Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Christian Limberg' _publ_contact_author_address ; Institut fur Chemie Humboldt-Universitat zu Berlin Brook-Taylor-Strasse 2 Berlin 12489 GERMANY ; _publ_contact_author_email CHRISTIAN.LIMBERG@CHEMIE.HU-BERLIN.DE _publ_section_title ; V2O5/SiO2 surface inspired, silsesquioxane-derived oxovanadium complexes and their properties ; loop_ _publ_author_name 'Christian Limberg' 'Marcus Brandt' 'Jens Dobler' 'Christian Ohde' 'J. Sauer' 'Burkhard Ziemer' data_MAN? _database_code_depnum_ccdc_archive 'CCDC 640134' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H166 O32 Si18 V2' _chemical_formula_sum 'C102 H166 O32 Si18 V2' _chemical_formula_weight 1255.92 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.076(4) _cell_length_b 14.748(3) _cell_length_c 18.540(5) _cell_angle_alpha 77.43(3) _cell_angle_beta 77.90(3) _cell_angle_gamma 67.34(3) _cell_volume 3188.7(15) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 22.0 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method none _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.8610 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20620 _diffrn_reflns_av_R_equivalents 0.1061 _diffrn_reflns_av_sigmaI/netI 0.1512 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 23.21 _reflns_number_total 8447 _reflns_number_gt 3804 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^2^] 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 8447 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1740 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.2591 _refine_ls_wR_factor_gt 0.2187 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8126(9) 0.5215(8) 0.3204(5) 0.068(3) Uani 1 1 d . . . H1 H 0.7537 0.5345 0.3649 0.081 Uiso 1 1 calc R . . C2 C 0.8191(11) 0.6200(9) 0.2782(7) 0.092(4) Uani 1 1 d . . . H2A H 0.8342 0.6191 0.2237 0.111 Uiso 1 1 calc R . . H2B H 0.7481 0.6752 0.2896 0.111 Uiso 1 1 calc R . . C3 C 0.9131(13) 0.6318(11) 0.3042(11) 0.133(6) Uani 1 1 d . . . H3A H 0.9509 0.6684 0.2634 0.160 Uiso 1 1 calc R . . H3B H 0.8844 0.6697 0.3467 0.160 Uiso 1 1 calc R . . C4 C 0.9897(15) 0.5347(14) 0.3267(13) 0.169(8) Uani 1 1 d . . . H4A H 1.0232 0.5348 0.3698 0.203 Uiso 1 1 calc R . . H4B H 1.0508 0.5135 0.2852 0.203 Uiso 1 1 calc R . . C5 C 0.9275(9) 0.4654(8) 0.3474(6) 0.077(3) Uani 1 1 d . . . H5A H 0.9181 0.4447 0.4021 0.093 Uiso 1 1 calc R . . H5B H 0.9685 0.4053 0.3232 0.093 Uiso 1 1 calc R . . C6 C 0.7201(9) 0.2631(8) 0.4537(5) 0.069(3) Uani 1 1 d . . . H6 H 0.8015 0.2376 0.4586 0.082 Uiso 1 1 calc R . . C7 C 0.6633(10) 0.3630(9) 0.4860(5) 0.084(4) Uani 1 1 d . . . H7A H 0.7203 0.3872 0.4941 0.101 Uiso 1 1 calc R . . H7B H 0.6142 0.4145 0.4517 0.101 Uiso 1 1 calc R . . C8 C 0.5970(16) 0.3389(11) 0.5579(8) 0.142(7) Uani 1 1 d . . . H8A H 0.6123 0.3652 0.5977 0.170 Uiso 1 1 calc R . . H8B H 0.5162 0.3710 0.5537 0.170 Uiso 1 1 calc R . . C9 C 0.6253(16) 0.2343(12) 0.5769(8) 0.149(7) Uani 1 1 d . . . H9A H 0.5586 0.2186 0.6032 0.179 Uiso 1 1 calc R . . H9B H 0.6837 0.2065 0.6102 0.179 Uiso 1 1 calc R . . C10 C 0.6672(11) 0.1908(9) 0.5067(5) 0.088(4) Uani 1 1 d . . . H10A H 0.6051 0.1875 0.4859 0.106 Uiso 1 1 calc R . . H10B H 0.7237 0.1231 0.5152 0.106 Uiso 1 1 calc R . . C11 C 0.7054(8) -0.0023(7) 0.3458(5) 0.066(3) Uani 1 1 d . . . H11 H 0.7480 -0.0288 0.3895 0.079 Uiso 1 1 calc R . . C12 C 0.5816(9) 0.0388(8) 0.3770(5) 0.075(3) Uani 1 1 d . . . H12A H 0.5701 0.0758 0.4184 0.090 Uiso 1 1 calc R . . H12B H 0.5374 0.0840 0.3376 0.090 Uiso 1 1 calc R . . C13 C 0.5474(11) -0.0513(9) 0.4047(7) 0.099(4) Uani 1 1 d . . . H13A H 0.5624 -0.0793 0.4566 0.119 Uiso 1 1 calc R . . H13B H 0.4668 -0.0337 0.4028 0.119 Uiso 1 1 calc R . . C14 C 0.6180(13) -0.1241(11) 0.3523(8) 0.120(5) Uani 1 1 d . . . H14A H 0.6466 -0.1919 0.3805 0.144 Uiso 1 1 calc R . . H14B H 0.5732 -0.1246 0.3156 0.144 Uiso 1 1 calc R . . C15 C 0.7132(10) -0.0916(9) 0.3134(7) 0.096(4) Uani 1 1 d . . . H15A H 0.7090 -0.0732 0.2591 0.115 Uiso 1 1 calc R . . H15B H 0.7853 -0.1465 0.3208 0.115 Uiso 1 1 calc R . . C16 C 0.6728(9) 0.4156(7) -0.0264(5) 0.070(3) Uani 1 1 d . . . H16 H 0.5989 0.4111 -0.0279 0.083 Uiso 1 1 calc R . . C17 C 0.7654(9) 0.3386(8) -0.0719(5) 0.077(3) Uani 1 1 d . . . H17A H 0.8330 0.3063 -0.0467 0.093 Uiso 1 1 calc R . . H17B H 0.7387 0.2868 -0.0782 0.093 Uiso 1 1 calc R . . C18 C 0.7907(11) 0.3983(11) -0.1475(6) 0.101(4) Uani 1 1 d . . . H18A H 0.8691 0.3672 -0.1702 0.121 Uiso 1 1 calc R . . H18B H 0.7399 0.4037 -0.1824 0.121 Uiso 1 1 calc R . . C19 C 0.7708(11) 0.4981(10) -0.1287(6) 0.101(4) Uani 1 1 d . . . H19A H 0.8376 0.4975 -0.1112 0.121 Uiso 1 1 calc R . . H19B H 0.7544 0.5499 -0.1731 0.121 Uiso 1 1 calc R . . C20 C 0.6741(10) 0.5181(8) -0.0691(5) 0.084(3) Uani 1 1 d . . . H20A H 0.6037 0.5559 -0.0907 0.100 Uiso 1 1 calc R . . H20B H 0.6818 0.5575 -0.0349 0.100 Uiso 1 1 calc R . . C21 C 0.4813(8) 0.6679(7) 0.1666(5) 0.065(3) Uani 1 1 d . . . H21 H 0.4196 0.6771 0.1386 0.078 Uiso 1 1 calc R . . C22 C 0.5565(12) 0.7209(9) 0.1169(7) 0.109(5) Uani 1 1 d . . . H22A H 0.6359 0.6763 0.1149 0.130 Uiso 1 1 calc R . . H22B H 0.5371 0.7406 0.0655 0.130 Uiso 1 1 calc R . . C23 C 0.5393(14) 0.8063(12) 0.1481(9) 0.135(6) Uani 1 1 d . . . H23A H 0.5326 0.8642 0.1081 0.162 Uiso 1 1 calc R . . H23B H 0.6040 0.7948 0.1732 0.162 Uiso 1 1 calc R . . C24 C 0.4355(12) 0.8270(10) 0.2029(7) 0.108(4) Uani 1 1 d . . . H24A H 0.3691 0.8708 0.1785 0.129 Uiso 1 1 calc R . . H24B H 0.4406 0.8584 0.2434 0.129 Uiso 1 1 calc R . . C25 C 0.4300(9) 0.7249(8) 0.2323(5) 0.084(4) Uani 1 1 d . . . H25A H 0.3516 0.7288 0.2491 0.101 Uiso 1 1 calc R . . H25B H 0.4733 0.6925 0.2747 0.101 Uiso 1 1 calc R . . C26 C 0.3449(8) 0.3785(7) 0.3422(5) 0.062(3) Uani 1 1 d . . . H26 H 0.2901 0.3956 0.3066 0.074 Uiso 1 1 calc R . . C27 C 0.3007(9) 0.4591(8) 0.3936(5) 0.078(3) Uani 1 1 d . . . H27A H 0.3637 0.4685 0.4089 0.093 Uiso 1 1 calc R . . H27B H 0.2541 0.5233 0.3676 0.093 Uiso 1 1 calc R . . C28 C 0.2315(12) 0.4213(11) 0.4609(7) 0.106(4) Uani 1 1 d . . . H28A H 0.2589 0.4194 0.5073 0.128 Uiso 1 1 calc R . . H28B H 0.1521 0.4660 0.4633 0.128 Uiso 1 1 calc R . . C29 C 0.2416(15) 0.3221(12) 0.4535(8) 0.150(7) Uani 1 1 d . . . H29A H 0.1730 0.3241 0.4375 0.180 Uiso 1 1 calc R . . H29B H 0.2520 0.2777 0.5019 0.180 Uiso 1 1 calc R . . C30 C 0.3383(9) 0.2852(8) 0.3978(6) 0.082(3) Uani 1 1 d . . . H30A H 0.3281 0.2378 0.3719 0.099 Uiso 1 1 calc R . . H30B H 0.4074 0.2514 0.4214 0.099 Uiso 1 1 calc R . . C31 C 0.5418(10) 0.1976(9) 0.1060(6) 0.086(3) Uani 1 1 d . . . H31 H 0.5030 0.2602 0.0733 0.104 Uiso 1 1 calc R . . C32 C 0.4571(15) 0.1542(15) 0.1444(9) 0.138(6) Uani 1 1 d . . . H32A H 0.3835 0.2073 0.1544 0.166 Uiso 1 1 calc R . . H32B H 0.4790 0.1132 0.1924 0.166 Uiso 1 1 calc R . . C33 C 0.4508(18) 0.0898(13) 0.0921(14) 0.171(9) Uani 1 1 d . . . H33A H 0.4253 0.0351 0.1196 0.205 Uiso 1 1 calc R . . H33B H 0.4023 0.1295 0.0534 0.205 Uiso 1 1 calc R . . C34 C 0.570(3) 0.0532(15) 0.0605(15) 0.205(11) Uani 1 1 d . . . H34A H 0.6097 -0.0087 0.0925 0.246 Uiso 1 1 calc R . . H34B H 0.5769 0.0364 0.0104 0.246 Uiso 1 1 calc R . . C35 C 0.6256(16) 0.1235(13) 0.0539(8) 0.133(6) Uani 1 1 d . . . H35A H 0.6350 0.1569 0.0018 0.159 Uiso 1 1 calc R . . H35B H 0.6997 0.0908 0.0715 0.159 Uiso 1 1 calc R . . C36 C 1.0872(9) 0.0572(8) 0.2726(5) 0.073(3) Uani 1 1 d . . . C37 C 1.0452(9) 0.1571(9) 0.2428(6) 0.078(3) Uani 1 1 d . . . H37 H 0.9775 0.1815 0.2219 0.093 Uiso 1 1 calc R . . C38 C 1.0973(10) 0.2215(9) 0.2423(6) 0.082(3) Uani 1 1 d . . . H38 H 1.0675 0.2884 0.2189 0.098 Uiso 1 1 calc R . . C39 C 1.1910(12) 0.1915(10) 0.2748(6) 0.098(4) Uani 1 1 d . . . H39 H 1.2248 0.2377 0.2762 0.117 Uiso 1 1 calc R . . C40 C 1.2376(13) 0.0918(11) 0.3063(8) 0.124(6) Uani 1 1 d . . . H40 H 1.3043 0.0692 0.3282 0.149 Uiso 1 1 calc R . . C41 C 1.1858(11) 0.0269(10) 0.3053(7) 0.095(4) Uani 1 1 d . . . H41 H 1.2173 -0.0405 0.3272 0.114 Uiso 1 1 calc R . . C42 C 1.0094(9) -0.1079(8) 0.3661(6) 0.077(3) Uani 1 1 d . . . C43 C 0.9602(10) -0.0558(10) 0.4293(6) 0.092(4) Uani 1 1 d . . . H43 H 0.9366 0.0147 0.4223 0.111 Uiso 1 1 calc R . . C44 C 0.9469(11) -0.1080(12) 0.5006(7) 0.104(4) Uani 1 1 d . . . H44 H 0.9153 -0.0733 0.5422 0.125 Uiso 1 1 calc R . . C45 C 0.9802(14) -0.2111(13) 0.5109(9) 0.112(5) Uani 1 1 d . . . H45 H 0.9708 -0.2468 0.5596 0.134 Uiso 1 1 calc R . . C46 C 1.0250(15) -0.2597(12) 0.4526(10) 0.126(6) Uani 1 1 d . . . H46 H 1.0467 -0.3300 0.4609 0.151 Uiso 1 1 calc R . . C47 C 1.0420(10) -0.2104(9) 0.3783(7) 0.091(4) Uani 1 1 d . . . H47 H 1.0749 -0.2473 0.3380 0.109 Uiso 1 1 calc R . . C48 C 1.0965(11) -0.1162(10) 0.2007(7) 0.101(4) Uani 1 1 d . . . H48A H 1.1006 -0.0764 0.1512 0.152 Uiso 1 1 calc R . . H48B H 1.0576 -0.1614 0.2009 0.152 Uiso 1 1 calc R . . H48C H 1.1724 -0.1550 0.2126 0.152 Uiso 1 1 calc R . . C49 C 0.850(2) 0.8466(13) 0.0348(9) 0.164(8) Uani 1 1 d . . . H49 H 0.7684 0.8666 0.0315 0.197 Uiso 1 1 calc R . . C50 C 0.903(3) 0.8969(15) -0.0315(12) 0.31(2) Uani 1 1 d . . . H50A H 0.9843 0.8667 -0.0341 0.368 Uiso 1 1 calc R . . H50B H 0.8787 0.9676 -0.0278 0.368 Uiso 1 1 calc R . . H50C H 0.8803 0.8898 -0.0766 0.368 Uiso 1 1 calc R . . C51 C 0.8622(19) 0.8566(13) 0.1064(10) 0.173(8) Uani 1 1 d . . . H51A H 0.8360 0.9273 0.1107 0.208 Uiso 1 1 calc R . . H51C H 0.9412 0.8252 0.1134 0.208 Uiso 1 1 calc R . . H51B H 0.8178 0.8242 0.1447 0.208 Uiso 1 1 calc R . . O1 O 0.7656(10) 0.7259(11) -0.0291(8) 0.244(10) Uani 1 1 d . . . O2 O 0.9790(5) 0.6104(5) -0.0718(3) 0.081(2) Uani 1 1 d . . . O3 O 0.8520(6) 0.5609(5) 0.0669(4) 0.088(2) Uani 1 1 d . . . O4 O 0.9057(16) 0.7374(12) 0.0337(6) 0.204(7) Uani 1 1 d . . . O5 O 0.8751(5) 0.4325(5) 0.1908(3) 0.0663(18) Uani 1 1 d . . . O6 O 0.7745(5) 0.3466(5) 0.3044(3) 0.0644(18) Uani 1 1 d . . . O7 O 0.7601(5) 0.1712(5) 0.3262(3) 0.0641(18) Uani 1 1 d . . . O8 O 0.6930(5) 0.1342(5) 0.2121(3) 0.0688(19) Uani 1 1 d . . . O9 O 0.5748(5) 0.3286(5) 0.3438(3) 0.0640(18) Uani 1 1 d . . . O10 O 0.6594(5) 0.5202(5) 0.2320(3) 0.0672(18) Uani 1 1 d . . . O11 O 0.8200(5) 0.3958(6) 0.0759(3) 0.075(2) Uani 1 1 d . . . O12 O 0.6020(5) 0.4861(5) 0.1137(3) 0.0692(19) Uani 1 1 d . . . O13 O 0.4772(5) 0.4777(5) 0.2447(3) 0.0623(17) Uani 1 1 d . . . O14 O 0.5156(5) 0.2966(5) 0.2265(3) 0.0650(18) Uani 1 1 d . . . O15 O 0.6846(6) 0.2949(5) 0.1185(3) 0.078(2) Uani 1 1 d . . . O16 O 0.8930(5) 0.0299(5) 0.2490(3) 0.0694(18) Uani 1 1 d . . . Si1 Si 0.8904(2) 0.4449(2) 0.10166(13) 0.0673(9) Uani 1 1 d . . . Si2 Si 0.7776(2) 0.4535(2) 0.26206(13) 0.0586(8) Uani 1 1 d . . . Si3 Si 0.7078(2) 0.27696(19) 0.35462(13) 0.0554(7) Uani 1 1 d . . . Si4 Si 0.7644(2) 0.0851(2) 0.28286(14) 0.0622(8) Uani 1 1 d . . . Si5 Si 0.6930(2) 0.3979(2) 0.07176(13) 0.0661(8) Uani 1 1 d . . . Si6 Si 0.5556(2) 0.5351(2) 0.18988(13) 0.0598(8) Uani 1 1 d . . . Si7 Si 0.4823(2) 0.3688(2) 0.28774(13) 0.0579(7) Uani 1 1 d . . . Si8 Si 0.6102(2) 0.2307(2) 0.16757(13) 0.0633(8) Uani 1 1 d . . . Si9 Si 1.0190(2) -0.0329(2) 0.27121(16) 0.0714(9) Uani 1 1 d . . . V V 0.88445(19) 0.65538(16) 0.00454(13) 0.1071(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.077(7) 0.070(7) 0.061(5) -0.013(5) -0.012(5) -0.029(6) C2 0.109(10) 0.075(8) 0.108(8) -0.014(7) -0.024(7) -0.045(7) C3 0.104(11) 0.085(11) 0.225(18) -0.021(11) -0.025(11) -0.050(9) C4 0.117(13) 0.133(16) 0.27(2) 0.024(15) -0.061(14) -0.071(13) C5 0.089(8) 0.074(7) 0.076(6) -0.011(6) -0.026(6) -0.029(6) C6 0.088(7) 0.073(7) 0.055(5) -0.002(5) -0.017(5) -0.041(6) C7 0.126(10) 0.088(9) 0.059(6) -0.019(6) 0.005(6) -0.066(8) C8 0.214(18) 0.087(10) 0.103(10) -0.034(8) 0.049(10) -0.056(11) C9 0.220(18) 0.138(14) 0.101(10) -0.034(10) 0.066(11) -0.112(14) C10 0.129(10) 0.089(9) 0.061(6) -0.004(6) -0.009(6) -0.060(8) C11 0.077(7) 0.054(6) 0.068(6) -0.011(5) -0.006(5) -0.027(5) C12 0.094(8) 0.065(7) 0.068(6) -0.020(5) 0.011(5) -0.035(6) C13 0.105(9) 0.090(9) 0.101(8) -0.018(7) 0.014(7) -0.047(8) C14 0.150(13) 0.104(11) 0.131(11) -0.038(9) 0.018(10) -0.080(10) C15 0.092(9) 0.075(8) 0.120(9) -0.028(7) 0.017(7) -0.038(7) C16 0.075(7) 0.065(7) 0.054(5) -0.017(5) 0.006(5) -0.014(5) C17 0.092(8) 0.086(8) 0.058(5) -0.027(6) 0.004(5) -0.035(7) C18 0.121(11) 0.123(12) 0.068(7) -0.030(7) 0.019(6) -0.060(9) C19 0.121(10) 0.104(11) 0.075(7) 0.001(7) 0.000(7) -0.054(9) C20 0.111(9) 0.071(7) 0.063(6) -0.014(6) -0.012(6) -0.025(7) C21 0.073(7) 0.065(7) 0.058(5) -0.013(5) -0.010(5) -0.022(5) C22 0.144(12) 0.061(8) 0.097(8) -0.016(7) 0.031(8) -0.034(8) C23 0.137(13) 0.107(12) 0.169(14) -0.024(11) 0.019(11) -0.071(11) C24 0.129(12) 0.082(9) 0.112(9) -0.026(8) -0.005(8) -0.038(8) C25 0.082(7) 0.072(8) 0.067(6) -0.008(6) 0.005(5) -0.001(6) C26 0.059(6) 0.074(7) 0.060(5) -0.010(5) -0.012(4) -0.030(5) C27 0.075(7) 0.084(8) 0.078(6) -0.019(6) 0.006(5) -0.037(6) C28 0.120(11) 0.114(12) 0.093(8) -0.047(8) 0.020(7) -0.050(9) C29 0.189(17) 0.126(13) 0.105(10) -0.015(9) 0.068(10) -0.071(12) C30 0.085(8) 0.083(8) 0.091(7) -0.012(6) 0.000(6) -0.049(7) C31 0.102(9) 0.075(8) 0.091(7) -0.048(7) -0.016(7) -0.020(7) C32 0.136(14) 0.197(18) 0.130(11) -0.062(12) -0.023(10) -0.090(14) C33 0.160(18) 0.086(12) 0.30(3) -0.048(15) -0.147(19) -0.015(12) C34 0.25(3) 0.102(15) 0.28(3) 0.012(17) -0.10(2) -0.075(19) C35 0.190(17) 0.116(13) 0.118(10) -0.045(10) -0.047(11) -0.055(13) C36 0.081(8) 0.068(7) 0.062(6) -0.013(5) 0.002(5) -0.021(6) C37 0.070(7) 0.076(8) 0.087(7) -0.014(6) -0.013(5) -0.022(6) C38 0.072(7) 0.077(8) 0.098(8) -0.001(6) -0.026(6) -0.028(7) C39 0.112(11) 0.102(10) 0.097(8) -0.006(8) -0.013(7) -0.064(9) C40 0.120(11) 0.111(12) 0.155(13) 0.039(10) -0.067(10) -0.063(10) C41 0.093(9) 0.088(9) 0.102(8) 0.006(7) -0.035(7) -0.031(8) C42 0.074(7) 0.060(7) 0.094(8) 0.002(6) -0.023(6) -0.024(6) C43 0.100(9) 0.109(10) 0.081(7) 0.008(8) -0.025(6) -0.057(8) C44 0.107(10) 0.120(12) 0.092(8) 0.002(8) -0.028(7) -0.050(9) C45 0.143(13) 0.118(14) 0.097(10) 0.014(10) -0.050(9) -0.072(11) C46 0.167(15) 0.094(11) 0.147(13) 0.044(11) -0.078(12) -0.084(11) C47 0.094(9) 0.079(9) 0.110(9) -0.011(7) -0.034(7) -0.034(7) C48 0.095(9) 0.092(9) 0.113(9) -0.042(8) -0.008(7) -0.018(7) C49 0.30(3) 0.089(12) 0.111(12) -0.046(10) 0.006(13) -0.082(15) C50 0.58(6) 0.110(15) 0.18(2) -0.030(14) 0.13(3) -0.16(3) C51 0.26(2) 0.091(12) 0.134(14) -0.047(11) -0.046(14) -0.006(13) O1 0.106(8) 0.193(13) 0.231(13) 0.103(11) 0.036(9) 0.063(8) O2 0.064(4) 0.088(5) 0.066(4) -0.001(4) 0.011(3) -0.017(4) O3 0.090(5) 0.074(5) 0.076(4) -0.001(4) 0.012(4) -0.020(4) O4 0.36(2) 0.180(13) 0.117(8) -0.087(9) 0.058(11) -0.164(15) O5 0.071(4) 0.077(5) 0.050(3) -0.011(3) 0.002(3) -0.030(4) O6 0.066(4) 0.060(4) 0.070(4) -0.013(3) 0.000(3) -0.028(3) O7 0.072(4) 0.058(4) 0.067(4) -0.022(3) -0.008(3) -0.024(3) O8 0.076(4) 0.066(4) 0.062(4) -0.009(3) -0.010(3) -0.023(4) O9 0.055(4) 0.072(4) 0.063(3) -0.007(3) -0.006(3) -0.023(3) O10 0.073(4) 0.065(4) 0.064(3) -0.011(3) -0.011(3) -0.023(4) O11 0.066(4) 0.101(6) 0.062(4) -0.029(4) -0.001(3) -0.031(4) O12 0.078(5) 0.073(5) 0.050(3) -0.013(3) -0.003(3) -0.022(4) O13 0.066(4) 0.058(4) 0.064(3) -0.013(3) -0.001(3) -0.024(3) O14 0.076(4) 0.070(4) 0.057(3) -0.017(3) 0.000(3) -0.034(4) O15 0.090(5) 0.069(5) 0.066(4) -0.009(3) 0.001(3) -0.024(4) O16 0.072(4) 0.062(4) 0.065(4) -0.016(3) -0.005(3) -0.014(3) Si1 0.0673(18) 0.0727(19) 0.0519(14) -0.0040(14) 0.0041(12) -0.0233(15) Si2 0.0688(17) 0.0622(17) 0.0499(13) -0.0055(13) -0.0014(11) -0.0341(15) Si3 0.0664(17) 0.0536(16) 0.0514(13) -0.0067(12) -0.0059(11) -0.0287(14) Si4 0.0702(18) 0.0553(17) 0.0594(14) -0.0097(14) -0.0023(12) -0.0235(14) Si5 0.0761(19) 0.0698(19) 0.0477(13) -0.0113(13) -0.0004(12) -0.0239(16) Si6 0.0661(17) 0.0604(17) 0.0490(13) -0.0098(12) -0.0008(11) -0.0213(14) Si7 0.0607(16) 0.0642(18) 0.0515(13) -0.0141(13) -0.0014(11) -0.0255(14) Si8 0.0694(18) 0.0663(19) 0.0545(14) -0.0183(13) -0.0063(12) -0.0208(15) Si9 0.0712(19) 0.068(2) 0.0728(17) -0.0172(15) -0.0070(14) -0.0210(16) V 0.1007(16) 0.0730(14) 0.1165(16) -0.0196(13) 0.0522(13) -0.0290(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.517(14) . ? C1 C5 1.539(14) . ? C1 Si2 1.848(11) . ? C1 H1 1.0000 . ? C2 C3 1.491(18) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.43(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.481(17) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C10 1.553(12) . ? C6 C7 1.559(15) . ? C6 Si3 1.838(9) . ? C6 H6 1.0000 . ? C7 C8 1.484(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.421(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.482(17) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C15 1.525(15) . ? C11 C12 1.525(13) . ? C11 Si4 1.832(8) . ? C11 H11 1.0000 . ? C12 C13 1.514(14) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.504(17) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.493(15) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.548(14) . ? C16 C20 1.551(14) . ? C16 Si5 1.842(10) . ? C16 H16 1.0000 . ? C17 C18 1.530(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.500(17) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.476(15) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C25 1.520(14) . ? C21 C22 1.525(13) . ? C21 Si6 1.819(10) . ? C21 H21 1.0000 . ? C22 C23 1.421(18) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.486(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.510(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.544(14) . ? C26 C30 1.549(12) . ? C26 Si7 1.837(8) . ? C26 H26 1.0000 . ? C27 C28 