Supplementary material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Rob Duchateau' 'Dianne D.Ellis' 'John R.Severn' 'Anthony L.Spek' 'R. van Santen' 'Glenn P.A.Yap' _publ_contact_author_name 'Dr Rob Duchateau' _publ_contact_author_address ; Department of Chemistry Eindhoven University of Technology Den Dolech 2 P.O.Box 513 Eindhoven 5600 MB NETHERLANDS ; _publ_contact_author_email R.DUCHATEAU@TUE.NL _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Silsesquioxane-Bonded Zirconocene Complexes; Soluble Models for Silica-Tethered Olefin Polymerization Catalysts. ; data_6b _database_code_CSD 201605 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H94 Cl2 O12 Si10 Zr, 2.5(C H2 Cl2)' _chemical_formula_sum 'C62.50 H99 Cl7 O12 Si10 Zr' _chemical_formula_weight 1662.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Zr Zr -2.9673 0.5597 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3551(4) _cell_length_b 18.1661(7) _cell_length_c 19.8473(8) _cell_angle_alpha 86.0297(17) _cell_angle_beta 83.156(2) _cell_angle_gamma 77.2346(18) _cell_volume 3960.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1738 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type multi-scan _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_reflns_number 30418 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13918 _reflns_number_gt 9162 _reflns_threshold_expression I>2\s(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0443P)^2^+4.2876P] 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_number_reflns 13918 _refine_ls_number_parameters 890 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1135 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Zr1 Zr -0.22909(4) 0.77908(2) 0.55847(2) 0.02897(12) Uani 1 1 d . . . Cl1 Cl -0.34188(11) 0.88262(6) 0.62670(5) 0.0389(3) Uani 1 1 d . . . Cl2 Cl -0.40521(11) 0.74738(6) 0.51879(5) 0.0403(3) Uani 1 1 d . . . Si1 Si -0.06470(10) 0.71851(6) 0.30781(5) 0.0231(3) Uani 1 1 d . . . Si2 Si 0.20252(11) 0.72600(7) 0.25793(6) 0.0316(3) Uani 1 1 d . . . Si3 Si 0.10891(11) 0.85218(6) 0.15069(6) 0.0315(3) Uani 1 1 d . . . Si4 Si -0.15900(10) 0.84361(6) 0.20097(5) 0.0249(3) Uani 1 1 d . . . Si5 Si -0.14533(13) 0.72026(7) 0.09643(6) 0.0378(3) Uani 1 1 d . . . Si6 Si -0.05130(12) 0.59368(6) 0.20448(6) 0.0339(3) Uani 1 1 d . . . Si7 Si 0.21237(12) 0.60272(7) 0.15355(6) 0.0371(3) Uani 1 1 d . . . Si8 Si 0.11915(13) 0.73001(7) 0.04602(6) 0.0422(3) Uani 1 1 d . . . Si9 Si -0.18166(13) 0.77269(7) 0.75675(6) 0.0405(3) Uani 1 1 d . . . Si10 Si -0.25231(12) 0.55693(7) 0.57018(6) 0.0354(3) Uani 1 1 d . . . O1 O 0.0763(2) 0.72310(15) 0.30521(13) 0.0319(7) Uani 1 1 d . . . O2 O 0.1801(3) 0.80303(17) 0.21036(16) 0.0458(8) Uani 1 1 d . . . O3 O -0.0344(2) 0.87035(15) 0.17550(14) 0.0335(7) Uani 1 1 d . . . O4 O -0.1403(2) 0.79301(14) 0.27126(13) 0.0289(6) Uani 1 1 d . . . O5 O -0.1162(3) 0.64331(16) 0.14353(15) 0.0538(9) Uani 1 1 d . . . O6 O 0.0934(3) 0.57056(15) 0.18182(15) 0.0435(8) Uani 1 1 d . A . O7 O 0.1869(3) 0.65432(15) 0.08519(14) 0.0381(7) Uani 1 1 d . A . O8 O -0.0235(3) 0.72926(18) 0.04851(15) 0.0496(9) Uani 1 1 d . A . O9 O -0.1875(3) 0.79123(15) 0.14500(14) 0.0358(7) Uani 1 1 d . . . O10 O -0.0745(3) 0.64414(15) 0.27064(13) 0.0344(7) Uani 1 1 d . . . O11 O 0.2396(3) 0.65375(17) 0.21064(14) 0.0396(7) Uani 1 1 d . A . O12 O 0.1338(3) 0.80258(16) 0.08442(15) 0.0477(9) Uani 1 1 d . A . C1 C -0.1298(4) 0.7108(2) 0.39688(19) 0.0268(9) Uani 1 1 d . . . H1A H -0.2134 0.7029 0.3973 0.032 Uiso 1 1 calc R . . H1B H -0.0817 0.6652 0.4187 0.032 Uiso 1 1 calc R . . C2 C -0.3422(5) 0.8003(3) 0.7928(2) 0.0562(14) Uani 1 1 d . . . H2A H -0.3870 0.8379 0.7621 0.084 Uiso 1 1 calc R . . H2B H -0.3464 0.8218 0.8372 0.084 Uiso 1 1 calc R . . H2C H -0.3783 0.7557 0.7982 0.084 Uiso 1 1 calc R . . C3 C -0.1038(5) 0.8534(3) 0.7447(3) 0.0623(16) Uani 1 1 d . . . H3A H -0.0989 0.8725 0.7890 0.093 Uiso 1 1 calc R . . H3B H -0.1498 0.8937 0.7168 0.093 Uiso 1 1 calc R . . H3C H -0.0217 0.8364 0.7219 0.093 Uiso 1 1 calc R . . C4 C -0.1040(5) 0.6984(3) 0.8159(2) 0.0539(14) Uani 1 1 d . . . H4A H -0.1102 0.7188 0.8609 0.081 Uiso 1 1 calc R . . H4B H -0.0182 0.6823 0.7986 0.081 Uiso 1 1 calc R . . H4C H -0.1428 0.6549 0.8193 0.081 Uiso 1 1 calc R . . C5 C -0.4124(4) 0.5626(3) 0.6025(3) 0.0496(13) Uani 1 1 d . . . H5A H -0.4387 0.5184 0.5891 0.074 Uiso 1 1 calc R . . H5B H -0.4624 0.6087 0.5836 0.074 Uiso 1 1 calc R . . H5C H -0.4216 0.5639 0.6522 0.074 Uiso 1 1 calc R . . C6 C -0.1532(5) 0.4733(2) 0.6095(3) 0.0563(15) Uani 1 1 d . . . H6A H -0.1740 0.4270 0.5966 0.084 Uiso 1 1 calc R . . H6B H -0.1655 0.4761 0.6590 0.084 Uiso 1 1 calc R . . H6C H -0.0680 0.4727 0.5934 0.084 Uiso 1 1 calc R . . C7 C -0.2306(5) 0.5463(3) 0.4773(2) 0.0558(15) Uani 1 1 d . . . H7A H -0.2804 0.5901 0.4551 0.084 Uiso 1 1 calc R . . H7B H -0.2550 0.5002 0.4669 0.084 Uiso 1 1 calc R . . H7C H -0.1449 0.5430 0.4607 0.084 Uiso 1 1 calc R . . C8 C -0.1688(4) 0.7250(2) 0.6745(2) 0.0319(10) Uani 1 1 d . . . C9 C -0.2487(4) 0.6821(2) 0.6556(2) 0.0303(10) Uani 1 1 d . . . H9 H -0.3271 0.6820 0.6786 0.036 Uiso 1 1 calc R . . C10 C -0.1977(4) 0.6393(2) 0.5984(2) 0.0306(10) Uani 1 1 d . . . C11 C -0.0831(4) 0.6576(2) 0.5793(2) 0.0304(10) Uani 1 1 d . . . H11 H -0.0268 0.6380 0.5422 0.037 Uiso 1 1 calc R . . C12 C -0.0664(4) 0.7107(2) 0.6255(2) 0.0340(10) Uani 1 1 d . . . H12 H 0.0024 0.7328 0.6236 0.041 Uiso 1 1 calc R . . C21 C 0.3244(4) 0.7273(2) 0.3103(2) 0.0397(11) Uani 1 1 d . . . H21 H 0.2940 0.7686 0.3429 0.048 Uiso 1 1 calc R . . C22 C 0.3728(4) 0.6543(3) 0.3517(3) 0.0514(14) Uani 1 1 d . . . H22A H 0.3219 0.6521 0.3956 0.062 Uiso 1 1 calc R . . H22B H 0.3724 0.6094 0.3263 0.062 Uiso 1 1 calc R . . C23 C 0.5019(5) 0.6569(4) 0.3633(4) 0.084(2) Uani 1 1 d . . . H23A H 0.5055 0.6679 0.4111 0.101 Uiso 1 1 calc R . . H23B H 0.5576 0.6079 0.3532 0.101 Uiso 1 1 calc R . . C24 C 0.5370(5) 0.7183(4) 0.3164(4) 0.106(3) Uani 1 1 d . . . H24A H 0.6165 0.6994 0.2901 0.127 Uiso 1 1 calc R . . H24B H 0.5436 0.7614 0.3426 0.127 Uiso 1 1 calc R . . C25 C 0.4403(5) 0.7426(4) 0.2696(3) 0.0755(19) Uani 1 1 d . . . H25A H 0.4603 0.7132 0.2280 0.091 Uiso 1 1 calc R . . H25B H 0.4309 0.7970 0.2563 0.091 Uiso 1 1 calc R . . C31 C 0.1614(4) 0.9407(2) 0.1311(2) 0.0353(11) Uani 1 1 d . . . H31 H 0.1596 0.9655 0.1747 0.042 Uiso 1 1 calc R . . C32 C 0.0835(4) 0.9966(3) 0.0842(3) 0.0528(14) Uani 1 1 d . . . H32A H 0.0544 0.9693 0.0503 0.063 Uiso 1 1 calc R . . H32B H 0.0122 1.0269 0.1109 0.063 Uiso 1 1 calc R . . C33 C 0.1633(6) 1.0467(4) 0.0496(3) 0.078(2) Uani 1 1 d . . . H33A H 0.1529 1.0534 0.0006 0.094 Uiso 1 1 calc R . . H33B H 0.1415 1.0970 0.0696 0.094 Uiso 1 1 calc R . . C34 C 0.2895(6) 1.0103(4) 0.0592(3) 0.095(3) Uani 1 1 d . . . H34A H 0.3236 1.0410 0.0881 0.114 Uiso 1 1 calc R . . H34B H 0.3400 1.0053 0.0148 0.114 Uiso 1 1 calc R . . C35 C 0.2890(4) 0.9326(3) 0.0934(3) 0.0544(14) Uani 1 1 d . . . H35A H 0.3515 0.9190 0.1256 0.065 Uiso 1 1 calc R . . H35B H 0.3043 0.8934 0.0593 0.065 Uiso 1 1 calc R . . C41 C -0.2847(4) 0.9266(2) 0.2136(2) 0.0279(9) Uani 1 1 d . . . H41 H -0.2713 0.9527 0.2539 0.033 Uiso 1 1 calc R . . C42 C -0.4134(4) 0.9126(2) 0.2252(2) 0.0370(11) Uani 1 1 d . . . H42A H -0.4251 0.8765 0.1927 0.044 Uiso 1 1 calc R . . H42B H -0.4313 0.8926 0.2720 0.044 Uiso 1 1 calc R . . C43 C -0.4934(4) 0.9905(3) 0.2131(3) 0.0465(12) Uani 1 1 d . . . H43A H -0.5035 1.0213 0.2535 0.056 Uiso 1 1 calc R . . H43B H -0.5744 0.9865 0.2021 0.056 Uiso 1 1 calc R . . C44 C -0.4239(5) 1.0245(3) 0.1529(3) 0.0676(16) Uani 1 1 d . . . H44A H -0.4551 1.0168 0.1099 0.081 Uiso 1 1 calc R . . H44B H -0.4328 1.0794 0.1577 0.081 Uiso 1 1 calc R . . C45 C -0.2914(4) 0.9841(3) 0.1527(2) 0.0470(13) Uani 1 1 d . . . H45A H -0.2402 1.0207 0.1572 0.056 Uiso 1 1 calc R . . H45B H -0.2626 0.9579 0.1097 0.056 Uiso 1 1 calc R . . C51 C -0.2673(5) 0.7166(3) 0.0455(2) 0.0489(14) Uani 1 1 d . . . H51 H -0.2353 0.6760 0.0123 0.059 Uiso 1 1 calc R . . C52 C -0.3793(6) 0.6974(4) 0.0871(3) 0.079(2) Uani 1 1 d . . . H52A H -0.3733 0.6421 0.0891 0.095 Uiso 1 1 calc R . . H52B H -0.3852 0.7140 0.1340 0.095 Uiso 1 1 calc R . . C53 C -0.4883(7) 0.7363(4) 0.0544(4) 0.100(2) Uani 1 1 d . . . H53A H -0.5475 0.7673 0.0876 0.119 Uiso 1 1 calc R . . H53B H -0.5278 0.6989 0.0374 0.119 Uiso 1 1 calc R . . C54 C -0.4469(5) 0.7860(4) -0.0038(3) 0.0738(18) Uani 1 1 d . . . H54A H -0.4502 0.7645 -0.0478 0.089 Uiso 1 1 calc R . . H54B H -0.4994 0.8374 -0.0027 0.089 Uiso 1 1 calc R . . C55 C -0.3180(5) 0.7890(3) 0.0052(3) 0.0553(15) Uani 1 1 d . . . H55A H -0.3164 0.8339 0.0303 0.066 Uiso 1 1 calc R . . H55B H -0.2695 0.7914 -0.0394 0.066 Uiso 1 1 calc R . . C61 C -0.1144(4) 0.5088(2) 0.2255(2) 0.0359(11) Uani 1 1 d . . . H61 H -0.0837 0.4731 0.1880 0.043 Uiso 1 1 calc R . . C62 C -0.2525(5) 0.5238(3) 0.2331(3) 0.0662(17) Uani 1 1 d . . . H62A H -0.2877 0.5720 0.2555 0.079 Uiso 1 1 calc R . . H62B H -0.2832 0.5265 0.1881 0.079 Uiso 1 1 calc R . . C63 C -0.2849(6) 0.4577(4) 0.2765(5) 0.115(3) Uani 1 1 d . . . H63A H -0.3533 0.4761 0.3112 0.137 Uiso 1 1 calc R . . H63B H -0.3101 0.4227 0.2478 0.137 Uiso 1 1 calc R . . C64 C -0.1769(5) 0.4179(3) 0.3099(3) 0.0534(14) Uani 1 1 d . . . H64A H -0.1462 0.3666 0.2926 0.064 Uiso 1 1 calc R . . H64B H -0.1975 0.4134 0.3597 0.064 Uiso 1 1 calc R . . C65 C -0.0808(4) 0.4664(2) 0.2923(2) 0.0414(12) Uani 1 1 d . . . H65A H -0.0847 0.5022 0.3284 0.050 Uiso 1 1 calc R . . H65B H 0.0020 0.4342 0.2865 0.050 Uiso 1 1 calc R . . C71 C 0.3410(6) 0.5223(3) 0.1358(3) 0.076(2) Uani 0.524(5) 1 d P A 1 H71 H 0.3117 0.4921 0.1036 0.091 Uiso 0.524(5) 1 calc PR A 1 C72 C 0.4466(9) 0.5305(5) 0.1067(6) 0.067(3) Uani 0.524(5) 1 d P A 1 H72A H 0.4762 0.5680 0.1304 0.080 Uiso 0.524(5) 1 calc PR A 1 H72B H 0.4407 0.5484 0.0587 0.080 Uiso 0.524(5) 1 calc PR A 1 C73 C 0.5335(10) 0.4535(6) 0.1107(7) 0.076(4) Uani 0.524(5) 1 d P A 1 H73A H 0.6132 0.4583 0.1233 0.091 Uiso 0.524(5) 1 calc PR A 1 H73B H 0.5460 0.4285 0.0668 0.091 Uiso 0.524(5) 1 calc PR A 1 C74 C 0.4650(7) 0.4070(4) 0.1694(5) 0.100(2) Uani 0.524(5) 1 d P A 1 H74A H 0.4316 0.3679 0.1504 0.120 Uiso 0.524(5) 1 calc PR A 1 H74B H 0.5190 0.3832 0.2041 0.120 Uiso 0.524(5) 1 calc PR A 1 C75 C 0.3702(8) 0.4679(4) 0.1961(4) 0.138(4) Uani 0.524(5) 1 d P A 1 H75A H 0.3986 0.4930 0.2318 0.166 Uiso 0.524(5) 1 calc PR A 1 H75B H 0.2977 0.4488 0.2157 0.166 Uiso 0.524(5) 1 calc PR A 1 C81 C 0.1844(8) 0.7361(3) -0.0426(3) 0.082(2) Uani 0.524(5) 1 d P A 1 H81 H 0.1776 0.6878 -0.0616 0.098 Uiso 0.524(5) 1 calc PR A 1 C82 C 0.2912(10) 0.7414(6) -0.0610(5) 0.053(3) Uani 0.524(5) 1 d P A 1 H82A H 0.3450 0.6904 -0.0622 0.064 Uiso 0.524(5) 1 calc PR A 1 H82B H 0.3190 0.7709 -0.0284 0.064 Uiso 0.524(5) 1 calc PR A 1 C83 C 0.2978(10) 0.7808(7) -0.1322(6) 0.072(4) Uani 0.524(5) 1 d P A 1 H83A H 0.3432 0.8216 -0.1330 0.086 Uiso 0.524(5) 1 calc PR A 1 H83B H 0.3400 0.7441 -0.1664 0.086 Uiso 0.524(5) 1 calc PR A 1 C84 C 0.1751(8) 0.8116(5) -0.1470(4) 0.105(3) Uani 0.524(5) 1 d P A 1 H84A H 0.1557 0.7846 -0.1845 0.126 Uiso 0.524(5) 1 calc PR A 1 H84B H 0.1657 0.8658 -0.1612 0.126 Uiso 0.524(5) 1 calc PR A 1 C85 C 0.0912(10) 0.8027(5) -0.0843(4) 0.049(3) Uani 0.524(5) 1 d P A 1 H85A H 0.0187 0.7854 -0.0945 0.058 Uiso 0.524(5) 1 calc PR A 1 H85B H 0.0654 0.8500 -0.0593 0.058 Uiso 0.524(5) 1 calc PR A 1 C90 C -0.1349(4) 0.7771(2) 0.4397(2) 0.0292(10) Uani 1 1 d . . . C91 C -0.2229(4) 0.8476(2) 0.4396(2) 0.0318(10) Uani 1 1 d . . . C92 C -0.3285(4) 0.8722(2) 0.4059(2) 0.0382(11) Uani 1 1 d . . . H92 H -0.3535 0.8389 0.3784 0.046 Uiso 1 1 calc R . . C93 C -0.3943(5) 0.9445(3) 0.4132(2) 0.0488(13) Uani 1 1 d . . . H93 H -0.4641 0.9615 0.3897 0.059 Uiso 1 1 calc R . . C94 C -0.3604(5) 0.9945(3) 0.4553(2) 0.0525(14) Uani 1 1 d . . . H94 H -0.4075 1.0446 0.4590 0.063 Uiso 1 1 calc R . . C95 C -0.2619(5) 0.9723(2) 0.4902(2) 0.0474(13) Uani 1 1 d . . . H95 H -0.2411 1.0058 0.5192 0.057 Uiso 1 1 calc R . . C96 C -0.1907(4) 0.8979(2) 0.4826(2) 0.0350(11) Uani 1 1 d . . . C97 C -0.0775(4) 0.8608(2) 0.5073(2) 0.0365(11) Uani 1 1 d . . . C98 C 0.0009(5) 0.8856(3) 0.5462(2) 0.0502(14) Uani 1 1 d . . . H98 H -0.0256 0.9313 0.5693 0.060 Uiso 1 1 calc R . . C99 C 0.1143(6) 0.8439(3) 0.5502(3) 0.0564(15) Uani 1 1 d . . . H99 H 0.1673 0.8610 0.5761 0.068 Uiso 1 1 calc R . . C100 C 0.1561(5) 0.7744(3) 0.5164(2) 0.0492(13) Uani 1 1 d . . . H100 H 0.2372 0.7469 0.5188 0.059 Uiso 1 1 calc R . . C101 C 0.0807(4) 0.7472(2) 0.4805(2) 0.0366(11) Uani 1 1 d . . . H101 H 0.1084 0.7001 0.4595 0.044 Uiso 1 1 calc R . . C102 C -0.0388(4) 0.7892(2) 0.4747(2) 0.0303(10) Uani 1 1 d . . . C71A C 0.3410(6) 0.5223(3) 0.1358(3) 0.076(2) Uani 0.476(5) 1 d P A 2 H71A H 0.4137 0.5451 0.1241 0.091 Uiso 0.476(5) 1 calc PR A 2 C72A C 0.3473(12) 0.4737(7) 0.0884(6) 0.079(4) Uani 0.476(5) 1 d P A 2 H72C H 0.3753 0.4951 0.0437 0.094 Uiso 0.476(5) 1 calc PR A 2 H72D H 0.2658 0.4635 0.0857 0.094 Uiso 0.476(5) 1 calc PR A 2 C73A C 0.4335(18) 0.4020(9) 0.1050(9) 0.121(7) Uani 0.476(5) 1 d P A 2 H73C H 0.3947 0.3585 0.1037 0.145 Uiso 0.476(5) 1 calc PR A 2 H73D H 0.5067 0.3949 0.0716 0.145 Uiso 0.476(5) 1 calc PR A 2 C74A C 0.4650(7) 0.4070(4) 0.1694(5) 0.100(2) Uani 0.476(5) 1 d P A 2 H74C H 0.5460 0.4193 0.1676 0.120 Uiso 0.476(5) 1 calc PR A 2 H74D H 0.4647 0.3594 0.1968 0.120 Uiso 0.476(5) 1 calc PR A 2 C75A C 0.3702(8) 0.4679(4) 0.1961(4) 0.138(4) Uani 0.476(5) 1 d P A 2 H75C H 0.3986 0.4930 0.2318 0.166 Uiso 0.476(5) 1 calc PR A 2 H75D H 0.2977 0.4488 0.2157 0.166 Uiso 0.476(5) 1 calc PR A 2 C81A C 0.1844(8) 0.7361(3) -0.0426(3) 0.082(2) Uani 0.476(5) 1 d P A 2 H81A H 0.2723 0.7193 -0.0359 0.098 Uiso 0.476(5) 1 calc PR A 2 C82A C 0.1799(11) 0.6914(6) -0.0894(5) 0.051(3) Uani 0.476(5) 1 d P A 2 H82C H 0.0974 0.6811 -0.0870 0.061 Uiso 0.476(5) 1 calc PR A 2 H82D H 0.2383 0.6427 -0.0833 0.061 Uiso 0.476(5) 1 calc PR A 2 C83A C 0.2123(13) 0.7301(8) -0.1589(5) 0.069(4) Uani 0.476(5) 1 d P A 2 H83C H 0.3005 0.7155 -0.1734 0.083 Uiso 0.476(5) 1 calc PR A 2 H83D H 0.1673 0.7163 -0.1942 0.083 Uiso 0.476(5) 1 calc PR A 2 C84A C 0.1751(8) 0.8116(5) -0.1470(4) 0.105(3) Uani 0.476(5) 1 d P A 2 H84C H 0.0908 0.8315 -0.1579 0.126 Uiso 0.476(5) 1 calc PR A 2 H84D H 0.2293 0.8396 -0.1760 0.126 Uiso 0.476(5) 1 calc PR A 2 C85A C 0.1843(13) 0.8208(6) -0.0719(5) 0.056(3) Uani 0.476(5) 1 d P A 2 H85C H 0.1136 0.8576 -0.0512 0.067 Uiso 0.476(5) 1 calc PR A 2 H85D H 0.2601 0.8363 -0.0651 0.067 Uiso 0.476(5) 1 calc PR A 2 Cl20 Cl 0.78518(16) 0.05747(9) 0.66138(9) 0.0800(5) Uani 1 1 d . . . Cl21 Cl 1.04343(16) 0.01864(10) 0.67439(9) 0.0899(5) Uani 1 1 d . . . C200 C 0.9199(5) 0.0847(3) 0.6487(3) 0.0720(18) Uani 1 1 d . . . H20A H 0.9120 0.1314 0.6732 0.086 Uiso 1 1 calc R . . H20B H 0.9368 0.0973 0.5996 0.086 Uiso 1 1 calc R . . Cl30 Cl 0.66935(16) 0.27059(8) 0.32901(9) 0.0826(5) Uani 1 1 d . . . Cl31 Cl 0.69388(17) 0.11201(8) 0.30701(8) 0.0805(5) Uani 1 1 d . . . C300 C 0.5998(6) 0.1963(3) 0.3279(4) 0.093(2) Uani 1 1 d . . . H30A H 0.5561 0.1896 0.3734 0.112 Uiso 1 1 calc R . . H30B H 0.5383 0.2093 0.2951 0.112 Uiso 1 1 calc R . . C400 C 0.9594(8) 0.4670(4) 0.0192(4) 0.271(4) Uani 0.50 1 d P . . Cl40 Cl 0.8467(5) 0.4922(2) 0.03640(19) 0.1013(13) Uani 0.50 1 d P B 1 Cl41 Cl 0.9594(8) 0.4670(4) 0.0192(4) 0.271(4) Uani 0.50 1 d P . 2 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 Zr1 0.0410(3) 0.0225(2) 0.0207(2) 0.00104(16) -0.00016(18) -0.00332(18) Cl1 0.0546(8) 0.0259(6) 0.0291(6) -0.0003(5) 0.0027(5) 0.0025(5) Cl2 0.0480(7) 0.0407(7) 0.0328(6) 0.0052(5) -0.0067(5) -0.0116(5) Si1 0.0299(7) 0.0196(6) 0.0195(6) 0.0000(4) -0.0019(5) -0.0050(5) Si2 0.0276(7) 0.0313(7) 0.0335(7) 0.0106(5) -0.0032(5) -0.0052(5) Si3 0.0338(7) 0.0244(6) 0.0316(7) 0.0075(5) 0.0040(6) -0.0030(5) Si4 0.0299(7) 0.0203(6) 0.0233(6) 0.0005(5) -0.0035(5) -0.0030(5) Si5 0.0652(9) 0.0216(6) 0.0270(7) -0.0001(5) -0.0188(7) -0.0031(6) Si6 0.0585(9) 0.0190(6) 0.0248(7) -0.0003(5) -0.0106(6) -0.0064(6) Si7 0.0489(8) 0.0249(6) 0.0270(7) 0.0028(5) 0.0069(6) 0.0074(6) Si8 0.0651(10) 0.0276(7) 0.0223(7) 0.0032(5) 0.0082(6) 0.0069(6) Si9 0.0630(9) 0.0302(7) 0.0254(7) -0.0021(5) -0.0067(6) -0.0025(6) Si10 0.0448(8) 0.0251(6) 0.0358(7) -0.0022(5) -0.0009(6) -0.0080(6) O1 0.0306(17) 0.0356(17) 0.0287(16) 0.0040(13) -0.0036(13) -0.0069(13) O2 0.042(2) 0.0398(19) 0.051(2) 0.0246(16) -0.0073(16) -0.0063(15) O3 0.0340(18) 0.0256(16) 0.0389(18) 0.0020(13) 0.0026(14) -0.0066(13) O4 0.0325(17) 0.0267(15) 0.0241(16) 0.0015(12) -0.0002(13) -0.0011(13) O5 0.101(3) 0.0250(17) 0.0385(19) 0.0043(14) -0.0326(19) -0.0085(18) O6 0.063(2) 0.0236(16) 0.0403(19) 0.0004(13) 0.0073(16) -0.0084(15) O7 0.050(2) 0.0281(16) 0.0291(17) 0.0014(13) 0.0023(15) 0.0015(14) O8 0.062(2) 0.051(2) 0.0276(18) -0.0004(15) -0.0106(16) 0.0091(17) O9 0.0467(19) 0.0300(17) 0.0320(17) -0.0068(13) -0.0144(14) -0.0038(14) O10 0.051(2) 0.0291(16) 0.0246(16) -0.0034(12) -0.0013(14) -0.0118(14) O11 0.0345(18) 0.0455(19) 0.0332(18) -0.0003(14) -0.0045(14) 0.0035(15) O12 0.071(2) 0.0298(17) 0.0365(19) 0.0002(14) 0.0189(17) -0.0109(16) C1 0.031(2) 0.024(2) 0.025(2) -0.0005(17) 0.0000(19) -0.0058(19) C2 0.077(4) 0.047(3) 0.036(3) -0.003(2) -0.001(3) 0.003(3) C3 0.092(5) 0.048(3) 0.055(4) -0.006(3) -0.022(3) -0.025(3) C4 0.082(4) 0.042(3) 0.033(3) -0.002(2) -0.013(3) 0.001(3) C5 0.054(3) 0.035(3) 0.059(3) 0.001(2) -0.007(3) -0.008(2) C6 0.056(3) 0.024(3) 0.090(4) -0.004(3) -0.012(3) -0.009(2) C7 0.085(4) 0.043(3) 0.045(3) -0.012(2) 0.005(3) -0.028(3) C8 0.048(3) 0.024(2) 0.021(2) 0.0052(18) -0.006(2) -0.003(2) C9 0.037(3) 0.025(2) 0.024(2) 0.0037(18) 0.003(2) -0.001(2) C10 0.042(3) 0.021(2) 0.026(2) 0.0037(18) -0.001(2) -0.0020(19) C11 0.042(3) 0.022(2) 0.023(2) -0.0013(18) 0.003(2) -0.001(2) C12 0.046(3) 0.023(2) 0.031(3) 0.0058(19) -0.006(2) -0.004(2) C21 0.033(3) 0.031(3) 0.056(3) 0.007(2) -0.012(2) -0.009(2) C22 0.054(3) 0.040(3) 0.064(4) 0.012(3) -0.029(3) -0.010(3) C23 0.053(4) 0.080(5) 0.124(6) 0.004(4) -0.042(4) -0.008(3) C24 0.043(4) 0.071(5) 0.210(9) 0.023(5) -0.045(5) -0.019(4) C25 0.046(4) 0.083(5) 0.105(5) 0.023(4) -0.014(3) -0.036(3) C31 0.038(3) 0.035(3) 0.033(3) 0.013(2) -0.006(2) -0.011(2) C32 0.047(3) 0.037(3) 0.076(4) 0.024(3) -0.012(3) -0.017(2) C33 0.082(5) 0.080(5) 0.078(4) 0.046(4) -0.018(4) -0.041(4) C34 0.075(5) 0.127(6) 0.092(5) 0.069(5) -0.020(4) -0.056(5) C35 0.043(3) 0.065(4) 0.058(3) 0.005(3) -0.001(3) -0.022(3) C41 0.028(2) 0.026(2) 0.029(2) -0.0015(18) -0.0019(19) -0.0050(19) C42 0.033(3) 0.033(3) 0.044(3) -0.001(2) -0.005(2) -0.007(2) C43 0.032(3) 0.047(3) 0.055(3) -0.001(2) -0.006(2) 0.003(2) C44 0.057(4) 0.063(4) 0.065(4) 0.021(3) -0.003(3) 0.015(3) C45 0.053(3) 0.031(3) 0.050(3) 0.013(2) -0.004(3) 0.001(2) C51 0.088(4) 0.031(3) 0.036(3) 0.007(2) -0.028(3) -0.021(3) C52 0.107(5) 0.085(5) 0.064(4) 0.035(3) -0.046(4) -0.055(4) C53 0.099(6) 0.105(6) 0.089(5) 0.042(5) -0.018(4) -0.017(5) C54 0.071(4) 0.081(4) 0.063(4) 0.026(3) -0.013(3) -0.008(3) C55 0.083(4) 0.050(3) 0.041(3) 0.014(2) -0.034(3) -0.024(3) C61 0.052(3) 0.023(2) 0.034(3) 0.0003(19) -0.013(2) -0.008(2) C62 0.057(4) 0.041(3) 0.104(5) 0.015(3) -0.029(3) -0.012(3) C63 0.061(4) 0.058(4) 0.226(9) 0.061(5) -0.040(5) -0.025(4) C64 0.067(4) 0.048(3) 0.050(3) 0.001(3) 0.000(3) -0.028(3) C65 0.060(3) 0.028(2) 0.041(3) 0.007(2) -0.014(2) -0.017(2) C71 0.090(5) 0.051(4) 0.052(4) 0.015(3) 0.027(3) 0.035(3) C72 0.048(7) 0.038(6) 0.105(9) 0.007(6) 0.027(6) -0.008(5) C73 0.055(7) 0.063(8) 0.098(10) 0.004(7) 0.002(7) 0.007(6) C74 0.101(6) 0.043(4) 0.147(8) 