17) Uani 1 1 d . . . H40A H 0.0057 0.1272 0.0311 0.117 Uiso 1 1 calc R . . H40B H -0.0930 0.0450 -0.0254 0.117 Uiso 1 1 calc R . . H40C H -0.0831 0.1211 -0.0538 0.117 Uiso 1 1 calc R . . C41 C 0.6893(2) 0.55598(17) 0.27408(17) 0.0154(7) Uani 1 1 d . . . H41A H 0.6643 0.5054 0.2829 0.018 Uiso 1 1 calc R . . H41B H 0.7632 0.5645 0.2827 0.018 Uiso 1 1 calc R . . C42 C 0.6877(2) 0.62735(17) 0.34148(17) 0.0164(7) Uani 1 1 d . . . H42A H 0.6138 0.6247 0.3270 0.020 Uiso 1 1 calc R . . H42B H 0.7253 0.6789 0.3399 0.020 Uiso 1 1 calc R . . C43 C 0.7364(2) 0.63102(18) 0.43158(18) 0.0184(7) Uani 1 1 d . . . C44 C 0.8482(2) 0.6281(2) 0.45536(19) 0.0283(8) Uani 1 1 d . . . H44A H 0.8801 0.6356 0.5146 0.042 Uiso 1 1 calc R . . H44B H 0.8901 0.6718 0.4463 0.042 Uiso 1 1 calc R . . H44C H 0.8460 0.5750 0.4205 0.042 Uiso 1 1 calc R . . C45 C 0.7409(3) 0.71175(18) 0.49094(19) 0.0267(8) Uani 1 1 d . . . H45A H 0.7643 0.7125 0.5480 0.040 Uiso 1 1 calc R . . H45B H 0.6709 0.7170 0.4727 0.040 Uiso 1 1 calc R . . H45C H 0.7903 0.7574 0.4900 0.040 Uiso 1 1 calc R . . C46 C 0.6735(2) 0.55909(18) 0.44339(19) 0.0199(7) Uani 1 1 d . . . H46A H 0.6704 0.5073 0.4042 0.024 Uiso 1 1 calc R . . H46B H 0.7107 0.5623 0.5012 0.024 Uiso 1 1 calc R . . C47 C 0.5638(3) 0.55768(19) 0.4285(2) 0.0239(8) Uani 1 1 d . . . C48 C 0.4544(3) 0.5960(2) 0.4925(2) 0.0350(9) Uani 1 1 d . . . H48A H 0.4362 0.6317 0.4625 0.053 Uiso 1 1 calc R . . H48B H 0.4559 0.6182 0.5484 0.053 Uiso 1 1 calc R . . H48C H 0.4018 0.5412 0.4611 0.053 Uiso 1 1 calc R . . C49 C 0.7248(2) 0.54209(18) -0.11929(19) 0.0178(7) Uani 1 1 d . . . H49A H 0.7966 0.5702 -0.0737 0.021 Uiso 1 1 calc R . . H49B H 0.7234 0.4892 -0.1552 0.021 Uiso 1 1 calc R . . C50 C 0.7019(2) 0.59406(18) -0.17191(19) 0.0185(7) Uani 1 1 d . . . H50A H 0.6990 0.6453 -0.1364 0.022 Uiso 1 1 calc R . . H50B H 0.6311 0.5643 -0.2186 0.022 Uiso 1 1 calc R . . C51 C 0.7792(2) 0.61713(19) -0.20964(19) 0.0202(7) Uani 1 1 d . . . C52 C 0.7313(3) 0.6579(2) -0.2689(2) 0.0399(10) Uani 1 1 d . . . H52A H 0.7186 0.7055 -0.2378 0.060 Uiso 1 1 calc R . . H52B H 0.6648 0.6189 -0.3147 0.060 Uiso 1 1 calc R . . H52C H 0.7801 0.6755 -0.2922 0.060 Uiso 1 1 calc R . . C53 C 0.8850(3) 0.6759(2) -0.1401(2) 0.0338(9) Uani 1 1 d . . . H53A H 0.8762 0.7263 -0.1105 0.051 Uiso 1 1 calc R . . H53B H 0.9342 0.6887 -0.1646 0.051 Uiso 1 1 calc R . . H53C H 0.9128 0.6505 -0.1007 0.051 Uiso 1 1 calc R . . C54 C 0.7918(3) 0.5383(2) -0.2592(2) 0.0269(8) Uani 1 1 d . . . H54A H 0.8226 0.5130 -0.2197 0.032 Uiso 1 1 calc R . . H54B H 0.7212 0.4994 -0.3004 0.032 