1.517(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.452(19) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.459(16) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.471(17) . ? C31 C35 1.556(19) . ? C31 Si8 1.830(12) . ? C31 H31 1.0000 . ? C32 C33 1.53(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.48(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.45(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.388(14) . ? C36 C41 1.412(16) . ? C36 Si9 1.871(12) . ? C37 C38 1.364(15) . ? C37 H37 0.9500 . ? C38 C39 1.354(16) . ? C38 H38 0.9500 . ? C39 C40 1.400(18) . ? C39 H39 0.9500 . ? C40 C41 1.374(17) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.384(15) . ? C42 C43 1.440(17) . ? C42 Si9 1.871(10) . ? C43 C44 1.390(14) . ? C43 H43 0.9500 . ? C44 C45 1.39(2) . ? C44 H44 0.9500 . ? C45 C46 1.33(2) . ? C45 H45 0.9500 . ? C46 C47 1.427(17) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 Si9 1.852(12) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C51 1.42(2) . ? C49 C50 1.48(2) . ? C49 O4 1.49(2) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51C 0.9800 . ? C51 H51B 0.9800 . ? O1 V 1.663(12) . ? O2 Si1 1.618(7) 2_765 ? O2 V 1.736(6) . ? O3 Si1 1.609(7) . ? O3 V 1.734(6) . ? O4 V 1.561(13) . ? O5 Si1 1.602(6) . ? O5 Si2 1.622(6) . ? O6 Si2 1.613(6) . ? O6 Si3 1.617(6) . ? O7 Si3 1.601(7) . ? O7 Si4 1.622(7) . ? O8 Si8 1.599(7) . ? O8 Si4 1.642(7) . ? O9 Si7 1.612(7) . ? O9 Si3 1.645(7) . ? O10 Si2 1.618(7) . ? O10 Si6 1.625(7) . ? O11 Si1 1.565(8) . ? O11 Si5 1.667(7) . ? O12 Si5 1.603(7) . ? O12 Si6 1.622(7) . ? O13 Si7 1.613(6) . ? O13 Si6 1.630(6) . ? O14 Si7 1.604(7) . ? O14 Si8 1.625(7) . ? O15 Si5 1.609(7) . ? O15 Si8 1.623(7) . ? O16 Si4 1.615(7) . ? O16 Si9 1.638(7) . ? Si1 O2 1.618(7) 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 C2 C1 C5 104.7(8) . . ? C2 C1 Si2 112.1(7) . . ? C5 C1 Si2 113.6(8) . . ? C2 C1 H1 108.8 . . ? C5 C1 H1 108.8 . . ? Si2 C1 H1 108.8 . . ? C3 C2 C1 105.5(10) . . ? C3 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? C3 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.8 . . ? C4 C3 C2 107.7(13) . . ? C4 C3 H3A 110.2 . . ? C2 C3 H3A 110.2 . . ? C4 C3 H3B 110.2 . . ? C2 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C3 C4 C5 108.2(13) . . ? C3 C4 H4A 110.1 . . ? C5 C4 H4A 110.1 . . ? C3 C4 H4B 110.1 . . ? C5 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C4 C5 C1 106.9(10) . . ? C4 C5 H5A 110.3 . . ? C1 C5 H5A 110.3 . . ? C4 C5 H5B 110.3 . . ? C1 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? C10 C6 C7 104.8(8) . . ? C10 C6 Si3 114.8(7) . . ? C7 C6 Si3 113.1(7) . . ? C10 C6 H6 107.9 . . ? C7 C6 H6 107.9 . . ? Si3 C6 H6 107.9 . . ? C8 C7 C6 104.9(9) . . ? C8 C7 H7A 110.8 . . ? C6 C7 H7A 110.8 . . ? C8 C7 H7B 110.8 . . ? C6 C7 H7B 110.8 . . ? H7A C7 H7B 108.8 . . ? C9 C8 C7 110.1(12) . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 107.8(11) . . ? C8 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? C8 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.5 . . ? C9 C10 C6 104.2(10) . . ? C9 C10 H10A 110.9 . . ? C6 C10 H10A 110.9 . . ? C9 C10 H10B 110.9 . . ? C6 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C15 C11 C12 102.3(8) . . ? C15 C11 Si4 115.8(7) . . ? C12 C11 Si4 117.0(7) . . ? C15 C11 H11 107.1 . . ? C12 C11 H11 107.1 . . ? Si4 C11 H11 107.1 . . ? C13 C12 C11 105.4(9) . . ? C13 C12 H12A 110.7 . . ? C11 C12 H12A 110.7 . . ? C13 C12 H12B 110.7 . . ? C11 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? C14 C13 C12 104.7(9) . . ? C14 C13 H13A 110.8 . . ? C12 C13 H13A 110.8 . . ? C14 C13 H13B 110.8 . . ? C12 C13 H13B 110.8 . . ? H13A C13 H13B 108.9 . . ? C15 C14 C13 107.3(10) . . ? C15 C14 H14A 110.3 . . ? C13 C14 H14A 110.3 . . ? C15 C14 H14B 110.3 . . ? C13 C14 H14B 110.3 . . ? H14A C14 H14B 108.5 . . ? C14 C15 C11 108.1(9) . . ? C14 C15 H15A 110.1 . . ? C11 C15 H15A 110.1 . . ? C14 C15 H15B 110.1 . . ? C11 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? C17 C16 C20 104.9(7) . . ? C17 C16 Si5 113.6(7) . . ? C20 C16 Si5 112.0(8) . . ? C17 C16 H16 108.7 . . ? C20 C16 H16 108.7 . . ? Si5 C16 H16 108.7 . . ? C18 C17 C16 105.2(9) . . ? C18 C17 H17A 110.7 . . ? C16 C17 H17A 110.7 . . ? C18 C17 H17B 110.7 . . ? C16 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C19 C18 C17 103.6(9) . . ? C19 C18 H18A 111.0 . . ? C17 C18 H18A 111.0 . . ? C19 C18 H18B 111.0 . . ? C17 C18 H18B 111.0 . . ? H18A C18 H18B 109.0 . . ? C20 C19 C18 106.4(9) . . ? C20 C19 H19A 110.4 . . ? C18 C19 H19A 110.4 . . ? C20 C19 H19B 110.4 . . ? C18 C19 H19B 110.4 . . ? H19A C19 H19B 108.6 . . ? C19 C20 C16 106.7(9) . . ? C19 C20 H20A 110.4 . . ? C16 C20 H20A 110.4 . . ? C19 C20 H20B 110.4 . . ? C16 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? C25 C21 C22 104.7(9) . . ? C25 C21 Si6 115.8(6) . . ? C22 C21 Si6 112.4(8) . . ? C25 C21 H21 107.9 . . ? C22 C21 H21 107.9 . . ? Si6 C21 H21 107.9 . . ? C23 C22 C21 107.4(9) . . ? C23 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? C23 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C22 C23 C24 109.3(11) . . ? C22 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? C22 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? C23 C24 C25 102.9(11) . . ? C23 C24 H24A 111.2 . . ? C25 C24 H24A 111.2 . . ? C23 C24 H24B 111.2 . . ? C25 C24 H24B 111.2 . . ? H24A C24 H24B 109.1 . . ? C24 C25 C21 104.7(8) . . ? C24 C25 H25A 110.8 . . ? C21 C25 H25A 110.8 . . ? C24 C25 H25B 110.8 . . ? C21 C25 H25B 110.8 . . ? H25A C25 H25B 108.9 . . ? C27 C26 C30 102.0(7) . . ? C27 C26 Si7 113.4(6) . . ? C30 C26 Si7 116.5(7) . . ? C27 C26 H26 108.2 . . ? C30 C26 H26 108.2 . . ? Si7 C26 H26 108.2 . . ? C28 C27 C26 105.7(8) . . ? C28 C27 H27A 110.6 . . ? C26 C27 H27A 110.6 . . ? C28 C27 H27B 110.6 . . ? C26 C27 H27B 110.6 . . ? H27A C27 H27B 108.7 . . ? C29 C28 C27 108.2(10) . . ? C29 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? C29 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? C28 C29 C30 107.7(11) . . ? C28 C29 H29A 110.2 . . ? C30 C29 H29A 110.2 . . ? C28 C29 H29B 110.2 . . ? C30 C29 H29B 110.2 . . ? H29A C29 H29B 108.5 . . ? C29 C30 C26 105.4(10) . . ? C29 C30 H30A 110.7 . . ? C26 C30 H30A 110.7 . . ? C29 C30 H30B 110.7 . . ? C26 C30 H30B 110.7 . . ? H30A C30 H30B 108.8 . . ? C32 C31 C35 106.5(12) . . ? C32 C31 Si8 114.9(9) . . ? C35 C31 Si8 113.1(10) . . ? C32 C31 H31 107.3 . . ? C35 C31 H31 107.3 . . ? Si8 C31 H31 107.3 . . ? C31 C32 C33 106.4(14) . . ? C31 C32 H32A 110.4 . . ? C33 C32 H32A 110.4 . . ? C31 C32 H32B 110.4 . . ? C33 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? C34 C33 C32 98.3(15) . . ? C34 C33 H33A 112.1 . . ? C32 C33 H33A 112.1 . . ? C34 C33 H33B 112.1 . . ? C32 C33 H33B 112.1 . . ? H33A C33 H33B 109.8 . . ? C35 C34 C33 114(2) . . ? C35 C34 H34A 108.8 . . ? C33 C34 H34A 108.8 . . ? C35 C34 H34B 108.8 . . ? C33 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C34 C35 C31 101.6(17) . . ? C34 C35 H35A 111.4 . . ? C31 C35 H35A 111.4 . . ? C34 C35 H35B 111.4 . . ? C31 C35 H35B 111.4 . . ? H35A C35 H35B 109.3 . . ? C37 C36 C41 115.5(11) . . ? C37 C36 Si9 123.2(9) . . ? C41 C36 Si9 121.3(9) . . ? C38 C37 C36 122.7(11) . . ? C38 C37 H37 118.7 . . ? C36 C37 H37 118.7 . . ? C39 C38 C37 120.9(11) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C38 C39 C40 119.3(12) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C41 C40 C39 119.3(13) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C40 C41 C36 122.2(12) . . ? C40 C41 H41 118.9 . . ? C36 C41 H41 118.9 . . ? C47 C42 C43 118.3(10) . . ? C47 C42 Si9 123.4(10) . . ? C43 C42 Si9 118.3(8) . . ? C44 C43 C42 120.4(13) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 119.9(15) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0(14) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 122.7(15) . . ? C45 C46 H46 118.6 . . ? C47 C46 H46 118.6 . . ? C42 C47 C46 118.7(14) . . ? C42 C47 H47 120.7 . . ? C46 C47 H47 120.7 . . ? Si9 C48 H48A 109.5 . . ? Si9 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si9 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C50 119(2) . . ? C51 C49 O4 102.9(16) . . ? C50 C49 O4 107.0(15) . . ? C51 C49 H49 109.3 . . ? C50 C49 H49 109.3 . . ? O4 C49 H49 109.3 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? H51C C51 H51B 109.5 . . ? Si1 O2 V 144.8(5) 2_765 . ? Si1 O3 V 148.0(5) . . ? C49 O4 V 136.9(18) . . ? Si1 O5 Si2 140.6(5) . . ? Si2 O6 Si3 151.2(4) . . ? Si3 O7 Si4 156.0(5) . . ? Si8 O8 Si4 148.3(5) . . ? Si7 O9 Si3 147.8(4) . . ? Si2 O10 Si6 152.0(5) . . ? Si1 O11 Si5 146.9(5) . . ? Si5 O12 Si6 147.6(4) . . ? Si7 O13 Si6 141.4(4) . . ? Si7 O14 Si8 149.4(5) . . ? Si5 O15 Si8 150.2(5) . . ? Si4 O16 Si9 143.6(4) . . ? O11 Si1 O5 110.9(3) . . ? O11 Si1 O3 109.4(4) . . ? O5 Si1 O3 110.0(4) . . ? O11 Si1 O2 108.3(4) . 