0.009(4) -0.030(5) 0.011(4) C75 0.144(7) 0.114(6) 0.081(5) 0.053(5) 0.034(5) 0.091(5) C81 0.147(7) 0.037(3) 0.029(3) 0.010(3) 0.031(4) 0.023(4) C82 0.046(7) 0.080(8) 0.029(6) -0.005(5) 0.004(5) -0.011(6) C83 0.050(7) 0.096(9) 0.063(8) 0.020(7) 0.012(6) -0.022(7) C84 0.148(8) 0.095(6) 0.062(5) 0.029(4) -0.006(5) -0.018(5) C85 0.063(7) 0.045(6) 0.032(6) 0.012(4) -0.007(5) -0.003(5) C90 0.039(3) 0.026(2) 0.022(2) 0.0009(18) 0.0013(19) -0.008(2) C91 0.047(3) 0.024(2) 0.020(2) 0.0059(18) 0.004(2) -0.005(2) C92 0.049(3) 0.037(3) 0.023(2) 0.004(2) 0.002(2) -0.002(2) C93 0.052(3) 0.045(3) 0.035(3) 0.015(2) 0.008(2) 0.009(3) C94 0.075(4) 0.033(3) 0.034(3) 0.008(2) 0.015(3) 0.008(3) C95 0.082(4) 0.026(3) 0.027(3) 0.002(2) 0.009(3) -0.005(3) C96 0.058(3) 0.025(2) 0.019(2) 0.0015(18) 0.008(2) -0.007(2) C97 0.058(3) 0.027(2) 0.026(2) -0.0010(19) 0.004(2) -0.017(2) C98 0.078(4) 0.037(3) 0.042(3) -0.003(2) -0.007(3) -0.025(3) C99 0.073(4) 0.056(4) 0.049(3) -0.001(3) -0.011(3) -0.032(3) C100 0.048(3) 0.055(3) 0.047(3) 0.004(3) -0.007(3) -0.017(3) C101 0.046(3) 0.035(3) 0.030(3) 0.000(2) 0.000(2) -0.015(2) C102 0.043(3) 0.028(2) 0.020(2) 0.0034(18) 0.000(2) -0.012(2) C71A 0.090(5) 0.051(4) 0.052(4) 0.015(3) 0.027(3) 0.035(3) C72A 0.090(10) 0.059(8) 0.067(9) -0.040(7) -0.028(7) 0.048(7) C73A 0.161(18) 0.080(12) 0.114(14) -0.056(10) -0.045(13) 0.021(11) C74A 0.101(6) 0.043(4) 0.147(8) 0.009(4) -0.030(5) 0.011(4) C75A 0.144(7) 0.114(6) 0.081(5) 0.053(5) 0.034(5) 0.091(5) C81A 0.147(7) 0.037(3) 0.029(3) 0.010(3) 0.031(4) 0.023(4) C82A 0.076(8) 0.046(7) 0.031(6) -0.012(5) 0.007(5) -0.016(6) C83A 0.100(10) 0.095(11) 0.021(6) -0.010(6) -0.002(6) -0.042(9) C84A 0.148(8) 0.095(6) 0.062(5) 0.029(4) -0.006(5) -0.018(5) C85A 0.092(10) 0.049(7) 0.031(6) 0.009(5) -0.010(6) -0.030(7) Cl20 0.0977(13) 0.0568(10) 0.0871(12) -0.0024(8) -0.0152(10) -0.0176(9) Cl21 0.0870(12) 0.0915(13) 0.1028(13) -0.0345(10) -0.0008(10) -0.0398(11) C200 0.093(5) 0.049(3) 0.066(4) 0.004(3) 0.023(3) -0.017(3) Cl30 0.1029(13) 0.0489(9) 0.0977(13) -0.0090(8) -0.0053(10) -0.0212(9) Cl31 0.1190(14) 0.0464(9) 0.0739(11) -0.0061(7) 0.0094(10) -0.0224(9) C300 0.058(4) 0.076(5) 0.149(7) -0.042(4) 0.010(4) -0.021(4) C400 0.348(10) 0.193(6) 0.292(8) -0.121(6) 0.138(7) -0.157(6) Cl40 0.157(4) 0.089(3) 0.063(2) -0.0130(19) -0.021(3) -0.029(3) Cl41 0.348(10) 0.193(6) 0.292(8) -0.121(6) 0.138(7) -0.157(6) _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 Zr1 Cl1 2.4262(11) . ? Zr1 Cl2 2.4288(12) . ? Zr1 C12 2.464(4) . ? Zr1 C90 2.470(4) . ? Zr1 C11 2.492(4) . ? Zr1 C9 2.544(4) . ? Zr1 C8 2.551(4) . ? Zr1 C10 2.567(4) . ? Zr1 C97 2.589(4) . ? Zr1 C91 2.591(4) . ? Zr1 C102 2.598(4) . ? Zr1 C96 2.632(4) . ? Si1 O4 1.610(3) . ? Si1 O10 1.614(3) . ? Si1 O1 1.616(3) . ? Si1 C1 1.841(4) . ? Si2 O11 1.616(3) . ? Si2 O2 1.622(3) . ? Si2 O1 1.626(3) . ? Si2 C21 1.833(4) . ? Si3 O12 1.608(3) . ? Si3 O3 1.610(3) . ? Si3 O2 1.617(3) . ? Si3 C31 1.836(4) . ? Si4 O3 1.611(3) . ? Si4 O9 1.616(3) . ? Si4 O4 1.626(3) . ? Si4 C41 1.841(4) . ? Si5 O8 1.615(4) . ? Si5 O9 1.616(3) . ? Si5 O5 1.620(3) . ? Si5 C51 1.824(5) . ? Si6 O5 1.609(3) . ? Si6 O10 1.616(3) . ? Si6 O6 1.620(3) . ? Si6 C61 1.842(4) . ? Si7 O11 1.611(3) . ? Si7 O7 1.613(3) . ? Si7 O6 1.613(3) . ? Si7 C71 1.843(5) . ? Si8 O12 1.616(3) . ? Si8 O7 1.617(3) . ? Si8 O8 1.618(4) . ? Si8 C81 1.831(5) . ? Si9 C2 1.850(5) . ? Si9 C3 1.860(5) . ? Si9 C4 1.866(5) . ? Si9 C8 1.876(4) . ? Si10 C5 1.838(5) . ? Si10 C7 1.848(5) . ? Si10 C6 1.864(5) . ? Si10 C10 1.883(4) . ? C1 C90 1.508(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C12 1.413(6) . ? C8 C9 1.416(6) . ? C9 C10 1.413(6) . ? C9 H9 0.9500 . ? C10 C11 1.415(6) . ? C11 C12 1.432(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C21 C25 1.530(7) . ? C21 C22 1.539(6) . ? C21 H21 1.0000 . ? C22 C23 1.522(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.494(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.495(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C31 C35 1.531(6) . ? C31 C32 1.531(6) . ? C31 H31 1.0000 . ? C32 C33 1.500(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.469(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.525(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C41 C42 1.525(5) . ? C41 C45 1.540(6) . ? C41 H41 1.0000 . ? C42 C43 1.524(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.524(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.521(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C51 C52 1.525(7) . ? C51 C55 1.526(6) . ? C51 H51 1.0000 . ? C52 C53 1.481(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.513(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.508(7) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C61 C62 1.523(7) . ? C61 C65 1.531(6) . ? C61 H61 1.0000 . ? C62 C63 1.515(7) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.485(8) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.542(6) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C71 C72 1.303(10) . ? C71 C75 1.519(8) . ? C71 H71 1.0000 . ? C72 C73 1.527(14) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.617(13) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.443(9) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C81 C82 1.247(10) . ? C81 C85 1.666(11) . ? C81 H81 1.0000 . ? C82 C83 1.540(14) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.439(12) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.498(11) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C90 C102 1.425(6) . ? C90 C91 1.440(6) . ? C91 C92 1.414(6) . ? C91 C96 1.425(6) . ? C92 C93 1.367(6) . ? C92 H92 0.9500 . ? C93 C94 1.417(7) . ? C93 H93 0.9500 . ? C94 C95 1.357(7) . ? C94 H94 0.9500 . ? C95 C96 1.421(6) . ? C95 H95 0.9500 . ? C96 C97 1.438(6) . ? C97 C98 1.406(6) . ? C97 C102 1.450(6) . ? C98 C99 1.350(7) . ? C98 H98 0.9500 . ? C99 C100 1.431(7) . ? C99 H99 0.9500 . ? C100 C101 1.365(6) . ? C100 H100 0.9500 . ? C101 C102 1.416(6) . ? C101 H101 0.9500 . ? C72A C73A 1.489(18) . ? C72A H72C 0.9900 . ? C72A H72D 0.9900 . ? C73A H73C 0.9900 . ? C73A H73D 0.9900 . ? C82A C83A 1.548(14) . ? C82A H82C 0.9900 . ? C82A H82D 0.9900 . ? C83A H83C 0.9900 . ? C83A H83D 0.9900 . ? C85A H85C 0.9900 . ? C85A H85D 0.9900 . ? Cl20 C200 1.695(6) . ? Cl21 C200 1.735(6) . ? C200 H20A 0.9900 . ? C200 H20B 0.9900 . ? Cl30 C300 1.711(6) . ? Cl31 C300 1.708(6) . ? C300 H30A 0.9900 . ? C300 H30B 0.9900 . ? C400 Cl40 1.274(8) . ? C400 Cl41 1.751(11) 2_765 ? 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 Cl1 Zr1 Cl2 96.00(4) . . ? Cl1 Zr1 C12 105.81(10) . . ? Cl2 Zr1 C12 134.44(10) . . ? Cl1 Zr1 C90 131.28(10) . . ? Cl2 Zr1 C90 88.33(10) . . ? C12 Zr1 C90 105.01(14) . . ? Cl1 Zr1 C11 135.99(9) . . ? Cl2 Zr1 C11 106.88(10) . . ? C12 Zr1 C11 33.60(13) . . ? C90 Zr1 C11 87.33(13) . . ? Cl1 Zr1 C9 92.38(10) . . ? Cl2 Zr1 C9 86.94(10) . . ? C12 Zr1 C9 53.31(14) . . ? C90 Zr1 C9 136.34(13) . . ? C11 Zr1 C9 53.11(13) . . ? Cl1 Zr1 C8 81.43(10) . . ? Cl2 Zr1 C8 118.14(10) . . ? C12 Zr1 C8 32.68(13) . . ? C90 Zr1 C8 137.52(14) . . ? C11 Zr1 C8 54.70(13) . . ? C9 Zr1 C8 32.28(13) . . ? Cl1 Zr1 C10 124.10(10) . . ? Cl2 Zr1 C10 79.96(10) . . ? C12 Zr1 C10 54.63(13) . . ? C90 Zr1 C10 104.47(13) . . ? C11 Zr1 C10 32.44(13) . . ? C9 Zr1 C10 32.10(12) . . ? C8 Zr1 C10 54.46(13) . . ? Cl1 Zr1 C97 90.46(10) . . ? Cl2 Zr1 C97 133.57(11) . . ? C12 Zr1 C97 86.48(15) . . ? C90 Zr1 C97 55.02(13) . . ? C11 Zr1 C97 99.44(14) . . ? C9 Zr1 C97 138.81(14) . . ? C8 Zr1 C97 108.29(14) . . ? C10 Zr1 C97 131.80(15) . . ? Cl1 Zr1 C91 99.93(10) . . ? Cl2 Zr1 C91 80.64(10) . . ? C12 Zr1 C91 131.85(14) . . ? C90 Zr1 C91 32.96(13) . . ? C11 Zr1 C91 120.26(13) . . ? C9 Zr1 C91 163.30(13) . . ? C8 Zr1 C91 161.07(14) . . ? C10 Zr1 C91 133.23(13) . . ? C97 Zr1 C91 52.99(14) . . ? Cl1 Zr1 C102 122.90(9) . . ? Cl2 Zr1 C102 120.74(9) . . ? C12 Zr1 C102 79.49(14) . . ? C90 Zr1 C102 32.54(13) . . ? C11 Zr1 C102 76.26(13) . . ? C9 Zr1 C102 128.30(14) . . ? C8 Zr1 C102 111.00(14) . . ? C10 Zr1 C102 105.45(13) . . ? C97 Zr1 C102 32.46(13) . . ? C91 Zr1 C102 52.39(14) . . ? Cl1 Zr1 C96 77.88(9) . . ? Cl2 Zr1 C96 105.24(11) . . ? C12 Zr1 C96 118.07(14) . . ? C90 Zr1 C96 54.42(13) . . ? C11 Zr1 C96 128.36(14) . . ? C9 Zr1 C96 165.00(13) . . ? C8 Zr1 C96 133.43(13) . . ? C10 Zr1 C96 157.29(14) . . ? C97 Zr1 C96 31.96(14) . . ? C91 Zr1 C96 31.64(12) . . ? C102 Zr1 C96 52.61(14) . . ? O4 Si1 O10 110.05(15) . . ? O4 Si1 O1 110.29(14) . . ? O10 Si1 O1 109.53(16) . . ? O4 Si1 C1 109.21(17) . . ? O10 Si1 C1 108.16(16) . . ? O1 Si1 C1 109.56(17) . . ? O11 Si2 O2 109.56(17) . . ? O11 Si2 O1 109.53(15) . . ? O2 Si2 O1 107.83(16) . . ? O11 Si2 C21 110.19(19) . . ? O2 Si2 C21 108.91(18) . . ? O1 Si2 C21 110.79(18) . . ? O12 Si3 O3 109.14(17) . . ? O12 Si3 O2 108.41(18) . . ? O3 Si3 O2 108.63(16) . . ? O12 Si3 C31 110.12(18) . . ? O3 Si3 C31 109.94(18) . . ? O2 Si3 C31 110.56(18) . . ? O3 Si4 O9 109.34(15) . . ? O3 Si4 O4 108.11(15) . . ? O9 Si4 O4 108.33(14) . . ? O3 Si4 C41 109.99(16) . . ? O9 Si4 C41 109.88(17) . . ? O4 Si4 C41 111.14(17) . . ? O8 Si5 O9 109.05(16) . . ? O8 Si5 O5 109.10(19) . . ? O9 Si5 O5 108.77(16) . . ? O8 Si5 C51 110.9(2) . . ? O9 Si5 C51 109.5(2) . . ? O5 Si5 C51 109.48(18) . . ? O5 Si6 O10 108.90(16) . . ? O5 Si6 O6 108.83(18) . . ? O10 Si6 O6 108.85(16) . . ? O5 Si6 C61 110.50(18) . . ? O10 Si6 C61 109.02(18) . . ? O6 Si6 C61 110.69(18) . . ? O11 Si7 O7 109.22(15) . . ? O11 Si7 O6 108.19(16) . . ? O7 Si7 O6 109.56(17) . . ? O11 Si7 C71 110.9(3) . . ? O7 Si7 C71 110.2(2) . . ? O6 Si7 C71 108.8(2) . . ? O12 Si8 O7 108.63(17) . . ? O12 Si8 O8 109.29(18) . . ? O7 Si8 O8 108.98(16) . . ? O12 Si8 C81 109.2(2) . . ? O7 Si8 C81 111.3(2) . . ? O8 Si8 C81 109.4(3) . . ? C2 Si9 C3 113.1(3) . . ? C2 Si9 C4 107.0(2) . . ? C3 Si9 C4 110.6(2) . . ? C2 Si9 C8 110.9(2) . . ? C3 Si9 C8 110.1(2) . . ? C4 Si9 C8 104.9(2) . . ? C5 Si10 C7 110.2(2) . . ? C5 Si10 C6 110.7(2) . . ? C7 Si10 C6 107.5(3) . . ? C5 Si10 C10 110.4(2) . . ? C7 Si10 C10 114.26(19) . . ? C6 Si10 C10 103.5(2) . . ? Si1 O1 Si2 146.83(19) . . ? Si3 O2 Si2 148.1(2) . . ? Si3 O3 Si4 151.39(19) . . ? Si1 O4 Si4 146.57(19) . . ? Si6 O5 Si5 151.7(2) . . ? Si7 O6 Si6 144.56(19) . . ? Si7 O7 Si8 151.5(2) . . ? Si5 O8 Si8 145.7(2) . . ? Si5 O9 Si4 150.4(2) . . ? Si1 O10 Si6 151.19(19) . . ? Si7 O11 Si2 151.8(2) . . ? Si3 O12 Si8 150.53(19) . . ? C90 C1 Si1 116.4(3) . . ? C90 C1 H1A 108.2 . . ? Si1 C1 H1A 108.2 . . ? C90 C1 H1B 108.2 . . ? Si1 C1 H1B 108.2 . . ? H1A C1 H1B 107.3 . . ? Si9 C2 H2A 109.5 . . ? Si9 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si9 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si9 C3 H3A 109.5 . . ? Si9 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si9 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si9 C4 H4A 109.5 . . ? Si9 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si9 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si10 C5 H5A 109.5 . . ? Si10 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si10 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si10 C6 H6A 109.5 . . ? Si10 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si10 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si10 C7 H7A 109.5 . . ? Si10 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si10 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 C8 C9 105.2(4) . . ? C12 C8 Si9 127.0(3) . . ? C9 C8 Si9 126.6(3) . . ? C12 C8 Zr1 70.3(2) . . ? C9 C8 Zr1 73.6(2) . . ? Si9 C8 Zr1 130.2(2) . . ? C10 C9 C8 111.7(4) . . ? C10 C9 Zr1 74.8(2) . . ? C8 C9 Zr1 74.1(2) . . ? C10 C9 H9 124.2 . . ? C8 C9 H9 124.2 . . ? Zr1 C9 H9 118.5 . . ? C9 C10 C11 105.5(3) . . ? C9 C10 Si10 125.5(3) . . ? C11 C10 Si10 127.0(3) . . ? C9 C10 Zr1 73.1(2) . . ? C11 C10 Zr1 70.8(2) . . ? Si10 C10 Zr1 133.0(2) . . ? C10 C11 C12 108.5(4) . . ? C10 C11 Zr1 76.7(2) . . ? C12 C11 Zr1 72.1(2) . . ? C10 C11 H11 125.8 . . ? C12 C11 H11 125.8 . . ? Zr1 C11 H11 117.3 . . ? C8 C12 C11 109.0(4) . . ? C8 C12 Zr1 77.0(2) . . ? C11 C12 Zr1 74.3(2) . . ? C8 C12 H12 125.5 . . ? C11 C12 H12 125.5 . . ? Zr1 C12 H12 115.3 . . ? C25 C21 C22 102.2(4) . . ? C25 C21 Si2 113.7(4) . . ? C22 C21 Si2 117.2(3) . . ? C25 C21 H21 107.8 . . ? C22 C21 H21 107.8 . . ? Si2 C21 H21 107.8 . . ? C23 C22 C21 106.0(4) . . ? C23 C22 H22A 110.5 . . ? C21 C22 H22A 110.5 . . ? C23 C22 H22B 110.5 . . ? C21 C22 H22B 110.5 . . ? H22A C22 H22B 108.7 . . ? C24 C23 C22 106.7(5) . . ? C24 C23 H23A 110.4 . . ? C22 C23 H23A 110.4 . . ? C24 C23 H23B 110.4 . . ? C22 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? C23 C24 C25 107.3(5) . . ? C23 C24 H24A 110.3 . . ? C25 C24 H24A 110.2 . . ? C23 C24 H24B 110.2 . . ? C25 C24 H24B 110.3 . . ? H24A C24 H24B 108.5 . . ? C24 C25 C21 105.0(5) . . ? C24 C25 H25A 110.8 . . ? C21 C25 H25A 110.8 . . ? C24 C25 H25B 110.8 . . ? C21 C25 H25B 110.8 . . ? H25A C25 H25B 108.8 . . ? C35 C31 C32 102.5(3) . . ? C35 C31 Si3 115.6(3) . . ? C32 C31 Si3 113.8(3) . . ? C35 C31 H31 108.2 . . ? C32 C31 H31 108.2 . . ? Si3 C31 H31 108.2 . . ? C33 C32 C31 106.5(4) . . ? C33 C32 H32A 110.4 . . ? C31 C32 H32A 110.4 . . ? C33 C32 H32B 110.4 . . ? C31 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? C34 C33 C32 107.7(5) . . ? C34 C33 H33A 110.2 . . ? C32 C33 H33A 110.2 . . ? C34 C33 H33B 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C33 C34 C35 107.5(4) . . ? C33 C34 H34A 110.2 . . ? C35 C34 H34A 110.2 . . ? C33 C34 H34B 110.2 . . ? C35 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C34 C35 C31 104.3(4) . . ? C34 C35 H35A 110.9 . . ? C31 C35 H35A 110.9 . . ? C34 C35 H35B 110.9 . . ? C31 C35 H35B 110.9 . . ? H35A C35 H35B 108.9 . . ? C42 C41 C45 102.7(3) . . ? C42 C41 Si4 117.4(3) . . ? C45 C41 Si4 113.3(3) . . ? C42 C41 H41 107.7 . . ? C45 C41 H41 107.7 . . ? Si4 C41 H41 107.7 . . ? C43 C42 C41 103.7(3) . . ? C43 C42 H42A 111.0 . . ? C41 C42 H42A 111.0 . . ? C43 C42 H42B 111.0 . . ? C41 C42 H42B 111.0 . . ? H42A C42 H42B 109.0 . . ? C42 C43 C44 103.6(4) . . ? C42 C43 H43A 111.0 . . ? C44 C43 H43A 111.0 . . ? C42 C43 H43B 111.0 . . ? C44 C43 H43B 111.0 . . ? H43A C43 H43B 109.0 . . ? C45 C44 C43 106.6(4) . . ? C45 C44 H44A 110.4 . . ? C43 C44 H44A 110.4 . . ? C45 C44 H44B 110.4 . . ? C43 C44 H44B 110.4 . . ? H44A C44 H44B 108.6 . . ? C44 C45 C41 106.7(4) . . ? C44 C45 H45A 110.4 . . ? C41 C45 H45A 110.4 . . ? C44 C45 H45B 110.4 . . ? C41 C45 H45B 110.4 . . ? H45A C45 H45B 108.6 . . ? C52 C51 C55 103.7(5) . . ? C52 C51 Si5 113.6(3) . . ? C55 C51 Si5 116.3(3) . . ? C52 C51 H51 107.6 . . ? C55 C51 H51 107.6 . . ? Si5 C51 H51 107.6 . . ? C53 C52 C51 108.7(5) . . ? C53 C52 H52A 110.0 . . ? C51 C52 H52A 110.0 . . ? C53 C52 H52B 110.0 . . ? C51 C52 H52B 110.0 . . ? H52A C52 H52B 108.3 . . ? C52 C53 C54 107.4(5) . . ? C52 C53 H53A 110.2 . . ? C54 C53 H53A 110.2 . . ? C52 C53 H53B 110.2 . . ? C54 C53 H53B 110.2 . . ? H53A C53 H53B 108.5 . . ? C55 C54 C53 106.4(5) . . ? C55 C54 H54A 110.5 . . ? C53 C54 H54A 110.5 . . ? C55 C54 H54B 110.5 . . ? C53 C54 H54B 110.5 . . ? H54A C54 H54B 108.6 . . ? C54 C55 C51 106.0(4) . . ? C54 C55 H55A 110.5 . . ? C51 C55 H55A 110.5 . . ? C54 C55 H55B 110.5 . . ? C51 C55 H55B 110.5 . . ? H55A C55 H55B 108.7 . . ? C62 C61 C65 103.5(4) . . ? C62 C61 Si6 114.4(3) . . ? C65 C61 Si6 115.2(3) . . ? C62 C61 H61 107.8 . . ? C65 C61 H61 107.8 . . ? Si6 C61 H61 107.8 . . ? C63 C62 C61 105.3(4) . . ? C63 C62 H62A 110.7 . . ? C61 C62 H62A 110.7 . . ? C63 C62 H62B 110.7 . . ? C61 C62 H62B 110.7 . . ? H62A C62 H62B 108.8 . . ? C64 C63 C62 108.7(5) . . ? C64 C63 H63A 109.9 . . ? C62 C63 H63A 109.9 . . ? C64 C63 H63B 109.9 . . ? C62 C63 H63B 109.9 . . ? H63A C63 H63B 108.3 . . ? C63 C64 C65 105.9(4) . . ? C63 C64 H64A 110.6 . . ? C65 C64 H64A 110.6 . . ? C63 C64 H64B 110.6 . . ? C65 C64 H64B 110.6 . . ? H64A C64 H64B 108.7 . . ? C61 C65 C64 104.3(4) . . ? C61 C65 H65A 110.9 . . ? C64 C65 H65A 110.9 . . ? C61 C65 H65B 110.9 . . ? C64 C65 H65B 110.9 . . ? H65A C65 H65B 108.9 . . ? C72 C71 C75 104.4(7) . . ? C72 C71 Si7 122.8(6) . . ? C75 C71 Si7 114.9(4) . . ? C72 C71 H71 104.3 . . ? C75 C71 H71 104.3 . . ? Si7 C71 H71 104.3 . . ? C71 C72 C73 107.3(8) . . ? C71 C72 H72A 110.3 . . ? C73 C72 H72A 110.3 . . ? C71 C72 H72B 110.3 . . ? C73 C72 H72B 110.3 . . ? H72A C72 H72B 108.5 . . ? C72 C73 C74 103.5(8) . . ? C72 C73 H73A 111.1 . . ? C74 C73 H73A 111.1 . . ? C72 C73 H73B 111.1 . . ? C74 C73 H73B 111.1 . . ? H73A C73 H73B 109.0 . . ? C75 C74 C73 99.6(6) . . ? C75 C74 H74A 111.8 . . ? C73 C74 H74A 111.8 . . ? C75 C74 H74B 111.8 . . ? C73 C74 H74B 111.8 . . ? H74A C74 H74B 109.6 . . ? C74 C75 C71 105.3(6) . . ? C74 C75 H75A 110.7 . . ? C71 C75 H75A 110.7 . . ? C74 C75 H75B 110.7 . . ? C71 C75 H75B 110.7 . . ? H75A C75 H75B 108.8 . . ? C82 C81 C85 108.8(7) . . ? C82 C81 Si8 124.6(7) . . ? C85 C81 Si8 108.6(5) . . ? C82 C81 H81 104.3 . . ? C85 C81 H81 104.3 . . ? Si8 C81 H81 104.3 . . ? C81 C82 C83 109.4(8) . . ? C81 C82 H82A 109.8 . . ? C83 C82 H82A 109.8 . . ? C81 C82 H82B 109.8 . . ? C83 C82 H82B 109.8 . . ? H82A C82 H82B 108.3 . . ? C84 C83 C82 107.4(8) . . ? C84 C83 H83A 110.2 . . ? C82 C83 H83A 110.2 . . ? C84 C83 H83B 110.2 . . ? C82 C83 H83B 110.2 . . ? H83A C83 H83B 108.5 . . ? C83 C84 C85 108.4(7) . . ? C83 C84 H84A 110.0 . . ? C85 C84 H84A 110.0 . . ? C83 C84 H84B 110.0 . . ? C85 C84 H84B 110.0 . . ? H84A C84 H84B 108.4 . . ? C84 C85 C81 98.9(7) . . ? C84 C85 H85A 112.0 . . ? C81 C85 H85A 112.0 . . ? C84 C85 H85B 112.0 . . ? C81 C85 H85B 112.0 . . ? H85A C85 H85B 109.7 . . ? C102 C90 C91 106.2(3) . . ? C102 C90 C1 125.8(4) . . ? C91 C90 C1 126.5(4) . . ? C102 C90 Zr1 78.7(2) . . ? C91 C90 Zr1 78.2(2) . . ? C1 C90 Zr1 120.6(2) . . ? C92 C91 C96 119.0(4) . . ? C92 C91 C90 131.7(4) . . ? C96 C91 C90 109.3(4) . . ? C92 C91 Zr1 121.8(3) . . ? C96 C91 Zr1 75.7(2) . . ? C90 C91 Zr1 68.9(2) . . ? C93 C92 C91 119.3(4) . . ? C93 C92 H92 120.3 . . ? C91 C92 H92 120.3 . . ? C92 C93 C94 121.3(5) . . ? C92 C93 H93 119.4 . . ? C94 C93 H93 119.4 . . ? C95 C94 C93 121.2(5) . . ? C95 C94 H94 119.4 . . ? C93 C94 H94 119.4 . . ? C94 C95 C96 118.7(5) . . ? C94 C95 H95 120.7 . . ? C96 C95 H95 120.7 . . ? C95 C96 C91 120.5(4) . . ? C95 C96 C97 131.6(4) . . ? C91 C96 C97 107.7(4) . . ? C95 C96 Zr1 124.5(3) . . ? C91 C96 Zr1 72.6(2) . . ? C97 C96 Zr1 72.4(2) . . ? C98 C97 C96 132.4(4) . . ? C98 C97 C102 120.1(5) . . ? C96 C97 C102 106.8(4) . . ? C98 C97 Zr1 123.0(3) . . ? C96 C97 Zr1 75.7(2) . . ? C102 C97 Zr1 74.1(2) . . ? C99 C98 C97 119.5(5) . . ? C99 C98 H98 120.2 . . ? C97 C98 H98 120.2 . . ? C98 C99 C100 121.3(5) . . ? C98 C99 H99 119.3 . . ? C100 C99 H99 119.3 . . ? C101 C100 C99 120.6(5) . . ? C101 C100 H100 119.7 . . ? C99 C100 H100 119.7 . . ? C100 C101 C102 119.9(4) . . ? C100 C101 H101 120.0 . . ? C102 C101 H101 120.0 . . ? C101 C102 C90 132.7(4) . . ? C101 C102 C97 118.4(4) . . ? C90 C102 C97 108.9(4) . . ? C101 C102 Zr1 125.6(3) . . ? C90 C102 Zr1 68.8(2) . . ? C97 C102 Zr1 73.4(2) . . ? C73A C72A H72C 109.8 . . ? C73A C72A H72D 109.8 . . ? H72C C72A H72D 108.2 . . ? C72A C73A H73C 110.2 . . ? C72A C73A H73D 110.2 . . ? H73C C73A H73D 108.5 . . ? C83A C82A H82C 110.1 . . ? C83A C82A H82D 110.1 . . ? H82C C82A H82D 108.4 . . ? C82A C83A H83C 110.9 . . ? C82A C83A H83D 110.9 . . ? H83C C83A H83D 108.9 . . ? H85C C85A H85D 109.5 . . ? Cl20 C200 Cl21 115.4(3) . . ? Cl20 C200 H20A 108.4 . . ? Cl21 C200 H20A 108.4 . . ? Cl20 C200 H20B 108.4 . . ? Cl21 C200 H20B 108.4 . . ? H20A C200 H20B 107.5 . . ? Cl31 C300 Cl30 115.5(4) . . ? Cl31 C300 H30A 108.4 . . ? Cl30 C300 H30A 108.4 . . ? Cl31 C300 H30B 108.4 . . ? Cl30 C300 H30B 108.4 . . ? H30A C300 H30B 107.5 . . ? Cl40 C400 Cl41 116.0(8) . 