Uiso 1 1 calc R . . C55 C 0.8590(3) 0.5503(2) -0.3049(2) 0.0316(9) Uani 1 1 d . . . C56 C 1.0244(3) 0.5603(2) -0.3058(2) 0.0369(10) Uani 1 1 d . . . H56A H 0.9930 0.5154 -0.3608 0.055 Uiso 1 1 calc R . . H56B H 1.0930 0.5588 -0.2720 0.055 Uiso 1 1 calc R . . H56C H 1.0333 0.6125 -0.3131 0.055 Uiso 1 1 calc R . . C57 C 0.6998(2) 0.33788(17) 0.03520(18) 0.0167(7) Uani 1 1 d . . . H57A H 0.7142 0.3181 -0.0146 0.020 Uiso 1 1 calc R . . H57B H 0.7681 0.3706 0.0841 0.020 Uiso 1 1 calc R . . C58 C 0.6478(2) 0.26397(17) 0.05014(19) 0.0188(7) Uani 1 1 d . . . H58A H 0.5761 0.2357 0.0044 0.023 Uiso 1 1 calc R . . H58B H 0.6404 0.2845 0.1032 0.023 Uiso 1 1 calc R . . C59 C 0.7040(2) 0.20032(18) 0.05514(19) 0.0178(7) Uani 1 1 d . . . C60 C 0.7118(3) 0.16288(19) -0.02746(19) 0.0251(8) Uani 1 1 d . . . H60A H 0.7602 0.2044 -0.0343 0.038 Uiso 1 1 calc R . . H60B H 0.6422 0.1432 -0.0742 0.038 Uiso 1 1 calc R . . H60C H 0.7380 0.1171 -0.0267 0.038 Uiso 1 1 calc R . . C61 C 0.6373(2) 0.13425(18) 0.0711(2) 0.0250(8) Uani 1 1 d . . . H61A H 0.6681 0.0907 0.0716 0.038 Uiso 1 1 calc R . . H61B H 0.5657 0.1115 0.0266 0.038 Uiso 1 1 calc R . . H61C H 0.6356 0.1583 0.1254 0.038 Uiso 1 1 calc R . . C62 C 0.8126(2) 0.24296(18) 0.12884(19) 0.0207(8) Uani 1 1 d . . . H62A H 0.8547 0.2831 0.1151 0.025 Uiso 1 1 calc R . . H62B H 0.8038 0.2740 0.1784 0.025 Uiso 1 1 calc R . . C63 C 0.8753(2) 0.1897(2) 0.1535(2) 0.0207(8) Uani 1 1 d . . . C64 C 1.0235(3) 0.1877(2) 0.2594(2) 0.0310(9) Uani 1 1 d . . . H64A H 0.9854 0.1382 0.2630 0.046 Uiso 1 1 calc R . . H64B H 1.0798 0.2235 0.3148 0.046 Uiso 1 1 calc R . . H64C H 1.0539 0.1727 0.2193 0.046 Uiso 1 1 calc R . . O1 O 0.02640(15) -0.07215(11) 0.37292(12) 0.0190(5) Uani 1 1 d . . . O2 O -0.00547(15) -0.14948(12) 0.46815(12) 0.0189(5) Uani 1 1 d . . . O3 O 0.01980(15) 0.07648(11) 0.39148(12) 0.0170(5) Uani 1 1 d . . . O4 O 0.17899(15) 0.05540(12) 0.49870(12) 0.0176(5) Uani 1 1 d . . . O5 O 0.15602(15) -0.02595(12) 0.59320(12) 0.0204(5) Uani 1 1 d . . . O6 O 0.16429(15) 0.12815(11) 0.63855(11) 0.0169(5) Uani 1 1 d . . . O7 O 0.55292(19) 0.08718(15) 0.32993(14) 0.0356(6) Uani 1 1 d . . . O8 O 0.41987(17) 0.02216(13) 0.20273(14) 0.0318(6) Uani 1 1 d . . . O9 O 0.1716(2) -0.27620(19) 0.12748(16) 0.0645(9) Uani 1 1 d . . . O10 O 0.0198(2) -0.37707(14) 0.05346(15) 0.0415(7) Uani 1 1 d . . . O11 O -0.2857(2) 0.37589(16) 0.29720(17) 0.0527(8) Uani 1 1 d . . . O12 O -0.43077(18) 0.26893(13) 0.24870(14) 0.0323(6) Uani 1 1 d . . . O13 O 0.50936(19) 0.10070(18) 0.54257(15) 0.0541(8) Uani 1 1 d . . . O14 O 0.68045(16) 