2_765 ? O5 Si1 O2 108.5(4) . 2_765 ? O3 Si1 O2 109.7(3) . 2_765 ? O6 Si2 O10 110.0(3) . . ? O6 Si2 O5 106.6(4) . . ? O10 Si2 O5 108.6(3) . . ? O6 Si2 C1 113.3(4) . . ? O10 Si2 C1 110.4(4) . . ? O5 Si2 C1 107.8(4) . . ? O7 Si3 O6 108.1(3) . . ? O7 Si3 O9 109.5(4) . . ? O6 Si3 O9 109.2(3) . . ? O7 Si3 C6 110.8(4) . . ? O6 Si3 C6 110.2(4) . . ? O9 Si3 C6 109.0(4) . . ? O16 Si4 O7 108.2(4) . . ? O16 Si4 O8 107.1(3) . . ? O7 Si4 O8 110.5(4) . . ? O16 Si4 C11 111.7(4) . . ? O7 Si4 C11 110.7(4) . . ? O8 Si4 C11 108.6(4) . . ? O12 Si5 O15 107.5(3) . . ? O12 Si5 O11 108.4(4) . . ? O15 Si5 O11 106.7(4) . . ? O12 Si5 C16 111.3(4) . . ? O15 Si5 C16 113.0(5) . . ? O11 Si5 C16 109.7(4) . . ? O12 Si6 O10 110.1(4) . . ? O12 Si6 O13 108.2(4) . . ? O10 Si6 O13 108.4(3) . . ? O12 Si6 C21 109.2(4) . . ? O10 Si6 C21 107.9(4) . . ? O13 Si6 C21 113.0(4) . . ? O14 Si7 O9 110.4(4) . . ? O14 Si7 O13 108.2(3) . . ? O9 Si7 O13 109.0(4) . . ? O14 Si7 C26 111.3(4) . . ? O9 Si7 C26 109.0(4) . . ? O13 Si7 C26 108.9(4) . . ? O8 Si8 O15 107.2(4) . . ? O8 Si8 O14 109.5(3) . . ? O15 Si8 O14 109.3(4) . . ? O8 Si8 C31 111.7(5) . . ? O15 Si8 C31 109.8(5) . . ? O14 Si8 C31 109.4(5) . . ? O16 Si9 C48 107.6(5) . . ? O16 Si9 C36 108.5(5) . . ? C48 Si9 C36 111.8(5) . . ? O16 Si9 C42 109.6(4) . . ? C48 Si9 C42 110.1(6) . . ? C36 Si9 C42 109.1(5) . . ? O4 V O1 98.4(10) . . ? O4 V O3 120.3(5) . . ? O1 V O3 104.4(5) . . ? O4 V O2 114.2(5) . . ? O1 V O2 105.4(6) . . ? O3 V O2 111.5(3) . . ? 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 C5 C1 C2 C3 -19.3(14) . . . . ? Si2 C1 C2 C3 -142.7(10) . . . . ? C1 C2 C3 C4 27.5(19) . . . . ? C2 C3 C4 C5 -25(2) . . . . ? C3 C4 C5 C1 12(2) . . . . ? C2 C1 C5 C4 5.0(15) . . . . ? Si2 C1 C5 C4 127.5(12) . . . . ? C10 C6 C7 C8 7.5(14) . . . . ? Si3 C6 C7 C8 133.3(11) . . . . ? C6 C7 C8 C9 10.7(19) . . . . ? C7 C8 C9 C10 -26(2) . . . . ? C8 C9 C10 C6 29.5(18) . . . . ? C7 C6 C10 C9 -22.0(14) . . . . ? Si3 C6 C10 C9 -146.8(11) . . . . ? C15 C11 C12 C13 34.5(11) . . . . ? Si4 C11 C12 C13 162.1(8) . . . . ? C11 C12 C13 C14 -32.9(14) . . . . ? C12 C13 C14 C15 17.8(16) . . . . ? C13 C14 C15 C11 3.8(16) . . . . ? C12 C11 C15 C14 -23.5(13) . . . . ? Si4 C11 C15 C14 -151.9(10) . . . . ? C20 C16 C17 C18 -15.8(12) . . . . ? Si5 C16 C17 C18 -138.4(8) . . . . ? C16 C17 C18 C19 32.1(13) . . . . ? C17 C18 C19 C20 -37.1(14) . . . . ? C18 C19 C20 C16 27.2(14) . . . . ? C17 C16 C20 C19 -6.6(13) . . . . ? Si5 C16 C20 C19 117.1(9) . . . . ? C25 C21 C22 C23 -5.7(15) . . . . ? Si6 C21 C22 C23 -132.2(12) . . . . ? C21 C22 C23 C24 -15.4(18) . . . . ? C22 C23 C24 C25 30.3(17) . . . . ? C23 C24 C25 C21 -32.6(14) . . . . ? C22 C21 C25 C24 23.9(13) . . . . ? Si6 C21 C25 C24 148.3(9) . . . . ? C30 C26 C27 C28 -22.4(12) . . . . ? Si7 C26 C27 C28 -148.5(9) . . . . ? C26 C27 C28 C29 4.6(16) . . . . ? C27 C28 C29 C30 16.7(19) . . . . ? C28 C29 C30 C26 -31.3(17) . . . . ? C27 C26 C30 C29 32.8(13) . . . . ? Si7 C26 C30 C29 156.8(11) . . . . ? C35 C31 C32 C33 -28.0(17) . . . . ? Si8 C31 C32 C33 -154.2(11) . . . . ? C31 C32 C33 C34 35.5(19) . . . . ? C32 C33 C34 C35 -33(2) . . . . ? C33 C34 C35 C31 17(2) . . . . ? C32 C31 C35 C34 7.8(18) . . . . ? Si8 C31 C35 C34 135.1(13) . . . . ? C41 C36 C37 C38 2.4(16) . . . . ? Si9 C36 C37 C38 -178.2(9) . . . . ? C36 C37 C38 C39 -3.4(18) . . . . ? C37 C38 C39 C40 3(2) . . . . ? C38 C39 C40 C41 -2(2) . . . . ? C39 C40 C41 C36 1(2) . . . . ? C37 C36 C41 C40 -1.0(18) . . . . ? Si9 C36 C41 C40 179.5(11) . . . . ? C47 C42 C43 C44 0.5(17) . . . . ? Si9 C42 C43 C44 177.3(9) . . . . ? C42 C43 C44 C45 -0.8(18) . . . . ? C43 C44 C45 C46 0(2) . . . . ? C44 C45 C46 C47 0(2) . . . . ? C43 C42 C47 C46 0.1(17) . . . . ? Si9 C42 C47 C46 -176.4(9) . . . . ? C45 C46 C47 C42 -1(2) . . . . ? C51 C49 O4 V 140.4(15) . . . . ? C50 C49 O4 V -94(2) . . . . ? Si5 O11 Si1 O5 65.9(9) . . . . ? Si5 O11 Si1 O3 -55.6(8) . . . . ? Si5 O11 Si1 O2 -175.1(7) . . . 2_765 ? Si2 O5 Si1 O11 -53.4(8) . . . . ? Si2 O5 Si1 O3 67.8(8) . . . . ? Si2 O5 Si1 O2 -172.3(6) . . . 2_765 ? V O3 Si1 O11 -110.5(11) . . . . ? V O3 Si1 O5 127.4(10) . . . . ? V O3 Si1 O2 8.2(12) . . . 2_765 ? Si3 O6 Si2 O10 -31.8(11) . . . . ? Si3 O6 Si2 O5 -149.3(9) . . . . ? Si3 O6 Si2 C1 92.3(10) . . . . ? Si6 O10 Si2 O6 -46.5(9) . . . . ? Si6 O10 Si2 O5 69.9(8) . . . . ? Si6 O10 Si2 C1 -172.2(8) . . . . ? Si1 O5 Si2 O6 108.6(7) . . . . ? Si1 O5 Si2 O10 -9.8(8) . . . . ? Si1 O5 Si2 C1 -129.5(7) . . . . ? C2 C1 Si2 O6 177.9(7) . . . . ? C5 C1 Si2 O6 59.6(7) . . . . ? C2 C1 Si2 O10 -58.3(8) . . . . ? C5 C1 Si2 O10 -176.6(6) . . . . ? C2 C1 Si2 O5 60.2(9) . . . . ? C5 C1 Si2 O5 -58.1(7) . . . . ? Si4 O7 Si3 O6 -104.1(9) . . . . ? Si4 O7 Si3 O9 14.7(10) . . . . ? Si4 O7 Si3 C6 135.0(9) . . . . ? Si2 O6 Si3 O7 144.1(9) . . . . ? Si2 O6 Si3 O9 25.0(11) . . . . ? Si2 O6 Si3 C6 -94.7(10) . . . . ? Si7 O9 Si3 O7 -58.5(9) . . . . ? Si7 O9 Si3 O6 59.7(9) . . . . ? Si7 O9 Si3 C6 -179.8(8) . . . . ? C10 C6 Si3 O7 -55.8(9) . . . . ? C7 C6 Si3 O7 -176.1(6) . . . . ? C10 C6 Si3 O6 -175.4(8) . . . . ? C7 C6 Si3 O6 64.4(8) . . . . ? C10 C6 Si3 O9 64.7(9) . . . . ? C7 C6 Si3 O9 -55.5(8) . . . . ? Si9 O16 Si4 O7 58.6(8) . . . . ? Si9 O16 Si4 O8 177.7(7) . . . . ? Si9 O16 Si4 C11 -63.5(9) . . . . ? Si3 O7 Si4 O16 144.7(9) . . . . ? Si3 O7 Si4 O8 27.7(10) . . . . ? Si3 O7 Si4 C11 -92.6(10) . . . . ? Si8 O8 Si4 O16 -125.3(8) . . . . ? Si8 O8 Si4 O7 -7.7(9) . . . . ? Si8 O8 Si4 C11 113.9(8) . . . . ? C15 C11 Si4 O16 -54.6(10) . . . . ? C12 C11 Si4 O16 -175.3(7) . . . . ? C15 C11 Si4 O7 -175.3(8) . . . . ? C12 C11 Si4 O7 64.0(9) . . . . ? C15 C11 Si4 O8 63.2(9) . . . . ? C12 C11 Si4 O8 -57.5(9) . . . . ? Si6 O12 Si5 O15 58.0(9) . . . . ? Si6 O12 Si5 O11 -56.9(9) . . . . ? Si6 O12 Si5 C16 -177.7(8) . . . . ? Si8 O15 Si5 O12 38.1(11) . . . . ? Si8 O15 Si5 O11 154.2(10) . . . . ? Si8 O15 Si5 C16 -85.2(11) . . . . ? Si1 O11 Si5 O12 -2.3(9) . . . . ? Si1 O11 Si5 O15 -117.8(8) . . . . ? Si1 O11 Si5 C16 119.4(8) . . . . ? C17 C16 Si5 O12 174.2(7) . . . . ? C20 C16 Si5 O12 55.5(8) . . . . ? C17 C16 Si5 O15 -64.7(8) . . . . ? C20 C16 Si5 O15 176.6(7) . . . . ? C17 C16 Si5 O11 54.2(9) . . . . ? C20 C16 Si5 O11 -64.5(8) . . . . ? Si5 O12 Si6 O10 36.2(9) . . . . ? Si5 O12 Si6 O13 -82.2(9) . . . . ? Si5 O12 Si6 C21 154.4(8) . . . . ? Si2 O10 Si6 O12 -44.2(9) . . . . ? Si2 O10 Si6 O13 74.0(9) . . . . ? Si2 O10 Si6 C21 -163.3(8) . . . . ? Si7 O13 Si6 O12 60.2(8) . . . . ? Si7 O13 Si6 O10 -59.2(8) . . . . ? Si7 O13 Si6 C21 -178.8(7) . . . . ? C25 C21 Si6 O12 178.7(8) . . . . ? C22 C21 Si6 O12 -61.0(9) . . . . ? C25 C21 Si6 O10 -61.6(8) . . . . ? C22 C21 Si6 O10 58.6(9) . . . . ? C25 C21 Si6 O13 58.3(9) . . . . ? C22 C21 Si6 O13 178.5(8) . . . . ? Si8 O14 Si7 O9 -43.7(9) . . . . ? Si8 O14 Si7 O13 75.5(9) . . . . ? Si8 O14 Si7 C26 -165.0(8) . . . . ? Si3 O9 Si7 O14 39.0(9) . . . . ? Si3 O9 Si7 O13 -79.7(9) . . . . ? Si3 O9 Si7 C26 161.6(8) . . . . ? Si6 O13 Si7 O14 -61.2(8) . . . . ? Si6 O13 Si7 O9 59.0(8) . . . . ? Si6 O13 Si7 C26 177.8(7) . . . . ? C27 C26 Si7 O14 -171.2(7) . . . . ? C30 C26 Si7 O14 70.8(8) . . . . ? C27 C26 Si7 O9 66.7(8) . . . . ? C30 C26 Si7 O9 -51.3(9) . . . . ? C27 C26 Si7 O13 -52.1(8) . . . . ? C30 C26 Si7 O13 -170.1(7) . . . . ? Si4 O8 Si8 O15 78.1(8) . . . . ? Si4 O8 Si8 O14 -40.4(9) . . . . ? Si4 O8 Si8 C31 -161.6(8) . . . . ? Si5 O15 Si8 O8 -162.1(10) . . . . ? Si5 O15 Si8 O14 -43.5(11) . . . . ? Si5 O15 Si8 C31 76.4(11) . . . . ? Si7 O14 Si8 O8 71.5(9) . . . . ? Si7 O14 Si8 O15 -45.7(9) . . . . ? Si7 O14 Si8 C31 -165.9(8) . . . . ? C32 C31 Si8 O8 71.2(12) . . . . ? C35 C31 Si8 O8 -51.5(10) . . . . ? C32 C31 Si8 O15 -170.1(11) . . . . ? C35 C31 Si8 O15 67.2(10) . . . . ? C32 C31 Si8 O14 -50.1(12) . . . . ? C35 C31 Si8 O14 -172.8(9) . . . . ? Si4 O16 Si9 C48 151.7(8) . . . . ? Si4 O16 Si9 C36 -87.2(8) . . . . ? Si4 O16 Si9 C42 32.0(9) . . . . ? C37 C36 Si9 O16 -13.3(10) . . . . ? C41 C36 Si9 O16 166.1(8) . . . . ? C37 C36 Si9 C48 105.2(10) . . . . ? C41 C36 Si9 C48 -75.4(10) . . . . ? C37 C36 Si9 C42 -132.8(9) . . . . ? C41 C36 Si9 C42 46.7(10) . . . . ? C47 C42 Si9 O16 109.6(9) . . . . ? C43 C42 Si9 O16 -67.0(10) . . . . ? C47 C42 Si9 C48 -8.6(11) . . . . ? C43 C42 Si9 C48 174.8(9) . . . . ? C47 C42 Si9 C36 -131.7(10) . . . . ? C43 C42 Si9 C36 51.8(10) . . . . ? C49 O4 V O1 -1.2(15) . . . . ? C49 O4 V O3 -113.4(14) . . . . ? C49 O4 V O2 109.9(14) . . . . ? Si1 O3 V O4 -110.0(13) . . . . ? Si1 O3 V O1 141.0(12) . . . . ? Si1 O3 V O2 27.7(12) . . . . ? Si1 O2 V O4 60.1(11) 2_765 . . . ? Si1 O2 V O1 167.0(10) 2_765 . . . ? Si1 O2 V O3 -80.3(9) 2_765 . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 23.21 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 1.085 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.110 # Attachment 'complex_3.CIF' data_c:\ziemer\co-20\ohde9 _database_code_depnum_ccdc_archive 'CCDC 640135' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H64 O14 Si7 V, C24 H20 P, 2(C H2 Cl2)' _chemical_formula_sum 'C61 H88 Cl4 O14 P Si7 V' _chemical_formula_weight 1465.65 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' P P 0.1023 0.0942 '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' V V 0.3005 0.5294 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.292(3) _cell_length_b 14.543(4) _cell_length_c 24.244(6) _cell_angle_alpha 87.33(3) _cell_angle_beta 88.66(3) _cell_angle_gamma 85.85(3) _cell_volume 3614.6(17) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 22.5 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method none _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7948 _exptl_absorpt_correction_T_max 0.9625 _exptl_absorpt_process_details ; The correction was carried out by ABSCOR (Stoe, 1997), a modification of DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166. In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones. ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a \f-axis diffractometer supplied with an area detector. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_measurement_device 'Stoe IPDS diffractometer' _diffrn_measurement_method '\f-oscill.,\f-incr.=1.2\%,200 exposures' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21258 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.1718 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 24.16 _reflns_number_total 10790 _reflns_number_gt 3992 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'IPDS2.87 (Stoe & Cie, 1997)' _computing_cell_refinement 'IPDS2.87 (Stoe & Cie, 1997)' _computing_data_reduction 'IPDS2.87 (Stoe & Cie, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (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^)+(0.1618P)^2^] 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 10790 _refine_ls_number_parameters 796 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.2055 _refine_ls_R_factor_gt 0.1085 _refine_ls_wR_factor_ref 0.3183 _refine_ls_wR_factor_gt 0.2673 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.095 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4250(8) 0.7777(4) 0.2501(3) 0.076(2) Uani 1 1 d . . . H1 H 0.4743 0.7937 0.2153 0.092 Uiso 1 1 calc R . . C2 C 0.4234(8) 0.8608(5) 0.2891(4) 0.096(3) Uani 1 1 d . . . H2A H 0.4223 0.9201 0.2673 0.115 Uiso 1 1 calc R . . H2B H 0.3460 0.8617 0.3141 0.115 Uiso 1 1 calc R . . C3 C 0.5471(10) 0.8446(7) 0.3214(5) 0.126(4) Uani 1 1 d . . . H3A H 0.6120 0.8874 0.3073 0.152 Uiso 1 1 calc R . . H3B H 0.5289 0.8560 0.3608 0.152 Uiso 1 1 calc R . . C4 C 0.5993(12) 0.7467(9) 0.3151(6) 0.176(5) Uani 1 1 d . . . H4A H 0.6849 0.7451 0.2956 0.211 Uiso 1 1 calc R . . H4B H 0.6109 0.7150 0.3519 0.211 Uiso 1 1 calc R . . C5 C 0.5060(8) 0.7000(5) 0.2833(4) 0.086(3) Uani 1 1 d . . . H5A H 0.4484 0.6648 0.3084 0.103 Uiso 1 1 calc R . . H5B H 0.5524 0.6568 0.2579 0.103 Uiso 1 1 calc R . . C6 C -0.1302(10) 0.4603(5) 0.2686(4) 0.130(4) Uani 1 1 d D . . H6 H -0.1135 0.4714 0.3081 0.155 Uiso 1 1 d R . . C7 C -0.0825(12) 0.3788(6) 0.2321(5) 0.224(7) Uani 1 1 d D . . H7A H -0.0440 0.3611 0.2685 0.269 Uiso 1 1 d R . . H7B H -0.0108 0.3868 0.2048 0.269 Uiso 1 1 d R . . C8 C -0.1705(11) 0.2996(6) 0.2514(5) 0.179(6) Uani 1 1 d D . . H8A H -0.1949 0.3048 0.2121 0.215 Uiso 1 1 d R . . H8B H -0.1381 0.2359 0.2627 0.215 Uiso 1 1 d R . . C9 C -0.2863(12) 0.3451(7) 0.2822(7) 0.211(7) Uani 1 1 d D . . H9A H -0.2676 0.3224 0.3206 0.253 Uiso 1 1 d R . . H9B H -0.3741 0.3273 0.2731 0.253 Uiso 1 1 d R . . C10 C -0.2637(11) 0.4532(6) 0.2824(7) 0.213(8) Uani 1 1 d D . . H10A H -0.3123 0.4799 0.2500 0.255 Uiso 1 1 d R . . H10B H -0.3003 0.4816 0.3162 0.255 Uiso 1 1 d R . . C11 C -0.2707(9) 0.9835(5) 0.1431(3) 0.092(3) Uani 1 1 d . . . H11 H -0.2811 0.9612 0.1052 0.111 Uiso 1 1 calc R . . C12 C -0.4079(9) 0.9980(6) 0.1706(5) 0.109(3) Uani 1 1 d . . . H12A H -0.4703 0.9608 0.1527 0.131 Uiso 1 1 calc R . . H12B H -0.4045 0.9788 0.2103 0.131 Uiso 1 1 calc R . . C13 C -0.4497(10) 1.0986(5) 0.1638(4) 0.112(3) Uani 1 1 d . . . H13A H -0.4554 1.1270 0.2001 0.134 Uiso 1 1 calc R . . H13B H -0.5364 1.1070 0.1466 0.134 Uiso 1 1 calc R . . C14 C -0.3498(9) 1.1427(6) 0.1274(5) 0.116(4) Uani 1 1 d . . . H14A H -0.3391 1.2067 0.1378 0.139 Uiso 1 1 calc R . . H14B H -0.3740 1.1435 0.0881 0.139 Uiso 1 1 calc R . . C15 C -0.2281(9) 1.0820(5) 0.1377(4) 0.106(3) Uani 1 1 d . . . H15A H -0.1868 1.0983 0.1721 0.127 Uiso 1 1 calc R . . H15B H -0.1649 1.0886 0.1066 0.127 Uiso 1 1 calc R . . C16 C 0.3126(11) 0.4717(6) 0.1662(4) 0.152(4) Uani 1 1 d . . . H16 H 0.3843 0.5007 0.1447 0.182 Uiso 1 1 calc R . . C17 C 0.3791(13) 0.4314(7) 0.2096(5) 0.168(5) Uani 1 1 d . . . H17A H 0.3190 0.4172 0.2408 0.201 Uiso 1 1 calc R . . H17B H 0.4442 0.4723 0.2223 0.201 Uiso 1 1 calc R . . C18 C 0.4477(15) 0.3410(8) 0.1873(6) 0.192(6) Uani 1 1 d . . . H18A H 0.5415 0.3476 0.1796 0.231 Uiso 1 1 calc R . . H18B H 0.4378 0.2878 0.2137 0.231 Uiso 1 1 calc R . . C19 C 0.3761(15) 0.3304(7) 0.1353(5) 0.232(6) Uani 1 1 d . . . H19A H 0.4376 0.3305 0.1033 0.278 Uiso 1 1 calc R . . H19B H 0.3345 0.2710 0.1372 0.278 Uiso 1 1 calc R . . C20 C 0.2756(15) 0.4079(8) 0.1286(6) 0.256(6) Uani 1 1 d . . . H20A H 0.2763 0.4348 0.0903 0.307 Uiso 1 1 calc R . . H20B H 0.1877 0.3876 0.1379 0.307 Uiso 1 1 calc R . . C21 C -0.3588(7) 0.6810(5) 0.1186(3) 0.075(2) Uani 1 1 d . . . H21 H -0.4252 0.6747 0.1490 0.090 Uiso 1 1 calc R . . C22 C -0.3558(8) 0.5955(5) 0.0838(4) 0.101(3) Uani 1 1 d . . . H22A H -0.2678 0.5824 0.0673 0.122 Uiso 1 1 calc R . . H22B H -0.3792 0.5409 0.1068 0.122 Uiso 1 1 calc R . . C23 C -0.4528(13) 0.6174(7) 0.0398(4) 0.142(4) Uani 1 1 d . . . H23A H -0.5341 0.5873 0.0494 0.170 Uiso 1 1 calc R . . H23B H -0.4181 0.5943 0.0043 0.170 Uiso 1 1 calc R . . C24 C -0.4800(12) 0.7195(8) 0.0349(5) 0.181(5) Uani 1 1 d . . . H24A H -0.4522 0.7434 -0.0021 0.217 Uiso 1 1 calc R . . H24B H -0.5745 0.7357 0.0399 0.217 Uiso 1 1 calc R . . C25 C -0.4064(9) 0.7601(5) 0.0783(4) 0.103(3) Uani 1 1 d . . . H25A H -0.4632 0.8064 0.0979 0.123 Uiso 1 1 calc R . . H25B H -0.3313 0.7910 0.0617 0.123 Uiso 1 1 calc R . . C26 C 0.2143(8) 0.9789(9) 0.1076(4) 0.182(6) Uani 1 1 d D . . H26 H 0.2487 1.0141 0.1378 0.218 Uiso 1 1 d R . . C27 C 0.1175(11) 1.0366(9) 0.0684(6) 0.255(10) Uani 1 1 d D . . H27A H 0.0721 1.0881 0.0881 0.305 Uiso 1 1 d R . . H27B H 0.0545 1.0014 0.0493 0.305 Uiso 1 1 d R . . C28 C 0.2111(14) 1.0805(9) 0.0246(6) 0.397(12) Uani 1 1 d D . . H28A H 0.1799 1.1177 -0.0083 0.476 Uiso 1 1 d R . . H28B H 0.2725 1.1155 0.0448 0.476 Uiso 1 1 d R . . C29 C 0.3205(17) 1.0137(12) 0.0166(4) 0.474(16) Uani 1 1 d D . . H29A H 0.4012 1.0216 -0.0057 0.569 Uiso 1 1 d R . . H29B H 0.2594 0.9829 -0.0062 0.569 Uiso 1 1 d R . . C30 C 0.3274(13) 0.9487(9) 0.0673(6) 0.218(8) Uani 1 1 d D . . H30A H 0.4142 0.9602 0.0811 0.262 Uiso 1 1 d R . . H30B H 0.3258 0.8824 0.0599 0.262 Uiso 1 1 d R . . C31 C 0.0594(11) 0.6567(13) 0.0062(4) 0.229(7) Uani 1 1 d D . . H31 H 0.0007 0.6052 0.0042 0.275 Uiso 1 1 calc R . . C32 C 0.1871(15) 0.6254(14) -0.0168(5) 0.311(10) Uani 1 1 d D . . H32A H 0.2186 0.5634 -0.0020 0.373 Uiso 1 1 calc R . . H32B H 0.2540 0.6700 -0.0123 0.373 Uiso 1 1 calc R . . C33 C 0.140(2) 0.6246(9) -0.0769(4) 0.281(9) Uani 1 1 d . . . H33A H 0.2148 0.6270 -0.1031 0.337 Uiso 1 1 calc R . . H33B H 0.0965 0.5671 -0.0824 0.337 Uiso 1 1 calc R . . C34 C 0.0521(18) 0.7011(9) -0.0869(4) 0.205(7) Uani 1 1 d . . . H34A H -0.0232 0.6840 -0.1079 0.246 Uiso 1 1 calc R . . H34B H 0.0950 0.7508 -0.1079 0.246 Uiso 1 1 calc R . . C35 C 0.0080(16) 0.7322(11) -0.0291(4) 0.198(7) Uani 1 1 d . . . H35A H 0.0453 0.7907 -0.0206 0.238 Uiso 1 1 calc R . . H35B H -0.0882 0.7402 -0.0258 0.238 Uiso 1 1 calc R . . C36 C 0.3314(7) 0.3253(4) 0.3729(2) 0.0591(18) Uani 1 1 d . . . C37 C 0.2063(8) 0.3698(4) 0.3673(3) 0.082(2) Uani 1 1 d . . . H37 H 0.1319 0.3347 0.3675 0.098 Uiso 1 1 calc R . . C38 C 0.1921(8) 0.4653(5) 0.3615(4) 0.091(3) Uani 1 1 d . . . H38 H 0.1077 0.4958 0.3584 0.109 Uiso 1 1 calc R . . C39 C 0.2973(8) 0.5146(5) 0.3603(3) 0.084(2) Uani 1 1 d . . . H39 H 0.2858 0.5798 0.3553 0.101 Uiso 1 1 calc R . . C40 C 0.4195(10) 0.4745(6) 0.3659(4) 0.106(3) Uani 1 1 d . . . H40 H 0.4925 0.5110 0.3651 0.127 Uiso 1 1 calc R . . C41 C 0.4365(8) 0.3777(5) 0.3728(4) 0.090(3) Uani 1 1 d . . . H41 H 0.5214 0.3487 0.3775 0.108 Uiso 1 1 calc R . . C42 C 0.2472(8) 0.1526(4) 0.3371(3) 0.078(2) Uani 1 1 d . . . C43 C 0.1938(8) 0.0705(6) 0.3551(5) 0.105(3) Uani 1 1 d . . . H43 H 0.2072 0.0448 0.3915 