2_765 ? 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 O4 Si1 O1 Si2 -64.3(4) . . . . ? O10 Si1 O1 Si2 56.9(4) . . . . ? C1 Si1 O1 Si2 175.4(3) . . . . ? O11 Si2 O1 Si1 -55.8(4) . . . . ? O2 Si2 O1 Si1 63.3(4) . . . . ? C21 Si2 O1 Si1 -177.6(3) . . . . ? O12 Si3 O2 Si2 -57.0(5) . . . . ? O3 Si3 O2 Si2 61.5(5) . . . . ? C31 Si3 O2 Si2 -177.8(4) . . . . ? O11 Si2 O2 Si3 55.3(5) . . . . ? O1 Si2 O2 Si3 -63.8(5) . . . . ? C21 Si2 O2 Si3 175.9(4) . . . . ? O12 Si3 O3 Si4 57.9(4) . . . . ? O2 Si3 O3 Si4 -60.1(4) . . . . ? C31 Si3 O3 Si4 178.8(4) . . . . ? O9 Si4 O3 Si3 -57.3(4) . . . . ? O4 Si4 O3 Si3 60.4(4) . . . . ? C41 Si4 O3 Si3 -178.1(4) . . . . ? O10 Si1 O4 Si4 -57.8(4) . . . . ? O1 Si1 O4 Si4 63.1(3) . . . . ? C1 Si1 O4 Si4 -176.4(3) . . . . ? O3 Si4 O4 Si1 -60.2(3) . . . . ? O9 Si4 O4 Si1 58.1(4) . . . . ? C41 Si4 O4 Si1 178.9(3) . . . . ? O10 Si6 O5 Si5 48.0(6) . . . . ? O6 Si6 O5 Si5 -70.5(6) . . . . ? C61 Si6 O5 Si5 167.8(5) . . . . ? O8 Si5 O5 Si6 69.3(6) . . . . ? O9 Si5 O5 Si6 -49.5(6) . . . . ? C51 Si5 O5 Si6 -169.1(5) . . . . ? O11 Si7 O6 Si6 65.2(4) . . . . ? O7 Si7 O6 Si6 -53.8(4) . . . . ? C71 Si7 O6 Si6 -174.3(4) . . . . ? O5 Si6 O6 Si7 54.0(4) . . . . ? O10 Si6 O6 Si7 -64.5(4) . . . . ? C61 Si6 O6 Si7 175.7(3) . . . . ? O11 Si7 O7 Si8 -49.0(5) . . . . ? O6 Si7 O7 Si8 69.3(5) . . . . ? C71 Si7 O7 Si8 -171.0(5) . . . . ? O12 Si8 O7 Si7 50.3(5) . . . . ? O8 Si8 O7 Si7 -68.7(5) . . . . ? C81 Si8 O7 Si7 170.5(5) . . . . ? O9 Si5 O8 Si8 66.9(4) . . . . ? O5 Si5 O8 Si8 -51.8(4) . . . . ? C51 Si5 O8 Si8 -172.5(4) . . . . ? O12 Si8 O8 Si5 -66.4(4) . . . . ? O7 Si8 O8 Si5 52.2(4) . . . . ? C81 Si8 O8 Si5 174.0(4) . . . . ? O8 Si5 O9 Si4 -55.7(4) . . . . ? O5 Si5 O9 Si4 63.2(4) . . . . ? C51 Si5 O9 Si4 -177.2(4) . . . . ? O3 Si4 O9 Si5 51.3(4) . . . . ? O4 Si4 O9 Si5 -66.3(4) . . . . ? C41 Si4 O9 Si5 172.1(4) . . . . ? O4 Si1 O10 Si6 61.9(5) . . . . ? O1 Si1 O10 Si6 -59.5(5) . . . . ? C1 Si1 O10 Si6 -178.9(4) . . . . ? O5 Si6 O10 Si1 -57.6(5) . . . . ? O6 Si6 O10 Si1 60.9(5) . . . . ? C61 Si6 O10 Si1 -178.2(4) . . . . ? O7 Si7 O11 Si2 56.8(5) . . . . ? O6 Si7 O11 Si2 -62.4(5) . . . . ? C71 Si7 O11 Si2 178.4(4) . . . . ? O2 Si2 O11 Si7 -59.0(5) . . . . ? O1 Si2 O11 Si7 59.0(5) . . . . ? C21 Si2 O11 Si7 -178.8(4) . . . . ? O3 Si3 O12 Si8 -52.3(5) . . . . ? O2 Si3 O12 Si8 65.9(5) . . . . ? C31 Si3 O12 Si8 -173.0(5) . . . . ? O7 Si8 O12 Si3 -63.2(5) . . . . ? O8 Si8 O12 Si3 55.6(5) . . . . ? C81 Si8 O12 Si3 175.3(5) . . . . ? O4 Si1 C1 C90 -57.3(3) . . . . ? O10 Si1 C1 C90 -177.1(3) . . . . ? O1 Si1 C1 C90 63.6(3) . . . . ? C2 Si9 C8 C12 165.4(4) . . . . ? C3 Si9 C8 C12 39.5(4) . . . . ? C4 Si9 C8 C12 -79.4(4) . . . . ? C2 Si9 C8 C9 -29.1(4) . . . . ? C3 Si9 C8 C9 -155.0(4) . . . . ? C4 Si9 C8 C9 86.1(4) . . . . ? C2 Si9 C8 Zr1 70.6(3) . . . . ? C3 Si9 C8 Zr1 -55.3(3) . . . . ? C4 Si9 C8 Zr1 -174.2(3) . . . . ? Cl1 Zr1 C8 C12 -138.2(2) . . . . ? Cl2 Zr1 C8 C12 129.6(2) . . . . ? C90 Zr1 C8 C12 7.2(3) . . . . ? C11 Zr1 C8 C12 38.2(2) . . . . ? C9 Zr1 C8 C12 113.3(4) . . . . ? C10 Zr1 C8 C12 78.2(3) . . . . ? C97 Zr1 C8 C12 -50.6(3) . . . . ? C91 Zr1 C8 C12 -42.6(5) . . . . ? C102 Zr1 C8 C12 -16.1(3) . . . . ? C96 Zr1 C8 C12 -74.0(3) . . . . ? Cl1 Zr1 C8 C9 108.5(2) . . . . ? Cl2 Zr1 C8 C9 16.3(3) . . . . ? C12 Zr1 C8 C9 -113.3(4) . . . . ? C90 Zr1 C8 C9 -106.1(3) . . . . ? C11 Zr1 C8 C9 -75.2(3) . . . . ? C10 Zr1 C8 C9 -35.1(2) . . . . ? C97 Zr1 C8 C9 -163.9(2) . . . . ? C91 Zr1 C8 C9 -155.9(4) . . . . ? C102 Zr1 C8 C9 -129.5(2) . . . . ? C96 Zr1 C8 C9 172.7(2) . . . . ? Cl1 Zr1 C8 Si9 -15.9(3) . . . . ? Cl2 Zr1 C8 Si9 -108.2(2) . . . . ? C12 Zr1 C8 Si9 122.2(4) . . . . ? C90 Zr1 C8 Si9 129.5(3) . . . . ? C11 Zr1 C8 Si9 160.4(3) . . . . ? C9 Zr1 C8 Si9 -124.4(4) . . . . ? C10 Zr1 C8 Si9 -159.5(4) . . . . ? C97 Zr1 C8 Si9 71.7(3) . . . . ? C91 Zr1 C8 Si9 79.7(5) . . . . ? C102 Zr1 C8 Si9 106.1(3) . . . . ? C96 Zr1 C8 Si9 48.3(4) . . . . ? C12 C8 C9 C10 2.4(5) . . . . ? Si9 C8 C9 C10 -165.6(3) . . . . ? Zr1 C8 C9 C10 66.0(3) . . . . ? C12 C8 C9 Zr1 -63.6(3) . . . . ? Si9 C8 C9 Zr1 128.3(3) . . . . ? Cl1 Zr1 C9 C10 171.8(2) . . . . ? Cl2 Zr1 C9 C10 75.9(2) . . . . ? C12 Zr1 C9 C10 -80.2(3) . . . . ? C90 Zr1 C9 C10 -8.4(3) . . . . ? C11 Zr1 C9 C10 -37.9(2) . . . . ? C8 Zr1 C9 C10 -118.4(4) . . . . ? C97 Zr1 C9 C10 -94.8(3) . . . . ? C91 Zr1 C9 C10 34.1(6) . . . . ? C102 Zr1 C9 C10 -51.7(3) . . . . ? C96 Zr1 C9 C10 -139.3(5) . . . . ? Cl1 Zr1 C9 C8 -69.8(2) . . . . ? Cl2 Zr1 C9 C8 -165.7(2) . . . . ? C12 Zr1 C9 C8 38.2(2) . . . . ? C90 Zr1 C9 C8 110.0(3) . . . . ? C11 Zr1 C9 C8 80.5(3) . . . . ? C10 Zr1 C9 C8 118.4(4) . . . . ? C97 Zr1 C9 C8 23.6(3) . . . . ? C91 Zr1 C9 C8 152.5(4) . . . . ? C102 Zr1 C9 C8 66.7(3) . . . . ? C96 Zr1 C9 C8 -20.9(7) . . . . ? C8 C9 C10 C11 -1.7(5) . . . . ? Zr1 C9 C10 C11 63.8(3) . . . . ? C8 C9 C10 Si10 163.2(3) . . . . ? Zr1 C9 C10 Si10 -131.2(3) . . . . ? C8 C9 C10 Zr1 -65.6(3) . . . . ? C5 Si10 C10 C9 23.5(4) . . . . ? C7 Si10 C10 C9 148.4(4) . . . . ? C6 Si10 C10 C9 -95.0(4) . . . . ? C5 Si10 C10 C11 -174.7(4) . . . . ? C7 Si10 C10 C11 -49.9(4) . . . . ? C6 Si10 C10 C11 66.8(4) . . . . ? C5 Si10 C10 Zr1 -76.7(3) . . . . ? C7 Si10 C10 Zr1 48.2(4) . . . . ? C6 Si10 C10 Zr1 164.8(3) . . . . ? Cl1 Zr1 C10 C9 -9.9(3) . . . . ? Cl2 Zr1 C10 C9 -100.4(2) . . . . ? C12 Zr1 C10 C9 75.7(3) . . . . ? C90 Zr1 C10 C9 174.0(2) . . . . ? C11 Zr1 C10 C9 113.7(4) . . . . ? C8 Zr1 C10 C9 35.3(2) . . . . ? C97 Zr1 C10 C9 118.3(3) . . . . ? C91 Zr1 C10 C9 -167.2(2) . . . . ? C102 Zr1 C10 C9 140.3(2) . . . . ? C96 Zr1 C10 C9 154.1(3) . . . . ? Cl1 Zr1 C10 C11 -123.6(2) . . . . ? Cl2 Zr1 C10 C11 145.9(2) . . . . ? C12 Zr1 C10 C11 -38.1(2) . . . . ? C90 Zr1 C10 C11 60.3(2) . . . . ? C9 Zr1 C10 C11 -113.7(4) . . . . ? C8 Zr1 C10 C11 -78.5(3) . . . . ? C97 Zr1 C10 C11 4.6(3) . . . . ? C91 Zr1 C10 C11 79.1(3) . . . . ? C102 Zr1 C10 C11 26.6(2) . . . . ? C96 Zr1 C10 C11 40.3(5) . . . . ? Cl1 Zr1 C10 Si10 113.2(2) . . . . ? Cl2 Zr1 C10 Si10 22.8(3) . . . . ? C12 Zr1 C10 Si10 -161.2(4) . . . . ? C90 Zr1 C10 Si10 -62.9(3) . . . . ? C11 Zr1 C10 Si10 -123.1(4) . . . . ? C9 Zr1 C10 Si10 123.1(4) . . . . ? C8 Zr1 C10 Si10 158.4(4) . . . . ? C97 Zr1 C10 Si10 -118.6(3) . . . . ? C91 Zr1 C10 Si10 -44.1(4) . . . . ? C102 Zr1 C10 Si10 -96.5(3) . . . . ? C96 Zr1 C10 Si10 -82.8(5) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? Si10 C10 C11 C12 -164.3(3) . . . . ? Zr1 C10 C11 C12 65.7(3) . . . . ? C9 C10 C11 Zr1 -65.4(3) . . . . ? Si10 C10 C11 Zr1 130.0(3) . . . . ? Cl1 Zr1 C11 C10 82.9(2) . . . . ? Cl2 Zr1 C11 C10 -35.2(2) . . . . ? C12 Zr1 C11 C10 114.7(3) . . . . ? C90 Zr1 C11 C10 -122.7(2) . . . . ? C9 Zr1 C11 C10 37.5(2) . . . . ? C8 Zr1 C11 C10 77.7(2) . . . . ? C97 Zr1 C11 C10 -176.5(2) . . . . ? C91 Zr1 C11 C10 -124.1(2) . . . . ? C102 Zr1 C11 C10 -153.6(2) . . . . ? C96 Zr1 C11 C10 -161.4(2) . . . . ? Cl1 Zr1 C11 C12 -31.9(3) . . . . ? Cl2 Zr1 C11 C12 -150.0(2) . . . . ? C90 Zr1 C11 C12 122.6(2) . . . . ? C9 Zr1 C11 C12 -77.3(3) . . . . ? C8 Zr1 C11 C12 -37.1(2) . . . . ? C10 Zr1 C11 C12 -114.7(3) . . . . ? C97 Zr1 C11 C12 68.7(3) . . . . ? C91 Zr1 C11 C12 121.2(2) . . . . ? C102 Zr1 C11 C12 91.6(2) . . . . ? C96 Zr1 C11 C12 83.9(3) . . . . ? C9 C8 C12 C11 -2.1(4) . . . . ? Si9 C8 C12 C11 165.9(3) . . . . ? Zr1 C8 C12 C11 -68.1(3) . . . . ? C9 C8 C12 Zr1 65.9(3) . . . . ? Si9 C8 C12 Zr1 -126.1(3) . . . . ? C10 C11 C12 C8 1.1(5) . . . . ? Zr1 C11 C12 C8 69.9(3) . . . . ? C10 C11 C12 Zr1 -68.8(3) . . . . ? Cl1 Zr1 C12 C8 43.2(2) . . . . ? Cl2 Zr1 C12 C8 -72.2(3) . . . . ? C90 Zr1 C12 C8 -175.0(2) . . . . ? C11 Zr1 C12 C8 -114.4(3) . . . . ? C9 Zr1 C12 C8 -37.7(2) . . . . ? C10 Zr1 C12 C8 -77.7(2) . . . . ? C97 Zr1 C12 C8 132.7(2) . . . . ? C91 Zr1 C12 C8 162.9(2) . . . . ? C102 Zr1 C12 C8 164.7(2) . . . . ? C96 Zr1 C12 C8 127.7(2) . . . . ? Cl1 Zr1 C12 C11 157.6(2) . . . . ? Cl2 Zr1 C12 C11 42.2(3) . . . . ? C90 Zr1 C12 C11 -60.6(3) . . . . ? C9 Zr1 C12 C11 76.6(2) . . . . ? C8 Zr1 C12 C11 114.4(3) . . . . ? C10 Zr1 C12 C11 36.7(2) . . . . ? C97 Zr1 C12 C11 -112.9(2) . . . . ? C91 Zr1 C12 C11 -82.8(3) . . . . ? C102 Zr1 C12 C11 -81.0(2) . . . . ? C96 Zr1 C12 C11 -117.9(2) . . . . ? O11 Si2 C21 C25 67.8(4) . . . . ? O2 Si2 C21 C25 -52.4(4) . . . . ? O1 Si2 C21 C25 -170.8(3) . . . . ? O11 Si2 C21 C22 -51.2(4) . . . . ? O2 Si2 C21 C22 -171.4(4) . . . . ? O1 Si2 C21 C22 70.2(4) . . . . ? C25 C21 C22 C23 30.1(6) . . . . ? Si2 C21 C22 C23 155.1(4) . . . . ? C21 C22 C23 C24 -13.3(7) . . . . ? C22 C23 C24 C25 -9.5(8) . . . . ? C23 C24 C25 C21 28.7(8) . . . . ? C22 C21 C25 C24 -35.9(6) . . . . ? Si2 C21 C25 C24 -163.2(4) . . . . ? O12 Si3 C31 C35 -47.8(4) . . . . ? O3 Si3 C31 C35 -168.1(3) . . . . ? O2 Si3 C31 C35 72.0(4) . . . . ? O12 Si3 C31 C32 70.4(4) . . . . ? O3 Si3 C31 C32 -49.9(4) . . . . ? O2 Si3 C31 C32 -169.9(3) . . . . ? C35 C31 C32 C33 -30.3(6) . . . . ? Si3 C31 C32 C33 -155.8(4) . . . . ? C31 C32 C33 C34 15.3(7) . . . . ? C32 C33 C34 C35 6.3(8) . . . . ? C33 C34 C35 C31 -25.3(7) . . . . ? C32 C31 C35 C34 33.5(5) . . . . ? Si3 C31 C35 C34 157.8(4) . . . . ? O3 Si4 C41 C42 169.1(3) . . . . ? O9 Si4 C41 C42 48.7(3) . . . . ? O4 Si4 C41 C42 -71.2(3) . . . . ? O3 Si4 C41 C45 49.6(3) . . . . ? O9 Si4 C41 C45 -70.8(3) . . . . ? O4 Si4 C41 C45 169.3(3) . . . . ? C45 C41 C42 C43 -39.2(4) . . . . ? Si4 C41 C42 C43 -164.2(3) . . . . ? C41 C42 C43 C44 39.4(5) . . . . ? C42 C43 C44 C45 -24.0(6) . . . . ? C43 C44 C45 C41 -0.3(6) . . . . ? C42 C41 C45 C44 24.3(5) . . . . ? Si4 C41 C45 C44 151.9(4) . . . . ? O8 Si5 C51 C52 172.1(4) . . . . ? O9 Si5 C51 C52 -67.5(4) . . . . ? O5 Si5 C51 C52 51.6(4) . . . . ? O8 Si5 C51 C55 -67.5(5) . . . . ? O9 Si5 C51 C55 52.9(5) . . . . ? O5 Si5 C51 C55 172.0(4) . . . . ? C55 C51 C52 C53 20.6(6) . . . . ? Si5 C51 C52 C53 147.9(5) . . . . ? C51 C52 C53 C54 -5.3(8) . . . . ? C52 C53 C54 C55 -12.5(8) . . . . ? C53 C54 C55 C51 25.5(7) . . . . ? C52 C51 C55 C54 -28.1(6) . . . . ? Si5 C51 C55 C54 -153.6(4) . . . . ? O5 Si6 C61 C62 -47.3(4) . . . . ? O10 Si6 C61 C62 72.4(4) . . . . ? O6 Si6 C61 C62 -167.9(3) . . . . ? O5 Si6 C61 C65 -167.0(3) . . . . ? O10 Si6 C61 C65 -47.4(4) . . . . ? O6 Si6 C61 C65 72.3(4) . . . . ? C65 C61 C62 C63 -31.5(6) . . . . ? Si6 C61 C62 C63 -157.7(5) . . . . ? C61 C62 C63 C64 15.9(8) . . . . ? C62 C63 C64 C65 6.1(8) . . . . ? C62 C61 C65 C64 35.2(5) . . . . ? Si6 C61 C65 C64 160.8(3) . . . . ? C63 C64 C65 C61 -25.7(6) . . . . ? O11 Si7 C71 C72 -67.4(9) . . . . ? O7 Si7 C71 C72 53.6(9) . . . . ? O6 Si7 C71 C72 173.7(8) . . . . ? O11 Si7 C71 C75 61.2(7) . . . . ? O7 Si7 C71 C75 -177.7(6) . . . . ? O6 Si7 C71 C75 -57.6(7) . . . . ? C75 C71 C72 C73 38.4(11) . . . . ? Si7 C71 C72 C73 171.4(7) . . . . ? C71 C72 C73 C74 -17.9(13) . . . . ? C72 C73 C74 C75 -11.1(11) . . . . ? C73 C74 C75 C71 32.4(10) . . . . ? C72 C71 C75 C74 -47.6(10) . . . . ? Si7 C71 C75 C74 175.1(6) . . . . ? O12 Si8 C81 C82 56.8(8) . . . . ? O7 Si8 C81 C82 -63.1(8) . . . . ? O8 Si8 C81 C82 176.4(7) . . . . ? O12 Si8 C81 C85 -73.5(6) . . . . ? O7 Si8 C81 C85 166.6(5) . . . . ? O8 Si8 C81 C85 46.1(6) . . . . ? C85 C81 C82 C83 -23.8(11) . . . . ? Si8 C81 C82 C83 -154.0(7) . . . . ? C81 C82 C83 C84 11.5(13) . . . . ? C82 C83 C84 C85 7.8(12) . . . . ? C83 C84 C85 C81 -18.8(10) . . . . ? C82 C81 C85 C84 27.4(10) . . . . ? Si8 C81 C85 C84 165.8(6) . . . . ? Si1 C1 C90 C102 -84.9(4) . . . . ? Si1 C1 C90 C91 78.7(5) . . . . ? Si1 C1 C90 Zr1 176.79(19) . . . . ? Cl1 Zr1 C90 C102 88.2(3) . . . . ? Cl2 Zr1 C90 C102 -175.3(2) . . . . ? C12 Zr1 C90 C102 -39.5(3) . . . . ? C11 Zr1 C90 C102 -68.3(2) . . . . ? C9 Zr1 C90 C102 -91.5(3) . . . . ? C8 Zr1 C90 C102 -43.5(3) . . . . ? C10 Zr1 C90 C102 -96.1(2) . . . . ? C97 Zr1 C90 C102 35.1(2) . . . . ? C91 Zr1 C90 C102 109.4(3) . . . . ? C96 Zr1 C90 C102 74.5(3) . . . . ? Cl1 Zr1 C90 C91 -21.2(3) . . . . ? Cl2 Zr1 C90 C91 75.3(2) . . . . ? C12 Zr1 C90 C91 -148.9(2) . . . . ? C11 Zr1 C90 C91 -177.7(2) . . . . ? C9 Zr1 C90 C91 159.1(2) . . . . ? C8 Zr1 C90 C91 -152.9(2) . . . . ? C10 Zr1 C90 C91 154.5(2) . . . . ? C97 Zr1 C90 C91 -74.3(3) . . . . ? C102 Zr1 C90 C91 -109.4(3) . . . . ? C96 Zr1 C90 C91 -34.9(2) . . . . ? Cl1 Zr1 C90 C1 -146.8(3) . . . . ? Cl2 Zr1 C90 C1 -50.3(3) . . . . ? C12 Zr1 C90 C1 85.6(3) . . . . ? C11 Zr1 C90 C1 56.7(3) . . . . ? C9 Zr1 C90 C1 33.5(4) . . . . ? C8 Zr1 C90 C1 81.5(4) . . . . ? C10 Zr1 C90 C1 28.9(3) . . . . ? C97 Zr1 C90 C1 160.2(4) . . . . ? C91 Zr1 C90 C1 -125.6(4) . . . . ? C102 Zr1 C90 C1 125.1(4) . . . . ? C96 Zr1 C90 C1 -160.4(4) . . . . ? C102 C90 C91 C92 171.3(4) . . . . ? C1 C90 C91 C92 5.1(7) . . . . ? Zr1 C90 C91 C92 -114.3(4) . . . . ? C102 C90 C91 C96 -8.9(4) . . . . ? C1 C90 C91 C96 -175.1(4) . . . . ? Zr1 C90 C91 C96 65.5(3) . . . . ? C102 C90 C91 Zr1 -74.4(3) . . . . ? C1 C90 C91 Zr1 119.5(4) . . . . ? Cl1 Zr1 C91 C92 -69.2(3) . . . . ? Cl2 Zr1 C91 C92 25.3(3) . . . . ? C12 Zr1 C91 C92 168.9(3) . . . . ? C90 Zr1 C91 C92 126.9(4) . . . . ? C11 Zr1 C91 C92 129.5(3) . . . . ? C9 Zr1 C91 C92 67.8(6) . . . . ? C8 Zr1 C91 C92 -161.7(4) . . . . ? C10 Zr1 C91 C92 91.9(4) . . . . ? C97 Zr1 C91 C92 -152.2(4) . . . . ? C102 Zr1 C91 C92 166.7(4) . . . . ? C96 Zr1 C91 C92 -115.5(5) . . . . ? Cl1 Zr1 C91 C96 46.3(3) . . . . ? Cl2 Zr1 C91 C96 140.8(3) . . . . ? C12 Zr1 C91 C96 -75.6(3) . . . . ? C90 Zr1 C91 C96 -117.6(4) . . . . ? C11 Zr1 C91 C96 -115.0(3) . . . . ? C9 Zr1 C91 C96 -176.7(4) . . . . ? C8 Zr1 C91 C96 -46.2(5) . . . . ? C10 Zr1 C91 C96 -152.6(3) . . . . ? C97 Zr1 C91 C96 -36.7(2) . . . . ? C102 Zr1 C91 C96 -77.8(3) . . . . ? Cl1 Zr1 C91 C90 164.0(2) . . . . ? Cl2 Zr1 C91 C90 -101.5(2) . . . . ? C12 Zr1 C91 C90 42.1(3) . . . . ? C11 Zr1 C91 C90 2.6(3) . . . . ? C9 Zr1 C91 C90 -59.1(6) . . . . ? C8 Zr1 C91 C90 71.4(5) . . . . ? C10 Zr1 C91 C90 -34.9(3) . . . . ? C97 Zr1 C91 C90 81.0(3) . . . . ? C102 Zr1 C91 C90 39.8(2) . . . . ? C96 Zr1 C91 C90 117.6(4) . . . . ? C96 C91 C92 C93 2.6(6) . . . . ? C90 C91 C92 C93 -177.6(4) . . . . ? Zr1 C91 C92 C93 93.3(4) . . . . ? C91 C92 C93 C94 -1.6(6) . . . . ? C92 C93 C94 C95 -0.6(7) . . . . ? C93 C94 C95 C96 1.6(7) . . . . ? C94 C95 C96 C91 -0.6(6) . . . . ? C94 C95 C96 C97 173.6(4) . . . . ? C94 C95 C96 Zr1 -89.6(5) . . . . ? C92 C91 C96 C95 -1.5(6) . . . . ? C90 C91 C96 C95 178.6(4) . . . . ? Zr1 C91 C96 C95 -120.2(4) . . . . ? C92 C91 C96 C97 -176.9(4) . . . . ? C90 C91 C96 C97 3.2(4) . . . . ? Zr1 C91 C96 C97 64.4(3) . . . . ? C92 C91 C96 Zr1 118.7(4) . . . . ? C90 C91 C96 Zr1 -61.1(3) . . . . ? Cl1 Zr1 C96 C95 -17.8(4) . . . . ? Cl2 Zr1 C96 C95 75.2(4) . . . . ? C12 Zr1 C96 C95 -119.4(4) . . . . ? C90 Zr1 C96 C95 151.8(5) . . . . ? C11 Zr1 C96 C95 -158.0(4) . . . . ? C9 Zr1 C96 C95 -68.2(7) . . . . ? C8 Zr1 C96 C95 -83.4(5) . . . . ? C10 Zr1 C96 C95 175.8(4) . . . . ? C97 Zr1 C96 C95 -128.9(5) . . . . ? C91 Zr1 C96 C95 115.4(5) . . . . ? C102 Zr1 C96 C95 -167.5(5) . . . . ? Cl1 Zr1 C96 C91 -133.2(3) . . . . ? Cl2 Zr1 C96 C91 -40.2(3) . . . . ? C12 Zr1 C96 C91 125.2(3) . . . . ? C90 Zr1 C96 C91 36.3(2) . . . . ? C11 Zr1 C96 C91 86.6(3) . . . . ? C9 Zr1 C96 C91 176.4(5) . . . . ? C8 Zr1 C96 C91 161.2(2) . . . . ? C10 Zr1 C96 C91 60.3(5) . . . . ? C97 Zr1 C96 C91 115.7(4) . . . . ? C102 Zr1 C96 C91 77.1(3) . . . . ? Cl1 Zr1 C96 C97 111.1(2) . . . . ? Cl2 Zr1 C96 C97 -155.9(2) . . . . ? C12 Zr1 C96 C97 9.5(3) . . . . ? C90 Zr1 C96 C97 -79.3(3) . . . . ? C11 Zr1 C96 C97 -29.1(3) . . . . ? C9 Zr1 C96 C97 60.7(6) . . . . ? C8 Zr1 C96 C97 45.5(3) . . . . ? C10 Zr1 C96 C97 -55.4(5) . . . . ? C91 Zr1 C96 C97 -115.7(4) . . . . ? C102 Zr1 C96 C97 -38.6(2) . . . . ? C95 C96 C97 C98 -1.0(8) . . . . ? C91 C96 C97 C98 173.7(4) . . . . ? Zr1 C96 C97 C98 -121.8(5) . . . . ? C95 C96 C97 C102 -171.1(4) . . . . ? C91 C96 C97 C102 3.6(4) . . . . ? Zr1 C96 C97 C102 68.1(3) . . . . ? C95 C96 C97 Zr1 120.8(5) . . . . ? C91 C96 C97 Zr1 -64.5(3) . . . . ? Cl1 Zr1 C97 C98 65.8(4) . . . . ? Cl2 Zr1 C97 C98 164.5(4) . . . . ? C12 Zr1 C97 C98 -40.0(4) . . . . ? C90 Zr1 C97 C98 -151.1(5) . . . . ? C11 Zr1 C97 C98 -71.1(4) . . . . ? C9 Zr1 C97 C98 -28.3(5) . . . . ? C8 Zr1 C97 C98 -15.3(4) . . . . ? C10 Zr1 C97 C98 -73.6(4) . . . . ? C91 Zr1 C97 C98 167.9(5) . . . . ? C102 Zr1 C97 C98 -115.9(5) . . . . ? C96 Zr1 C97 C98 131.6(5) . . . . ? Cl1 Zr1 C97 C96 -65.8(2) . . . . ? Cl2 Zr1 C97 C96 32.9(3) . . . . ? C12 Zr1 C97 C96 -171.6(2) . . . . ? C90 Zr1 C97 C96 77.3(3) . . . . ? C11 Zr1 C97 C96 157.3(2) . . . . ? C9 Zr1 C97 C96 -160.0(2) . . . . ? C8 Zr1 C97 C96 -146.9(2) . . . . ? C10 Zr1 C97 C96 154.8(2) . . . . ? C91 Zr1 C97 C96 36.3(2) . . . . ? C102 Zr1 C97 C96 112.5(4) . . . . ? Cl1 Zr1 C97 C102 -178.3(2) . . . . ? Cl2 Zr1 C97 C102 -79.6(3) . . . . ? C12 Zr1 C97 C102 75.9(3) . . . . ? C90 Zr1 C97 C102 -35.2(2) . . . . ? C11 Zr1 C97 C102 44.8(3) . . . . ? C9 Zr1 C97 C102 87.6(3) . . . . ? C8 Zr1 C97 C102 100.6(3) . . . . ? C10 Zr1 C97 C102 42.3(3) . . . . ? C91 Zr1 C97 C102 -76.2(3) . . . . ? C96 Zr1 C97 C102 -112.5(4) . . . . ? C96 C97 C98 C99 -166.0(5) . . . . ? C102 C97 C98 C99 3.0(7) . . . . ? Zr1 C97 C98 C99 92.9(5) . . . . ? C97 C98 C99 C100 -0.7(7) . . . . ? C98 C99 C100 C101 -2.0(8) . . . . ? C99 C100 C101 C102 2.2(7) . . . . ? C100 C101 C102 C90 177.7(4) . . . . ? C100 C101 C102 C97 0.1(6) . . . . ? C100 C101 C102 Zr1 -89.2(4) . . . . ? C91 C90 C102 C101 -166.6(4) . . . . ? C1 C90 C102 C101 -0.3(7) . . . . ? Zr1 C90 C102 C101 119.4(5) . . . . ? C91 C90 C102 C97 11.1(4) . . . . ? C1 C90 C102 C97 177.4(4) . . . . ? Zr1 C90 C102 C97 -62.9(3) . . . . ? C91 C90 C102 Zr1 74.0(3) . . . . ? C1 C90 C102 Zr1 -119.7(4) . . . . ? C98 C97 C102 C101 -2.7(6) . . . . ? C96 C97 C102 C101 168.8(4) . . . . ? Zr1 C97 C102 C101 -121.9(4) . . . . ? C98 C97 C102 C90 179.2(4) . . . . ? C96 C97 C102 C90 -9.3(4) . . . . ? Zr1 C97 C102 C90 59.9(3) . . . . ? C98 C97 C102 Zr1 119.2(4) . . . . ? C96 C97 C102 Zr1 -69.2(3) . . . . ? Cl1 Zr1 C102 C101 115.4(3) . . . . ? Cl2 Zr1 C102 C101 -122.6(3) . . . . ? C12 Zr1 C102 C101 13.3(3) . . . . ? C90 Zr1 C102 C101 -128.0(5) . . . . ? C11 Zr1 C102 C101 -20.9(3) . . . . ? C9 Zr1 C102 C101 -9.6(4) . . . . ? C8 Zr1 C102 C101 22.1(4) . . . . ? C10 Zr1 C102 C101 -35.2(4) . . . . ? C97 Zr1 C102 C101 113.4(5) . . . . ? C91 Zr1 C102 C101 -168.4(4) . . . . ? C96 Zr1 C102 C101 151.4(4) . . . . ? Cl1 Zr1 C102 C90 -116.5(2) . . . . ? Cl2 Zr1 C102 C90 5.4(3) . . . . ? C12 Zr1 C102 C90 141.3(3) . . . . ? C11 Zr1 C102 C90 107.1(2) . . . . ? C9 Zr1 C102 C90 118.4(2) . . . . ? C8 Zr1 C102 C90 150.1(2) . . . . ? C10 Zr1 C102 C90 92.8(2) . . . . ? C97 Zr1 C102 C90 -118.6(4) . . . . ? C91 Zr1 C102 C90 -40.4(2) . . . . ? C96 Zr1 C102 C90 -80.6(3) . . . . ? Cl1 Zr1 C102 C97 2.0(3) . . . . ? Cl2 Zr1 C102 C97 124.0(2) . . . . ? C12 Zr1 C102 C97 -100.1(3) . . . . ? C90 Zr1 C102 C97 118.6(4) . . . . ? C11 Zr1 C102 C97 -134.3(3) . . . . ? C9 Zr1 C102 C97 -123.0(3) . . . . ? C8 Zr1 C102 C97 -91.3(3) . . . . ? C10 Zr1 C102 C97 -148.6(3) . . . . ? C91 Zr1 C102 C97 78.2(3) . . . . ? C96 Zr1 C102 C97 38.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.836 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.076 data_5b _database_code_CSD 201606 # # NOTE: faint disordered hexane density modelled with dummy carbon atoms. # _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H82 O12 Si8 Sn, 0.25(C6 H14)' _chemical_formula_sum 'C53.5 H85.5 O12 Si8 Sn' _chemical_formula_weight 1264.15 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P c' _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 10.9320(3) _cell_length_b 17.9730(4) _cell_length_c 32.0160(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.0678(8) _cell_angle_gamma 90.00 _cell_volume 6274.