0.12473(12) 0.61152(12) 0.0242(5) Uani 1 1 d . . . O15 O 0.49807(15) 0.34829(11) -0.03988(12) 0.0175(5) Uani 1 1 d . . . O16 O 0.62815(16) 0.46221(11) 0.10684(11) 0.0187(5) Uani 1 1 d . . . O17 O 0.48774(15) 0.51884(11) 0.14360(12) 0.0175(5) Uani 1 1 d . . . O18 O 0.65047(15) 0.61912(11) 0.14474(11) 0.0167(5) Uani 1 1 d . . . O19 O 0.66098(16) 0.46019(12) -0.02641(12) 0.0192(5) Uani 1 1 d . . . O20 O 0.64333(15) 0.60632(11) -0.00445(12) 0.0179(5) Uani 1 1 d . . . O21 O 0.0854(2) 0.18653(15) -0.06038(17) 0.0485(7) Uani 1 1 d . . . O22 O 0.0134(2) 0.05979(14) -0.07268(16) 0.0491(8) Uani 1 1 d . . . O23 O 0.48975(19) 0.52993(16) 0.36202(14) 0.0448(7) Uani 1 1 d . . . O24 O 0.55632(17) 0.59149(13) 0.50082(13) 0.0282(6) Uani 1 1 d . . . O25 O 0.8320(2) 0.5575(2) -0.37085(17) 0.0744(11) Uani 1 1 d . . . O26 O 0.95627(18) 0.55144(13) -0.26368(14) 0.0296(6) Uani 1 1 d . . . O27 O 0.86356(18) 0.12141(14) 0.11122(15) 0.0361(6) Uani 1 1 d . . . O28 O 0.95175(16) 0.23008(12) 0.23161(13) 0.0243(5) Uani 1 1 d . . . Si1 Si 0.09676(6) 0.02149(5) 0.40119(5) 0.0141(2) Uani 1 1 d . . . Si2 Si -0.05465(6) -0.14629(5) 0.37642(5) 0.0137(2) Uani 1 1 d . . . Si3 Si -0.05867(7) 0.10546(5) 0.43045(5) 0.0144(2) Uani 1 1 d . . . Si4 Si 0.21018(6) 0.06244(5) 0.59464(5) 0.0139(2) Uani 1 1 d . . . Si5 Si 0.62024(7) 0.40396(5) 0.01881(5) 0.0143(2) Uani 1 1 d . . . Si6 Si 0.37608(7) 0.34237(5) -0.07321(5) 0.0140(2) Uani 1 1 d . . . Si7 Si 0.61172(7) 0.53928(5) 0.16513(5) 0.0144(2) Uani 1 1 d . . . Si8 Si 0.63283(7) 0.52201(5) -0.07284(5) 0.0146(2) Uani 1 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 C1 0.0143(18) 0.0213(17) 0.0187(17) 0.0086(15) 0.0096(14) 0.0073(14) C2 0.0203(19) 0.0192(17) 0.0218(18) 0.0071(15) 0.0125(15) 0.0067(15) C3 0.0169(19) 0.0174(17) 0.0248(18) 0.0098(15) 0.0117(15) 0.0073(14) C4 0.031(2) 0.037(2) 0.035(2) 0.0208(18) 0.0229(18) 0.0181(18) C5 0.024(2) 0.0227(18) 0.046(2) 0.0129(18) 0.0226(18) 0.0077(16) C6 0.0188(19) 0.0215(17) 0.0286(19) 0.0100(16) 0.0164(16) 0.0070(15) C7 0.026(2) 0.0185(18) 0.032(2) 0.0121(17) 0.0193(18) 0.0092(16) C8 0.035(2) 0.042(2) 0.044(2) 0.004(2) 0.032(2) 0.0014(19) C9 0.0142(18) 0.0219(17) 0.0219(18) 0.0045(15) 0.0077(15) 0.0067(15) C10 0.024(2) 0.0275(19) 0.032(2) 0.0087(17) 0.0084(17) 0.0115(16) C11 0.020(2) 0.0220(18) 0.032(2) 0.0013(17) 0.0178(17) 0.0061(15) C12 0.038(2) 0.030(2) 0.045(2) 0.0045(19) 0.023(2) 0.0090(18) C13 0.046(3) 0.035(2) 0.043(2) 0.014(2) 0.022(2) 0.0221(19) C14 0.048(3) 0.030(2) 0.038(2) 0.0108(19) 0.019(2) 0.0100(19) C15 0.023(2) 0.051(3) 0.036(2) 0.017(2) 0.013(2) 