0.126 Uiso 1 1 calc R . . C44 C 0.1200(11) 0.0279(6) 0.3176(5) 0.128(4) Uani 1 1 d . . . H44 H 0.0782 -0.0260 0.3292 0.153 Uiso 1 1 calc R . . C45 C 0.1063(10) 0.0620(6) 0.2642(4) 0.116(3) Uani 1 1 d . . . H45 H 0.0632 0.0280 0.2385 0.140 Uiso 1 1 calc R . . C46 C 0.1536(12) 0.1434(7) 0.2477(4) 0.146(4) Uani 1 1 d . . . H46 H 0.1373 0.1705 0.2119 0.175 Uiso 1 1 calc R . . C47 C 0.2291(11) 0.1871(6) 0.2865(4) 0.121(4) Uani 1 1 d . . . H47 H 0.2672 0.2427 0.2753 0.145 Uiso 1 1 calc R . . C48 C 0.3078(9) 0.1770(5) 0.4556(3) 0.083(2) Uani 1 1 d . . . C49 C 0.2307(11) 0.2326(7) 0.4864(3) 0.119(4) Uani 1 1 d . . . H49 H 0.2012 0.2915 0.4711 0.143 Uiso 1 1 calc R . . C50 C 0.1912(12) 0.2079(8) 0.5404(4) 0.165(4) Uani 1 1 d . . . H50 H 0.1280 0.2461 0.5594 0.198 Uiso 1 1 calc R . . C51 C 0.2423(11) 0.1313(7) 0.5647(4) 0.119(4) Uani 1 1 d . . . H51 H 0.2218 0.1173 0.6024 0.143 Uiso 1 1 calc R . . C52 C 0.3229(10) 0.0730(7) 0.5367(3) 0.118(4) Uani 1 1 d . . . H52 H 0.3553 0.0161 0.5539 0.141 Uiso 1 1 calc R . . C53 C 0.3593(9) 0.0959(6) 0.4819(3) 0.099(3) Uani 1 1 d . . . H53 H 0.4196 0.0558 0.4627 0.119 Uiso 1 1 calc R . . C54 C 0.5143(8) 0.1633(5) 0.3751(3) 0.075(2) Uani 1 1 d . . . C55 C 0.6113(9) 0.1868(6) 0.4111(4) 0.095(3) Uani 1 1 d . . . H55 H 0.5866 0.2225 0.4419 0.114 Uiso 1 1 calc R . . C56 C 0.7439(11) 0.1586(7) 0.4024(4) 0.118(4) Uani 1 1 d . . . H56 H 0.8082 0.1754 0.4269 0.142 Uiso 1 1 calc R . . C57 C 0.7777(10) 0.1069(7) 0.3583(4) 0.116(4) Uani 1 1 d . . . H57 H 0.8667 0.0879 0.3515 0.139 Uiso 1 1 calc R . . C58 C 0.6834(10) 0.0817(5) 0.3234(4) 0.098(3) Uani 1 1 d . . . H58 H 0.7075 0.0417 0.2944 0.118 Uiso 1 1 calc R . . C59 C 0.5566(9) 0.1134(4) 0.3299(3) 0.079(2) Uani 1 1 d . . . H59 H 0.4956 0.1009 0.3029 0.095 Uiso 1 1 calc R . . C60 C 0.2931(13) 0.7394(8) 0.4328(8) 0.106(6) Uiso 0.50 1 d PD . . H60A H 0.2241 0.7061 0.4525 0.127 Uiso 0.50 1 calc PR . . H60B H 0.2845 0.7307 0.3928 0.127 Uiso 0.50 1 calc PR . . C61 C 0.0959(11) 0.8615(9) 0.4538(7) 0.107(6) Uiso 0.50 1 d PD . . H61A H 0.0557 0.8596 0.4172 0.129 Uiso 0.50 1 calc PR . . H61B H 0.0727 0.8060 0.4760 0.129 Uiso 0.50 1 calc PR . . C62 C -0.355(4) 0.409(3) 0.4960(16) 0.144(12) Uiso 0.33 1 d P . . C63 C -0.158(4) 0.520(3) 0.4352(17) 0.155(12) Uiso 0.33 1 d PU . . C64 C -0.136(6) 0.445(4) 0.494(3) 0.238(16) Uiso 0.33 1 d PU A . O1 O -0.0497(5) 0.8212(3) 0.3256(2) 0.0924(17) Uani 1 1 d . . . O2 O 0.0545(7) 0.6826(4) 0.3875(2) 0.107(2) Uani 1 1 d . . . O3 O 0.1754(5) 0.7359(4) 0.2874(2) 0.1035(19) Uani 1 1 d . . . O4 O -0.0619(6) 0.6371(4) 0.2920(2) 0.1034(19) Uani 1 1 d . . . O5 O -0.1575(5) 0.9277(3) 0.2448(2) 0.0842(15) Uani 1 1 d . . . H5 H -0.105(7) 0.884(5) 0.264(3) 0.101 Uiso 1 1 d . . . O6 O 0.2737(5) 0.6533(3) 0.2002(2) 0.0907(17) Uani 1 1 d . . . O7 O 0.2001(7) 0.8287(4) 0.1911(2) 0.146(2) Uani 1 1 d . . . O8 O 0.0749(6) 0.5500(3) 0.2153(2) 0.0952(18) Uani 1 1 d . . . O9 O -0.1648(6) 0.6179(3) 0.1956(2) 0.0900(17) Uani 1 1 d . . . O10 O -0.2037(5) 0.7967(3) 0.1772(2) 0.0799(15) Uani 1 1 d . . . O11 O -0.0148(6) 0.9063(4) 0.1530(3) 0.113(2) Uani 1 1 d . . . O12 O 0.1413(6) 0.6095(4) 0.1155(2) 0.111(2) Uani 1 1 d . . . O13 O -0.0898(5) 0.6964(3) 0.10020(19) 0.0853(16) Uani 1 1 d U . . O14 O 0.1222(6) 0.7861(5) 0.0928(2) 0.106(2) Uani 1 1 d . . . P P 0.3476(2) 0.20357(12) 0.38470(7) 0.0705(6) Uani 1 1 d . . . Si1 Si 0.2635(2) 0.74909(14) 0.23232(8) 0.0776(6) Uani 1 1 d . . . Si2 Si -0.0698(3) 0.56925(13) 0.24154(9) 0.0816(7) Uani 1 1 d . . . Si3 Si -0.1569(2) 0.90022(12) 0.18082(8) 0.0714(6) Uani 1 1 d . . . Si4 Si 0.1951(2) 0.57412(15) 0.17525(9) 0.0938(7) Uani 1 1 d . . . Si5 Si -0.2011(2) 0.69911(12) 0.14886(8) 0.0688(6) Uani 1 1 d U . . Si6 Si 0.1286(3) 0.86822(19) 0.13603(10) 0.0990(8) Uani 1 1 d . . . Si7 Si 0.0606(3) 0.6914(2) 0.08113(8) 0.1033(9) Uani 1 1 d U . . V V 0.02558(13) 0.72141(8) 0.32489(5) 0.0738(4) Uani 1 1 d . . . Cl1 Cl 0.2671(4) 0.8582(2) 0.44486(11) 0.1453(12) Uani 1 1 d D . . Cl2 Cl 0.0310(8) 0.9607(5) 0.4867(3) 0.181(3) Uiso 0.50 1 d PD . . Cl3 Cl 0.4447(5) 0.6902(3) 0.4536(2) 0.1119(15) Uiso 0.50 1 d PD . . Cl4S Cl -0.177(2) 0.3495(11) 0.4463(11) 0.274(11) Uiso 0.264(6) 1 d PDU A 2 Cl4 Cl -0.1005(10) 0.3885(7) 0.4467(5) 0.305(5) Uiso 0.736(6) 1 d PDU A 1 Cl5 Cl -0.2948(10) 0.5419(7) 0.4652(5) 0.314(5) Uiso 0.736(6) 1 d PDU A 1 Cl5S Cl -0.097(2) 0.5353(12) 0.4699(11) 0.274(10) Uiso 0.264(6) 1 d PDU 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 C1 0.094(5) 0.056(4) 0.074(4) 0.008(3) 0.025(4) 0.015(4) C2 0.092(6) 0.064(4) 0.134(7) -0.006(5) 0.021(6) -0.023(4) C3 0.119(8) 0.122(7) 0.144(8) -0.026(6) -0.003(7) -0.034(6) C4 0.141(9) 0.157(10) 0.232(13) -0.042(9) -0.089(9) 0.021(8) C5 0.081(5) 0.073(5) 0.102(6) 0.015(4) -0.002(5) 0.002(4) C6 0.202(11) 0.069(5) 0.121(7) -0.012(5) -0.022(8) -0.023(6) C7 0.405(19) 0.121(8) 0.160(10) -0.040(7) 0.110(12) -0.130(10) C8 0.277(16) 0.088(7) 0.177(12) -0.003(7) 0.036(12) -0.062(9) C9 0.238(15) 0.149(10) 0.245(17) 0.052(11) 0.053(14) -0.069(10) C10 0.121(9) 0.113(8) 0.39(2) 0.111(11) -0.004(13) -0.013(7) C11 0.126(7) 0.053(4) 0.098(5) 0.003(4) -0.036(5) 0.002(4) C12 0.096(6) 0.076(5) 0.154(8) 0.010(5) -0.042(6) 0.001(4) C13 0.115(7) 0.068(5) 0.149(8) -0.009(5) -0.016(6) 0.025(5) C14 0.111(7) 0.079(5) 0.147(8) 0.032(5) 0.016(7) 0.033(5) C15 0.091(6) 0.079(5) 0.141(8) 0.038(5) 0.000(6) 0.012(4) C16 0.182(9) 0.127(6) 0.144(7) -0.079(5) -0.068(6) 0.083(6) C17 0.216(11) 0.105(6) 0.174(10) -0.053(6) -0.052(9) 0.084(7) C18 0.254(14) 0.127(8) 0.183(12) -0.031(8) -0.005(11) 0.091(9) C19 0.376(15) 0.156(7) 0.145(8) -0.084(6) -0.084(10) 0.181(8) C20 0.305(13) 0.189(8) 0.271(11) -0.166(7) -0.165(10) 0.157(8) C21 0.086(5) 0.065(4) 0.074(4) -0.012(3) -0.016(4) 0.011(4) C22 0.105(6) 0.072(4) 0.131(6) -0.037(4) -0.041(5) -0.004(4) C23 0.222(11) 0.099(6) 0.109(7) -0.022(5) -0.050(7) -0.020(7) C24 0.257(10) 0.124(8) 0.171(8) -0.003(7) -0.147(7) -0.039(8) C25 0.126(6) 0.059(4) 0.127(6) -0.015(4) -0.059(5) -0.010(4) C26 0.040(5) 0.377(18) 0.113(7) 0.097(9) 0.002(6) 0.019(8) C27 0.261(19) 0.133(11) 0.35(2) 0.082(13) 0.116(19) 0.018(12) C28 0.45(2) 0.148(12) 0.56(3) 0.104(14) 0.40(2) 0.000(14) C29 0.72(4) 0.54(3) 0.107(9) -0.063(14) -0.151(16) 0.39(3) C30 0.210(14) 0.174(12) 0.261(18) -0.018(13) -0.064(14) 0.072(11) C31 0.188(10) 0.413(19) 0.053(5) 0.026(8) 0.003(7) 0.175(11) C32 0.39(2) 0.40(2) 0.112(8) -0.120(10) -0.080(11) 0.216(18) C33 0.56(2) 0.186(9) 0.062(6) -0.032(6) -0.011(10) 0.211(12) C34 0.41(2) 0.145(9) 0.067(6) -0.002(6) -0.032(10) -0.093(12) C35 0.261(15) 0.245(14) 0.071(6) -0.014(8) -0.015(8) 0.105(12) C36 0.079(4) 0.054(3) 0.043(3) -0.001(3) -0.004(3) 0.005(3) C37 0.085(5) 0.046(4) 0.113(6) 0.009(4) -0.021(5) -0.002(3) C38 0.088(5) 0.066(4) 0.115(6) 0.003(4) -0.015(5) 0.021(4) C39 0.096(6) 0.060(4) 0.095(5) -0.003(4) -0.004(5) 0.002(4) C40 0.120(7) 0.083(5) 0.115(7) 0.024(5) -0.011(6) -0.019(5) C41 0.080(5) 0.076(5) 0.111(6) 0.012(4) -0.006(5) 0.008(4) C42 0.086(5) 0.050(4) 0.095(5) -0.010(4) 0.021(5) 0.003(4) C43 0.092(6) 0.073(5) 0.151(8) -0.004(5) -0.024(6) -0.010(4) C44 0.154(9) 0.070(5) 0.159(9) -0.003(6) -0.033(8) -0.004(6) C45 0.131(7) 0.089(5) 0.137(7) -0.051(5) -0.010(6) -0.032(5) C46 0.225(11) 0.129(7) 0.095(6) -0.041(5) -0.013(7) -0.069(8) C47 0.210(10) 0.081(5) 0.077(5) -0.007(4) -0.018(6) -0.044(6) C48 0.119(6) 0.060(4) 0.065(4) 0.007(3) 0.019(5) 0.013(4) C49 0.167(9) 0.108(6) 0.073(5) 0.009(5) 0.015(6) 0.048(6) C50 0.208(9) 0.185(8) 0.076(6) 0.018(6) 0.039(7) 0.132(7) C51 0.135(8) 0.131(8) 0.082(6) 0.004(6) 0.013(6) 0.039(6) C52 0.130(8) 0.141(7) 0.069(5) 0.039(5) 0.024(6) 0.042(6) C53 0.112(7) 0.096(6) 0.083(5) 0.006(5) 0.018(5) 0.023(5) C54 0.097(6) 0.072(4) 0.052(4) 0.009(3) 0.004(4) 0.013(4) C55 0.097(6) 0.096(6) 0.088(5) 0.006(5) 0.006(5) 0.017(5) C56 0.115(8) 0.126(8) 0.111(7) 0.006(6) 0.007(7) 0.000(6) C57 0.103(7) 0.114(7) 0.121(8) 0.030(6) 0.017(7) 0.020(6) C58 0.117(7) 0.063(4) 0.111(6) -0.011(4) 0.026(6) 0.016(5) C59 0.110(6) 0.054(4) 0.073(4) -0.012(3) 0.008(5) 0.002(4) O1 0.123(4) 0.068(3) 0.082(3) -0.011(2) -0.032(3) 0.036(3) O2 0.155(5) 0.100(4) 0.061(3) -0.002(3) -0.029(3) 0.028(4) O3 0.067(3) 0.132(4) 0.116(4) -0.055(3) 0.002(3) -0.006(3) O4 0.105(4) 0.126(4) 0.084(3) -0.044(3) -0.006(3) -0.016(3) O5 0.116(4) 0.055(2) 0.082(3) -0.014(2) -0.037(3) 0.007(2) O6 0.098(4) 0.082(3) 0.089(3) -0.017(3) -0.019(3) 0.027(3) O7 0.240(6) 0.092(4) 0.098(4) -0.015(3) -0.085(4) 0.081(4) O8 0.116(4) 0.064(3) 0.102(4) -0.009(3) -0.017(3) 0.029(3) O9 0.131(4) 0.058(3) 0.080(3) 0.006(2) -0.035(3) 0.004(3) O10 0.110(4) 0.047(2) 0.083(3) -0.016(2) -0.014(3) 0.005(2) O11 0.107(4) 0.080(3) 0.145(5) 0.047(3) 0.025(4) 0.013(3) O12 0.122(4) 0.132(4) 0.071(3) -0.030(3) -0.011(3) 0.058(3) O13 