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2658 _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type multi-scan _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Kappa-CCD _diffrn_reflns_number 55788 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.0 _reflns_number_total 21590 _reflns_number_gt 18097 _reflns_threshold_expression I>2\s(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0715P)^2^+27.5450P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(2) _refine_ls_number_reflns 21590 _refine_ls_number_parameters 1349 _refine_ls_number_restraints 260 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1738 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.084 _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 Sn11 Sn 1.14955(5) 0.53313(3) 0.631593(19) 0.02859(14) Uani 1 1 d D . . Si11 Si 1.03390(18) 0.49863(14) 0.48306(7) 0.0231(5) Uani 1 1 d D . . Si12 Si 1.09867(18) 0.62179(13) 0.41957(7) 0.0238(5) Uani 1 1 d D . . Si13 Si 0.82551(18) 0.62490(13) 0.38288(7) 0.0242(5) Uani 1 1 d D . . Si14 Si 0.76118(17) 0.50262(13) 0.44687(7) 0.0227(5) Uani 1 1 d D . . Si15 Si 0.81830(18) 0.38051(13) 0.38214(7) 0.0230(5) Uani 1 1 d D . . Si16 Si 1.08901(18) 0.37450(13) 0.41919(7) 0.0244(5) Uani 1 1 d D . . Si17 Si 1.15970(18) 0.49837(14) 0.35612(7) 0.0251(5) Uani 1 1 d D . . Si18 Si 0.88949(19) 0.50396(13) 0.31856(7) 0.0223(5) Uani 1 1 d D . . O11 O 1.0895(5) 0.5708(3) 0.46118(16) 0.0295(13) Uani 1 1 d D . . O12 O 0.9614(4) 0.6450(3) 0.40185(19) 0.0350(14) Uani 1 1 d D . . O13 O 0.7603(5) 0.5747(3) 0.41708(18) 0.0334(14) Uani 1 1 d D . . O14 O 0.8859(4) 0.5014(3) 0.47734(17) 0.0288(14) Uani 1 1 d D . . O15 O 0.9520(4) 0.3521(3) 0.40119(18) 0.0326(14) Uani 1 1 d D . . O16 O 1.1534(5) 0.4253(4) 0.38516(17) 0.0312(15) Uani 1 1 d D . . O17 O 1.0379(4) 0.5009(3) 0.32443(18) 0.0330(15) Uani 1 1 d D . . O18 O 0.8360(5) 0.4315(3) 0.34108(17) 0.0349(14) Uani 1 1 d D . . O19 O 0.7569(5) 0.4286(3) 0.41748(17) 0.0284(13) Uani 1 1 d D . . O20 O 1.0812(5) 0.4235(3) 0.46130(17) 0.0304(13) Uani 1 1 d D . . O21 O 1.1630(5) 0.5734(4) 0.38505(18) 0.0341(15) Uani 1 1 d D . . O22 O 0.8372(5) 0.5770(3) 0.34063(17) 0.0340(14) Uani 1 1 d D . . C1 C 1.0910(7) 0.4925(4) 0.5388(2) 0.0233(17) Uani 1 1 d D . . H1A H 1.0590 0.4458 0.5503 0.028 Uiso 1 1 calc R . . H1B H 1.1814 0.4878 0.5398 0.028 Uiso 1 1 calc R . . C2 C 1.3405(9) 0.5243(6) 0.6246(3) 0.048(3) Uani 1 1 d D . . H2A H 1.3834 0.5133 0.6518 0.072 Uiso 1 1 calc R . . H2B H 1.3710 0.5714 0.6139 0.072 Uiso 1 1 calc R . . H2C H 1.3555 0.4842 0.6049 0.072 Uiso 1 1 calc R . . C3 C 1.1160(10) 0.6286(5) 0.6692(3) 0.054(3) Uani 1 1 d D . . H3A H 1.0318 0.6460 0.6627 0.081 Uiso 1 1 calc R . . H3B H 1.1737 0.6682 0.6632 0.081 Uiso 1 1 calc R . . H3C H 1.1270 0.6151 0.6989 0.081 Uiso 1 1 calc R . . C4 C 1.0930(12) 0.4328(7) 0.6512(4) 0.077(4) Uiso 1 1 d D . . H4A H 1.1261 0.3936 0.6339 0.116 Uiso 1 1 calc R . . H4B H 1.0032 0.4308 0.6486 0.116 Uiso 1 1 calc R . . H4C H 1.1224 0.4253 0.6805 0.116 Uiso 1 1 calc R . . C21 C 1.1843(7) 0.7092(4) 0.4295(2) 0.0251(17) Uani 1 1 d D . . H21 H 1.1527 0.7332 0.4548 0.030 Uiso 1 1 calc R . . C22 C 1.1646(8) 0.7652(5) 0.3918(3) 0.040(2) Uani 1 1 d D . . H22A H 1.1547 0.7381 0.3649 0.048 Uiso 1 1 calc R . . H22B H 1.0912 0.7964 0.3949 0.048 Uiso 1 1 calc R . . C23 C 1.2817(9) 0.8132(6) 0.3941(3) 0.056(3) Uani 1 1 d D . . H23A H 1.3222 0.8099 0.3675 0.067 Uiso 1 1 calc R . . H23B H 1.2612 0.8660 0.3991 0.067 Uiso 1 1 calc R . . C24 C 1.3642(9) 0.7837(6) 0.4294(3) 0.051(3) Uani 1 1 d D . . H24A H 1.3560 0.8137 0.4550 0.062 Uiso 1 1 calc R . . H24B H 1.4508 0.7854 0.4223 0.062 Uiso 1 1 calc R . . C25 C 1.3251(6) 0.7048(5) 0.4362(3) 0.032(2) Uani 1 1 d D . . H25A H 1.3509 0.6877 0.4649 0.038 Uiso 1 1 calc R . . H25B H 1.3595 0.6708 0.4157 0.038 Uiso 1 1 calc R . . C31 C 0.7322(6) 0.7080(4) 0.3690(2) 0.0240(17) Uani 1 1 d D . . H31 H 0.7252 0.7392 0.3945 0.029 Uiso 1 1 calc R . . C32 C 0.7865(7) 0.7561(5) 0.3342(3) 0.037(2) Uani 1 1 d D . . H32A H 0.8096 0.8061 0.3449 0.044 Uiso 1 1 calc R . . H32B H 0.8599 0.7319 0.3238 0.044 Uiso 1 1 calc R . . C33 C 0.6851(10) 0.7612(10) 0.2999(4) 0.095(6) Uani 1 1 d D . . H33A H 0.6791 0.8127 0.2890 0.114 Uiso 1 1 calc R . . H33B H 0.7027 0.7277 0.2765 0.114 Uiso 1 1 calc R . . C34 C 0.5702(10) 0.7398(8) 0.3170(4) 0.085(5) Uani 1 1 d D . . H34A H 0.5142 0.7169 0.2950 0.102 Uiso 1 1 calc R . . H34B H 0.5293 0.7838 0.3282 0.102 Uiso 1 1 calc R . . C35 C 0.6017(7) 0.6856(6) 0.3508(3) 0.055(3) Uani 1 1 d D . . H35A H 0.6017 0.6343 0.3395 0.066 Uiso 1 1 calc R . . H35B H 0.5422 0.6884 0.3726 0.066 Uiso 1 1 calc R . . C41 C 0.6231(7) 0.5075(5) 0.4772(3) 0.033(2) Uani 1 1 d D . . H41 H 0.6346 0.5487 0.4981 0.040 Uiso 1 1 calc R . . C42 C 0.5068(9) 0.5216(9) 0.4505(4) 0.072(4) Uani 1 1 d D . . H42A H 0.5045 0.4907 0.4249 0.086 Uiso 1 1 calc R . . H42B H 0.5011 0.5746 0.4423 0.086 Uiso 1 1 calc R . . C43 C 0.4024(9) 0.5009(7) 0.4768(4) 0.061(3) Uani 1 1 d D . . H43A H 0.3393 0.4719 0.4602 0.073 Uiso 1 1 calc R . . H43B H 0.3636 0.5461 0.4877 0.073 Uiso 1 1 calc R . . C44 C 0.4606(9) 0.4546(8) 0.5124(4) 0.067(4) Uani 1 1 d D . . H44A H 0.4638 0.4827 0.5390 0.081 Uiso 1 1 calc R . . H44B H 0.4138 0.4081 0.5158 0.081 Uiso 1 1 calc R . . C45 C 0.5880(9) 0.4378(6) 0.4999(3) 0.049(3) Uani 1 1 d D . . H45A H 0.5880 0.3939 0.4812 0.059 Uiso 1 1 calc R . . H45B H 0.6449 0.4285 0.5248 0.059 Uiso 1 1 calc R . . C51 C 0.7199(7) 0.3004(5) 0.3660(2) 0.0301(19) Uani 1 1 d D . . H51 H 0.7083 0.2688 0.3911 0.036 Uiso 1 1 calc R . . C52 C 0.7754(8) 0.2523(5) 0.3324(3) 0.039(2) Uani 1 1 d D . . H52A H 0.8358 0.2813 0.3175 0.047 Uiso 1 1 calc R . . H52B H 0.8169 0.2082 0.3453 0.047 Uiso 1 1 calc R . . C53 C 0.6711(10) 0.2293(8) 0.3030(4) 0.080(4) Uani 1 1 d D . . H53A H 0.6867 0.2447 0.2742 0.096 Uiso 1 1 calc R . . H53B H 0.6627 0.1744 0.3033 0.096 Uiso 1 1 calc R . . C54 C 0.5609(10) 0.2628(8) 0.3150(4) 0.081(4) Uani 1 1 d D . . H54A H 0.5092 0.2249 0.3277 0.098 Uiso 1 1 calc R . . H54B H 0.5143 0.2835 0.2900 0.098 Uiso 1 1 calc R . . C55 C 0.5915(7) 0.3236(6) 0.3460(3) 0.054(3) Uani 1 1 d D . . H55A H 0.5305 0.3261 0.3673 0.065 Uiso 1 1 calc R . . H55B H 0.5952 0.3725 0.3319 0.065 Uiso 1 1 calc R . . C61 C 1.1784(7) 0.2898(5) 0.4290(3) 0.034(2) Uani 1 1 d D . . H61 H 1.1370 0.2599 0.4503 0.041 Uiso 1 1 calc R . . C62 C 1.3125(10) 0.2985(7) 0.4446(4) 0.074(4) Uani 1 1 d D . . H62A H 1.3529 0.3377 0.4288 0.089 Uiso 1 1 calc R . . H62B H 1.3203 0.3112 0.4748 0.089 Uiso 1 1 calc R . . C63 C 1.3669(12) 0.2237(8) 0.4370(5) 0.087(5) Uani 1 1 d D . . H63A H 1.3665 0.1930 0.4626 0.104 Uiso 1 1 calc R . . H63B H 1.4530 0.2295 0.4297 0.104 Uiso 1 1 calc R . . C64 C 1.2927(11) 0.1860(6) 0.4015(4) 0.068(4) Uani 1 1 d D . . H64A H 1.3428 0.1776 0.3773 0.081 Uiso 1 1 calc R . . H64B H 1.2603 0.1376 0.4105 0.081 Uiso 1 1 calc R . . C65 C 1.1903(11) 0.2399(6) 0.3904(3) 0.056(3) Uani 1 1 d D . . H65A H 1.1127 0.2128 0.3835 0.068 Uiso 1 1 calc R . . H65B H 1.2094 0.2704 0.3660 0.068 Uiso 1 1 calc R . . C71 C 1.2951(7) 0.4903(5) 0.3258(2) 0.0308(19) Uani 1 1 d D . . H71 H 1.3684 0.4849 0.3461 0.037 Uiso 1 1 calc R . . C72 C 1.2924(9) 0.4236(6) 0.2966(3) 0.053(3) Uani 1 1 d D . . H72A H 1.3286 0.3795 0.3113 0.063 Uiso 1 1 calc R . . H72B H 1.2070 0.4117 0.2865 0.063 Uiso 1 1 calc R . . C73 C 1.3667(11) 0.4450(8) 0.2605(3) 0.068(4) Uani 1 1 d D . . H73A H 1.4550 0.4348 0.2670 0.081 Uiso 1 1 calc R . . H73B H 1.3385 0.4178 0.2347 0.081 Uiso 1 1 calc R . . C74 C 1.3437(18) 0.5243(8) 0.2560(4) 0.107(7) Uani 1 1 d D . . H74A H 1.2726 0.5327 0.2356 0.128 Uiso 1 1 calc R . . H74B H 1.4161 0.5489 0.2452 0.128 Uiso 1 1 calc R . . C75 C 1.3185(10) 0.5570(6) 0.2970(3) 0.055(3) Uani 1 1 d D . . H75A H 1.2457 0.5898 0.2941 0.066 Uiso 1 1 calc R . . H75B H 1.3896 0.5865 0.3085 0.066 Uiso 1 1 calc R . . C81 C 0.8413(7) 0.5030(5) 0.2625(2) 0.035(2) Uani 1 1 d D . . H81 H 0.8795 0.5471 0.2495 0.042 Uiso 1 1 calc R . . C82 C 0.8826(10) 0.4342(6) 0.2398(3) 0.054(3) Uani 1 1 d D . . H82A H 0.9670 0.4407 0.2312 0.065 Uiso 1 1 calc R . . H82B H 0.8806 0.3899 0.2582 0.065 Uiso 1 1 calc R . . C83 C 0.7943(12) 0.4256(8) 0.2026(4) 0.087(5) Uani 1 1 d D . . H83A H 0.8276 0.4487 0.1777 0.105 Uiso 1 1 calc R . . H83B H 0.7787 0.3723 0.1966 0.105 Uiso 1 1 calc R . . C84 C 0.6819(11) 0.4625(11) 0.2122(4) 0.102(6) Uani 1 1 d D . . H84A H 0.6173 0.4249 0.2158 0.123 Uiso 1 1 calc R . . H84B H 0.6537 0.4955 0.1887 0.123 Uiso 1 1 calc R . . C85 C 0.7020(8) 0.5075(7) 0.2517(3) 0.058(3) Uani 1 1 d D . . H85A H 0.6562 0.4860 0.2744 0.070 Uiso 1 1 calc R . . H85B H 0.6756 0.5597 0.2469 0.070 Uiso 1 1 calc R . . C90 C 1.0600(7) 0.5564(4) 0.5682(2) 0.032(2) Uani 1 1 d D . . C91 C 0.9284(8) 0.5708(6) 0.5772(3) 0.051(3) Uani 1 1 d D . . C92 C 0.8376(8) 0.5196(6) 0.5838(3) 0.047(3) Uani 1 1 d D . . H92 H 0.8530 0.4676 0.5830 0.056 Uiso 1 1 calc R . . C93 C 0.7178(11) 0.5483(10) 0.5920(4) 0.083(5) Uani 1 1 d D . . H93 H 0.6505 0.5159 0.5953 0.100 Uiso 1 1 calc R . . C94 C 0.7052(13) 0.6256(10) 0.5949(4) 0.087(5) Uani 1 1 d D . . H94 H 0.6277 0.6444 0.6016 0.104 Uiso 1 1 calc R . . C95 C 0.7948(12) 0.6759(10) 0.5889(4) 0.106(7) Uani 1 1 d D . . H95 H 0.7801 0.7277 0.5914 0.127 Uiso 1 1 calc R . . C96 C 0.9107(9) 0.6490(5) 0.5789(3) 0.049(3) Uani 1 1 d D . . C97 C 1.0190(11) 0.6893(7) 0.5684(4) 0.073(4) Uani 1 1 d D . . C98 C 1.0431(14) 0.7680(6) 0.5658(4) 0.077(4) Uani 1 1 d D . . H98 H 0.9843 0.8047 0.5718 0.092 Uiso 1 1 calc R . . C99 C 1.1553(16) 0.7856(10) 0.5541(5) 0.101(6) Uani 1 1 d D . . H99 H 1.1767 0.8368 0.5532 0.121 Uiso 1 1 calc R . . C100 C 1.2425(16) 0.7336(8) 0.5432(4) 0.100(6) Uani 1 1 d D . . H100 H 1.3175 0.7497 0.5329 0.120 Uiso 1 1 calc R . . C101 C 1.2184(11) 0.6572(6) 0.5474(3) 0.060(3) Uani 1 1 d D . . H101 H 1.2790 0.6213 0.5420 0.072 Uiso 1 1 calc R . . C102 C 1.1042(9) 0.6348(5) 0.5598(3) 0.043(2) Uani 1 1 d D . . Sn21 Sn 0.62986(4) 0.99752(3) -0.064270(18) 0.02677(14) Uani 1 1 d D . . Si21 Si 0.73156(17) 0.97489(12) 0.08529(6) 0.0154(4) Uani 1 1 d D . . Si22 Si 0.67603(17) 1.09981(11) 0.14785(6) 0.0150(4) Uani 1 1 d D . . Si23 Si 0.94459(17) 1.09313(11) 0.18583(6) 0.0172(4) Uani 1 1 d D . . Si24 Si 1.00164(18) 0.96983(12) 0.12273(7) 0.0195(5) Uani 1 1 d D . . Si25 Si 0.92850(19) 0.84828(12) 0.18669(7) 0.0230(5) Uani 1 1 d D . . Si26 Si 0.65836(19) 0.85395(11) 0.14958(7) 0.0178(4) Uani 1 1 d D . . Si27 Si 0.60083(17) 0.97868(11) 0.21204(7) 0.0142(4) Uani 1 1 d D . . Si28 Si 0.86859(18) 0.97172(12) 0.24973(7) 0.0189(4) Uani 1 1 d D . . O211 O 0.6780(4) 1.0485(3) 0.10579(16) 0.0212(11) Uani 1 1 d D . . O212 O 0.8148(4) 1.1216(3) 0.16368(18) 0.0262(12) Uani 1 1 d D . . O213 O 1.0115(5) 1.0418(3) 0.15276(19) 0.0326(15) Uani 1 1 d D A . O214 O 0.8792(4) 0.9764(3) 0.09145(16) 0.0195(11) Uani 1 1 d D A . O215 O 0.7900(5) 0.8272(3) 0.17012(19) 0.0322(13) Uani 1 1 d D A . O216 O 0.5911(5) 0.9063(3) 0.18231(17) 0.0254(12) Uani 1 1 d D A . O217 O 0.7200(5) 0.9704(3) 0.24436(17) 0.0290(13) Uani 1 1 d D A . O218 O 0.9215(5) 0.8986(3) 0.22864(16) 0.0292(13) Uani 1 1 d D A . O219 O 0.9901(5) 0.8963(3) 0.15113(18) 0.0331(14) Uani 1 1 d D A . O220 O 0.6796(5) 0.9020(3) 0.10817(16) 0.0225(12) Uani 1 1 d D A . O221 O 0.6159(5) 1.0523(3) 0.18434(18) 0.0265(12) Uiso 1 1 d D A . O222 O 0.9175(5) 1.0440(3) 0.22641(17) 0.0288(13) Uani 1 1 d D A . C5 C 0.6755(6) 0.9676(4) 0.0293(2) 0.0207(17) Uani 1 1 d D . . H5A H 0.6905 0.9160 0.0201 0.025 Uiso 1 1 calc R . . H5B H 0.5856 0.9749 0.0276 0.025 Uiso 1 1 calc R . . C6 C 0.6726(8) 0.8895(5) -0.0839(3) 0.041(2) Uani 1 1 d D . . H6A H 0.6028 0.8690 -0.1010 0.061 Uiso 1 1 calc R . . H6B H 0.6905 0.8578 -0.0593 0.061 Uiso 1 1 calc R . . H6C H 0.7446 0.8914 -0.1005 0.061 Uiso 1 1 calc R . . C7 C 0.6863(8) 1.0806(5) -0.1064(3) 0.035(2) Uani 1 1 d D . . H7A H 0.7752 1.0774 -0.1084 0.052 Uiso 1 1 calc R . . H7B H 0.6653 1.1300 -0.0960 0.052 Uiso 1 1 calc R . . H7C H 0.6445 1.0727 -0.1341 0.052 Uiso 1 1 calc R . . C8 C 0.4382(7) 1.0040(6) -0.0566(3) 0.035(2) Uani 1 1 d D . . H8A H 0.3929 1.0034 -0.0841 0.053 Uiso 1 1 calc R . . H8B H 0.4202 1.0501 -0.0419 0.053 Uiso 1 1 calc R . . H8C H 0.4132 0.9613 -0.0401 0.053 Uiso 1 1 calc R . . C221 C 0.5860(6) 1.1850(4) 0.1387(2) 0.0217(16) Uiso 1 1 d D . . H221 H 0.6178 1.2120 0.1144 0.026 Uiso 1 1 calc R . . C222 C 0.4466(7) 1.1708(5) 0.1292(3) 0.043(2) Uani 1 1 d D . . H22C H 0.4263 1.1629 0.0989 0.051 Uiso 1 1 calc R . . H22D H 0.4188 1.1272 0.1449 0.051 Uiso 1 1 calc R . . C223 C 0.3889(11) 1.2433(7) 0.1444(4) 0.077(4) Uani 1 1 d D . . H22E H 0.3832 1.2807 0.1216 0.092 Uiso 1 1 calc R . . H22F H 0.3054 1.2336 0.1532 0.092 Uiso 1 1 calc R . . C224 C 0.4694(11) 1.2706(10) 0.1801(5) 0.104(7) Uani 1 1 d D . . H22G H 0.4364 1.2556 0.2069 0.124 Uiso 1 1 calc R . . H22H H 0.4748 1.3256 0.1794 0.124 Uiso 1 1 calc R . . C225 C 0.5927(8) 1.2370(5) 0.1764(3) 0.039(2) Uani 1 1 d D . . H22I H 0.6179 1.2089 0.2022 0.047 Uiso 1 1 calc R . . H22J H 0.6539 1.2767 0.1728 0.047 Uiso 1 1 calc R . . C231 C 1.0402(6) 1.1732(4) 0.2032(2) 0.0249(17) Uani 1 1 d D . . H231 H 1.0576 1.2037 0.1782 0.030 Uiso 1 1 calc R . . C232 C 0.9779(7) 1.2234(5) 0.2351(3) 0.0293(19) Uani 1 1 d D . . H23C H 0.9496 1.2706 0.2217 0.035 Uiso 1 1 calc R . . H23D H 0.9064 1.1977 0.2458 0.035 Uiso 1 1 calc R . . C233 C 1.0741(9) 1.2384(7) 0.2702(3) 0.054(3) Uani 1 1 d D . . H23E H 1.0764 1.2922 0.2771 0.065 Uiso 1 1 calc R . . H23F H 1.0549 1.2105 0.2956 0.065 Uiso 1 1 calc R . . C234 C 1.1945(8) 1.2142(5) 0.2562(3) 0.048(3) Uani 1 1 d D . . H23G H 1.2497 1.1979 0.2803 0.057 Uiso 1 1 calc R . . H23H H 1.2344 1.2552 0.2416 0.057 Uiso 1 1 calc R . . C235 C 1.1644(7) 1.1502(5) 0.2267(3) 0.042(2) Uani 1 1 d D . . H23I H 1.1556 1.1032 0.2424 0.051 Uiso 1 1 calc R . . H23J H 1.2290 1.1437 0.2068 0.051 Uiso 1 1 calc R . . C241 C 1.1382(6) 0.9647(5) 0.0924(3) 0.033(2) Uani 0.488(13) 1 d PD A 1 H241 H 1.1151 0.9968 0.0675 0.039 Uiso 0.488(13) 1 calc PR A 1 C242 C 1.1780(14) 0.8960(10) 0.0734(6) 0.049(6) Uani 0.488(13) 1 d PD A 1 H24C H 1.1204 0.8818 0.0494 0.058 Uiso 0.488(13) 1 calc PR A 1 H24D H 1.1816 0.8550 0.0941 0.058 Uiso 0.488(13) 1 calc PR A 1 C243 C 1.3042(16) 0.9113(13) 0.0587(7) 0.059(7) Uani 0.488(13) 1 d PD A 1 H24E H 1.3527 0.8650 0.0578 0.070 Uiso 0.488(13) 1 calc PR A 1 H24F H 1.2984 0.9344 0.0306 0.070 Uiso 0.488(13) 1 calc PR A 1 C244 C 1.3607(10) 0.9644(10) 0.0912(5) 0.097(6) Uani 0.488(13) 1 d PD A 1 H24G H 1.4132 0.9372 0.1125 0.117 Uiso 0.488(13) 1 calc PR A 1 H24H H 1.4113 1.0022 0.0779 0.117 Uiso 0.488(13) 1 calc PR A 1 C245 C 1.2551(13) 1.0008(12) 0.1108(7) 0.053(7) Uani 0.488(13) 1 d PD A 1 H24I H 1.2540 1.0548 0.1048 0.063 Uiso 0.488(13) 1 calc PR A 1 H24J H 1.2630 0.9937 0.1416 0.063 Uiso 0.488(13) 1 calc PR A 1 C251 C 1.0217(7) 0.7651(5) 0.1996(3) 0.036(2) Uani 1 1 d D A . H251 H 1.0247 0.7336 0.1739 0.043 Uiso 1 1 calc R . . C252 C 0.9715(9) 0.7187(6) 0.2345(3) 0.048(3) Uani 1 1 d D . . H25C H 0.9021 0.7447 0.2464 0.057 Uiso 1 1 calc R A . H25D H 0.9423 0.6698 0.2235 0.057 Uiso 1 1 calc R . . C253 C 1.0734(12) 0.7089(13) 0.2666(4) 0.138(10) Uani 1 1 d D A . H25E H 1.0506 0.7308 0.2933 0.166 Uiso 1 1 calc R . . H25F H 1.0885 0.6551 0.2712 0.166 Uiso 1 1 calc R . . C254 C 1.1798(15) 0.7425(9) 0.2547(5) 0.121(8) Uani 1 1 d D . . H25G H 1.2424 0.7040 0.2502 0.145 Uiso 1 1 calc R A . H25H H 1.2130 0.7761 0.2772 0.145 Uiso 1 1 calc R . . C255 C 1.1534(8) 0.7851(6) 0.2159(4) 0.057(3) Uani 1 1 d D A . H25I H 1.2120 0.7718 0.1949 0.068 Uiso 1 1 calc R . . H25J H 1.1602 0.8392 0.2215 0.068 Uiso 1 1 calc R . . C261 C 0.5608(8) 0.7741(4) 0.1378(3) 0.036(2) Uani 1 1 d D A . H261 H 0.4828 0.7924 0.1231 0.043 Uiso 1 1 calc R . . C262 C 0.6123(17) 0.7129(8) 0.1108(5) 0.123(7) Uani 1 1 d D . . H26A H 0.5776 0.7167 0.0814 0.148 Uiso 1 1 calc R A . H26B H 0.7027 0.7162 0.1112 0.148 Uiso 1 1 calc R . . C263 C 0.575(5) 0.6430(9) 0.1299(13) 0.48(5) Uani 1 1 d D A . H26C H 0.6475 0.6174 0.1433 0.576 Uiso 1 1 calc R . . H26D H 0.5365 0.6097 0.1080 0.576 Uiso 1 1 calc R . . C264 C 0.483(3) 0.6596(10) 0.1628(7) 0.203(15) Uani 1 1 d D . . H26E H 0.3975 0.6623 0.1502 0.244 Uiso 1 1 calc R A . H26F H 0.4877 0.6225 0.1857 0.244 Uiso 1 1 calc R . . C265 C 0.5280(16) 0.7319(7) 0.1769(4) 0.102(6) Uani 1 1 d D A . H26G H 0.6012 0.7263 0.1967 0.123 Uiso 1 1 calc R . . H26H H 0.4641 0.7591 0.1912 0.123 Uiso 1 1 calc R . . C271 C 0.4637(7) 0.9877(4) 0.2418(2) 0.0270(18) Uani 1 1 d D A . H271 H 0.3910 0.9947 0.2214 0.032 Uiso 1 1 calc R . . C272 C 0.4718(9) 1.0551(5) 0.2712(3) 0.044(3) Uani 1 1 d D . . H27A H 0.5586 1.0673 0.2792 0.053 Uiso 1 1 calc R A . H27B H 0.4325 1.0990 0.2572 0.053 Uiso 1 1 calc R . . C273 C 0.4070(16) 1.0350(8) 0.3091(4) 0.091(5) Uani 1 1 d D A . H27C H 0.4513 1.0555 0.3346 0.109 Uiso 1 1 calc R . . H27D H 0.3227 1.0554 0.3069 0.109 Uiso 1 1 calc R . . C274 C 0.4039(12) 0.9538(7) 0.3110(4) 0.071(4) Uani 1 1 d D . . H27E H 0.3207 0.9370 0.3170 0.086 Uiso 1 1 calc R A . H27F H 0.4623 0.9361 0.3339 0.086 Uiso 1 1 calc R . . C275 C 0.4376(12) 0.9221(6) 0.2702(4) 0.066(4) Uani 1 1 d D A . H27G H 0.3693 0.8917 0.2574 0.080 Uiso 1 1 calc R . . H27H H 0.5111 0.8901 0.2746 0.080 Uiso 1 1 calc R . . C281 C 0.9178(7) 0.9748(4) 0.3058(2) 0.0206(16) Uani 1 1 d D A . H281 H 0.8779 0.9323 0.3197 0.025 Uiso 1 1 calc R . . C282 C 0.8825(8) 1.0463(4) 0.3278(2) 0.0300(19) Uani 1 1 d D . . H28A H 0.8907 1.0900 0.3093 0.036 Uiso 1 1 calc R A . H28B H 0.7970 1.0437 0.3360 0.036 Uiso 1 1 calc R . . C283 C 0.9716(9) 1.0513(6) 0.3659(3) 0.050(3) Uani 1 1 d D A . H28C H 0.9820 1.1036 0.3752 0.060 Uiso 1 1 calc R . . H28D H 0.9426 1.0215 0.3892 0.060 Uiso 1 1 calc R . . C284 C 1.0873(9) 1.0214(9) 0.3522(4) 0.080(5) Uani 1 1 d D . . H28E H 1.1322 0.9948 0.3756 0.095 Uiso 1 1 calc R A . H28F H 1.1397 1.0624 0.3432 0.095 Uiso 1 1 calc R . . C285 C 1.0572(7) 0.9686(6) 0.3162(3) 0.039(2) Uani 1 1 d D A . H28G H 1.0799 0.9170 0.3243 0.047 Uiso 1 1 calc R . . H28H H 1.1022 0.9827 0.2916 0.047 Uiso 1 1 calc R . . C290 C 0.7279(6) 1.0195(3) -0.0022(2) 0.0162(14) Uani 1 1 d D . . C291 C 0.8611(7) 1.0123(4) -0.0116(2) 0.0260(18) Uani 1 1 d D . . C292 C 0.9295(7) 0.9479(5) -0.0146(2) 0.0305(19) Uani 1 1 d D . . H292 H 0.8959 0.9007 -0.0086 0.037 Uiso 1 1 calc R . . C293 C 1.0513(7) 0.9547(6) -0.0267(3) 0.044(3) Uani 1 1 d D . . H293 H 1.1002 0.9118 -0.0301 0.053 Uiso 1 1 calc R . . C294 C 1.0973(8) 1.0243(7) -0.0337(3) 0.052(3) Uani 1 1 d D . . H294 H 1.1792 1.0281 -0.0415 0.062 Uiso 1 1 calc R . . C295 C 1.0328(8) 1.0877(6) -0.0300(3) 0.044(2) Uani 1 1 d D . . H295 H 1.0678 1.1348 -0.0355 0.053 Uiso 1 1 calc R . . C296 C 0.9116(7) 1.0819(5) -0.0176(2) 0.0292(19) Uani 1 1 d D . . C297 C 0.8183(8) 1.1383(4) -0.0110(3) 0.032(2) Uani 1 1 d D . . C298 C 0.8227(9) 1.2163(5) -0.0146(3) 0.041(2) Uani 1 1 d D . . H298 H 0.8941 1.2407 -0.0230 0.049 Uiso 1 1 calc R . . C299 C 0.7233(10) 1.2550(6) -0.0060(3) 0.052(3) Uani 1 1 d D . . H299 H 0.7228 1.3072 -0.0103 0.063 Uiso 1 1 calc R . . C300 C 0.6176(10) 1.2208(6) 0.0095(3) 0.057(3) Uani 1 1 d D . . H300 H 0.5516 1.2505 0.0179 0.069 Uiso 1 1 calc R . . C301 C 0.6126(8) 1.1429(4) 0.0124(3) 0.0305(19) Uani 1 1 d D . . H301 H 0.5419 1.1189 0.0215 0.037 Uiso 1 1 calc R . . C302 C 0.7120(7) 1.1019(4) 0.0016(2) 0.0257(17) Uani 1 1 d D . . C240 C 1.1382(6) 0.9647(5) 0.0924(3) 0.033(2) Uani 0.512(13) 1 d P A 2 H240 H 1.1187 0.9283 0.0692 0.039 Uiso 0.512(13) 1 calc PR A 2 C246 C 1.1813(13) 1.0282(10) 0.0739(5) 0.028(4) Uani 0.512(13) 1 d P A 2 H24K H 1.1847 1.0702 0.0940 0.033 Uiso 0.512(13) 1 calc PR A 2 H24L H 1.1272 1.0422 0.0491 0.033 Uiso 0.512(13) 1 calc PR A 2 C247 C 1.3121(15) 1.0087(8) 0.0610(6) 0.025(4) Uani 0.512(13) 1 d P A 2 H24M H 1.3076 0.9828 0.0336 0.030 Uiso 0.512(13) 1 calc PR A 2 H24N H 1.3618 1.0544 0.0588 0.030 Uiso 0.512(13) 1 calc PR A 2 C248 C 1.3607(10) 0.9644(10) 0.0912(5) 0.097(6) Uani 0.512(13) 1 d P A 2 H24O H 1.4222 0.9929 0.1089 0.117 Uiso 0.512(13) 1 calc PR A 2 H24P H 1.4037 0.9227 0.0783 0.117 Uiso 0.512(13) 1 calc PR A 2 C249 C 1.2577(14) 0.9308(12) 0.1207(7) 0.046(6) Uani 0.512(13) 1 d P A 2 H24Q H 1.2653 0.9513 0.1495 0.055 Uiso 0.512(13) 1 calc PR A 2 H24R H 1.2580 0.8758 0.1216 0.055 Uiso 0.512(13) 1 calc PR A 2 C400 C 0.781(3) 0.738(2) -0.0028(11) 0.118(12) Uiso 0.50 1 d PD . . H40A H 0.7109 0.7046 -0.0026 0.177 Uiso 0.50 1 calc PR . . H40B H 0.8296 0.7261 -0.0265 0.177 Uiso 0.50 1 calc PR . . H40C H 0.7521 0.7898 -0.0055 0.177 Uiso 0.50 1 calc PR . . C401 C 0.859(3) 0.730(4) 0.0372(15) 0.20(2) Uiso 0.50 1 d PD . . H40D H 0.8339 0.7678 0.0573 0.244 Uiso 0.50 1 calc PR . . H40E H 0.8439 0.6804 0.0492 0.244 Uiso 0.50 1 calc PR . . C402 C 0.991(3) 0.738(3) 0.0331(13) 0.20(2) Uiso 0.50 1 d PD . . H40F H 1.0059 0.7865 0.0199 0.237 Uiso 0.50 1 calc PR . . H40G H 1.0170 0.6986 0.0139 0.237 Uiso 0.50 1 calc PR . . C403 C 1.070(3) 0.733(2) 0.0728(10) 0.116(12) Uiso 0.50 1 d PD . . H40H H 1.0466 0.6889 0.0891 0.139 Uiso 0.50 1 calc PR . . H40I H 1.0592 0.7779 0.0900 0.139 Uiso 0.50 1 calc PR . . C404 C 1.204(4) 0.726(3) 0.0617(15) 0.17(2) Uiso 0.50 1 d PD . . 