0.000(2) C16 0.044(3) 0.060(3) 0.051(3) 0.020(2) 0.032(2) 0.019(2) C17 0.0167(18) 0.0138(16) 0.0180(17) 0.0062(14) 0.0062(14) 0.0041(14) C18 0.0143(18) 0.0240(18) 0.0175(17) 0.0093(15) 0.0062(14) 0.0077(15) C19 0.0147(18) 0.0180(17) 0.0221(18) 0.0070(15) 0.0080(15) 0.0073(14) C20 0.027(2) 0.041(2) 0.037(2) 0.0157(19) 0.0193(18) 0.0218(18) C21 0.023(2) 0.0209(18) 0.038(2) 0.0068(17) 0.0077(17) 0.0127(16) C22 0.020(2) 0.0229(18) 0.0263(19) 0.0127(16) 0.0070(16) 0.0116(15) C23 0.027(2) 0.029(2) 0.030(2) 0.0164(18) 0.0103(17) 0.0139(18) C24 0.027(2) 0.057(3) 0.054(3) 0.030(2) 0.012(2) 0.029(2) C25 0.0132(18) 0.0181(16) 0.0169(17) 0.0051(14) 0.0056(14) 0.0077(14) C26 0.0130(18) 0.0195(17) 0.0282(19) 0.0076(16) 0.0084(15) 0.0079(14) C27 0.0106(18) 0.0185(17) 0.0266(19) 0.0017(16) 0.0068(15) 0.0030(14) C28 0.020(2) 0.061(3) 0.028(2) -0.014(2) 0.0073(17) 0.008(2) C29 0.020(2) 0.0222(19) 0.082(3) 0.013(2) 0.020(2) 0.0066(17) C30 0.0105(18) 0.0242(18) 0.0202(18) 0.0051(15) 0.0047(14) 0.0044(14) C31 0.019(2) 0.0271(19) 0.030(2) 0.0089(17) 0.0122(18) 0.0081(16) C32 0.031(2) 0.050(2) 0.030(2) 0.0055(19) 0.0214(18) 0.0087(19) C33 0.0165(19) 0.0185(17) 0.0191(17) 0.0060(15) 0.0039(15) 0.0040(14) C34 0.0148(18) 0.0177(17) 0.0192(17) 0.0092(15) 0.0043(14) 0.0017(14) C35 0.022(2) 0.0155(17) 0.0255(19) 0.0082(16) 0.0110(16) 0.0047(15) C36 0.040(2) 0.0251(19) 0.050(2) 0.0173(19) 0.028(2) 0.0168(18) C37 0.032(2) 0.030(2) 0.039(2) 0.0245(18) 0.0119(18) 0.0070(17) C38 0.026(2) 0.0186(17) 0.0279(19) 0.0083(16) 0.0126(17) 0.0023(15) C39 0.021(2) 0.026(2) 0.037(2) 0.0110(19) 0.0137(18) 0.0034(17) C40 0.074(4) 0.055(3) 0.106(4) 0.000(3) 0.079(3) -0.002(3) C41 0.0170(18) 0.0151(16) 0.0137(16) 0.0063(14) 0.0055(14) 0.0054(14) C42 0.0150(18) 0.0154(16) 0.0179(17) 0.0065(15) 0.0064(14) 0.0044(14) C43 0.0172(19) 0.0202(17) 0.0128(17) 0.0037(15) 0.0047(14) 0.0032(14) C44 0.018(2) 0.041(2) 0.0182(18) 0.0076(17) 0.0035(15) 0.0068(17) C45 0.027(2) 0.0238(18) 0.0183(18) -0.0006(16) 0.0074(16) 0.0024(16) C46 0.022(2) 0.0220(17) 0.0157(17) 0.0084(15) 0.0071(15) 0.0068(15) C47 0.024(2) 0.0229(18) 0.024(2) 0.0117(17) 0.0117(18) 0.0014(16) C48 0.024(2) 0.035(2) 0.053(2) 0.019(2) 0.0216(19) 0.0107(17) C49 0.0144(18) 0.0197(17) 0.0229(18) 0.0105(15) 0.0092(15) 0.0070(14) C50 0.0189(19) 0.0194(17) 0.0239(18) 0.0116(15) 0.0132(15) 0.0078(14) C51 0.0165(19) 0.0246(18) 0.0220(18) 0.0119(16) 0.0088(15) 0.0064(15) C52 0.043(3) 0.048(2) 0.053(3) 0.038(2) 0.031(2) 0.020(2) C53 0.030(2) 0.032(2) 0.034(2) 0.0072(18) 0.0191(18) -0.0034(17) C54 0.024(2) 0.034(2) 