0.093(3) 0.089(3) 0.074(3) -0.024(2) -0.023(3) 0.013(3) O14 0.091(4) 0.167(5) 0.059(3) 0.000(3) -0.002(3) -0.007(4) P 0.1049(15) 0.0511(9) 0.0515(9) 0.0016(7) 0.0084(10) 0.0167(9) Si1 0.0912(14) 0.0780(12) 0.0588(10) -0.0081(9) -0.0103(11) 0.0326(11) Si2 0.1160(17) 0.0455(9) 0.0829(13) -0.0063(9) -0.0205(13) 0.0055(10) Si3 0.0910(15) 0.0486(9) 0.0729(12) -0.0008(9) -0.0106(11) 0.0076(9) Si4 0.1113(17) 0.0845(12) 0.0810(12) -0.0326(10) -0.0224(12) 0.0486(12) Si5 0.0874(14) 0.0523(9) 0.0666(10) -0.0171(8) -0.0152(10) 0.0095(9) Si6 0.0886(16) 0.1210(18) 0.0799(14) 0.0334(13) -0.0111(13) 0.0218(14) Si7 0.1005(17) 0.156(2) 0.0486(10) -0.0265(12) -0.0103(12) 0.0417(16) V 0.0882(9) 0.0700(7) 0.0617(7) -0.0101(6) -0.0107(7) 0.0135(6) Cl1 0.202(3) 0.130(2) 0.0997(17) -0.0093(16) -0.021(2) 0.023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.559(10) . ? C1 C2 1.568(10) . ? C1 Si1 1.809(8) . ? C1 H1 1.0000 . ? C2 C3 1.508(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.499(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.467(14) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C10 1.416(14) . ? C6 C7 1.556(11) . ? C6 Si2 1.831(8) . ? C6 H6 1.0000 . ? C7 C8 1.563(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.606(12) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C15 1.527(11) . ? C11 C12 1.552(12) . ? C11 Si3 1.848(8) . ? C11 H11 1.0000 . ? C12 C13 1.497(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.499(13) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.499(12) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.356(14) . ? C16 C20 1.408(14) . ? C16 Si4 1.867(9) . ? C16 H16 1.0000 . ? C17 C18 1.560(14) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.493(18) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.479(16) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.533(10) . ? C21 C25 1.534(10) . ? C21 Si5 1.838(8) . ? C21 H21 1.0000 . ? C22 C23 1.485(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.490(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.480(12) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C30 1.553(16) . ? C26 C27 1.564(12) . ? C26 Si6 1.979(12) . ? C26 H26 1.0000 . ? C27 C28 1.562(14) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.448(15) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.517(14) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C35 1.438(18) . ? C31 C32 1.466(14) . ? C31 Si7 1.909(11) . ? C31 H31 1.0000 . ? C32 C33 1.549(17) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.39(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.539(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C41 1.368(11) . ? C36 C37 1.405(10) . ? C36 P 1.777(6) . ? C37 C38 1.387(10) . ? C37 H37 0.9500 . ? C38 C39 1.341(11) . ? C38 H38 0.9500 . ? C39 C40 1.354(12) . ? C39 H39 0.9500 . ? C40 C41 1.408(11) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.318(11) . ? C42 C43 1.397(11) . ? C42 P 1.786(8) . ? C43 C44 1.394(14) . ? C43 H43 0.9500 . ? C44 C45 1.370(14) . ? C44 H44 0.9500 . ? C45 C46 1.352(13) . ? C45 H45 0.9500 . ? C46 C47 1.432(13) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.333(12) . ? C48 C53 1.391(11) . ? C48 P 1.789(8) . ? C49 C50 1.400(13) . ? C49 H49 0.9500 . ? C50 C51 1.315(14) . ? C50 H50 0.9500 . ? C51 C52 1.339(13) . ? C51 H51 0.9500 . ? C52 C53 1.403(12) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C59 1.386(10) . ? C54 C55 1.413(11) . ? C54 P 1.786(8) . ? C55 C56 1.410(13) . ? C55 H55 0.9500 . ? C56 C57 1.360(14) . ? C56 H56 0.9500 . ? C57 C58 1.383(13) . ? C57 H57 0.9500 . ? C58 C59 1.360(12) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 Cl3 1.745(12) . ? C60 Cl1 1.766(12) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 Cl2 1.763(13) . ? C61 Cl1 1.767(12) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? O1 V 1.596(5) . ? O2 V 1.621(5) . ? O3 Si1 1.609(6) . ? O3 V 1.791(6) . ? O4 Si2 1.615(5) . ? O4 V 1.797(5) . ? O5 Si3 1.620(5) . ? O5 H5 0.92(8) . ? O6 Si4 1.603(6) . ? O6 Si1 1.623(5) . ? O7 Si6 1.602(6) . ? O7 Si1 1.606(6) . ? O8 Si4 1.604(6) . ? O8 Si2 1.616(6) . ? O9 Si2 1.604(5) . ? O9 Si5 1.629(5) . ? O10 Si5 1.604(4) . ? O10 Si3 1.620(5) . ? O11 Si6 1.590(7) . ? O11 Si3 1.603(7) . ? O12 Si4 1.612(6) . ? O12 Si7 1.612(6) . ? O13 Si7 1.603(6) . ? O13 Si5 1.625(6) . ? O14 Si7 1.597(7) . ? O14 Si6 1.630(7) . ? Cl2 Cl2 1.441(14) 2_576 ? Cl3 C62 2.10(4) 2_566 ? 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 C5 C1 C2 102.5(6) . . ? C5 C1 Si1 114.8(5) . . ? C2 C1 Si1 113.0(5) . . ? C5 C1 H1 108.8 . . ? C2 C1 H1 108.8 . . ? Si1 C1 H1 108.8 . . ? C3 C2 C1 104.9(7) . . ? C3 C2 H2A 110.8 . . ? C1 C2 H2A 110.8 . . ? C3 C2 H2B 110.8 . . ? C1 C2 H2B 110.8 . . ? H2A C2 H2B 108.8 . . ? C4 C3 C2 108.4(8) . . ? C4 C3 H3A 110.0 . . ? C2 C3 H3A 110.0 . . ? C4 C3 H3B 110.0 . . ? C2 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C5 C4 C3 108.3(9) . . ? C5 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? C5 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C4 C5 C1 106.1(7) . . ? C4 C5 H5A 110.5 . . ? C1 C5 H5A 110.5 . . ? C4 C5 H5B 110.5 . . ? C1 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? C10 C6 C7 108.9(8) . . ? C10 C6 Si2 121.3(7) . . ? C7 C6 Si2 111.4(7) . . ? C10 C6 H6 89.2 . . ? C7 C6 H6 130.7 . . ? Si2 C6 H6 95.0 . . ? C6 C7 C8 104.0(8) . . ? C6 C7 H7A 76.6 . . ? C8 C7 H7A 80.1 . . ? C6 C7 H7B 119.5 . . ? C8 C7 H7B 136.5 . . ? H7A C7 H7B 108.4 . . ? C9 C8 C7 106.4(7) . . ? C9 C8 H8A 104.9 . . ? C7 C8 H8A 81.9 . . ? C9 C8 H8B 119.3 . . ? C7 C8 H8B 125.0 . . ? H8A C8 H8B 111.7 . . ? C8 C9 C10 106.6(8) . . ? C8 C9 H9A 100.7 . . ? C10 C9 H9A 103.9 . . ? C8 C9 H9B 117.5 . . ? C10 C9 H9B 117.8 . . ? H9A C9 H9B 108.1 . . ? C6 C10 C9 105.7(8) . . ? C6 C10 H10A 105.8 . . ? C9 C10 H10A 103.8 . . ? C6 C10 H10B 119.2 . . ? C9 C10 H10B 111.9 . . ? H10A C10 H10B 109.2 . . ? C15 C11 C12 101.9(6) . . ? C15 C11 Si3 114.8(6) . . ? C12 C11 Si3 114.7(6) . . ? C15 C11 H11 108.3 . . ? C12 C11 H11 108.3 . . ? Si3 C11 H11 108.3 . . ? C13 C12 C11 107.4(7) . . ? C13 C12 H12A 110.2 . . ? C11 C12 H12A 110.2 . . ? C13 C12 H12B 110.2 . . ? C11 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C12 C13 C14 107.4(8) . . ? C12 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? C12 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? C13 C14 C15 103.3(7) . . ? C13 C14 H14A 111.1 . . ? C15 C14 H14A 111.1 . . ? C13 C14 H14B 111.1 . . ? C15 C14 H14B 111.1 . . ? H14A C14 H14B 109.1 . . ? C14 C15 C11 105.9(7) . . ? C14 C15 H15A 110.6 . . ? C11 C15 H15A 110.6 . . ? C14 C15 H15B 110.6 . . ? C11 C15 H15B 110.6 . . ? H15A C15 H15B 108.7 . . ? C17 C16 C20 113.1(9) . . ? C17 C16 Si4 121.0(7) . . ? C20 C16 Si4 115.5(8) . . ? C17 C16 H16 100.8 . . ? C20 C16 H16 100.8 . . ? Si4 C16 H16 100.8 . . ? C16 C17 C18 105.0(10) . . ? C16 C17 H17A 110.7 . . ? C18 C17 H17A 110.7 . . ? C16 C17 H17B 110.7 . . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C19 C18 C17 102.3(10) . . ? C19 C18 H18A 111.3 . . ? C17 C18 H18A 111.3 . . ? C19 C18 H18B 111.3 . . ? C17 C18 H18B 111.3 . . ? H18A C18 H18B 109.2 . . ? C20 C19 C18 108.8(9) . . ? C20 C19 H19A 109.9 . . ? C18 C19 H19A 109.9 . . ? C20 C19 H19B 109.9 . . ? C18 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C16 C20 C19 103.4(11) . . ? C16 C20 H20A 111.1 . . ? C19 C20 H20A 111.1 . . ? C16 C20 H20B 111.1 . . ? C19 C20 H20B 111.1 . . ? H20A C20 H20B 109.0 . . ? C22 C21 C25 103.7(6) . . ? C22 C21 Si5 113.6(5) . . ? C25 C21 Si5 113.0(5) . . ? C22 C21 H21 108.8 . . ? C25 C21 H21 108.8 . . ? Si5 C21 H21 108.8 . . ? C23 C22 C21 106.1(7) . . ? 