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 Sn11 0.0362(3) 0.0282(3) 0.0210(3) -0.0003(2) -0.0011(2) 0.0081(3) Si11 0.0156(9) 0.0389(16) 0.0146(11) -0.0016(9) 0.0011(8) -0.0019(9) Si12 0.0164(9) 0.0374(15) 0.0176(11) -0.0019(9) 0.0011(8) -0.0022(9) Si13 0.0166(10) 0.0359(15) 0.0202(11) 0.0001(9) 0.0026(8) 0.0000(9) Si14 0.0127(9) 0.0390(16) 0.0167(11) 0.0006(9) 0.0030(8) -0.0008(9) Si15 0.0189(10) 0.0315(14) 0.0187(11) -0.0019(9) 0.0016(8) -0.0027(9) Si16 0.0177(10) 0.0365(15) 0.0190(11) -0.0013(9) 0.0004(8) 0.0020(9) Si17 0.0147(9) 0.0473(17) 0.0136(11) -0.0027(10) 0.0035(8) -0.0025(9) Si18 0.0178(9) 0.0327(15) 0.0165(11) -0.0020(9) 0.0008(8) -0.0014(9) O11 0.023(3) 0.044(4) 0.021(3) -0.002(3) -0.002(2) -0.001(2) O12 0.022(3) 0.047(4) 0.035(3) 0.001(3) -0.008(2) -0.005(3) O13 0.022(3) 0.052(4) 0.027(3) 0.013(3) 0.009(2) 0.003(3) O14 0.015(2) 0.053(4) 0.019(3) -0.003(3) 0.003(2) 0.000(2) O15 0.021(3) 0.039(4) 0.036(3) -0.005(3) -0.007(2) -0.001(2) O16 0.034(3) 0.035(4) 0.026(3) 0.007(2) 0.014(3) -0.003(2) O17 0.015(3) 0.058(5) 0.026(3) -0.003(3) 0.001(2) -0.003(2) O18 0.037(3) 0.041(4) 0.027(3) -0.002(3) 0.006(3) -0.017(3) O19 0.024(3) 0.038(4) 0.024(3) -0.009(3) 0.003(2) -0.004(2) O20 0.031(3) 0.038(4) 0.023(3) -0.006(3) 0.000(2) 0.008(3) O21 0.027(3) 0.047(4) 0.029(4) -0.012(3) 0.010(3) -0.012(3) O22 0.035(3) 0.041(4) 0.026(3) -0.004(3) 0.000(3) 0.010(3) C1 0.022(4) 0.027(5) 0.021(4) -0.002(3) -0.001(3) 0.003(3) C2 0.054(6) 0.046(7) 0.043(6) -0.001(5) -0.002(5) 0.018(5) C3 0.058(7) 0.047(7) 0.057(7) -0.004(5) 0.005(5) -0.001(5) C21 0.032(4) 0.022(4) 0.021(4) 0.002(3) 0.006(3) 0.002(3) C22 0.045(5) 0.046(6) 0.030(5) 0.006(4) -0.005(4) -0.015(4) C23 0.059(7) 0.055(7) 0.054(7) 0.018(6) 0.003(5) -0.026(6) C24 0.044(5) 0.048(7) 0.061(7) 0.011(5) -0.004(5) -0.017(5) C25 0.016(3) 0.036(5) 0.044(5) -0.002(4) 0.000(3) -0.008(3) C31 0.023(4) 0.023(5) 0.026(4) 0.001(3) 0.003(3) 0.006(3) C32 0.035(5) 0.039(6) 0.038(5) 0.012(4) 0.008(4) -0.005(4) C33 0.049(7) 0.191(18) 0.044(8) 0.061(9) 0.002(6) 0.021(9) C34 0.057(7) 0.103(11) 0.088(10) 0.051(9) -0.038(7) -0.023(7) C35 0.021(4) 0.074(8) 0.070(8) 0.016(6) 0.006(5) 0.015(5) C41 0.018(4) 0.051(6) 0.032(5) -0.001(4) 0.007(3) -0.006(4) C42 0.027(5) 0.139(13) 0.049(8) 0.019(8) 0.003(5) 0.015(6) C43 0.021(4) 0.069(8) 0.093(10) 0.006(7) 0.021(6) 0.002(5) C44 0.036(6) 0.107(11) 0.061(8) -0.016(8) 0.019(6) -0.018(6) C45 0.045(6) 0.059(7) 0.045(6) 0.004(5) 0.012(5) -0.002(5) C51 0.026(4) 0.042(6) 0.023(4) -0.001(4) 0.006(3) 0.001(4) C52 0.038(5) 0.038(6) 0.042(5) -0.007(4) 0.004(4) -0.014(4) C53 0.064(8) 0.104(11) 0.069(9) -0.048(8) -0.016(7) -0.010(7) C54 0.050(7) 0.103(12) 0.086(10) -0.036(8) -0.026(7) 0.013(7) C55 0.019(4) 0.079(8) 0.063(7) -0.006(6) -0.005(4) -0.012(5) C61 0.039(5) 0.034(5) 0.030(5) 0.006(4) 0.001(4) 0.013(4) C62 0.052(7) 0.084(10) 0.081(9) -0.020(7) -0.024(6) 0.030(6) C63 0.059(8) 0.082(10) 0.115(12) -0.011(9) -0.022(8) 0.033(7) C64 0.077(8) 0.047(7) 0.081(9) -0.011(7) 0.021(7) 0.029(6) C65 0.085(8) 0.039(7) 0.043(6) -0.014(5) -0.013(6) 0.012(6) C71 0.022(4) 0.044(6) 0.027(5) 0.000(4) 0.005(3) -0.005(4) C72 0.037(5) 0.073(8) 0.050(6) -0.030(6) 0.015(5) -0.003(5) C73 0.055(7) 0.118(12) 0.030(6) -0.016(6) 0.013(5) 0.006(7) C74 0.166(17) 0.134(15) 0.027(7) 0.039(8) 0.047(8) 0.083(12) C75 0.051(6) 0.058(8) 0.059(7) 0.003(6) 0.019(5) -0.016(5) C81 0.029(4) 0.058(7) 0.017(4) -0.002(4) -0.003(3) 0.005(4) C82 0.060(7) 0.060(7) 0.042(6) -0.029(5) -0.004(5) 0.023(5) C83 0.099(11) 0.076(10) 0.081(10) -0.032(8) -0.033(8) 0.022(8) C84 0.045(7) 0.200(19) 0.061(9) -0.050(11) -0.014(6) 0.018(9) C85 0.036(5) 0.104(10) 0.033(6) -0.012(6) -0.015(4) 0.021(6) C90 0.031(4) 0.039(6) 0.025(4) 0.004(4) -0.007(3) 0.007(4) C91 0.035(5) 0.091(9) 0.026(5) -0.006(5) -0.004(4) 0.016(5) C92 0.043(6) 0.066(8) 0.031(5) 0.006(5) 0.007(4) -0.007(5) C93 0.056(8) 0.160(17) 0.033(7) -0.005(8) -0.003(6) -0.004(9) C94 0.059(8) 0.155(17) 0.046(8) -0.015(9) 0.004(6) 0.026(10) C95 0.091(11) 0.161(17) 0.062(9) -0.027(10) -0.022(8) 0.101(12) C96 0.074(7) 0.044(6) 0.025(5) -0.007(4) -0.014(5) 0.036(6) C97 0.081(9) 0.093(11) 0.043(7) 0.001(7) -0.020(6) 0.003(8) C98 0.115(12) 0.047(8) 0.060(8) 0.007(6) -0.053(8) 0.001(7) C99 0.133(16) 0.095(13) 0.066(10) 0.009(9) -0.048(11) -0.005(12) C100 0.161(16) 0.100(12) 0.036(7) 0.016(8) -0.021(9) -0.087(12) C101 0.099(9) 0.053(7) 0.025(5) 0.009(5) -0.013(5) -0.039(6) C102 0.076(7) 0.029(5) 0.021(4) -0.002(4) -0.012(4) 0.013(5) Sn21 0.0205(2) 0.0436(4) 0.0162(2) -0.0008(2) 0.00149(18) 0.0003(2) Si21 0.0175(9) 0.0130(12) 0.0159(11) 0.0018(8) 0.0030(8) -0.0037(7) Si22 0.0185(9) 0.0066(10) 0.0203(10) 0.0039(8) 0.0039(8) -0.0030(7) Si23 0.0161(9) 0.0162(12) 0.0197(10) -0.0009(8) 0.0032(8) -0.0046(8) Si24 0.0157(9) 0.0232(13) 0.0200(11) -0.0030(9) 0.0038(8) -0.0018(8) Si25 0.0285(11) 0.0191(12) 0.0210(11) -0.0025(9) -0.0009(9) 0.0112(9) Si26 0.0297(10) 0.0048(10) 0.0193(10) -0.0019(8) 0.0056(8) -0.0038(8) Si27 0.0191(9) 0.0015(10) 0.0225(11) 0.0007(7) 0.0050(8) -0.0018(7) Si28 0.0207(10) 0.0192(12) 0.0164(11) 0.0008(8) -0.0007(8) 0.0042(8) O211 0.024(3) 0.013(3) 0.026(3) 0.009(2) 0.000(2) 0.000(2) O212 0.021(3) 0.016(3) 0.040(3) 0.006(2) -0.007(2) -0.006(2) O213 0.021(3) 0.039(4) 0.039(4) -0.018(3) 0.011(3) -0.008(2) O214 0.020(3) 0.015(3) 0.024(3) 0.001(2) 0.002(2) -0.0003(19) O215 0.039(3) 0.017(3) 0.040(3) -0.003(3) -0.006(3) 0.009(2) O216 0.037(3) 0.008(3) 0.032(3) 0.000(2) 0.010(3) -0.005(2) O217 0.024(3) 0.039(4) 0.023(3) 0.003(2) -0.002(2) 0.004(2) O218 0.043(3) 0.026(3) 0.019(3) -0.008(2) 0.002(2) 0.011(3) O219 0.039(3) 0.023(3) 0.038(4) 0.007(3) 0.005(3) 0.012(2) O220 0.031(3) 0.015(3) 0.021(3) 0.004(2) 0.003(2) -0.010(2) O222 0.037(3) 0.025(3) 0.024(3) 0.006(2) -0.002(2) -0.005(2) C5 0.021(4) 0.023(5) 0.018(4) 0.004(3) 0.001(3) -0.008(3) C6 0.039(5) 0.036(6) 0.047(6) -0.002(5) 0.007(4) -0.005(4) C7 0.042(5) 0.032(5) 0.031(5) 0.006(4) 0.009(4) -0.004(4) C8 0.014(4) 0.054(7) 0.038(5) -0.009(5) 0.001(3) 0.002(4) C222 0.031(5) 0.033(6) 0.062(7) -0.011(5) -0.017(4) 0.012(4) C223 0.066(8) 0.070(9) 0.093(10) -0.042(8) -0.003(7) 0.041(7) C224 0.067(8) 0.149(16) 0.093(11) -0.081(11) -0.008(8) 0.045(9) C225 0.049(5) 0.018(5) 0.048(6) -0.005(4) -0.005(4) 0.008(4) C231 0.019(4) 0.028(5) 0.027(4) 0.001(3) -0.002(3) -0.008(3) C232 0.030(4) 0.017(5) 0.041(5) -0.011(4) 0.008(4) 0.000(3) C233 0.051(6) 0.058(7) 0.052(7) -0.029(6) 0.000(5) -0.001(5) C234 0.047(6) 0.024(5) 0.070(7) -0.011(5) -0.013(5) -0.012(4) C235 0.021(4) 0.042(6) 0.062(7) -0.017(5) -0.011(4) 0.000(4) C241 0.013(3) 0.059(7) 0.026(5) -0.018(4) 0.006(3) -0.005(4) C242 0.030(10) 0.072(16) 0.044(12) -0.006(11) 0.001(8) 0.019(10) C243 0.045(12) 0.073(18) 0.058(15) -0.019(13) 0.009(11) 0.009(11) C244 0.029(6) 0.173(18) 0.094(12) -0.017(12) 0.027(7) 0.009(8) C245 0.015(8) 0.092(19) 0.051(13) -0.003(13) 0.004(8) -0.034(10) C251 0.046(5) 0.037(6) 0.025(4) 0.006(4) 0.004(4) 0.030(4) C252 0.056(6) 0.042(6) 0.046(6) 0.015(5) 0.011(5) 0.010(5) C253 0.070(10) 0.28(3) 0.067(11) 0.090(14) 0.017(8) 0.058(14) C254 0.146(16) 0.069(10) 0.133(15) 0.068(10) -0.087(13) -0.022(10) C255 0.033(5) 0.049(7) 0.087(9) 0.019(6) -0.003(5) 0.016(5) C261 0.059(6) 0.016(5) 0.032(5) 0.001(4) 0.004(4) -0.011(4) C262 0.136(16) 0.099(13) 0.139(17) -0.052(12) 0.045(13) -0.054(11) C263 0.96(12) 0.025(11) 0.52(7) -0.02(2) 0.52(8) -0.09(3) C264 0.35(4) 0.098(16) 0.18(2) -0.007(15) 0.13(2) -0.15(2) C265 0.180(16) 0.077(10) 0.051(8) 0.005(7) 0.014(9) -0.099(11) C271 0.022(4) 0.028(5) 0.031(5) -0.005(4) 0.005(3) -0.007(3) C272 0.051(6) 0.033(6) 0.053(6) -0.009(5) 0.026(5) 0.009(4) C273 0.117(13) 0.097(13) 0.064(10) -0.031(9) 0.032(9) 0.013(9) C274 0.066(8) 0.090(11) 0.062(9) 0.029(7) 0.031(7) 0.020(7) C275 0.090(9) 0.041(7) 0.076(9) 0.008(6) 0.056(7) -0.011(6) C281 0.024(4) 0.011(4) 0.027(4) 0.004(3) 0.001(3) 0.000(3) C282 0.043(5) 0.023(5) 0.023(4) 0.002(3) 0.001(4) 0.003(4) C283 0.053(6) 0.060(7) 0.036(6) -0.025(5) -0.009(5) 0.002(5) C284 0.034(6) 0.162(14) 0.042(7) -0.048(8) -0.003(5) -0.012(7) C285 0.032(5) 0.052(6) 0.031(5) -0.001(4) -0.008(4) 0.015(4) C290 0.023(3) 0.010(4) 0.016(3) 0.005(3) 0.001(3) -0.003(3) C291 0.030(4) 0.039(5) 0.008(3) -0.002(3) -0.006(3) -0.010(4) C292 0.031(4) 0.041(6) 0.018(4) -0.004(4) -0.005(3) 0.015(4) C293 0.023(4) 0.082(8) 0.026(5) -0.009(5) -0.002(4) 0.017(5) C294 0.030(5) 0.107(10) 0.018(4) 0.001(5) 0.001(4) -0.011(6) C295 0.035(5) 0.068(8) 0.030(5) 0.006(5) 0.003(4) -0.013(5) C296 0.029(4) 0.042(5) 0.017(4) -0.002(4) 0.001(3) -0.012(4) C297 0.048(5) 0.020(4) 0.027(4) 0.003(4) -0.010(4) -0.017(4) C298 0.055(6) 0.030(5) 0.036(5) 0.006(4) -0.011(4) -0.020(4) C299 0.073(8) 0.036(6) 0.046(6) -0.004(5) -0.006(5) -0.012(5) C300 0.063(7) 0.064(8) 0.041(6) -0.008(5) -0.022(5) 0.025(6) C301 0.045(5) 0.016(4) 0.029(4) -0.004(3) -0.008(4) 0.004(4) C302 0.037(4) 0.025(4) 0.015(4) 0.004(3) -0.004(3) -0.002(3) C240 0.013(3) 0.059(7) 0.026(5) -0.018(4) 0.006(3) -0.005(4) C246 0.016(7) 0.042(11) 0.025(9) 0.013(7) -0.002(6) -0.007(7) C247 0.035(9) 0.006(7) 0.037(10) -0.008(6) 0.026(8) 0.001(6) C248 0.029(6) 0.173(18) 0.094(12) -0.017(12) 0.027(7) 0.009(8) C249 0.017(8) 0.053(13) 0.069(14) 0.033(11) 0.011(8) 0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn11 C4 2.021(11) . ? Sn11 C2 2.121(9) . ? Sn11 C3 2.142(9) . ? Sn11 C90 2.228(7) . ? Si11 O11 1.614(6) . ? Si11 O14 1.616(5) . ? Si11 O20 1.621(6) . ? Si11 C1 1.851(7) . ? Si12 O21 1.607(6) . ? Si12 O12 1.620(5) . ? Si12 O11 1.626(6) . ? Si12 C21 1.844(7) . ? Si13 O12 1.606(5) . ? Si13 O22 1.616(6) . ? Si13 O13 1.622(5) . ? Si13 C31 1.846(7) . ? Si14 O13 1.609(6) . ? Si14 O14 1.620(5) . ? Si14 O19 1.628(6) . ? Si14 C41 1.854(7) . ? Si15 O19 1.608(5) . ? Si15 O18 1.625(6) . ? Si15 O15 1.625(5) . ? Si15 C51 1.849(8) . ? Si16 O15 1.617(5) . ? Si16 O20 1.618(6) . ? Si16 O16 1.620(5) . ? Si16 C61 1.824(8) . ? Si17 O16 1.614(6) . ? Si17 O17 1.617(5) . ? Si17 O21 1.635(6) . ? Si17 C71 1.832(7) . ? Si18 O22 1.615(6) . ? Si18 O18 1.618(6) . ? Si18 O17 1.621(5) . ? Si18 C81 1.835(7) . ? C1 C90 1.539(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C21 C25 1.541(9) . ? C21 C22 1.574(10) . ? C21 H21 1.0000 . ? C22 C23 1.541(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.494(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.503(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C31 C35 1.556(10) . ? C31 C32 1.559(10) . ? C31 H31 1.0000 . ? C32 C33 1.506(12) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.457(13) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.478(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C41 C42 1.503(13) . ? C41 C45 1.511(12) . ? C41 H41 1.0000 . ? C42 C43 1.513(14) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.513(15) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.507(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C51 C52 1.538(10) . ? C51 C55 1.557(11) . ? C51 H51 1.0000 . ? C52 C53 1.485(12) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.424(14) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.497(13) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C61 C62 1.524(12) . ? C61 C65 1.538(11) . ? C61 H61 1.0000 . ? C62 C63 1.497(15) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.510(17) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.504(13) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C71 C72 1.519(11) . ? C71 C75 1.545(11) . ? C71 H71 1.0000 . ? C72 C73 1.511(12) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.454(16) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.482(13) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C81 C82 1.518(11) . ? C81 C85 1.541(10) . ? C81 H81 1.0000 . ? C82 C83 1.489(12) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.448(14) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.502(13) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C90 C91 1.509(10) . ? C90 C102 1.522(11) . ? C91 C92 1.381(12) . ? C91 C96 1.421(12) . ? C92 C93 1.448(13) . ? C92 H92 0.9500 . ? C93 C94 1.401(17) . ? C93 H93 0.9500 . ? C94 C95 1.356(17) . ? C94 H94 0.9500 . ? C95 C96 1.415(13) . ? C95 H95 0.9500 . ? C96 C97 1.447(14) . ? C97 C102 1.392(13) . ? C97 C98 1.444(14) . ? C98 C99 1.345(17) . ? C98 H98 0.9500 . ? C99 C100 1.397(17) . ? C99 H99 0.9500 . ? C100 C101 1.407(14) . ? C100 H100 0.9500 . ? C101 C102 1.395(12) . ? C101 H101 0.9500 . ? Sn21 C6 2.103(8) . ? Sn21 C8 2.131(7) . ? Sn21 C7 2.132(8) . ? Sn21 C290 2.225(6) . ? Si21 O211 1.606(5) . ? Si21 O214 1.613(5) . ? Si21 O220 1.623(5) . ? Si21 C5 1.858(7) . ? Si22 O212 1.614(5) . ? Si22 O221 1.623(6) . ? Si22 O211 1.633(5) . ? Si22 C221 1.833(7) . ? Si23 O222 1.616(5) . ? Si23 O213 1.617(5) . ? Si23 O212 1.623(5) . ? Si23 C231 1.841(7) . ? Si24 O213 1.611(6) . ? Si24 O219 1.615(6) . ? Si24 O214 1.618(5) . ? Si24 C241 1.841(7) . ? Si25 O219 1.613(6) . ? Si25 O215 1.613(6) . ? Si25 O218 1.626(5) . ? Si25 C251 1.840(7) . ? Si26 O220 1.613(5) . ? Si26 O215 1.613(5) . ? Si26 O216 1.623(5) . ? Si26 C261 1.812(8) . ? Si27 O221 1.608(6) . ? Si27 O216 1.610(5) . ? Si27 O217 1.612(5) . ? Si27 C271 1.840(7) . ? Si28 O218 1.604(5) . ? Si28 O222 1.608(5) . ? Si28 O217 1.622(5) . ? Si28 C281 1.838(7) . ? C5 C290 1.515(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C221 C225 1.526(10) . ? C221 C222 1.554(10) . ? C221 H221 1.0000 . ? C222 C223 1.540(12) . ? C222 H22C 0.9900 . ? C222 H22D 0.9900 . ? C223 C224 1.477(14) . ? C223 H22E 0.9900 . ? C223 H22F 0.9900 . ? C224 C225 1.489(12) . ? C224 H22G 0.9900 . ? C224 H22H 0.9900 . ? C225 H22I 0.9900 . ? C225 H22J 0.9900 . ? C231 C232 1.556(10) . ? C231 C235 1.561(10) . ? C231 H231 1.0000 . ? C232 C233 1.510(11) . ? C232 H23C 0.9900 . ? C232 H23D 0.9900 . ? C233 C234 1.486(12) . ? C233 H23E 0.9900 . ? C233 H23F 0.9900 . ? C234 C235 1.510(11) . ? C234 H23G 0.9900 . ? C234 H23H 0.9900 . ? C235 H23I 0.9900 . ? C235 H23J 0.9900 . ? C241 C242 1.458(16) . ? C241 C245 1.515(14) . ? C241 H241 1.0000 . ? C242 C243 1.514(19) . ? C242 H24C 0.9900 . ? C242 H24D 0.9900 . ? C243 C244 1.511(18) . ? C243 H24E 0.9900 . ? C243 H24F 0.9900 . ? C244 C245 1.502(17) . ? C244 H24G 0.9900 . ? C244 H24H 0.9900 . ? C245 H24I 0.9900 . ? C245 H24J 0.9900 . ? C251 C252 1.527(11) . ? C251 C255 1.539(11) . ? C251 H251 1.0000 . ? C252 C253 1.472(13) . ? C252 H25C 0.9900 . ? C252 H25D 0.9900 . ? C253 C254 1.387(16) . ? C253 H25E 0.9900 . ? C253 H25F 0.9900 . ? C254 C255 1.472(13) . ? C254 H25G 0.9900 . ? C254 H25H 0.9900 . ? C255 H25I 0.9900 . ? C255 H25J 0.9900 . ? C261 C265 1.528(11) . ? C261 C262 1.531(14) . ? C261 H261 1.0000 . ? C262 C263 1.469(18) . ? C262 H26A 0.9900 . ? C262 H26B 0.9900 . ? C263 C264 1.54(2) . ? C263 H26C 0.9900 . ? C263 H26D 0.9900 . ? C264 C265 1.451(16) . ? C264 H26E 0.9900 . ? C264 H26F 0.9900 . ? C265 H26G 0.9900 . ? C265 H26H 0.9900 . ? C271 C275 1.529(11) . ? C271 C272 1.532(11) . ? C271 H271 1.0000 . ? C272 C273 1.490(13) . ? C272 H27A 0.9900 . ? C272 H27B 0.9900 . ? C273 C274 1.462(16) . ? C273 H27C 0.9900 . ? C273 H27D 0.9900 . ? C274 C275 1.494(13) . ? C274 H27E 0.9900 . ? C274 H27F 0.9900 . ? C275 H27G 0.9900 . ? C275 H27H 0.9900 . ? C281 C282 1.528(10) . ? C281 C285 1.540(10) . ? C281 H281 1.0000 . ? C282 C283 1.508(10) . ? C282 H28A 0.9900 . ? C282 H28B 0.9900 . ? C283 C284 1.469(12) . ? C283 H28C 0.9900 . ? C283 H28D 0.9900 . ? C284 C285 1.513(12) . ? C284 H28E 0.9900 . ? C284 H28F 0.9900 . ? C285 H28G 0.9900 . ? C285 H28H 0.9900 . ? C290 C302 1.496(9) . ? C290 C291 1.513(9) . ? C291 C292 1.384(11) . ? C291 C296 1.386(10) . ? C292 C293 1.419(11) . ? C292 H292 0.9500 . ? C293 C294 1.371(14) . ? C293 H293 0.9500 . ? C294 C295 1.350(14) . ? C294 H294 0.9500 . ? C295 C296 1.414(10) . ? C295 H295 0.9500 . ? C296 C297 1.464(11) . ? C297 C298 1.409(11) . ? C297 C302 1.417(10) . ? C298 C299 1.335(13) . ? C298 H298 0.9500 . ? C299 C300 1.428(14) . ? C299 H299 0.9500 . ? C300 C301 1.405(12) . ? C300 H300 0.9500 . ? C301 C302 1.377(10) . ? C301 H301 0.9500 . ? C246 C247 1.56(2) . ? C246 H24K 0.9900 . ? C246 H24L 0.9900 . ? C247 H24M 0.9900 . ? C247 H24N 0.9900 . ? C249 H24Q 0.9900 . ? C249 H24R 0.9900 . ? C400 C401 1.50(3) . ? C400 H40A 0.9800 . ? C400 H40B 0.9800 . ? C400 H40C 0.9800 . ? C401 C402 1.46(3) . ? C401 H40D 0.9900 . ? C401 H40E 0.9900 . ? C402 C403 1.49(3) . ? C402 H40F 0.9900 . ? C402 H40G 0.9900 . ? C403 C404 1.54(3) . ? C403 H40H 0.9900 . ? C403 H40I 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 C4 Sn11 C2 106.9(5) . . ? C4 Sn11 C3 118.2(5) . . ? C2 Sn11 C3 109.2(4) . . ? C4 Sn11 C90 109.0(4) . . ? C2 Sn11 C90 106.9(4) . . ? C3 Sn11 C90 106.2(4) . . ? O11 Si11 O14 109.3(3) . . ? O11 Si11 O20 110.0(3) . . ? O14 Si11 O20 108.9(3) . . ? O11 Si11 C1 110.8(3) . . ? O14 Si11 C1 112.2(3) . . ? O20 Si11 C1 105.6(3) . . ? O21 Si12 O12 109.8(3) . . ? O21 Si12 O11 108.3(3) . . ? O12 Si12 O11 108.8(3) . . ? O21 Si12 C21 109.8(3) . . ? O12 Si12 C21 106.7(3) . . ? O11 Si12 C21 113.5(3) . . ? O12 Si13 O22 108.1(3) . . ? O12 Si13 O13 108.0(3) . . ? O22 Si13 O13 109.5(3) . . ? O12 Si13 C31 112.9(3) . . ? O22 Si13 C31 107.7(3) . . ? O13 Si13 C31 110.6(3) . . ? O13 Si14 O14 109.7(3) . . ? O13 Si14 O19 108.5(3) . . ? O14 Si14 O19 109.0(3) . . ? O13 Si14 C41 107.6(3) . . ? O14 Si14 C41 111.5(4) . . ? O19 Si14 C41 110.5(4) . . ? O19 Si15 O18 110.2(3) . . ? O19 Si15 O15 108.3(3) . . ? O18 Si15 O15 109.0(3) . . ? O19 Si15 C51 110.6(3) . . ? O18 Si15 C51 108.2(3) . . ? O15 Si15 C51 110.5(3) . . ? O15 Si16 O20 109.2(3) . . ? O15 Si16 O16 109.7(3) . . ? O20 Si16 O16 107.8(3) . . ? O15 Si16 C61 108.9(4) . . ? O20 Si16 C61 111.8(3) . . ? O16 Si16 C61 109.4(4) . . ? O16 Si17 O17 