0.0275(19) 0.0117(17) 0.0179(17) 0.0072(16) C55 0.027(2) 0.041(2) 0.028(2) 0.0109(19) 0.0165(18) 0.0095(18) C56 0.031(2) 0.038(2) 0.052(2) 0.012(2) 0.033(2) 0.0093(18) C57 0.0143(18) 0.0171(16) 0.0184(17) 0.0076(15) 0.0062(14) 0.0048(14) C58 0.0180(19) 0.0180(17) 0.0225(18) 0.0089(15) 0.0088(15) 0.0085(14) C59 0.0138(18) 0.0168(16) 0.0258(18) 0.0107(15) 0.0087(15) 0.0072(14) C60 0.028(2) 0.0218(18) 0.0275(19) 0.0104(16) 0.0105(16) 0.0134(16) C61 0.020(2) 0.0219(18) 0.032(2) 0.0122(16) 0.0082(16) 0.0071(15) C62 0.0202(19) 0.0172(17) 0.0264(19) 0.0094(16) 0.0093(16) 0.0092(15) C63 0.0144(19) 0.0242(19) 0.027(2) 0.0137(17) 0.0090(16) 0.0063(15) C64 0.025(2) 0.042(2) 0.036(2) 0.0260(19) 0.0100(17) 0.0212(18) O1 0.0181(13) 0.0179(11) 0.0246(12) 0.0086(10) 0.0130(10) 0.0056(10) O2 0.0198(13) 0.0209(11) 0.0175(12) 0.0071(10) 0.0078(10) 0.0103(10) O3 0.0155(12) 0.0218(11) 0.0192(11) 0.0103(10) 0.0096(10) 0.0099(10) O4 0.0131(12) 0.0241(12) 0.0161(11) 0.0075(10) 0.0061(9) 0.0073(10) O5 0.0134(12) 0.0207(11) 0.0309(13) 0.0137(10) 0.0102(10) 0.0065(10) O6 0.0105(12) 0.0204(11) 0.0170(11) 0.0034(10) 0.0050(9) 0.0067(9) O7 0.0203(15) 0.0528(16) 0.0373(15) 0.0174(13) 0.0157(13) 0.0128(13) O8 0.0252(14) 0.0323(14) 0.0301(14) -0.0009(12) 0.0186(12) 0.0002(11) O9 0.0404(19) 0.086(2) 0.0468(18) 0.0087(17) 0.0235(15) -0.0039(17) O10 0.0437(17) 0.0375(15) 0.0400(16) 0.0042(14) 0.0237(14) 0.0113(13) O11 0.0339(17) 0.0379(16) 0.078(2) 0.0362(15) 0.0027(15) 0.0133(14) O12 0.0185(14) 0.0342(13) 0.0427(15) 0.0188(12) 0.0055(12) 0.0131(11) O13 0.0212(16) 0.098(2) 0.0203(14) -0.0007(15) 0.0033(13) 0.0165(15) O14 0.0201(13) 0.0303(13) 0.0231(13) 0.0064(11) 0.0131(11) 0.0088(11) O15 0.0133(12) 0.0162(11) 0.0208(12) 0.0056(10) 0.0049(10) 0.0061(9) O16 0.0240(13) 0.0181(11) 0.0142(11) 0.0054(10) 0.0078(10) 0.0092(10) O17 0.0153(12) 0.0205(11) 0.0170(11) 0.0079(10) 0.0074(10) 0.0047(10) O18 0.0138(12) 0.0175(11) 0.0171(11) 0.0093(10) 0.0041(9) 0.0027(9) O19 0.0193(13) 0.0206(11) 0.0214(12) 0.0119(10) 0.0091(10) 0.0078(10) O20 0.0204(13) 0.0156(11) 0.0201(12) 0.0059(10) 0.0123(10) 0.0055(9) O21 0.0534(19) 0.0315(15) 0.081(2) 0.0246(15) 0.0450(16) 0.0215(14) O22 0.0483(18) 0.0321(14) 0.0667(19) 0.0054(14) 0.0437(16) -0.0014(13) O23 0.0199(15) 0.0743(19) 0.0222(14) 0.0131(14) 0.0032(12) -0.0024(13) O24 0.0194(14) 0.0336(13) 0.0289(14) 0.0068(12) 0.0111(11) 0.0088(11) O25 0.047(2) 0.172(3) 0.0365(17) 0.060(2) 0.0295(15) 0.052(2) O26 0.0283(15) 0.0357(14) 0.0383(14) 0.0179(12) 0.0232(12) 0.0160(12) O27 0.0370(16) 0.0240(14) 0.0409(15) 0.0094(13) 0.0068(12) 