108.5(3) . . ? O16 Si17 O21 110.2(3) . . ? O17 Si17 O21 108.5(3) . . ? O16 Si17 C71 108.0(3) . . ? O17 Si17 C71 109.3(3) . . ? O21 Si17 C71 112.3(3) . . ? O22 Si18 O18 108.0(3) . . ? O22 Si18 O17 111.1(3) . . ? O18 Si18 O17 108.1(3) . . ? O22 Si18 C81 110.5(4) . . ? O18 Si18 C81 109.9(4) . . ? O17 Si18 C81 109.2(3) . . ? Si11 O11 Si12 148.8(4) . . ? Si13 O12 Si12 152.0(4) . . ? Si14 O13 Si13 149.7(4) . . ? Si11 O14 Si14 149.6(4) . . ? Si16 O15 Si15 147.3(4) . . ? Si17 O16 Si16 152.2(4) . . ? Si17 O17 Si18 147.9(4) . . ? Si18 O18 Si15 151.9(4) . . ? Si15 O19 Si14 148.2(4) . . ? Si16 O20 Si11 148.1(4) . . ? Si12 O21 Si17 147.4(4) . . ? Si18 O22 Si13 148.3(4) . . ? C90 C1 Si11 118.2(5) . . ? C90 C1 H1A 107.8 . . ? Si11 C1 H1A 107.8 . . ? C90 C1 H1B 107.8 . . ? Si11 C1 H1B 107.8 . . ? H1A C1 H1B 107.1 . . ? Sn11 C2 H2A 109.5 . . ? Sn11 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sn11 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Sn11 C3 H3A 109.5 . . ? Sn11 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Sn11 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Sn11 C4 H4A 109.5 . . ? Sn11 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Sn11 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C25 C21 C22 102.7(6) . . ? C25 C21 Si12 118.0(5) . . ? C22 C21 Si12 111.8(5) . . ? C25 C21 H21 107.9 . . ? C22 C21 H21 107.9 . . ? Si12 C21 H21 107.9 . . ? C23 C22 C21 104.8(7) . . ? C23 C22 H22A 110.8 . . ? C21 C22 H22A 110.8 . . ? C23 C22 H22B 110.8 . . ? C21 C22 H22B 110.8 . . ? H22A C22 H22B 108.9 . . ? C24 C23 C22 106.9(7) . . ? C24 C23 H23A 110.3 . . ? C22 C23 H23A 110.3 . . ? C24 C23 H23B 110.3 . . ? C22 C23 H23B 110.3 . . ? H23A C23 H23B 108.6 . . ? C23 C24 C25 106.4(8) . . ? C23 C24 H24A 110.4 . . ? C25 C24 H24A 110.4 . . ? C23 C24 H24B 110.4 . . ? C25 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? C24 C25 C21 102.9(7) . . ? C24 C25 H25A 111.2 . . ? C21 C25 H25A 111.2 . . ? C24 C25 H25B 111.2 . . ? C21 C25 H25B 111.2 . . ? H25A C25 H25B 109.1 . . ? C35 C31 C32 105.2(6) . . ? C35 C31 Si13 110.9(6) . . ? C32 C31 Si13 112.9(5) . . ? C35 C31 H31 109.2 . . ? C32 C31 H31 109.2 . . ? Si13 C31 H31 109.2 . . ? C33 C32 C31 104.9(7) . . ? C33 C32 H32A 110.8 . . ? C31 C32 H32A 110.8 . . ? C33 C32 H32B 110.8 . . ? C31 C32 H32B 110.8 . . ? H32A C32 H32B 108.8 . . ? C34 C33 C32 108.7(8) . . ? C34 C33 H33A 110.0 . . ? C32 C33 H33A 110.0 . . ? C34 C33 H33B 110.0 . . ? C32 C33 H33B 110.0 . . ? H33A C33 H33B 108.3 . . ? C33 C34 C35 106.7(9) . . ? C33 C34 H34A 110.4 . . ? C35 C34 H34A 110.4 . . ? C33 C34 H34B 110.4 . . ? C35 C34 H34B 110.4 . . ? H34A C34 H34B 108.6 . . ? C34 C35 C31 105.2(8) . . ? C34 C35 H35A 110.7 . . ? C31 C35 H35A 110.7 . . ? C34 C35 H35B 110.7 . . ? C31 C35 H35B 110.7 . . ? H35A C35 H35B 108.8 . . ? C42 C41 C45 100.3(8) . . ? C42 C41 Si14 113.4(7) . . ? C45 C41 Si14 117.1(6) . . ? C42 C41 H41 108.5 . . ? C45 C41 H41 108.5 . . ? Si14 C41 H41 108.5 . . ? C41 C42 C43 106.5(9) . . ? C41 C42 H42A 110.4 . . ? C43 C42 H42A 110.4 . . ? C41 C42 H42B 110.4 . . ? C43 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C42 C43 C44 105.0(8) . . ? C42 C43 H43A 110.7 . . ? C44 C43 H43A 110.7 . . ? C42 C43 H43B 110.7 . . ? C44 C43 H43B 110.7 . . ? H43A C43 H43B 108.8 . . ? C45 C44 C43 105.0(8) . . ? C45 C44 H44A 110.7 . . ? C43 C44 H44A 110.7 . . ? C45 C44 H44B 110.7 . . ? C43 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? C44 C45 C41 103.4(9) . . ? C44 C45 H45A 111.1 . . ? C41 C45 H45A 111.1 . . ? C44 C45 H45B 111.1 . . ? C41 C45 H45B 111.1 . . ? H45A C45 H45B 109.0 . . ? C52 C51 C55 104.6(7) . . ? C52 C51 Si15 112.5(5) . . ? C55 C51 Si15 113.4(6) . . ? C52 C51 H51 108.8 . . ? C55 C51 H51 108.8 . . ? Si15 C51 H51 108.8 . . ? C53 C52 C51 106.1(7) . . ? C53 C52 H52A 110.5 . . ? C51 C52 H52A 110.5 . . ? C53 C52 H52B 110.5 . . ? C51 C52 H52B 110.5 . . ? H52A C52 H52B 108.7 . . ? C54 C53 C52 109.7(9) . . ? C54 C53 H53A 109.7 . . ? C52 C53 H53A 109.7 . . ? C54 C53 H53B 109.7 . . ? C52 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C53 C54 C55 109.5(9) . . ? C53 C54 H54A 109.8 . . ? C55 C54 H54A 109.8 . . ? C53 C54 H54B 109.8 . . ? C55 C54 H54B 109.8 . . ? H54A C54 H54B 108.2 . . ? C54 C55 C51 103.3(8) . . ? C54 C55 H55A 111.1 . . ? C51 C55 H55A 111.1 . . ? C54 C55 H55B 111.1 . . ? C51 C55 H55B 111.1 . . ? H55A C55 H55B 109.1 . . ? C62 C61 C65 100.9(8) . . ? C62 C61 Si16 117.5(7) . . ? C65 C61 Si16 115.0(6) . . ? C62 C61 H61 107.6 . . ? C65 C61 H61 107.6 . . ? Si16 C61 H61 107.6 . . ? C63 C62 C61 103.7(9) . . ? C63 C62 H62A 111.0 . . ? C61 C62 H62A 111.0 . . ? C63 C62 H62B 111.0 . . ? C61 C62 H62B 111.0 . . ? H62A C62 H62B 109.0 . . ? C62 C63 C64 109.2(9) . . ? C62 C63 H63A 109.8 . . ? C64 C63 H63A 109.8 . . ? C62 C63 H63B 109.8 . . ? C64 C63 H63B 109.8 . . ? H63A C63 H63B 108.3 . . ? C65 C64 C63 103.8(8) . . ? C65 C64 H64A 111.0 . . ? C63 C64 H64A 111.0 . . ? C65 C64 H64B 111.0 . . ? C63 C64 H64B 111.0 . . ? H64A C64 H64B 109.0 . . ? C64 C65 C61 106.9(8) . . ? C64 C65 H65A 110.3 . . ? C61 C65 H65A 110.3 . . ? C64 C65 H65B 110.3 . . ? C61 C65 H65B 110.3 . . ? H65A C65 H65B 108.6 . . ? C72 C71 C75 104.0(7) . . ? C72 C71 Si17 114.0(6) . . ? C75 C71 Si17 115.4(6) . . ? C72 C71 H71 107.7 . . ? C75 C71 H71 107.7 . . ? Si17 C71 H71 107.7 . . ? C73 C72 C71 106.4(8) . . ? C73 C72 H72A 110.5 . . ? C71 C72 H72A 110.5 . . ? C73 C72 H72B 110.5 . . ? C71 C72 H72B 110.5 . . ? H72A C72 H72B 108.6 . . ? C74 C73 C72 103.1(9) . . ? C74 C73 H73A 111.1 . . ? C72 C73 H73A 111.1 . . ? C74 C73 H73B 111.1 . . ? C72 C73 H73B 111.1 . . ? H73A C73 H73B 109.1 . . ? C73 C74 C75 110.1(9) . . ? C73 C74 H74A 109.6 . . ? C75 C74 H74A 109.6 . . ? C73 C74 H74B 109.6 . . ? C75 C74 H74B 109.6 . . ? H74A C74 H74B 108.2 . . ? C74 C75 C71 105.7(9) . . ? C74 C75 H75A 110.6 . . ? C71 C75 H75A 110.6 . . ? C74 C75 H75B 110.6 . . ? C71 C75 H75B 110.6 . . ? H75A C75 H75B 108.7 . . ? C82 C81 C85 104.9(7) . . ? C82 C81 Si18 113.6(6) . . ? C85 C81 Si18 115.5(6) . . ? C82 C81 H81 107.5 . . ? C85 C81 H81 107.5 . . ? Si18 C81 H81 107.5 . . ? C83 C82 C81 105.6(8) . . ? C83 C82 H82A 110.6 . . ? C81 C82 H82A 110.6 . . ? C83 C82 H82B 110.6 . . ? C81 C82 H82B 110.6 . . ? H82A C82 H82B 108.7 . . ? C84 C83 C82 107.0(9) . . ? C84 C83 H83A 110.3 . . ? C82 C83 H83A 110.3 . . ? C84 C83 H83B 110.3 . . ? C82 C83 H83B 110.3 . . ? H83A C83 H83B 108.6 . . ? C83 C84 C85 110.5(9) . . ? C83 C84 H84A 109.5 . . ? C85 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? C85 C84 H84B 109.5 . . ? H84A C84 H84B 108.1 . . ? C84 C85 C81 104.1(8) . . ? C84 C85 H85A 110.9 . . ? C81 C85 H85A 110.9 . . ? C84 C85 H85B 110.9 . . ? C81 C85 H85B 110.9 . . ? H85A C85 H85B 108.9 . . ? C91 C90 C102 101.2(7) . . ? C91 C90 C1 119.9(7) . . ? C102 C90 C1 119.7(7) . . ? C91 C90 Sn11 102.8(5) . . ? C102 C90 Sn11 102.2(5) . . ? C1 C90 Sn11 108.5(5) . . ? C92 C91 C96 123.5(9) . . ? C92 C91 C90 128.3(9) . . ? C96 C91 C90 108.1(8) . . ? C91 C92 C93 117.3(11) . . ? C91 C92 H92 121.3 . . ? C93 C92 H92 121.3 . . ? C94 C93 C92 117.5(12) . . ? C94 C93 H93 121.3 . . ? C92 C93 H93 121.3 . . ? C95 C94 C93 125.1(12) . . ? C95 C94 H94 117.4 . . ? C93 C94 H94 117.4 . . ? C94 C95 C96 118.2(13) . . ? C94 C95 H95 120.9 . . ? C96 C95 H95 120.9 . . ? C95 C96 C91 118.3(11) . . ? C95 C96 C97 129.9(11) . . ? C91 C96 C97 111.8(8) . . ? C102 C97 C98 123.4(11) . . ? C102 C97 C96 105.3(9) . . ? C98 C97 C96 131.3(11) . . ? C99 C98 C97 114.9(13) . . ? C99 C98 H98 122.6 . . ? C97 C98 H98 122.6 . . ? C98 C99 C100 124.4(15) . . ? C98 C99 H99 117.8 . . ? C100 C99 H99 117.8 . . ? C99 C100 C101 119.6(14) . . ? C99 C100 H100 120.2 . . ? C101 C100 H100 120.2 . . ? C102 C101 C100 119.1(12) . . ? C102 C101 H101 120.5 . . ? C100 C101 H101 120.5 . . ? C97 C102 C101 118.6(9) . . ? C97 C102 C90 113.0(9) . . ? C101 C102 C90 128.2(8) . . ? C6 Sn21 C8 109.0(4) . . ? C6 Sn21 C7 112.2(4) . . ? C8 Sn21 C7 111.5(4) . . ? C6 Sn21 C290 109.1(3) . . ? C8 Sn21 C290 107.6(3) . . ? C7 Sn21 C290 107.3(3) . . ? O211 Si21 O214 109.1(3) . . ? O211 Si21 O220 109.3(3) . . ? O214 Si21 O220 109.7(3) . . ? O211 Si21 C5 110.4(3) . . ? O214 Si21 C5 112.2(3) . . ? O220 Si21 C5 106.1(3) . . ? O212 Si22 O221 108.8(3) . . ? O212 Si22 O211 109.2(3) . . ? O221 Si22 O211 109.0(3) . . ? O212 Si22 C221 109.3(3) . . ? O221 Si22 C221 108.3(3) . . ? O211 Si22 C221 112.2(3) . . ? O222 Si23 O213 109.4(3) . . ? O222 Si23 O212 108.6(3) . . ? O213 Si23 O212 108.4(3) . . ? O222 Si23 C231 108.5(3) . . ? O213 Si23 C231 111.7(3) . . ? O212 Si23 C231 110.2(3) . . ? O213 Si24 O219 109.0(4) . . ? O213 Si24 O214 109.2(3) . . ? O219 Si24 O214 108.3(3) . . ? O213 Si24 C241 109.4(3) . . ? O219 Si24 C241 110.8(4) . . ? O214 Si24 C241 110.1(3) . . ? O219 Si25 O215 108.8(3) . . ? O219 Si25 O218 109.4(3) . . ? O215 Si25 O218 107.7(3) . . ? O219 Si25 C251 109.9(3) . . ? O215 Si25 C251 112.0(4) . . ? O218 Si25 C251 109.0(3) . . ? O220 Si26 O215 108.6(3) . . ? O220 Si26 O216 108.6(3) . . ? O215 Si26 O216 110.0(3) . . ? O220 Si26 C261 111.7(3) . . ? O215 Si26 C261 110.1(4) . . ? O216 Si26 C261 107.9(3) . . ? O221 Si27 O216 110.1(3) . . ? O221 Si27 O217 108.7(3) . . ? O216 Si27 O217 108.7(3) . . ? O221 Si27 C271 109.4(3) . . ? O216 Si27 C271 110.8(3) . . ? O217 Si27 C271 109.0(3) . . ? O218 Si28 O222 108.9(3) . . ? O218 Si28 O217 109.4(3) . . ? O222 Si28 O217 109.0(3) . . ? O218 Si28 C281 110.3(3) . . ? O222 Si28 C281 110.2(3) . . ? O217 Si28 C281 109.0(3) . . ? Si21 O211 Si22 146.0(3) . . ? Si22 O212 Si23 146.5(4) . . ? Si24 O213 Si23 146.6(4) . . ? Si21 O214 Si24 148.4(4) . . ? Si26 O215 Si25 148.6(4) . . ? Si27 O216 Si26 146.7(4) . . ? Si27 O217 Si28 145.6(4) . . ? Si28 O218 Si25 147.5(4) . . ? Si25 O219 Si24 152.7(4) . . ? Si26 O220 Si21 151.5(4) . . ? Si27 O221 Si22 153.1(4) . . ? Si28 O222 Si23 154.3(4) . . ? C290 C5 Si21 119.0(5) . . ? C290 C5 H5A 107.6 . . ? Si21 C5 H5A 107.6 . . ? C290 C5 H5B 107.6 . . ? Si21 C5 H5B 107.6 . . ? H5A C5 H5B 107.0 . . ? Sn21 C6 H6A 109.5 . . ? Sn21 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Sn21 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Sn21 C7 H7A 109.5 . . ? Sn21 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Sn21 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Sn21 C8 H8A 109.5 . . ? Sn21 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Sn21 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C225 C221 C222 104.2(6) . . ? C225 C221 Si22 113.0(5) . . ? C222 C221 Si22 113.8(5) . . ? C225 C221 H221 108.6 . . ? C222 C221 H221 108.6 . . ? Si22 C221 H221 108.6 . . ? C223 C222 C221 102.6(7) . . ? C223 C222 H22C 111.2 . . ? C221 C222 H22C 111.2 . . ? C223 C222 H22D 111.2 . . ? C221 C222 H22D 111.2 . . ? H22C C222 H22D 109.2 . . ? C224 C223 C222 106.9(9) . . ? C224 C223 H22E 110.3 . . ? C222 C223 H22E 110.3 . . ? C224 C223 H22F 110.3 . . ? C222 C223 H22F 110.3 . . ? H22E C223 H22F 108.6 . . ? C223 C224 C225 107.3(8) . . ? C223 C224 H22G 110.3 . . ? C225 C224 H22G 110.3 . . ? C223 C224 H22H 110.3 . . ? C225 C224 H22H 110.3 . . ? H22G C224 H22H 108.5 . . ? C224 C225 C221 108.5(7) . . ? C224 C225 H22I 110.0 . . ? C221 C225 H22I 110.0 . . ? C224 C225 H22J 110.0 . . ? C221 C225 H22J 110.0 . . ? H22I C225 H22J 108.4 . . ? C232 C231 C235 104.1(6) . . ? C232 C231 Si23 112.7(5) . . ? C235 C231 Si23 113.2(5) . . ? C232 C231 H231 108.9 . . ? C235 C231 H231 108.9 . . ? Si23 C231 H231 108.9 . . ? C233 C232 C231 106.2(6) . . ? C233 C232 H23C 110.5 . . ? C231 C232 H23C 110.5 . . ? C233 C232 H23D 110.5 . . ? C231 C232 H23D 110.5 . . ? H23C C232 H23D 108.7 . . ? C234 C233 C232 107.8(7) . . ? C234 C233 H23E 110.1 . . ? C232 C233 H23E 110.1 . . ? C234 C233 H23F 110.1 . . ? C232 C233 H23F 110.1 . . ? H23E C233 H23F 108.5 . . ? C233 C234 C235 104.8(7) . . ? C233 C234 H23G 110.8 . . ? C235 C234 H23G 110.8 . . ? C233 C234 H23H 110.8 . . ? C235 C234 H23H 110.8 . . ? H23G C234 H23H 108.9 . . ? C234 C235 C231 104.0(7) . . ? C234 C235 H23I 111.0 . . ? C231 C235 H23I 111.0 . . ? C234 C235 H23J 111.0 . . ? C231 C235 H23J 111.0 . . ? H23I C235 H23J 109.0 . . ? C242 C241 C245 104.9(10) . . ? C242 C241 Si24 122.7(9) . . ? C245 C241 Si24 117.8(8) . . ? C242 C241 H241 102.9 . . ? C245 C241 H241 102.9 . . ? Si24 C241 H241 102.9 . . ? C241 C242 C243 106.3(13) . . ? C241 C242 H24C 110.5 . . ? C243 C242 H24C 110.5 . . ? C241 C242 H24D 110.5 . . ? C243 C242 H24D 110.5 . . ? H24C C242 H24D 108.7 . . ? C244 C243 C242 103.8(13) . . ? C244 C243 H24E 111.0 . . ? C242 C243 H24E 111.0 . . ? C244 C243 H24F 111.0 . . ? C242 C243 H24F 111.0 . . ? H24E C243 H24F 109.0 . . ? C245 C244 C243 105.9(11) . . ? C245 C244 H24G 110.6 . . ? C243 C244 H24G 110.6 . . ? C245 C244 H24H 110.6 . . ? C243 C244 H24H 110.6 . . ? H24G C244 H24H 108.7 . . ? C244 C245 C241 107.6(12) . . ? C244 C245 H24I 110.2 . . ? C241 C245 H24I 110.2 . . ? C244 C245 H24J 110.2 . . ? C241 C245 H24J 110.2 . . ? H24I C245 H24J 108.5 . . ? C252 C251 C255 104.8(7) . . ? C252 C251 Si25 112.7(6) . . ? C255 C251 Si25 112.0(6) . . ? C252 C251 H251 109.1 . . ? C255 C251 H251 109.1 . . ? Si25 C251 H251 109.1 . . ? C253 C252 C251 106.4(9) . . ? C253 C252 H25C 110.5 . . ? C251 C252 H25C 110.5 . . ? C253 C252 H25D 110.5 . . ? C251 C252 H25D 110.5 . . ? H25C C252 H25D 108.6 . . ? C254 C253 C252 111.4(10) . . ? C254 C253 H25E 109.3 . . ? C252 C253 H25E 109.3 . . ? C254 C253 H25F 109.3 . . ? C252 C253 H25F 109.3 . . ? H25E C253 H25F 108.0 . . ? C253 C254 C255 109.8(10) . . ? C253 C254 H25G 109.7 . . ? C255 C254 H25G 109.7 . . ? C253 C254 H25H 109.7 . . ? C255 C254 H25H 109.7 . . ? H25G C254 H25H 108.2 . . ? C254 C255 C251 106.7(9) . . ? C254 C255 H25I 110.4 . . ? C251 C255 H25I 110.4 . . ? C254 C255 H25J 110.4 . . ? C251 C255 H25J 110.4 . . ? H25I C255 H25J 108.6 . . ? C265 C261 C262 102.9(10) . . ? C265 C261 Si26 113.0(6) . . ? C262 C261 Si26 116.9(8) . . ? C265 C261 H261 107.9 . . ? C262 C261 H261 107.9 . . ? Si26 C261 H261 107.9 . . ? C263 C262 C261 104.7(12) . . ? C263 C262 H26A 110.8 . . ? C261 C262 H26A 110.8 . . ? C263 C262 H26B 110.8 . . ? C261 C262 H26B 110.8 . . ? H26A C262 H26B 108.9 . . ? C262 C263 C264 109.6(14) . . ? C262 C263 H26C 109.8 . . ? C264 C263 H26C 109.8 . . ? C262 C263 H26D 109.8 . . ? C264 C263 H26D 109.8 . . ? H26C C263 H26D 108.2 . . ? C265 C264 C263 99.4(15) . . ? C265 C264 H26E 111.9 . . ? C263 C264 H26E 111.9 . . ? C265 C264 H26F 111.9 . . ? C263 C264 H26F 111.9 . . ? H26E C264 H26F 109.6 . . ? C264 C265 C261 106.5(10) . . ? C264 C265 H26G 110.4 . . ? C261 C265 H26G 110.4 . . ? C264 C265 H26H 110.4 . . ? C261 C265 H26H 110.4 . . ? H26G C265 H26H 108.6 . . ? C275 C271 C272 104.5(7) . . ? C275 C271 Si27 115.7(6) . . ? C272 C271 Si27 112.0(5) . . ? C275 C271 H271 108.1 . . ? C272 C271 H271 108.1 . . ? Si27 C271 H271 108.1 . . ? C273 C272 C271 107.3(8) . . ? C273 C272 H27A 110.2 . . ? C271 C272 H27A 110.2 . . ? C273 C272 H27B 110.2 . . ? C271 C272 H27B 110.2 . . ? H27A C272 H27B 108.5 . . ? C274 C273 C272 106.9(9) . . ? C274 C273 H27C 110.3 . . ? C272 C273 H27C 110.3 . . ? C274 C273 H27D 110.3 . . ? C272 C273 H27D 110.3 . . ? H27C C273 H27D 108.6 . . ? C273 C274 C275 109.6(9) . . ? C273 C274 H27E 109.8 . . ? C275 C274 H27E 109.8 . . ? C273 C274 H27F 109.8 . . ? C275 C274 H27F 109.8 . . ? H27E C274 H27F 108.2 . . ? C274 C275 C271 107.0(8) . . ? C274 C275 H27G 110.3 . . ? C271 C275 H27G 110.3 . . ? C274 C275 H27H 110.3 . . ? C271 C275 H27H 110.3 . . ? H27G C275 H27H 108.6 . . ? C282 C281 C285 103.9(6) . . ? C282 C281 Si28 114.2(5) . . ? C285 C281 Si28 115.1(6) . . ? C282 C281 H281 107.8 . . ? C285 C281 H281 107.8 . . ? Si28 C281 H281 107.8 . . ? C283 C282 C281 104.6(6) . . ? C283 C282 H28A 110.8 . . ? C281 C282 H28A 110.8 . . ? C283 C282 H28B 110.8 . . ? C281 C282 H28B 110.8 . . ? H28A C282 H28B 108.9 . . ? C284 C283 C282 104.9(7) . . ? C284 C283 H28C 110.8 . . ? C282 C283 H28C 110.8 . . ? C284 C283 H28D 110.8 . . ? C282 C283 H28D 110.8 . . ? H28C C283 H28D 108.8 . . ? C283 C284 C285 108.1(7) . . ? C283 C284 H28E 110.1 . . ? C285 C284 H28E 110.1 . . ? C283 C284 H28F 110.1 . . ? C285 C284 H28F 110.1 . . ? H28E C284 H28F 108.4 . . ? C284 C285 C281 106.1(7) . . ? C284 C285 H28G 110.5 . . ? C281 C285 H28G 110.5 . . ? C284 C285 H28H 110.5 . . ? C281 C285 H28H 110.5 . . ? H28G C285 H28H 108.7 . . ? C302 C290 C291 102.7(5) . . ? C302 C290 C5 120.2(6) . . ? C291 C290 C5 119.6(6) . . ? C302 C290 Sn21 101.4(4) . . ? C291 C290 Sn21 102.4(4) . . ? C5 C290 Sn21 107.7(4) . . ? C292 C291 C296 121.5(7) . . ? C292 C291 C290 128.1(7) . . ? C296 C291 C290 110.4(7) . . ? C291 C292 C293 118.0(9) . . ? C291 C292 H292 121.0 . . ? C293 C292 H292 121.0 . . ? C294 C293 C292 119.0(9) . . ? C294 C293 H293 120.5 . . ? C292 C293 H293 120.5 . . ? C295 C294 C293 123.8(9) . . ? C295 C294 H294 118.1 . . ? C293 C294 H294 118.1 . . ? C294 C295 C296 117.9(9) . . ? C294 C295 H295 121.1 . . ? C296 C295 H295 121.1 . . ? C291 C296 C295 119.7(8) . . ? C291 C296 C297 108.5(6) . . ? C295 C296 C297 131.7(8) . . ? C298 C297 C302 121.2(8) . . ? C298 C297 C296 130.5(8) . . ? C302 C297 C296 108.3(7) . . ? C299 C298 C297 117.8(9) . . ? C299 C298 H298 121.1 . . ? C297 C298 H298 121.1 . . ? C298 C299 C300 122.7(10) . . ? C298 C299 H299 118.7 . . ? C300 C299 H299 118.7 . . ? C301 C300 C299 119.1(9) . . ? C301 C300 H300 120.4 . . ? C299 C300 H300 120.4 . . ? C302 C301 C300 118.9(9) . . ? C302 C301 H301 120.6 . . ? C300 C301 H301 120.6 . . ? C301 C302 C297 120.1(7) . . ? C301 C302 C290 130.4(7) . . ? C297 C302 C290 109.4(6) . . ? C247 C246 H24K 110.5 . . ? C247 C246 H24L 110.5 . . ? H24K C246 H24L 108.7 . . ? C246 C247 H24M 110.6 . . ? C246 C247 H24N 110.6 . . ? H24M C247 H24N 108.8 . . ? H24Q C249 H24R 110.1 . . ? C401 C400 H40A 109.5 . . ? C401 C400 H40B 109.5 . . ? H40A C400 H40B 109.5 . . ? C401 C400 H40C 109.5 . . ? H40A C400 H40C 109.5 . . ? H40B C400 H40C 109.5 . . ? C402 C401 C400 115(4) . . ? C402 C401 H40D 108.6 . . ? C400 C401 H40D 108.6 . . ? C402 C401 H40E 108.6 . . ? C400 C401 H40E 108.6 . . ? H40D C401 H40E 107.5 . . ? C401 C402 C403 116(4) . . ? C401 C402 H40F 108.4 . . ? C403 C402 H40F 108.4 . . ? C401 C402 H40G 108.4 . . ? C403 C402 H40G 108.4 . . ? H40F C402 H40G 107.5 . . ? C402 C403 C404 108(3) . . ? C402 C403 H40H 110.1 . . ? C404 C403 H40H 110.1 . . ? C402 C403 H40I 110.1 . . ? C404 C403 H40I 110.1 . . ? H40H C403 H40I 108.4 . . ? 