0.0189(12) O28 0.0177(13) 0.0283(12) 0.0294(14) 0.0161(11) 0.0068(11) 0.0113(11) Si1 0.0117(5) 0.0168(5) 0.0162(5) 0.0072(4) 0.0074(4) 0.0052(4) Si2 0.0106(5) 0.0157(4) 0.0145(5) 0.0050(4) 0.0050(4) 0.0054(4) Si3 0.0126(5) 0.0161(5) 0.0170(5) 0.0078(4) 0.0071(4) 0.0060(4) Si4 0.0100(5) 0.0159(4) 0.0159(5) 0.0055(4) 0.0056(4) 0.0053(4) Si5 0.0148(5) 0.0146(4) 0.0151(5) 0.0070(4) 0.0064(4) 0.0060(4) Si6 0.0133(5) 0.0133(4) 0.0164(5) 0.0066(4) 0.0064(4) 0.0050(4) Si7 0.0158(5) 0.0143(4) 0.0139(5) 0.0059(4) 0.0063(4) 0.0058(4) Si8 0.0135(5) 0.0160(5) 0.0166(5) 0.0077(4) 0.0072(4) 0.0057(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 C1 C2 1.527(4) . ? C1 Si1 1.836(3) . ? C2 C3 1.535(4) . ? C3 C4 1.521(4) . ? C3 C5 1.528(4) . ? C3 C6 1.557(4) . ? C6 C7 1.499(4) . ? C7 O7 1.206(4) . ? C7 O8 1.340(4) . ? C8 O8 1.440(3) . ? C9 C10 1.523(4) . ? C9 Si2 1.828(3) . ? C10 C11 1.546(4) . ? C11 C12 1.526(4) . ? C11 C13 1.531(4) . ? C11 C14 1.533(4) . ? C14 C15 1.475(5) . ? C15 O9 1.197(4) . ? C15 O10 1.350(4) . ? C16 O10 1.444(4) . ? C17 C18 1.537(4) . ? C17 Si3 1.833(3) . ? C18 C19 1.542(4) . ? C19 C21 1.523(4) . ? C19 C20 1.530(4) . ? C19 C22 1.537(4) . ? C22 C23 1.505(4) . ? C23 O11 1.207(4) . ? C23 O12 1.337(4) . ? C24 O12 1.449(4) . ? C25 C26 1.530(4) . ? C25 Si4 1.829(3) . ? C26 C27 1.547(4) . ? C27 C28 1.517(4) . ? C27 C30 1.532(4) . ? C27 C29 1.534(4) . ? C30 C31 1.497(4) . ? C31 O13 1.197(4) . ? C31 O14 1.344(4) . ? C32 O14 1.444(4) . ? C33 C34 1.536(4) . ? C33 Si6 1.834(3) . ? C34 C35 1.541(4) . ? C35 C36 1.531(4) . ? C35 C37 1.534(4) . ? C35 C38 1.543(4) . ? C38 C39 1.497(4) . ? C39 O21 1.199(4) . ? C39 O22 1.334(4) . ? C40 O22 1.453(4) . ? C41 C42 1.528(4) . ? C41 Si7 1.825(3) . ? C42 C43 1.535(4) . ? C43 C44 1.531(4) . ? C43 C45 1.532(4) . ? C43 C46 1.537(4) . ? C46 C47 1.498(4) . ? C47 O23 1.193(4) . ? C47 O24 1.347(4) . ? C48 O24 1.442(4) . ? C49 C50 1.531(4) . ? C49 Si8 1.829(3) . ? C50 C51 1.543(4) . ? C51 C53 1.523(4) . ? C51 C52 1.533(4) . ? C51 C54 1.545(4) . ? C54 C55 1.501(4) . ? C55 O25 1.190(4) . ? C55 O26 1.336(4) . ? C56 O26 1.450(4) . ? C57 C58 1.534(4) . ? C57 Si5 1.833(3) . ? C58 C59 1.542(4) . ? C59 C60 1.530(4) . ? C59 C62 1.530(4) . ? C59 C61 1.532(4) . ? C62 C63 1.506(4) . ? C63 O27 1.202(4) . ? C63 O28 1.343(4) . ? C64 O28 1.448(3) . ? O1 Si1 1.614(2) . ? O1 Si2 1.617(2) . ? O2 Si2 1.611(2) . ? O2 Si3 1.625(2) 2_556 ? O3 Si3 1.625(2) . ? O3 Si1 1.632(2) . ? O4 Si1 1.618(2) . ? O4 Si4 1.621(2) . ? O5 Si4 1.616(2) . ? O5 Si3 1.619(2) 2_556 ? O6 Si2 1.623(2) 2_556 ? O6 Si4 1.626(2) . ? O15 Si6 1.617(2) . ? O15 Si5 1.622(2) . ? O16 Si5 1.613(2) . ? O16 Si7 1.617(2) . ? O17 Si7 1.623(2) . ? O17 Si8 1.623(2) 2_665 ? O18 Si6 1.623(2) 2_665 ? O18 Si7 1.627(2) . ? O19 Si5 1.619(2) . ? O19 Si8 1.620(2) . ? O20 Si6 1.614(2) 2_665 ? O20 Si8 1.621(2) . ? Si2 O6 1.623(2) 2_556 ? Si3 O5 1.619(2) 2_556 ? Si3 O2 1.625(2) 2_556 ? Si6 O20 1.614(2) 2_665 ? Si6 O18 1.623(2) 2_665 ? Si8 O17 1.623(2) 2_665 ? 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 C2 C1 Si1 114.6(2) . . ? C1 C2 C3 117.6(2) . . ? C4 C3 C5 109.9(3) . . ? C4 C3 C2 110.8(3) . . ? C5 C3 C2 107.4(2) . . ? C4 C3 C6 111.5(3) . . ? C5 C3 C6 109.1(2) . . ? C2 C3 C6 108.1(2) . . ? C7 C6 C3 113.4(2) . . ? O7 C7 O8 122.2(3) . . ? O7 C7 C6 125.3(3) . . ? O8 C7 C6 112.5(3) . . ? C10 C9 Si2 115.0(2) . . ? C9 C10 C11 116.9(3) . . ? C12 C11 C13 109.6(3) . . ? C12 C11 C14 112.1(3) . . ? C13 C11 C14 109.6(3) . . ? C12 C11 C10 110.0(3) . . ? C13 C11 C10 106.4(3) . . ? C14 C11 C10 108.9(3) . . ? C15 C14 C11 115.7(3) . . ? O9 C15 O10 120.3(3) . . ? O9 C15 C14 125.6(4) . . ? O10 C15 C14 114.1(3) . . ? C18 C17 Si3 111.9(2) . . ? C17 C18 C19 117.5(2) . . ? C21 C19 C20 109.6(3) . . ? C21 C19 C22 111.0(3) . . ? C20 C19 C22 110.0(3) . . ? C21 C19 C18 111.0(2) . . ? C20 C19 C18 107.9(2) . . ? C22 C19 C18 107.3(2) . . ? C23 C22 C19 115.1(3) . . ? O11 C23 O12 122.8(3) . . ? O11 C23 C22 125.4(3) . . ? O12 C23 C22 111.8(3) . . ? C26 C25 Si4 113.0(2) . . ? C25 C26 C27 116.9(3) . . ? C28 C27 C30 107.8(3) . . ? C28 C27 C29 109.0(3) . . ? C30 C27 C29 109.0(3) . . ? C28 C27 C26 109.6(3) . . ? C30 C27 C26 112.8(2) . . ? C29 C27 C26 108.5(3) . . ? C31 C30 C27 115.7(3) . . ? O13 C31 O14 122.5(3) . . ? O13 C31 C30 125.9(3) . . ? O14 C31 C30 111.6(3) . . ? C34 C33 Si6 112.5(2) . . ? C33 C34 C35 116.8(2) . . ? C36 C35 C37 109.4(3) . . ? C36 C35 C38 107.2(3) . . ? C37 C35 C38 109.2(3) . . ? C36 C35 C34 109.9(3) . . ? C37 C35 C34 107.8(3) . . ? C38 C35 C34 113.2(3) . . ? C39 C38 C35 114.4(3) . . ? O21 C39 O22 122.8(3) . . ? O21 C39 C38 125.5(3) . . ? O22 C39 C38 111.7(3) . . ? C42 C41 Si7 116.8(2) . . ? C41 C42 C43 115.9(2) . . ? C44 C43 C45 108.7(2) . . ? C44 C43 C42 110.8(2) . . ? C45 C43 C42 108.3(2) . . ? C44 C43 C46 107.0(2) . . ? C45 C43 C46 109.7(2) . . ? C42 C43 C46 112.3(2) . . ? C47 C46 C43 113.2(2) . . ? O23 C47 O24 122.2(3) . . ? O23 C47 C46 126.1(3) . . ? O24 C47 C46 111.8(3) . . ? C50 C49 Si8 114.4(2) . . ? C49 C50 C51 117.5(3) . . ? C53 C51 C52 110.2(3) . . ? C53 C51 C50 110.2(3) . . ? C52 C51 C50 107.4(3) . . ? C53 C51 C54 110.3(3) . . ? C52 C51 C54 110.0(3) . . ? C50 C51 C54 