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 O14 Si11 O11 Si12 -55.8(8) . . . . ? O20 Si11 O11 Si12 63.7(8) . . . . ? C1 Si11 O11 Si12 -179.9(7) . . . . ? O21 Si12 O11 Si11 -64.9(8) . . . . ? O12 Si12 O11 Si11 54.4(8) . . . . ? C21 Si12 O11 Si11 173.0(7) . . . . ? O22 Si13 O12 Si12 -56.8(10) . . . . ? O13 Si13 O12 Si12 61.6(10) . . . . ? C31 Si13 O12 Si12 -175.8(8) . . . . ? O21 Si12 O12 Si13 56.8(10) . . . . ? O11 Si12 O12 Si13 -61.6(10) . . . . ? C21 Si12 O12 Si13 175.6(9) . . . . ? O14 Si14 O13 Si13 55.5(9) . . . . ? O19 Si14 O13 Si13 -63.4(9) . . . . ? C41 Si14 O13 Si13 177.0(8) . . . . ? O12 Si13 O13 Si14 -54.8(10) . . . . ? O22 Si13 O13 Si14 62.6(9) . . . . ? C31 Si13 O13 Si14 -178.9(8) . . . . ? O11 Si11 O14 Si14 61.1(9) . . . . ? O20 Si11 O14 Si14 -59.1(9) . . . . ? C1 Si11 O14 Si14 -175.6(8) . . . . ? O13 Si14 O14 Si11 -60.4(9) . . . . ? O19 Si14 O14 Si11 58.2(9) . . . . ? C41 Si14 O14 Si11 -179.5(8) . . . . ? O20 Si16 O15 Si15 62.6(8) . . . . ? O16 Si16 O15 Si15 -55.3(8) . . . . ? C61 Si16 O15 Si15 -175.0(7) . . . . ? O19 Si15 O15 Si16 -63.9(8) . . . . ? O18 Si15 O15 Si16 56.0(8) . . . . ? C51 Si15 O15 Si16 174.8(7) . . . . ? O17 Si17 O16 Si16 -60.1(10) . . . . ? O21 Si17 O16 Si16 58.6(10) . . . . ? C71 Si17 O16 Si16 -178.4(9) . . . . ? O15 Si16 O16 Si17 59.4(10) . . . . ? O20 Si16 O16 Si17 -59.5(10) . . . . ? C61 Si16 O16 Si17 178.8(9) . . . . ? O16 Si17 O17 Si18 59.3(9) . . . . ? O21 Si17 O17 Si18 -60.4(9) . . . . ? C71 Si17 O17 Si18 176.9(8) . . . . ? O22 Si18 O17 Si17 59.1(9) . . . . ? O18 Si18 O17 Si17 -59.3(9) . . . . ? C81 Si18 O17 Si17 -178.8(8) . . . . ? O22 Si18 O18 Si15 -58.5(10) . . . . ? O17 Si18 O18 Si15 61.8(10) . . . . ? C81 Si18 O18 Si15 -179.1(9) . . . . ? O19 Si15 O18 Si18 56.9(10) . . . . ? O15 Si15 O18 Si18 -61.8(10) . . . . ? C51 Si15 O18 Si18 177.9(9) . . . . ? O18 Si15 O19 Si14 -54.6(8) . . . . ? O15 Si15 O19 Si14 64.5(8) . . . . ? C51 Si15 O19 Si14 -174.2(7) . . . . ? O13 Si14 O19 Si15 57.6(8) . . . . ? O14 Si14 O19 Si15 -61.8(8) . . . . ? C41 Si14 O19 Si15 175.3(7) . . . . ? O15 Si16 O20 Si11 -61.9(8) . . . . ? O16 Si16 O20 Si11 57.2(8) . . . . ? C61 Si16 O20 Si11 177.5(7) . . . . ? O11 Si11 O20 Si16 -58.6(8) . . . . ? O14 Si11 O20 Si16 61.2(8) . . . . ? C1 Si11 O20 Si16 -178.2(7) . . . . ? O12 Si12 O21 Si17 -60.0(9) . . . . ? O11 Si12 O21 Si17 58.7(9) . . . . ? C21 Si12 O21 Si17 -176.9(8) . . . . ? O16 Si17 O21 Si12 -55.6(9) . . . . ? O17 Si17 O21 Si12 63.1(9) . . . . ? C71 Si17 O21 Si12 -176.1(8) . . . . ? O18 Si18 O22 Si13 58.7(9) . . . . ? O17 Si18 O22 Si13 -59.7(9) . . . . ? C81 Si18 O22 Si13 178.9(8) . . . . ? O12 Si13 O22 Si18 58.3(9) . . . . ? O13 Si13 O22 Si18 -59.1(9) . . . . ? C31 Si13 O22 Si18 -179.4(7) . . . . ? O11 Si11 C1 C90 61.3(7) . . . . ? O14 Si11 C1 C90 -61.2(7) . . . . ? O20 Si11 C1 C90 -179.6(6) . . . . ? O21 Si12 C21 C25 -46.5(7) . . . . ? O12 Si12 C21 C25 -165.3(6) . . . . ? O11 Si12 C21 C25 74.9(7) . . . . ? O21 Si12 C21 C22 72.4(6) . . . . ? O12 Si12 C21 C22 -46.5(7) . . . . ? O11 Si12 C21 C22 -166.3(5) . . . . ? C25 C21 C22 C23 -25.4(10) . . . . ? Si12 C21 C22 C23 -153.0(7) . . . . ? C21 C22 C23 C24 2.5(12) . . . . ? C22 C23 C24 C25 22.4(13) . . . . ? C23 C24 C25 C21 -38.6(11) . . . . ? C22 C21 C25 C24 38.9(9) . . . . ? Si12 C21 C25 C24 162.5(6) . . . . ? O12 Si13 C31 C35 -180.0(6) . . . . ? O22 Si13 C31 C35 60.8(7) . . . . ? O13 Si13 C31 C35 -58.8(7) . . . . ? O12 Si13 C31 C32 62.3(7) . . . . ? O22 Si13 C31 C32 -57.0(6) . . . . ? O13 Si13 C31 C32 -176.6(6) . . . . ? C35 C31 C32 C33 2.4(11) . . . . ? Si13 C31 C32 C33 123.5(9) . . . . ? C31 C32 C33 C34 16.4(16) . . . . ? C32 C33 C34 C35 -29.9(18) . . . . ? C33 C34 C35 C31 30.5(16) . . . . ? C32 C31 C35 C34 -19.9(12) . . . . ? Si13 C31 C35 C34 -142.2(9) . . . . ? O13 Si14 C41 C42 50.0(9) . . . . ? O14 Si14 C41 C42 170.4(8) . . . . ? O19 Si14 C41 C42 -68.2(9) . . . . ? O13 Si14 C41 C45 166.2(7) . . . . ? O14 Si14 C41 C45 -73.4(8) . . . . ? O19 Si14 C41 C45 48.0(8) . . . . ? C45 C41 C42 C43 37.5(13) . . . . ? Si14 C41 C42 C43 163.2(9) . . . . ? C41 C42 C43 C44 -16.5(15) . . . . ? C42 C43 C44 C45 -11.4(15) . . . . ? C43 C44 C45 C41 35.0(12) . . . . ? C42 C41 C45 C44 -44.3(11) . . . . ? Si14 C41 C45 C44 -167.4(7) . . . . ? O19 Si15 C51 C52 -179.6(6) . . . . ? O18 Si15 C51 C52 59.6(7) . . . . ? O15 Si15 C51 C52 -59.7(7) . . . . ? O19 Si15 C51 C55 62.1(7) . . . . ? O18 Si15 C51 C55 -58.8(7) . . . . ? O15 Si15 C51 C55 -178.0(6) . . . . ? C55 C51 C52 C53 -18.0(11) . . . . ? Si15 C51 C52 C53 -141.4(9) . . . . ? C51 C52 C53 C54 3.2(16) . . . . ? C52 C53 C54 C55 14.0(18) . . . . ? C53 C54 C55 C51 -24.7(16) . . . . ? C52 C51 C55 C54 25.5(11) . . . . ? Si15 C51 C55 C54 148.3(9) . . . . ? O15 Si16 C61 C62 177.8(8) . . . . ? O20 Si16 C61 C62 -61.4(9) . . . . ? O16 Si16 C61 C62 57.9(9) . . . . ? O15 Si16 C61 C65 59.2(8) . . . . ? O20 Si16 C61 C65 180.0(7) . . . . ? O16 Si16 C61 C65 -60.7(8) . . . . ? C65 C61 C62 C63 -37.5(13) . . . . ? Si16 C61 C62 C63 -163.4(9) . . . . ? C61 C62 C63 C64 25.9(16) . . . . ? C62 C63 C64 C65 -2.7(17) . . . . ? C63 C64 C65 C61 -21.6(14) . . . . ? C62 C61 C65 C64 37.1(12) . . . . ? Si16 C61 C65 C64 164.6(8) . . . . ? O16 Si17 C71 C72 61.5(8) . . . . ? O17 Si17 C71 C72 -56.4(8) . . . . ? O21 Si17 C71 C72 -176.8(7) . . . . ? O16 Si17 C71 C75 -178.1(6) . . . . ? O17 Si17 C71 C75 64.0(7) . . . . ? O21 Si17 C71 C75 -56.4(7) . . . . ? C75 C71 C72 C73 24.9(11) . . . . ? Si17 C71 C72 C73 151.4(7) . . . . ? C71 C72 C73 C74 -33.1(13) . . . . ? C72 C73 C74 C75 29.0(16) . . . . ? C73 C74 C75 C71 -13.8(16) . . . . ? C72 C71 C75 C74 -7.3(12) . . . . ? Si17 C71 C75 C74 -133.0(10) . . . . ? O22 Si18 C81 C82 -177.6(7) . . . . ? O18 Si18 C81 C82 -58.5(8) . . . . ? O17 Si18 C81 C82 60.0(8) . . . . ? O22 Si18 C81 C85 -56.2(9) . . . . ? O18 Si18 C81 C85 62.9(9) . . . . ? O17 Si18 C81 C85 -178.7(7) . . . . ? C85 C81 C82 C83 28.3(13) . . . . ? Si18 C81 C82 C83 155.4(9) . . . . ? C81 C82 C83 C84 -24.3(17) . . . . ? C82 C83 C84 C85 11(2) . . . . ? C83 C84 C85 C81 6.9(19) . . . . ? C82 C81 C85 C84 -21.4(14) . . . . ? Si18 C81 C85 C84 -147.4(11) . . . . ? Si11 C1 C90 C91 65.0(9) . . . . ? Si11 C1 C90 C102 -60.9(9) . . . . ? Si11 C1 C90 Sn11 -177.5(4) . . . . ? C4 Sn11 C90 C91 71.4(7) . . . . ? C2 Sn11 C90 C91 -173.4(6) . . . . ? C3 Sn11 C90 C91 -57.0(7) . . . . ? C4 Sn11 C90 C102 176.0(6) . . . . ? C2 Sn11 C90 C102 -68.8(6) . . . . ? C3 Sn11 C90 C102 47.6(6) . . . . ? C4 Sn11 C90 C1 -56.6(7) . . . . ? C2 Sn11 C90 C1 58.6(6) . . . . ? C3 Sn11 C90 C1 175.0(5) . . . . ? C102 C90 C91 C92 174.1(9) . . . . ? C1 C90 C91 C92 39.9(13) . . . . ? Sn11 C90 C91 C92 -80.4(10) . . . . ? C102 C90 C91 C96 -7.1(9) . . . . ? C1 C90 C91 C96 -141.3(7) . . . . ? Sn11 C90 C91 C96 98.4(7) . . . . ? C96 C91 C92 C93 1.2(15) . . . . ? C90 C91 C92 C93 179.9(9) . . . . ? C91 C92 C93 C94 -3.5(16) . . . . ? C92 C93 C94 C95 3(2) . . . . ? C93 C94 C95 C96 0(2) . . . . ? C94 C95 C96 C91 -2.4(17) . . . . ? C94 C95 C96 C97 175.7(12) . . . . ? C92 C91 C96 C95 1.8(15) . . . . ? C90 C91 C96 C95 -177.1(9) . . . . ? C92 C91 C96 C97 -176.7(9) . . . . ? C90 C91 C96 C97 4.5(11) . . . . ? C95 C96 C97 C102 -177.6(10) . . . . ? C91 C96 C97 C102 0.6(11) . . . . ? C95 C96 C97 C98 1(2) . . . . ? C91 C96 C97 C98 179.6(11) . . . . ? C102 C97 C98 C99 0.2(17) . . . . ? C96 C97 C98 C99 -178.7(12) . . . . ? C97 C98 C99 C100 3(2) . . . . ? C98 C99 C100 C101 -5(2) . . . . ? C99 C100 C101 C102 4.4(17) . . . . ? C98 C97 C102 C101 -0.8(15) . . . . ? C96 C97 C102 C101 178.3(8) . . . . ? C98 C97 C102 C90 175.4(9) . . . . ? C96 C97 C102 C90 -5.6(11) . . . . ? C100 C101 C102 C97 -1.5(14) . . . . ? C100 C101 C102 C90 -177.0(9) . . . . ? C91 C90 C102 C97 7.9(9) . . . . ? C1 C90 C102 C97 142.2(8) . . . . ? Sn11 C90 C102 C97 -98.0(8) . . . . ? C91 C90 C102 C101 -176.4(9) . . . . ? C1 C90 C102 C101 -42.1(12) . . . . ? Sn11 C90 C102 C101 77.7(9) . . . . ? O214 Si21 O211 Si22 -54.1(7) . . . . ? O220 Si21 O211 Si22 65.8(7) . . . . ? C5 Si21 O211 Si22 -177.9(6) . . . . ? O212 Si22 O211 Si21 54.6(7) . . . . ? O221 Si22 O211 Si21 -64.1(7) . . . . ? C221 Si22 O211 Si21 175.9(6) . . . . ? O221 Si22 O212 Si23 46.1(8) . . . . ? O211 Si22 O212 Si23 -72.8(8) . . . . ? C221 Si22 O212 Si23 164.2(7) . . . . ? O222 Si23 O212 Si22 -45.2(8) . . . . ? O213 Si23 O212 Si22 73.5(8) . . . . ? C231 Si23 O212 Si22 -164.0(7) . . . . ? O219 Si24 O213 Si23 -63.7(9) . . . . ? O214 Si24 O213 Si23 54.5(9) . . . . ? C241 Si24 O213 Si23 175.0(8) . . . . ? O222 Si23 O213 Si24 61.9(9) . . . . ? O212 Si23 O213 Si24 -56.3(9) . . . . ? C231 Si23 O213 Si24 -177.9(8) . . . . ? O211 Si21 O214 Si24 70.9(7) . . . . ? O220 Si21 O214 Si24 -48.8(7) . . . . ? C5 Si21 O214 Si24 -166.5(6) . . . . ? O213 Si24 O214 Si21 -70.0(7) . . . . ? O219 Si24 O214 Si21 48.6(7) . . . . ? C241 Si24 O214 Si21 169.8(7) . . . . ? O220 Si26 O215 Si25 50.6(9) . . . . ? O216 Si26 O215 Si25 -68.1(9) . . . . ? C261 Si26 O215 Si25 173.1(8) . . . . ? O219 Si25 O215 Si26 -50.0(9) . . . . ? O218 Si25 O215 Si26 68.5(9) . . . . ? C251 Si25 O215 Si26 -171.7(8) . . . . ? O221 Si27 O216 Si26 62.9(8) . . . . ? O217 Si27 O216 Si26 -56.0(8) . . . . ? C271 Si27 O216 Si26 -175.9(6) . . . . ? O220 Si26 O216 Si27 -65.0(7) . . . . ? O215 Si26 O216 Si27 53.7(8) . . . . ? C261 Si26 O216 Si27 173.8(7) . . . . ? O221 Si27 O217 Si28 -48.0(8) . . . . ? O216 Si27 O217 Si28 71.8(7) . . . . ? C271 Si27 O217 Si28 -167.2(7) . . . . ? O218 Si28 O217 Si27 -71.5(8) . . . . ? O222 Si28 O217 Si27 47.5(8) . . . . ? C281 Si28 O217 Si27 167.8(7) . . . . ? O222 Si28 O218 Si25 -61.2(8) . . . . ? O217 Si28 O218 Si25 57.9(8) . . . . ? C281 Si28 O218 Si25 177.7(7) . . . . ? O219 Si25 O218 Si28 61.7(8) . . . . ? O215 Si25 O218 Si28 -56.4(8) . . . . ? C251 Si25 O218 Si28 -178.1(7) . . . . ? O215 Si25 O219 Si24 67.0(10) . . . . ? O218 Si25 O219 Si24 -50.5(10) . . . . ? C251 Si25 O219 Si24 -170.1(9) . . . . ? O213 Si24 O219 Si25 51.8(10) . . . . ? O214 Si24 O219 Si25 -66.9(10) . . . . ? C241 Si24 O219 Si25 172.3(9) . . . . ? O215 Si26 O220 Si21 -65.8(8) . . . . ? O216 Si26 O220 Si21 53.7(8) . . . . ? C261 Si26 O220 Si21 172.6(8) . . . . ? O211 Si21 O220 Si26 -54.1(8) . . . . ? O214 Si21 O220 Si26 65.5(8) . . . . ? C5 Si21 O220 Si26 -173.1(7) . . . . ? O216 Si27 O221 Si22 -46.1(9) . . . . ? O217 Si27 O221 Si22 72.9(9) . . . . ? C271 Si27 O221 Si22 -168.1(8) . . . . ? O212 Si22 O221 Si27 -72.3(9) . . . . ? O211 Si22 O221 Si27 46.7(9) . . . . ? C221 Si22 O221 Si27 169.0(8) . . . . ? O218 Si28 O222 Si23 47.9(10) . . . . ? O217 Si28 O222 Si23 -71.4(10) . . . . ? C281 Si28 O222 Si23 169.0(9) . . . . ? O213 Si23 O222 Si28 -47.8(10) . . . . ? O212 Si23 O222 Si28 70.3(10) . . . . ? C231 Si23 O222 Si28 -169.9(9) . . . . ? O211 Si21 C5 C290 73.1(6) . . . . ? O214 Si21 C5 C290 -48.8(7) . . . . ? O220 Si21 C5 C290 -168.6(5) . . . . ? O212 Si22 C221 C225 -53.5(6) . . . . ? O221 Si22 C221 C225 64.9(6) . . . . ? O211 Si22 C221 C225 -174.7(5) . . . . ? O212 Si22 C221 C222 -172.0(6) . . . . ? O221 Si22 C221 C222 -53.7(7) . . . . ? O211 Si22 C221 C222 66.7(7) . . . . ? C225 C221 C222 C223 29.4(10) . . . . ? Si22 C221 C222 C223 152.9(8) . . . . ? C221 C222 C223 C224 -32.1(15) . . . . ? C222 C223 C224 C225 22.1(18) . . . . ? C223 C224 C225 C221 -2.7(17) . . . . ? C222 C221 C225 C224 -17.3(12) . . . . ? Si22 C221 C225 C224 -141.2(10) . . . . ? O222 Si23 C231 C232 -59.3(6) . . . . ? O213 Si23 C231 C232 -180.0(5) . . . . ? O212 Si23 C231 C232 59.5(6) . . . . ? O222 Si23 C231 C235 58.6(7) . . . . ? O213 Si23 C231 C235 -62.1(7) . . . . ? O212 Si23 C231 C235 177.4(6) . . . . ? C235 C231 C232 C233 10.2(9) . . . . ? Si23 C231 C232 C233 133.3(7) . . . . ? C231 C232 C233 C234 12.4(11) . . . . ? C232 C233 C234 C235 -30.9(12) . . . . ? C233 C234 C235 C231 36.7(11) . . . . ? C232 C231 C235 C234 -28.6(9) . . . . ? Si23 C231 C235 C234 -151.4(7) . . . . ? O213 Si24 C241 C242 159.1(11) . . . . ? O219 Si24 C241 C242 38.8(12) . . . . ? O214 Si24 C241 C242 -81.0(12) . . . . ? O213 Si24 C241 C245 26.0(13) . . . . ? O219 Si24 C241 C245 -94.3(13) . . . . ? O214 Si24 C241 C245 145.9(12) . . . . ? C245 C241 C242 C243 -31.5(19) . . . . ? Si24 C241 C242 C243 -169.5(12) . . . . ? C241 C242 C243 C244 34(2) . . . . ? C242 C243 C244 C245 -23(2) . . . . ? C243 C244 C245 C241 4(2) . . . . ? C242 C241 C245 C244 17(2) . . . . ? Si24 C241 C245 C244 157.2(13) . . . . ? O219 Si25 C251 C252 177.6(7) . . . . ? O215 Si25 C251 C252 -61.4(8) . . . . ? O218 Si25 C251 C252 57.7(8) . . . . ? O219 Si25 C251 C255 59.6(7) . . . . ? O215 Si25 C251 C255 -179.3(6) . . . . ? O218 Si25 C251 C255 -60.3(7) . . . . ? C255 C251 C252 C253 -4.3(14) . . . . ? Si25 C251 C252 C253 -126.4(12) . . . . ? C251 C252 C253 C254 -1(2) . . . . ? C252 C253 C254 C255 7(3) . . . . ? C253 C254 C255 C251 -9(2) . . . . ? C252 C251 C255 C254 8.1(13) . . . . ? Si25 C251 C255 C254 130.6(11) . . . . ? O220 Si26 C261 C265 -174.1(9) . . . . ? O215 Si26 C261 C265 65.2(10) . . . . ? O216 Si26 C261 C265 -54.8(10) . . . . ? O220 Si26 C261 C262 66.8(11) . . . . ? O215 Si26 C261 C262 -53.9(11) . . . . ? O216 Si26 C261 C262 -174.0(10) . . . . ? C265 C261 C262 C263 15(3) . . . . ? Si26 C261 C262 C263 139(3) . . . . ? C261 C262 C263 C264 10(4) . . . . ? C262 C263 C264 C265 -32(4) . . . . ? C263 C264 C265 C261 41(3) . . . . ? C262 C261 C265 C264 -36(2) . . . . ? Si26 C261 C265 C264 -163.4(15) . . . . ? O221 Si27 C271 C275 -179.4(7) . . . . ? O216 Si27 C271 C275 59.0(8) . . . . ? O217 Si27 C271 C275 -60.6(8) . . . . ? O221 Si27 C271 C272 -59.8(7) . . . . ? O216 Si27 C271 C272 178.6(6) . . . . ? O217 Si27 C271 C272 58.9(7) . . . . ? C275 C271 C272 C273 -20.7(13) . . . . ? Si27 C271 C272 C273 -146.7(9) . . . . ? C271 C272 C273 C274 21.5(15) . . . . ? C272 C273 C274 C275 -13.6(16) . . . . ? C273 C274 C275 C271 0.4(15) . . . . ? C272 C271 C275 C274 12.4(12) . . . . ? Si27 C271 C275 C274 136.0(9) . . . . ? O218 Si28 C281 C282 174.3(5) . . . . ? O222 Si28 C281 C282 54.0(6) . . . . ? O217 Si28 C281 C282 -65.6(6) . . . . ? O218 Si28 C281 C285 54.2(7) . . . . ? O222 Si28 C281 C285 -66.1(7) . . . . ? O217 Si28 C281 C285 174.3(6) . . . . ? C285 C281 C282 C283 -31.3(9) . . . . ? Si28 C281 C282 C283 -157.5(6) . . . . ? C281 C282 C283 C284 35.5(12) . . . . ? C282 C283 C284 C285 -25.7(14) . . . . ? C283 C284 C285 C281 5.9(14) . . . . ? C282 C281 C285 C284 15.8(11) . . . . ? Si28 C281 C285 C284 141.3(9) . . . . ? Si21 C5 C290 C302 -61.5(8) . . . . ? Si21 C5 C290 C291 67.1(8) . . . . ? Si21 C5 C290 Sn21 -176.7(4) . . . . ? C6 Sn21 C290 C302 166.9(5) . . . . ? C8 Sn21 C290 C302 -74.9(5) . . . . ? C7 Sn21 C290 C302 45.2(5) . . . . ? C6 Sn21 C290 C291 61.0(5) . . . . ? C8 Sn21 C290 C291 179.2(5) . . . . ? C7 Sn21 C290 C291 -60.7(5) . . . . ? C6 Sn21 C290 C5 -65.9(5) . . . . ? C8 Sn21 C290 C5 52.2(5) . . . . ? C7 Sn21 C290 C5 172.3(5) . . . . ? C302 C290 C291 C292 173.6(7) . . . . ? C5 C290 C291 C292 37.4(10) . . . . ? Sn21 C290 C291 C292 -81.5(8) . . . . ? C302 C290 C291 C296 -6.5(7) . . . . ? C5 C290 C291 C296 -142.7(6) . . . . ? Sn21 C290 C291 C296 98.4(6) . . . . ? C296 C291 C292 C293 -4.2(11) . . . . ? C290 C291 C292 C293 175.6(7) . . . . ? C291 C292 C293 C294 2.2(12) . . . . ? C292 C293 C294 C295 -0.7(14) . . . . ? C293 C294 C295 C296 1.0(14) . . . . ? C292 C291 C296 C295 4.7(11) . . . . ? C290 C291 C296 C295 -175.2(7) . . . . ? C292 C291 C296 C297 -177.9(7) . . . . ? C290 C291 C296 C297 2.2(8) . . . . ? C294 C295 C296 C291 -2.9(12) . . . . ? C294 C295 C296 C297 -179.7(9) . . . . ? C291 C296 C297 C298 -177.6(8) . . . . ? C295 C296 C297 C298 -0.6(15) . . . . ? C291 C296 C297 C302 3.3(9) . . . . ? C295 C296 C297 C302 -179.6(8) . . . . ? C302 C297 C298 C299 -0.1(13) . . . . ? C296 C297 C298 C299 -179.0(9) . . . . ? C297 C298 C299 C300 4.6(15) . . . . ? C298 C299 C300 C301 -5.9(15) . . . . ? C299 C300 C301 C302 2.5(13) . . . . ? C300 C301 C302 C297 1.7(12) . . . . ? C300 C301 C302 C290 -173.7(8) . . . . ? C298 C297 C302 C301 -3.1(12) . . . . ? C296 C297 C302 C301 176.1(7) . . . . ? C298 C297 C302 C290 173.2(7) . . . . ? C296 C297 C302 C290 -7.6(9) . . . . ? C291 C290 C302 C301 -175.7(8) . . . . ? C5 C290 C302 C301 -39.8(11) . . . . ? Sn21 C290 C302 C301 78.6(9) . . . . ? C291 C290 C302 C297 8.5(8) . . . . ? C5 C290 C302 C297 144.4(6) . . . . ? Sn21 C290 C302 C297 -97.2(6) . . . . ? C400 C401 C402 C403 177(4) . . . . ? C401 C402 C403 C404 169(5) . . . . ? _diffrn_measured_fraction_theta_max 0.99 _diffrn_reflns_theta_full 26.0 _diffrn_measured_fraction_theta_full 0.99 _refine_diff_density_max 4.100 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.127 data_rd010 _database_code_CSD 201607 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H86 O12 Si8' _chemical_formula_weight 1163.96 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.489(1) _cell_length_b 30.222(3) _cell_length_c 19.520(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.441(2) _cell_angle_gamma 90.00 _cell_volume 6186(1) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 'reflections from 60 data frames' _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 20.82 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.659615 _exptl_absorpt_correction_T_max 0.928078 _exptl_absorpt_process_details 'Blessing,R., Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (435 frames), and at phi = 180 deg (230 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 203(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 48896 _diffrn_reflns_av_R_equivalents 0.1528 _diffrn_reflns_av_sigmaI/netI 0.1721 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 20.82 _reflns_number_total 6485 _reflns_number_gt 3958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0600P)^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 6485 _refine_ls_number_parameters 731 _refine_ls_number_restraints 204 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.006 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 1.28462(13) 0.42549(4) -0.25399(7) 0.0303(4) Uani 1 1 d . . . Si2 Si 1.55701(13) 0.38096(4) -0.25052(7) 0.0300(4) Uani 1 1 d . . . Si3 Si 1.19255(13) 0.36027(5) -0.36688(7) 0.0335(4) Uani 1 1 d . . . Si4 Si 1.19400(13) 0.36202(5) -0.14177(7) 0.0325(4) Uani 1 1 d . . . Si5 Si 1.46772(13) 0.31654(5) -0.13896(7) 0.0348(4) Uani 1 1 d . . . Si6 Si 1.46482(13) 0.31487(4) -0.36223(7) 0.0327(4) Uani 1 1 d . . . Si7 Si 1.10060(13) 0.29740(4) -0.25392(7) 0.0338(4) Uani 1 1 d . . . Si8 Si 1.37379(13) 0.25131(4) -0.25004(8) 0.0347(4) Uani 1 1 d . . . O1 O 1.4326(3) 0.41309(9) -0.25257(16) 0.0321(8) Uani 1 1 d . . . O2 O 1.2155(3) 0.40522(10) -0.32197(16) 0.0355(9) Uani 1 1 d . . . O3 O 1.2178(3) 0.40701(10) -0.18585(15) 0.0354(9) Uani 1 1 d . . . O4 O 1.5539(3) 0.35081(10) -0.18178(16) 0.0400(9) Uani 1 1 d . . . O5 O 1.5512(3) 0.34872(10) -0.31652(16) 0.0378(9) Uani 1 1 d . . . O6 O 1.3295(3) 0.33761(11) -0.38017(16) 0.0398(9) Uani 1 1 d . . . O7 O 1.1042(3) 0.32689(10) -0.32339(16) 0.0402(9) Uani 1 1 d . . . O8 O 1.1029(3) 0.32946(10) -0.18717(16) 0.0393(9) Uani 1 1 d . . . O9 O 1.3293(3) 0.33862(11) -0.12669(17) 0.0460(10) Uani 1 1 d . . . O10 O 1.4467(3) 0.27142(10) -0.18309(16) 0.0402(9) Uani 1 1 d . A . O11 O 1.4398(3) 0.27010(10) -0.31813(16) 0.0378(9) Uani 1 1 d . A . O12 O 1.2276(3) 0.26646(10) -0.24988(17) 0.0399(9) Uani 1 1 d . A . C1 C 1.2671(5) 0.48684(15) -0.2560(3) 0.0342(13) Uani 1 1 d . . . H1A H 1.1756 0.4949 -0.2574 0.041 Uiso 1 1 calc R . . C2 C 1.3337(5) 0.50737(16) -0.3161(3) 0.0334(13) Uani 1 1 d . . . C3 C 1.3102(5) 0.50258(18) -0.3856(3) 0.0482(15) Uani 1 1 d . . . H3A H 1.2427 0.4847 -0.4018 0.058 Uiso 1 1 calc R . . C4 C 1.3870(6) 0.5244(2) -0.4310(3) 0.0568(17) Uani 1 1 d . . . H4A H 1.3708 0.5213 -0.4783 0.068 Uiso 1 1 calc R . . C5 C 1.4863(6) 0.5505(2) -0.4084(4) 0.0589(17) Uani 1 1 d . . . H5A H 1.5380 0.5648 -0.4402 0.071 Uiso 1 1 calc R . . C6 C 1.5104(5) 0.55591(16) -0.3393(4) 0.0513(16) Uani 1 1 d . . . H6A H 1.5777 0.5742 -0.3239 0.062 Uiso 1 1 calc R . . C7 C 1.4345(5) 0.53414(16) -0.2920(3) 0.0374(14) Uani 1 1 d . . . C8 C 1.4334(5) 0.53496(16) -0.2177(3) 0.0382(14) Uani 1 1 d . . . C9 C 1.5110(5) 0.55757(18) -0.1704(3) 0.0544(16) Uani 1 1 d . . . H9A H 1.5787 0.5753 -0.1851 0.065 Uiso 1 1 calc R . . C10 C 1.4863(6) 0.5534(2) -0.1014(4) 0.0645(18) Uani 1 1 d . . . H10A H 1.5387 0.5680 -0.0689 0.077 Uiso 1 1 calc R . . C11 C 1.3857(6) 0.5280(2) -0.0797(3) 0.0673(19) Uani 1 1 d . . . H11A H 1.3693 0.5261 -0.0327 0.081 Uiso 1 1 calc R . . C12 C 1.3082(5) 0.50508(17) -0.1267(3) 0.0497(15) Uani 1 1 d . . . H12A H 1.2402 0.4876 -0.1118 0.060 Uiso 1 1 calc R . . C13 C 1.3330(5) 0.50849(16) -0.1955(3) 0.0350(13) Uani 1 1 d . . . C14 C 1.7038(5) 0.44317(18) -0.3177(3) 0.0513(16) Uani 1 1 d . . . H14A H 1.7085 0.4230 -0.3568 0.062 Uiso 1 1 calc R . . H14B H 1.6246 