108.7(2) . . ? C55 C54 C51 114.8(3) . . ? O25 C55 O26 121.7(3) . . ? O25 C55 C54 126.0(3) . . ? O26 C55 C54 112.3(3) . . ? C58 C57 Si5 113.7(2) . . ? C57 C58 C59 117.1(2) . . ? C60 C59 C62 111.5(3) . . ? C60 C59 C61 110.1(2) . . ? C62 C59 C61 110.2(2) . . ? C60 C59 C58 110.2(2) . . ? C62 C59 C58 108.1(2) . . ? C61 C59 C58 106.6(2) . . ? C63 C62 C59 117.2(3) . . ? O27 C63 O28 122.5(3) . . ? O27 C63 C62 127.2(3) . . ? O28 C63 C62 110.3(3) . . ? Si1 O1 Si2 155.88(13) . . ? Si2 O2 Si3 151.82(14) . 2_556 ? Si3 O3 Si1 139.61(13) . . ? Si1 O4 Si4 152.19(14) . . ? Si4 O5 Si3 155.20(14) . 2_556 ? Si2 O6 Si4 140.15(13) 2_556 . ? C7 O8 C8 115.5(3) . . ? C15 O10 C16 116.4(3) . . ? C23 O12 C24 115.6(3) . . ? C31 O14 C32 114.9(3) . . ? Si6 O15 Si5 148.14(13) . . ? Si5 O16 Si7 153.23(14) . . ? Si7 O17 Si8 147.90(13) . 2_665 ? Si6 O18 Si7 143.47(13) 2_665 . ? Si5 O19 Si8 143.70(14) . . ? Si6 O20 Si8 152.99(13) 2_665 . ? C39 O22 C40 115.5(3) . . ? C47 O24 C48 115.8(3) . . ? C55 O26 C56 115.1(3) . . ? C63 O28 C64 115.3(2) . . ? O1 Si1 O4 109.18(11) . . ? O1 Si1 O3 108.85(11) . . ? O4 Si1 O3 108.54(10) . . ? O1 Si1 C1 108.38(12) . . ? O4 Si1 C1 110.06(12) . . ? O3 Si1 C1 111.79(12) . . ? O2 Si2 O1 108.56(11) . . ? O2 Si2 O6 108.99(10) . 2_556 ? O1 Si2 O6 108.58(11) . 2_556 ? O2 Si2 C9 111.60(13) . . ? O1 Si2 C9 107.91(12) . . ? O6 Si2 C9 111.11(12) 2_556 . ? O5 Si3 O3 108.98(11) 2_556 . ? O5 Si3 O2 109.30(11) 2_556 2_556 ? O3 Si3 O2 108.80(11) . 2_556 ? O5 Si3 C17 109.80(12) 2_556 . ? O3 Si3 C17 111.69(12) . . ? O2 Si3 C17 108.24(12) 2_556 . ? O5 Si4 O4 108.44(11) . . ? O5 Si4 O6 109.08(11) . . ? O4 Si4 O6 108.54(11) . . ? O5 Si4 C25 111.19(12) . . ? O4 Si4 C25 111.00(12) . . ? O6 Si4 C25 108.54(12) . . ? O16 Si5 O19 109.14(10) . . ? O16 Si5 O15 108.11(11) . . ? O19 Si5 O15 109.52(11) . . ? O16 Si5 C57 110.89(12) . . ? O19 Si5 C57 109.52(12) . . ? O15 Si5 C57 109.63(12) . . ? O20 Si6 O15 108.83(11) 2_665 . ? O20 Si6 O18 109.61(10) 2_665 2_665 ? O15 Si6 O18 109.06(10) . 2_665 ? O20 Si6 C33 109.07(12) 2_665 . ? O15 Si6 C33 109.06(13) . . ? O18 Si6 C33 111.18(12) 2_665 . ? O16 Si7 O17 109.11(11) . . ? O16 Si7 O18 109.39(10) . . ? O17 Si7 O18 108.46(11) . . ? O16 Si7 C41 107.17(12) . . ? O17 Si7 C41 111.55(12) . . ? O18 Si7 C41 111.12(12) . . ? O19 Si8 O20 109.05(11) . . ? O19 Si8 O17 109.23(11) . 2_665 ? O20 Si8 O17 108.33(11) . 2_665 ? O19 Si8 C49 108.53(12) . . ? O20 Si8 C49 110.26(12) . . ? O17 Si8 C49 111.40(13) 2_665 . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.541 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.065