0.4602 -0.3228 0.062 Uiso 1 1 calc R . . C15 C 1.8171(6) 0.4750(2) -0.3187(4) 0.076(2) Uani 1 1 d . . . H15A H 1.8966 0.4579 -0.3193 0.092 Uiso 1 1 calc R . . H15B H 1.8120 0.4929 -0.3605 0.092 Uiso 1 1 calc R . . C16 C 1.8189(5) 0.5050(2) -0.2568(4) 0.072(2) Uani 1 1 d . . . H16A H 1.8947 0.5240 -0.2575 0.086 Uiso 1 1 calc R . . H16B H 1.7434 0.5241 -0.2584 0.086 Uiso 1 1 calc R . . C17 C 1.8203(6) 0.4784(2) -0.1921(4) 0.077(2) Uani 1 1 d . . . H17A H 1.8178 0.4985 -0.1528 0.093 Uiso 1 1 calc R . . H17B H 1.9001 0.4616 -0.1886 0.093 Uiso 1 1 calc R . . C18 C 1.7082(5) 0.44661(18) -0.1894(3) 0.0545(16) Uani 1 1 d . . . H18A H 1.6290 0.4637 -0.1870 0.065 Uiso 1 1 calc R . . H18B H 1.7163 0.4287 -0.1477 0.065 Uiso 1 1 calc R . . C19 C 1.7001(4) 0.41595(16) -0.2514(3) 0.0383(14) Uani 1 1 d . . . H19A H 1.7757 0.3964 -0.2498 0.046 Uiso 1 1 calc R . . C20 C 1.0002(5) 0.40566(19) -0.4403(3) 0.0539(16) Uani 1 1 d . . . H20A H 0.9367 0.3910 -0.4121 0.065 Uiso 1 1 calc R . . H20B H 1.0292 0.4323 -0.4158 0.065 Uiso 1 1 calc R . . C21 C 0.9376(6) 0.4192(2) -0.5081(3) 0.0699(19) Uani 1 1 d . . . H21A H 0.8973 0.3933 -0.5296 0.084 Uiso 1 1 calc R . . H21B H 0.8706 0.4410 -0.4995 0.084 Uiso 1 1 calc R . . C22 C 1.0324(6) 0.4388(2) -0.5563(3) 0.072(2) Uani 1 1 d . . . H22A H 0.9895 0.4456 -0.6002 0.087 Uiso 1 1 calc R . . H22B H 1.0661 0.4665 -0.5370 0.087 Uiso 1 1 calc R . . C23 C 1.1401(6) 0.4075(2) -0.5679(3) 0.0674(19) Uani 1 1 d . . . H23A H 1.2019 0.4215 -0.5978 0.081 Uiso 1 1 calc R . . H23B H 1.1072 0.3809 -0.5911 0.081 Uiso 1 1 calc R . . C24 C 1.2073(5) 0.39405(19) -0.5007(3) 0.0512(16) Uani 1 1 d . . . H24A H 1.2493 0.4200 -0.4803 0.061 Uiso 1 1 calc R . . H24B H 1.2733 0.3721 -0.5103 0.061 Uiso 1 1 calc R . . C25 C 1.1140(4) 0.37445(16) -0.4489(2) 0.0387(14) Uani 1 1 d . . . H25A H 1.0802 0.3466 -0.4690 0.046 Uiso 1 1 calc R . . C26 C 1.0046(5) 0.40694(19) -0.0707(3) 0.0486(15) Uani 1 1 d . . . H26A H 0.9404 0.3927 -0.1006 0.058 Uiso 1 1 calc R . . H26B H 1.0330 0.4339 -0.0935 0.058 Uiso 1 1 calc R . . C27 C 0.9435(5) 0.4194(2) -0.0028(3) 0.0609(18) Uani 1 1 d . . . H27A H 0.8742 0.4405 -0.0116 0.073 Uiso 1 1 calc R . . H27B H 0.9070 0.3929 0.0180 0.073 Uiso 1 1 calc R . . C28 C 1.0406(6) 0.4395(2) 0.0459(3) 0.0654(18) Uani 1 1 d . . . H28A H 1.0003 0.4465 0.0894 0.078 Uiso 1 1 calc R . . H28B H 1.0725 0.4672 0.0265 0.078 Uiso 1 1 calc R . . C29 C 1.1509(5) 0.4081(2) 0.0590(3) 0.0629(18) Uani 1 1 d . . . H29A H 1.1200 0.3813 0.0816 0.075 Uiso 1 1 calc R . . H29B H 1.2141 0.4222 0.0897 0.075 Uiso 1 1 calc R . . C30 C 1.2139(5) 0.39532(19) -0.0079(3) 0.0504(16) Uani 1 1 d . . . H30A H 1.2811 0.3735 0.0019 0.060 Uiso 1 1 calc R . . H30B H 1.2539 0.4216 -0.0275 0.060 Uiso 1 1 calc R . . C31 C 1.1178(4) 0.37581(16) -0.0607(2) 0.0356(13) Uani 1 1 d . . . H31A H 1.0850 0.3479 -0.0413 0.043 Uiso 1 1 calc R . . C32 C 1.6113(5) 0.34403(17) -0.0224(3) 0.0478(15) Uani 1 1 d . . . H32A H 1.6750 0.3564 -0.0530 0.057 Uiso 1 1 calc R . . H32B H 1.5464 0.3668 -0.0153 0.057 Uiso 1 1 calc R . . C33 C 1.6757(6) 0.3326(2) 0.0463(3) 0.0629(18) Uani 1 1 d . . . H33A H 1.7196 0.3588 0.0648 0.075 Uiso 1 1 calc R . . H33B H 1.6109 0.3237 0.0789 0.075 Uiso 1 1 calc R . . C34 C 1.7706(6) 0.2955(2) 0.0386(3) 0.078(2) Uani 1 1 d . . . H34A H 1.8069 0.2877 0.0838 0.093 Uiso 1 1 calc R . . H34B H 1.8404 0.3056 0.0100 0.093 Uiso 1 1 calc R . . C35 C 1.7096(7) 0.2548(2) 0.0063(3) 0.086(2) Uani 1 1 d . . . H35A H 1.6459 0.2427 0.0370 0.103 Uiso 1 1 calc R . . H35B H 1.7749 0.2321 -0.0002 0.103 Uiso 1 1 calc R . . C36 C 1.6457(5) 0.26617(18) -0.0631(3) 0.0604(17) Uani 1 1 d . . . H36A H 1.7112 0.2750 -0.0953 0.072 Uiso 1 1 calc R . . H36B H 1.6029 0.2398 -0.0816 0.072 Uiso 1 1 calc R . . C37 C 1.5482(4) 0.30358(16) -0.0570(2) 0.0360(13) Uani 1 1 d . . . H37A H 1.4817 0.2930 -0.0259 0.043 Uiso 1 1 calc R . . C38 C 1.6060(5) 0.34061(17) -0.4763(3) 0.0497(15) Uani 1 1 d . . . H38A H 1.5387 0.3624 -0.4861 0.060 Uiso 1 1 calc R . . H38B H 1.6695 0.3545 -0.4455 0.060 Uiso 1 1 calc R . . C39 C 1.6693(6) 0.3280(2) -0.5432(3) 0.0685(19) Uani 1 1 d . . . H39A H 1.7085 0.3543 -0.5633 0.082 Uiso 1 1 calc R . . H39B H 1.6048 0.3167 -0.5759 0.082 Uiso 1 1 calc R . . C40 C 1.7712(6) 0.2927(2) -0.5300(3) 0.085(2) Uani 1 1 d . . . H40A H 1.8084 0.2839 -0.5735 0.101 Uiso 1 1 calc R . . H40B H 1.8394 0.3048 -0.5004 0.101 Uiso 1 1 calc R . . C41 C 1.7127(7) 0.2526(2) -0.4958(4) 0.093(3) Uani 1 1 d . . . H41A H 1.6492 0.2392 -0.5271 0.112 Uiso 1 1 calc R . . H41B H 1.7794 0.2305 -0.4863 0.112 Uiso 1 1 calc R . . C42 C 1.6497(5) 0.26501(19) -0.4295(3) 0.0651(19) Uani 1 1 d . . . H42A H 1.7148 0.2758 -0.3967 0.078 Uiso 1 1 calc R . . H42B H 1.6103 0.2387 -0.4099 0.078 Uiso 1 1 calc R . . C43 C 1.5482(5) 0.30067(16) -0.4405(3) 0.0389(14) Uani 1 1 d . . . H43A H 1.4834 0.2881 -0.4727 0.047 Uiso 1 1 calc R . . C44 C 0.9651(5) 0.22867(17) -0.3143(3) 0.0466(15) Uani 1 1 d . . . H44A H 1.0485 0.2141 -0.3131 0.056 Uiso 1 1 calc R . . H44B H 0.9571 0.2451 -0.3575 0.056 Uiso 1 1 calc R . . C45 C 0.8597(5) 0.1930(2) -0.3127(3) 0.0631(18) Uani 1 1 d . . . H45A H 0.7763 0.2071 -0.3202 0.076 Uiso 1 1 calc R . . H45B H 0.8724 0.1718 -0.3498 0.076 Uiso 1 1 calc R . . C46 C 0.8617(5) 0.16929(18) -0.2458(3) 0.0615(18) Uani 1 1 d . . . H46A H 0.9428 0.1535 -0.2398 0.074 Uiso 1 1 calc R . . H46B H 0.7927 0.1474 -0.2457 0.074 Uiso 1 1 calc R . . C47 C 0.8456(5) 0.2013(2) -0.1873(3) 0.0627(18) Uani 1 1 d . . . H47A H 0.8487 0.1851 -0.1438 0.075 Uiso 1 1 calc R . . H47B H 0.7621 0.2157 -0.1918 0.075 Uiso 1 1 calc R . . C48 C 0.9498(5) 0.23632(18) -0.1866(3) 0.0501(16) Uani 1 1 d . . . H48A H 1.0319 0.2221 -0.1759 0.060 Uiso 1 1 calc R . . H48B H 0.9331 0.2577 -0.1502 0.060 Uiso 1 1 calc R . . C49 C 0.9590(5) 0.26106(16) -0.2549(3) 0.0402(14) Uani 1 1 d . . . H49A H 0.8819 0.2797 -0.2614 0.048 Uiso 1 1 calc R . . C50 C 1.2770(14) 0.1655(5) -0.2522(14) 0.071(5) Uani 0.435(14) 1 d PDU A 1 H50A H 1.2483 0.1730 -0.2989 0.085 Uiso 0.435(14) 1 calc PR A 1 H50B H 1.2105 0.1750 -0.2210 0.085 Uiso 0.435(14) 1 calc PR A 1 C51 C 1.2926(17) 0.1152(5) -0.2468(15) 0.096(7) Uani 0.435(14) 1 d PDU A 1 H51A H 1.2925 0.1070 -0.1982 0.116 Uiso 0.435(14) 1 calc PR A 1 H51B H 1.2180 0.1013 -0.2689 0.116 Uiso 0.435(14) 1 calc PR A 1 C52 C 1.4020(15) 0.0976(5) -0.2755(12) 0.060(5) Uani 0.435(14) 1 d PDU A 1 H52A H 1.3923 0.0987 -0.3255 0.072 Uiso 0.435(14) 1 calc PR A 1 H52B H 1.4098 0.0665 -0.2621 0.072 Uiso 0.435(14) 1 calc PR A 1 C53 C 1.5235(15) 0.1216(6) -0.2543(14) 0.071(6) Uani 0.435(14) 1 d PDU A 1 H53A H 1.5930 0.1118 -0.2833 0.086 Uiso 0.435(14) 1 calc PR A 1 H53B H 1.5464 0.1140 -0.2067 0.086 Uiso 0.435(14) 1 calc PR A 1 C54 C 1.5080(19) 0.1719(6) -0.2606(14) 0.074(6) Uani 0.435(14) 1 d PDU A 1 H54A H 1.5803 0.1859 -0.2363 0.088 Uiso 0.435(14) 1 calc PR A 1 H54B H 1.5137 0.1798 -0.3091 0.088 Uiso 0.435(14) 1 calc PR A 1 C55 C 1.395(2) 0.1903(6) -0.2357(14) 0.048(6) Uani 0.435(14) 1 d PDU A 1 H55A H 1.4051 0.1875 -0.1853 0.058 Uiso 0.435(14) 1 calc PR A 1 C50' C 1.3047(15) 0.1686(4) -0.2049(8) 0.062(4) Uani 0.565(14) 1 d PDU A 2 H50C H 1.3453 0.1771 -0.1611 0.075 Uiso 0.565(14) 1 calc PR A 2 H50D H 1.2174 0.1802 -0.2055 0.075 Uiso 0.565(14) 1 calc PR A 2 C51' C 1.2993(13) 0.1180(4) -0.2090(7) 0.051(4) Uani 0.565(14) 1 d PDU A 2 H51C H 1.2790 0.1063 -0.1637 0.061 Uiso 0.565(14) 1 calc PR A 2 H51D H 1.2296 0.1095 -0.2408 0.061 Uiso 0.565(14) 1 calc PR A 2 C52' C 1.4135(14) 0.0976(4) -0.2308(10) 0.070(5) Uani 0.565(14) 1 d PDU A 2 H52C H 1.3927 0.0672 -0.2446 0.084 Uiso 0.565(14) 1 calc PR A 2 H52D H 1.4723 0.0957 -0.1911 0.084 Uiso 0.565(14) 1 calc PR A 2 C53' C 1.4824(18) 0.1186(5) -0.2876(7) 0.067(5) Uani 0.565(14) 1 d PDU A 2 H53C H 1.4415 0.1095 -0.3310 0.080 Uiso 0.565(14) 1 calc PR A 2 H53D H 1.5699 0.1072 -0.2870 0.080 Uiso 0.565(14) 1 calc PR A 2 C54' C 1.4879(14) 0.1692(5) -0.2856(6) 0.030(3) Uani 0.565(14) 1 d PDU A 2 H54C H 1.5603 0.1783 -0.2562 0.036 Uiso 0.565(14) 1 calc PR A 2 H54D H 1.5030 0.1802 -0.3319 0.036 Uiso 0.565(14) 1 calc PR A 2 C55' C 1.3747(16) 0.1892(5) -0.2609(11) 0.049(5) Uani 0.565(14) 1 d PDU A 2 H55B H 1.3146 0.1852 -0.3003 0.058 Uiso 0.565(14) 1 calc PR A 2 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 0.0352(10) 0.0158(8) 0.0397(9) -0.0006(7) 0.0002(7) 0.0016(7) Si2 0.0321(9) 0.0171(8) 0.0408(9) -0.0005(7) 0.0009(7) -0.0013(7) Si3 0.0333(9) 0.0228(9) 0.0444(10) -0.0014(7) -0.0013(7) -0.0003(7) Si4 0.0326(9) 0.0220(9) 0.0429(10) 0.0005(7) 0.0038(7) 0.0024(7) Si5 0.0330(9) 0.0270(9) 0.0442(10) 0.0064(7) 0.0007(7) 0.0030(7) Si6 0.0355(9) 0.0177(9) 0.0450(10) -0.0049(7) 0.0032(7) -0.0007(7) Si7 0.0295(9) 0.0224(9) 0.0495(10) -0.0030(8) 0.0028(7) -0.0015(7) Si8 0.0323(9) 0.0163(8) 0.0556(11) -0.0006(8) 0.0044(7) -0.0004(7) O1 0.030(2) 0.0199(19) 0.047(2) 0.0009(16) -0.0038(15) 0.0019(16) O2 0.047(2) 0.019(2) 0.041(2) -0.0006(16) -0.0059(16) 0.0042(16) O3 0.046(2) 0.021(2) 0.039(2) -0.0019(16) 0.0054(16) 0.0041(16) O4 0.043(2) 0.034(2) 0.043(2) 0.0128(18) 0.0005(17) -0.0063(17) O5 0.039(2) 0.028(2) 0.047(2) -0.0094(17) 0.0025(17) -0.0049(16) O6 0.034(2) 0.041(2) 0.045(2) -0.0029(18) 0.0043(16) 0.0071(17) O7 0.041(2) 0.032(2) 0.047(2) 0.0028(18) -0.0005(17) -0.0078(17) O8 0.039(2) 0.027(2) 0.052(2) -0.0070(18) 0.0054(17) -0.0023(16) O9 0.031(2) 0.049(3) 0.057(2) 0.0098(19) 0.0006(17) 0.0103(18) O10 0.041(2) 0.027(2) 0.053(2) 0.0035(18) -0.0054(17) -0.0007(17) O11 0.043(2) 0.018(2) 0.052(2) 0.0001(17) 0.0063(17) -0.0005(16) O12 0.029(2) 0.031(2) 0.060(2) -0.0033(19) 0.0008(17) -0.0009(17) C1 0.036(3) 0.016(3) 0.050(4) -0.003(3) -0.005(3) 0.011(2) C2 0.045(4) 0.014(3) 0.041(4) 0.006(3) 0.000(3) 0.007(3) C3 0.061(4) 0.030(4) 0.053(4) 0.008(3) -0.008(3) 0.006(3) C4 0.072(5) 0.044(4) 0.055(4) 0.015(3) -0.001(4) 0.006(4) C5 0.068(5) 0.042(4) 0.067(5) 0.013(4) 0.017(4) 0.000(4) C6 0.049(4) 0.016(3) 0.089(5) 0.006(3) 0.010(4) 0.000(3) C7 0.044(4) 0.012(3) 0.056(4) -0.001(3) 0.004(3) 0.011(3) C8 0.040(4) 0.011(3) 0.064(4) -0.007(3) -0.004(3) 0.007(3) C9 0.058(4) 0.034(4) 0.071(5) -0.008(3) -0.003(4) -0.001(3) C10 0.073(5) 0.044(4) 0.077(6) -0.021(4) -0.007(4) -0.009(4) C11 0.087(5) 0.059(5) 0.056(4) -0.013(4) 0.010(4) 0.006(4) C12 0.063(4) 0.025(4) 0.061(5) -0.008(3) 0.004(3) 0.001(3) C13 0.047(4) 0.016(3) 0.043(4) -0.007(3) 0.002(3) 0.009(3) C14 0.064(4) 0.034(4) 0.057(4) -0.002(3) 0.016(3) -0.017(3) C15 0.080(5) 0.044(4) 0.107(6) 0.005(4) 0.026(4) -0.025(4) C16 0.054(4) 0.028(4) 0.133(7) 0.000(5) -0.006(4) -0.017(3) C17 0.074(5) 0.047(5) 0.110(6) -0.018(4) -0.031(4) -0.025(4) C18 0.068(4) 0.040(4) 0.054(4) -0.008(3) -0.016(3) -0.009(3) C19 0.031(3) 0.029(3) 0.055(4) -0.003(3) 0.001(3) -0.001(3) C20 0.043(4) 0.052(4) 0.066(4) 0.010(3) -0.003(3) 0.007(3) C21 0.062(5) 0.067(5) 0.079(5) 0.016(4) -0.022(4) 0.015(4) C22 0.085(5) 0.064(5) 0.067(5) 0.019(4) -0.017(4) 0.000(4) C23 0.079(5) 0.075(5) 0.049(4) 0.014(4) -0.002(3) 0.003(4) C24 0.061(4) 0.046(4) 0.046(4) -0.003(3) 0.005(3) 0.008(3) C25 0.037(3) 0.028(3) 0.051(4) -0.003(3) -0.001(3) -0.004(3) C26 0.041(4) 0.056(4) 0.049(4) -0.006(3) 0.000(3) 0.014(3) C27 0.059(4) 0.060(4) 0.065(5) -0.007(4) 0.018(4) 0.007(3) C28 0.079(5) 0.064(5) 0.054(4) -0.011(4) 0.017(4) -0.003(4) C29 0.071(5) 0.075(5) 0.042(4) -0.004(3) 0.003(3) -0.002(4) C30 0.059(4) 0.052(4) 0.040(4) 0.004(3) 0.003(3) 0.002(3) C31 0.039(3) 0.021(3) 0.046(3) 0.004(3) 0.002(3) -0.007(3) C32 0.053(4) 0.038(4) 0.053(4) 0.008(3) 0.004(3) 0.000(3) C33 0.074(5) 0.064(5) 0.050(4) 0.003(3) -0.013(3) -0.005(4) C34 0.078(5) 0.079(6) 0.074(5) 0.001(4) -0.039(4) 0.009(4) C35 0.103(6) 0.058(5) 0.094(6) 0.010(4) -0.043(4) 0.028(4) C36 0.066(4) 0.038(4) 0.076(5) -0.009(3) -0.020(3) 0.014(3) C37 0.032(3) 0.026(3) 0.050(4) 0.007(3) -0.001(3) 0.000(3) C38 0.056(4) 0.038(4) 0.055(4) -0.009(3) 0.009(3) -0.003(3) C39 0.075(5) 0.071(5) 0.060(4) -0.007(4) 0.022(4) -0.019(4) C40 0.080(5) 0.085(6) 0.090(6) -0.006(4) 0.049(4) 0.007(5) C41 0.102(6) 0.057(5) 0.124(7) -0.009(4) 0.067(5) 0.016(4) C42 0.069(4) 0.046(4) 0.082(5) 0.004(4) 0.037(4) 0.015(3) C43 0.037(3) 0.024(3) 0.055(4) -0.010(3) 0.004(3) -0.005(3) C44 0.044(4) 0.040(4) 0.056(4) 0.001(3) -0.002(3) -0.013(3) C45 0.061(4) 0.053(4) 0.075(5) -0.022(4) 0.000(3) -0.020(3) C46 0.047(4) 0.037(4) 0.100(6) 0.010(4) 0.000(4) -0.014(3) C47 0.052(4) 0.058(5) 0.078(5) 0.014(4) 0.008(3) -0.017(3) C48 0.047(4) 0.045(4) 0.058(4) -0.003(3) 0.010(3) -0.010(3) C49 0.030(3) 0.034(3) 0.056(4) 0.004(3) -0.004(3) 0.005(3) C50 0.055(8) 0.027(7) 0.132(15) -0.022(10) 0.010(11) 0.005(7) C51 0.058(8) 0.017(7) 0.22(2) 0.001(12) 0.026(12) -0.020(7) C52 0.066(9) 0.009(7) 0.106(14) -0.001(10) 0.031(11) -0.013(6) C53 0.057(8) 0.022(7) 0.136(16) -0.012(11) 0.009(10) 0.001(7) C54 0.047(8) 0.014(7) 0.159(17) -0.023(10) -0.027(10) 0.000(6) C55 0.071(10) 0.009(7) 0.067(14) -0.017(8) 0.033(10) -0.015(6) C50' 0.066(9) 0.027(6) 0.096(10) 0.000(7) 0.047(8) 0.002(6) C51' 0.070(7) 0.022(6) 0.061(8) 0.014(6) 0.029(6) -0.006(5) C52' 0.071(9) 0.024(6) 0.117(12) 0.029(8) 0.036(8) 0.014(6) C53' 0.096(12) 0.034(6) 0.072(10) -0.006(7) 0.044(8) 0.017(8) C54' 0.047(7) 0.027(6) 0.017(6) -0.005(5) 0.011(5) -0.014(5) C55' 0.037(8) 0.019(6) 0.092(14) 0.013(7) 0.031(7) -0.002(6) _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 1.596(3) . ? Si1 O3 1.618(3) . ? Si1 O2 1.617(3) . ? Si1 C1 1.863(5) . ? Si2 O5 1.615(3) . ? Si2 O4 1.623(3) . ? Si2 O1 1.626(3) . ? Si2 C19 1.836(5) . ? Si3 O6 1.618(3) . ? Si3 O7 1.624(3) . ? Si3 O2 1.631(3) . ? Si3 C25 1.834(5) . ? Si4 O9 1.607(3) . ? Si4 O8 1.620(3) . ? Si4 O3 1.632(3) . ? Si4 C31 1.839(5) . ? Si5 O4 1.620(3) . ? Si5 O9 1.621(3) . ? Si5 O10 1.625(3) . ? Si5 C37 1.832(5) . ? Si6 O6 1.607(3) . ? Si6 O5 1.619(3) . ? Si6 O11 1.628(3) . ? Si6 C43 1.830(5) . ? Si7 O8 1.623(3) . ? Si7 O7 1.624(3) . ? Si7 O12 1.627(3) . ? Si7 C49 1.847(5) . ? Si8 O12 1.601(3) . ? Si8 O10 1.616(3) . ? Si8 O11 1.617(3) . ? Si8 C55 1.88(2) . ? Si8 C55' 1.888(16) . ? C1 C13 1.502(6) . ? C1 C2 1.514(7) . ? C2 C3 1.379(7) . ? C2 C7 1.403(7) . ? C3 C4 1.379(7) . ? C4 C5 1.372(7) . ? C5 C6 1.377(7) . ? C6 C7 1.398(7) . ? C7 C8 1.450(7) . ? C8 C9 1.394(7) . ? C8 C13 1.400(7) . ? C9 C10 1.383(8) . ? C10 C11 1.380(8) . ? C11 C12 1.394(7) . ? C12 C13 1.377(7) . ? C14 C15 1.529(7) . ? C14 C19 1.535(7) . ? C15 C16 1.511(8) . ? C16 C17 1.496(8) . ? C17 C18 1.520(7) . ? C18 C19 1.524(7) . ? C20 C21 1.519(7) . ? C20 C25 1.534(6) . ? C21 C22 1.508(8) . ? C22 C23 1.496(8) . ? C23 C24 1.528(7) . ? C24 C25 1.542(7) . ? C26 C31 1.523(6) . ? C26 C27 1.533(7) . ? C27 C28 1.505(7) . ? C28 C29 1.514(7) . ? C29 C30 1.527(7) . ? C30 C31 1.540(6) . ? C32 C33 1.527(7) . ? C32 C37 1.538(7) . ? C33 C34 1.508(8) . ? C34 C35 1.517(8) . ? C35 C36 1.535(7) . ? C36 C37 1.531(6) . ? C38 C39 1.528(7) . ? C38 C43 1.528(6) . ? C39 C40 1.528(8) . ? C40 C41 1.521(8) . ? C41 C42 1.516(8) . ? C42 C43 1.526(7) . ? C44 C49 1.520(7) . ? C44 C45 1.544(7) . ? C45 C46 1.489(7) . ? C46 C47 1.510(8) . ? C47 C48 1.521(7) . ? C48 C49 1.534(7) . ? C50 C55 1.476(17) . ? C50 C51 1.532(14) . ? C51 C52 1.395(14) . ? C52 C53 1.514(15) . ? C53 C54 1.533(14) . ? C54 C55 1.406(14) . ? C50' C51' 1.533(12) . ? C50' C55' 1.472(15) . ? C51' C52' 1.421(12) . ? C52' C53' 1.481(13) . ? C53' C54' 1.531(12) . ? C54' C55' 1.427(11) . ? 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 O3 110.21(17) . . ? O1 Si1 O2 109.94(17) . . ? O3 Si1 O2 110.45(17) . . ? O1 Si1 C1 109.2(2) . . ? O3 Si1 C1 108.4(2) . . ? O2 Si1 C1 108.6(2) . . ? O5 Si2 O4 108.64(18) . . ? O5 Si2 O1 109.05(17) . . ? O4 Si2 O1 108.81(17) . . ? O5 Si2 C19 110.8(2) . . ? O4 Si2 C19 111.4(2) . . ? O1 Si2 C19 108.1(2) . . ? O6 Si3 O7 109.98(18) . . ? O6 Si3 O2 108.60(17) . . ? O7 Si3 O2 108.35(17) . . ? O6 Si3 C25 109.9(2) . . ? O7 Si3 C25 110.6(2) . . ? O2 Si3 C25 109.4(2) . . ? O9 Si4 O8 109.83(18) . . ? O9 Si4 O3 108.47(18) . . ? O8 Si4 O3 108.29(17) . . ? O9 Si4 C31 110.1(2) . . ? O8 Si4 C31 110.20(19) . . ? O3 Si4 C31 109.9(2) . . ? O4 Si5 O9 109.03(18) . . ? O4 Si5 O10 109.44(18) . . ? O9 Si5 O10 108.30(18) . . ? O4 Si5 C37 109.7(2) . . ? O9 Si5 C37 110.7(2) . . ? O10 Si5 C37 109.7(2) . . ? O6 Si6 O5 109.17(18) . . ? O6 Si6 O11 108.50(18) . . ? O5 Si6 O11 109.20(18) . . ? O6 Si6 C43 110.9(2) . . ? O5 Si6 C43 109.6(2) . . ? O11 Si6 C43 109.5(2) . . ? O8 Si7 O7 110.02(17) . . ? O8 Si7 O12 107.98(18) . . ? O7 Si7 O12 108.65(18) . . ? O8 Si7 C49 111.0(2) . . ? O7 Si7 C49 110.7(2) . . ? O12 Si7 C49 108.4(2) . . ? O12 Si8 O10 108.96(18) . . ? O12 Si8 O11 109.34(18) . . ? O10 Si8 O11 109.19(17) . . ? O12 Si8 C55 113.0(6) . . ? O10 Si8 C55 101.3(8) . . ? O11 Si8 C55 114.6(8) . . ? O12 Si8 C55' 107.0(5) . . ? O10 Si8 C55' 117.4(7) . . ? O11 Si8 C55' 104.7(5) . . ? C55 Si8 C55' 16.3(12) . . ? Si1 O1 Si2 156.9(2) . . ? Si1 O2 Si3 144.5(2) . . ? Si1 O3 Si4 142.8(2) . . ? Si5 O4 Si2 144.0(2) . . ? Si2 O5 Si6 146.1(2) . . ? Si6 O6 Si3 158.2(2) . . ? Si7 O7 Si3 143.4(2) . . ? Si4 O8 Si7 143.0(2) . . ? Si4 O9 Si5 160.9(2) . . ? Si8 O10 Si5 143.1(2) . . ? Si8 O11 Si6 143.6(2) . . ? Si8 O12 Si7 161.3(2) . . ? C13 C1 C2 102.6(4) . . ? C13 C1 Si1 112.0(3) . . ? C2 C1 Si1 112.1(3) . . ? C3 C2 C7 120.3(5) . . ? C3 C2 C1 130.1(5) . . ? C7 C2 C1 109.5(5) . . ? C4 C3 C2 119.2(5) . . ? C5 C4 C3 121.3(6) . . ? C4 C5 C6 120.1(6) . . ? C5 C6 C7 119.9(5) . . ? C6 C7 C2 119.1(5) . . ? C6 C7 C8 132.1(5) . . ? C2 C7 C8 108.7(5) . . ? C9 C8 C13 120.4(5) . . ? C9 C8 C7 130.6(5) . . ? C13 C8 C7 109.0(5) . . ? C10 C9 C8 118.6(6) . . ? C11 C10 C9 120.9(6) . . ? C10 C11 C12 120.8(6) . . ? C13 C12 C11 118.9(5) . . ? C12 C13 C8 120.4(5) . . ? C12 C13 C1 129.7(5) . . ? C8 C13 C1 109.9(5) . . ? C15 C14 C19 112.6(5) . . ? C16 C15 C14 111.2(5) . . ? C17 C16 C15 110.5(5) . . ? C16 C17 C18 112.2(5) . . ? C17 C18 C19 112.7(5) . . ? C18 C19 C14 109.9(4) . . ? C18 C19 Si2 111.9(4) . . ? C14 C19 Si2 110.8(3) . . ? C21 C20 C25 113.0(5) . . ? C22 C21 C20 111.8(5) . . ? C23 C22 C21 111.0(5) . . ? C22 C23 C24 111.9(5) . . ? C23 C24 C25 112.2(5) . . ? C20 C25 C24 110.2(4) . . ? C20 C25 Si3 112.4(4) . . ? C24 C25 Si3 112.5(3) . . ? C31 C26 C27 112.5(4) . . ? C28 C27 C26 110.7(5) . . ? C27 C28 C29 110.8(5) . . ? C28 C29 C30 111.0(5) . . ? C29 C30 C31 112.3(4) . . ? C26 C31 C30 110.1(4) . . ? C26 C31 Si4 112.6(3) . . ? C30 C31 Si4 111.8(3) . . ? C33 C32 C37 112.4(4) . . ? C34 C33 C32 111.0(5) . . ? C33 C34 C35 111.9(5) . . ? C34 C35 C36 110.7(5) . . ? C37 C36 C35 112.1(5) . . ? C36 C37 C32 109.9(4) . . ? C36 C37 Si5 112.6(4) . . ? C32 C37 Si5 113.4(3) . . ? C39 C38 C43 112.4(4) . . ? C38 C39 C40 110.3(5) . . ? C41 C40 C39 110.1(5) . . ? C42 C41 C40 111.4(5) . . ? C41 C42 C43 111.9(5) . . ? C42 C43 C38 109.8(4) . . ? C42 C43 Si6 113.3(4) . . ? C38 C43 Si6 113.6(3) . . ? C49 C44 C45 112.9(4) . . ? C46 C45 C44 111.1(5) . . ? C45 C46 C47 110.8(5) . . ? C46 C47 C48 111.0(5) . . ? C47 C48 C49 113.1(4) . . ? C44 C49 C48 110.7(4) . . ? C44 C49 Si7 110.0(3) . . ? C48 C49 Si7 110.4(3) . . ? C55 C50 C51 113.6(14) . . ? C52 C51 C50 116.0(13) . . ? C51 C52 C53 113.8(15) . . ? C52 C53 C54 111.4(14) . . ? C55 C54 C53 117.0(15) . . ? C54 C55 C50 115.7(16) . . ? C54 C55 Si8 115.8(13) . . ? C50 C55 Si8 111.7(16) . . ? C51' C50' C55' 113.7(11) . . ? C52' C51' C50' 114.8(10) . . ? C51' C52' C53' 117.9(11) . . ? C52' C53' C54' 115.4(10) . . ? C55' C54' C53' 113.7(10) . . ? C54' C55' C50' 120.4(12) . . ? C54' C55' Si8 117.8(9) . . ? C50' C55' Si8 109.5(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.312 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.058