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 . . ? C22 C23 C24 108.5(8) . . ? C22 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? C22 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? C25 C24 C23 107.7(8) . . ? C25 C24 H24A 110.2 . . ? C23 C24 H24A 110.2 . . ? C25 C24 H24B 110.2 . . ? C23 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? C24 C25 C21 107.3(7) . . ? C24 C25 H25A 110.3 . . ? C21 C25 H25A 110.3 . . ? C24 C25 H25B 110.3 . . ? C21 C25 H25B 110.3 . . ? H25A C25 H25B 108.5 . . ? C30 C26 C27 102.4(8) . . ? C30 C26 Si6 109.0(9) . . ? C27 C26 Si6 108.1(7) . . ? C30 C26 H26 109.7 . . ? C27 C26 H26 114.7 . . ? Si6 C26 H26 112.3 . . ? C28 C27 C26 102.5(8) . . ? C28 C27 H27A 106.9 . . ? C26 C27 H27A 110.5 . . ? C28 C27 H27B 109.2 . . ? C26 C27 H27B 116.2 . . ? H27A C27 H27B 110.8 . . ? C29 C28 C27 107.1(10) . . ? C29 C28 H28A 117.1 . . ? C27 C28 H28A 123.1 . . ? C29 C28 H28B 86.0 . . ? C27 C28 H28B 107.5 . . ? H28A C28 H28B 109.5 . . ? C28 C29 C30 107.5(10) . . ? C28 C29 H29A 128.1 . . ? C30 C29 H29A 118.5 . . ? C28 C29 H29B 84.3 . . ? C30 C29 H29B 100.7 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C26 108.2(9) . . ? C29 C30 H30A 100.6 . . ? C26 C30 H30A 113.0 . . ? C29 C30 H30B 115.1 . . ? C26 C30 H30B 110.7 . . ? H30A C30 H30B 109.0 . . ? C35 C31 C32 107.3(12) . . ? C35 C31 Si7 110.8(11) . . ? C32 C31 Si7 114.8(8) . . ? C35 C31 H31 107.9 . . ? C32 C31 H31 107.9 . . ? Si7 C31 H31 107.8 . . ? C31 C32 C33 94.6(11) . . ? C31 C32 H32A 112.7 . . ? C33 C32 H32A 112.8 . . ? C31 C32 H32B 112.9 . . ? C33 C32 H32B 112.9 . . ? H32A C32 H32B 110.3 . . ? C34 C33 C32 108.9(10) . . ? C34 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? C34 C33 H33B 109.9 . . ? C32 C33 H33B 110.0 . . ? H33A C33 H33B 108.3 . . ? C33 C34 C35 104.9(10) . . ? C33 C34 H34A 110.8 . . ? C35 C34 H34A 110.8 . . ? C33 C34 H34B 110.8 . . ? C35 C34 H34B 110.8 . . ? H34A C34 H34B 108.9 . . ? C31 C35 C34 102.2(11) . . ? C31 C35 H35A 111.4 . . ? C34 C35 H35A 111.3 . . ? C31 C35 H35B 111.3 . . ? C34 C35 H35B 111.3 . . ? H35A C35 H35B 109.2 . . ? C41 C36 C37 118.9(6) . . ? C41 C36 P 121.8(5) . . ? C37 C36 P 119.1(5) . . ? C38 C37 C36 119.5(7) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C39 C38 C37 120.1(8) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 122.2(8) . . ? C38 C39 H39 118.9 . . ? C40 C39 H39 118.9 . . ? C39 C40 C41 118.8(9) . . ? C39 C40 H40 120.6 . . ? C41 C40 H40 120.6 . . ? C36 C41 C40 120.4(8) . . ? C36 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C47 C42 C43 120.8(8) . . ? C47 C42 P 122.4(6) . . ? C43 C42 P 116.7(7) . . ? C44 C43 C42 117.3(9) . . ? C44 C43 H43 121.4 . . ? C42 C43 H43 121.4 . . ? C45 C44 C43 121.6(10) . . ? C45 C44 H44 119.2 . . ? C43 C44 H44 119.2 . . ? C46 C45 C44 120.7(9) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 117.3(9) . . ? C45 C46 H46 121.3 . . ? C47 C46 H46 121.3 . . ? C42 C47 C46 122.0(9) . . ? C42 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C49 C48 C53 116.2(7) . . ? C49 C48 P 123.3(6) . . ? C53 C48 P 120.5(6) . . ? C48 C49 C50 122.9(9) . . ? C48 C49 H49 118.6 . . ? C50 C49 H49 118.6 . . ? C51 C50 C49 119.5(9) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C50 C51 C52 120.7(9) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C51 C52 C53 119.8(9) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C48 C53 C52 120.5(8) . . ? C48 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C59 C54 C55 116.5(8) . . ? C59 C54 P 122.0(6) . . ? C55 C54 P 121.3(6) . . ? C56 C55 C54 121.7(8) . . ? C56 C55 H55 119.1 . . ? C54 C55 H55 119.1 . . ? C57 C56 C55 118.5(10) . . ? C57 C56 H56 120.8 . . ? C55 C56 H56 120.8 . . ? C56 C57 C58 120.4(10) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C59 C58 C57 121.0(8) . . ? C59 C58 H58 119.5 . . ? C57 C58 H58 119.5 . . ? C58 C59 C54 121.5(8) . . ? C58 C59 H59 119.2 . . ? C54 C59 H59 119.2 . . ? Cl3 C60 Cl1 114.1(8) . . ? Cl3 C60 H60A 108.7 . . ? Cl1 C60 H60A 108.7 . . ? Cl3 C60 H60B 108.7 . . ? Cl1 C60 H60B 108.7 . . ? H60A C60 H60B 107.6 . . ? Cl2 C61 Cl1 112.9(8) . . ? Cl2 C61 H61A 109.0 . . ? Cl1 C61 H61A 109.0 . . ? Cl2 C61 H61B 109.0 . . ? Cl1 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? Si1 O3 V 154.3(4) . . ? Si2 O4 V 148.1(4) . . ? Si3 O5 H5 108(5) . . ? Si4 O6 Si1 146.0(4) . . ? Si6 O7 Si1 154.9(4) . . ? Si4 O8 Si2 153.7(4) . . ? Si2 O9 Si5 151.6(4) . . ? Si5 O10 Si3 151.9(4) . . ? Si6 O11 Si3 155.3(4) . . ? Si4 O12 Si7 145.4(4) . . ? Si7 O13 Si5 150.2(3) . . ? Si7 O14 Si6 145.4(4) . . ? C36 P C42 108.5(3) . . ? C36 P C54 109.4(3) . . ? C42 P C54 110.5(3) . . ? C36 P C48 108.6(3) . . ? C42 P C48 113.8(4) . . ? C54 P C48 106.0(4) . . ? O7 Si1 O3 111.6(4) . . ? O7 Si1 O6 107.8(3) . . ? O3 Si1 O6 108.8(3) . . ? O7 Si1 C1 109.2(4) . . ? O3 Si1 C1 110.0(3) . . ? O6 Si1 C1 109.4(3) . . ? O9 Si2 O4 109.2(3) . . ? O9 Si2 O8 109.9(3) . . ? O4 Si2 O8 108.6(3) . . ? O9 Si2 C6 111.1(4) . . ? O4 Si2 C6 108.6(4) . . ? O8 Si2 C6 109.5(4) . . ? O11 Si3 O5 111.0(3) . . ? O11 Si3 O10 110.0(3) . . ? O5 Si3 O10 109.4(3) . . ? O11 Si3 C11 108.2(4) . . ? O5 Si3 C11 108.2(3) . . ? O10 Si3 C11 110.0(3) . . ? O6 Si4 O8 110.5(3) . . ? O6 Si4 O12 109.1(3) . . ? O8 Si4 O12 109.4(3) . . ? O6 Si4 C16 107.4(4) . . ? O8 Si4 C16 111.9(4) . . ? O12 Si4 C16 108.5(4) . . ? O10 Si5 O13 108.8(3) . . ? O10 Si5 O9 108.4(3) . . ? O13 Si5 O9 109.4(3) . . ? O10 Si5 C21 111.6(3) . . ? O13 Si5 C21 108.7(3) . . ? O9 Si5 C21 109.9(3) . . ? O11 Si6 O7 107.8(4) . . ? O11 Si6 O14 109.9(4) . . ? O7 Si6 O14 109.9(3) . . ? O11 Si6 C26 104.4(4) . . ? O7 Si6 C26 108.7(4) . . ? O14 Si6 C26 115.7(4) . . ? O14 Si7 O13 110.0(3) . . ? O14 Si7 O12 108.0(3) . . ? O13 Si7 O12 110.2(3) . . ? O14 Si7 C31 117.2(6) . . ? O13 Si7 C31 104.2(4) . . ? O12 Si7 C31 107.1(5) . . ? O1 V O2 110.0(3) . . ? O1 V O3 106.2(3) . . ? O2 V O3 110.3(3) . . ? O1 V O4 113.9(3) . . ? O2 V O4 107.5(3) . . ? O3 V O4 108.8(3) . . ? C60 Cl1 C61 97.4(6) . . ? Cl2 Cl2 C61 176.0(10) 2_576 . ? C60 Cl3 C62 90.9(12) . 2_566 ? 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 C5 C1 C2 C3 28.0(9) . . . . ? Si1 C1 C2 C3 152.1(6) . . . . ? C1 C2 C3 C4 -15.5(11) . . . . ? C2 C3 C4 C5 -4.3(14) . . . . ? C3 C4 C5 C1 22.5(12) . . . . ? C2 C1 C5 C4 -31.1(10) . . . . ? Si1 C1 C5 C4 -154.0(7) . . . . ? C10 C6 C7 C8 -29.2(13) . . . . ? Si2 C6 C7 C8 -165.7(8) . . . . ? C6 C7 C8 C9 17.3(14) . . . . ? C7 C8 C9 C10 -1.5(15) . . . . ? C7 C6 C10 C9 28.2(14) . . . . ? Si2 C6 C10 C9 159.5(9) . . . . ? C8 C9 C10 C6 -16.6(16) . . . . ? C15 C11 C12 C13 16.3(10) . . . . ? Si3 C11 C12 C13 140.9(7) . . . . ? C11 C12 C13 C14 6.7(11) . . . . ? C12 C13 C14 C15 -27.4(11) . . . . ? C13 C14 C15 C11 38.3(10) . . . . ? C12 C11 C15 C14 -33.6(10) . . . . ? Si3 C11 C15 C14 -158.2(7) . . . . ? C20 C16 C17 C18 27.7(16) . . . . ? Si4 C16 C17 C18 171.1(9) . . . . ? C16 C17 C18 C19 -15.7(15) . . . . ? C17 C18 C19 C20 0.0(16) . . . . ? C17 C16 C20 C19 -27.5(17) . . . . ? Si4 C16 C20 C19 -173.0(9) . . . . ? C18 C19 C20 C16 15.0(17) . . . . ? C25 C21 C22 C23 -25.9(9) . . . . ? Si5 C21 C22 C23 -148.9(7) . . . . ? C21 C22 C23 C24 18.8(12) . . . . ? C22 C23 C24 C25 -3.7(13) . . . . ? C23 C24 C25 C21 -13.0(12) . . . . ? C22 C21 C25 C24 23.9(10) . . . . ? Si5 C21 C25 C24 147.3(7) . . . . ? C30 C26 C27 C28 -32.4(14) . . . . ? Si6 C26 C27 C28 -147.4(9) . . . . ? C26 C27 C28 C29 34.5(16) . . . . ? C27 C28 C29 C30 -21.8(19) . . . . ? C28 C29 C30 C26 0.3(19) . . . . ? C27 C26 C30 C29 20.7(15) . . . . ? Si6 C26 C30 C29 135.1(11) . . . . ? C35 C31 C32 C33 -46.4(16) . . . . ? Si7 C31 C32 C33 -170.1(11) . . . . ? C31 C32 C33 C34 39.2(19) . . . . ? C32 C33 C34 C35 -18(2) . . . . ? C32 C31 C35 C34 38.0(17) . . . . ? Si7 C31 C35 C34 164.1(10) . . . . ? C33 C34 C35 C31 -10.6(18) . . . . ? C41 C36 C37 C38 0.5(11) . . . . ? P C36 C37 C38 176.0(6) . . . . ? C36 C37 C38 C39 1.2(13) . . . . ? C37 C38 C39 C40 -1.6(14) . . . . ? C38 C39 C40 C41 0.4(14) . . . . ? C37 C36 C41 C40 -1.6(12) . . . . ? P C36 C41 C40 -177.1(7) . . . . ? C39 C40 C41 C36 1.2(13) . . . . ? C47 C42 C43 C44 -0.7(13) . . . . ? P C42 C43 C44 -177.3(7) . . . . ? C42 C43 C44 C45 3.7(15) . . . . ? C43 C44 C45 C46 -6.6(17) . . . . ? C44 C45 C46 C47 6.2(17) . . . . ? C43 C42 C47 C46 0.6(15) . . . . ? P C42 C47 C46 177.0(8) . . . . ? C45 C46 C47 C42 -3.3(17) . . . . ? C53 C48 C49 C50 -6.6(16) . . . . ? P C48 C49 C50 174.5(9) . . . . ? C48 C49 C50 C51 7.6(19) . . . . ? C49 C50 C51 C52 -5.8(19) . . . . ? C50 C51 C52 C53 3.7(18) . . . . ? C49 C48 C53 C52 4.3(15) . . . . ? P C48 C53 C52 -176.7(8) . . . . ? C51 C52 C53 C48 -2.9(16) . . . . ? C59 C54 C55 C56 -1.8(12) . . . . ? P C54 C55 C56 -177.2(7) . . . . ? C54 C55 C56 C57 -0.5(14) . . . . ? C55 C56 C57 C58 -0.9(15) . . . . ? C56 C57 C58 C59 4.8(14) . . . . ? C57 C58 C59 C54 -7.3(13) . . . . ? C55 C54 C59 C58 5.7(11) . . . . ? P C54 C59 C58 -178.9(6) . . . . ? Cl5S C63 C64 Cl4 -126(4) . . . . ? Cl5 C63 C64 Cl4 130(3) . . . . ? Cl5 C63 C64 Cl5S -104(3) . . . . ? Cl4 C63 C64 Cl5S 126(4) . . . . ? Cl5S C63 C64 Cl4S -155(4) . . . . ? Cl5 C63 C64 Cl4S 101(2) . . . . ? Cl4 C63 C64 Cl4S -29.2(14) . . . . ? Cl5S C63 C64 Cl5 104(3) . . . . ? Cl4 C63 C64 Cl5 -130(3) . . . . ? C41 C36 P C42 -137.7(6) . . . . ? C37 C36 P C42 46.9(6) . . . . ? C41 C36 P C54 -17.2(7) . . . . ? C37 C36 P C54 167.4(5) . . . . ? C41 C36 P C48 98.1(7) . . . . ? C37 C36 P C48 -77.3(6) . . . . ? C47 C42 P C36 34.9(9) . . . . ? C43 C42 P C36 -148.6(6) . . . . ? C47 C42 P C54 -85.0(8) . . . . ? C43 C42 P C54 91.5(7) . . . . ? C47 C42 P C48 155.9(8) . . . . ? C43 C42 P C48 -27.6(7) . . . . ? C59 C54 P C36 -108.5(6) . . . . ? C55 C54 P C36 66.6(7) . . . . ? C59 C54 P C42 10.8(7) . . . . ? C55 C54 P C42 -174.0(6) . . . . ? C59 C54 P C48 134.6(6) . . . . ? C55 C54 P C48 -50.2(7) . . . . ? C49 C48 P C36 24.8(10) . . . . ? C53 C48 P C36 -154.1(7) . . . . ? C49 C48 P C42 -96.2(9) . . . . ? C53 C48 P C42 84.9(8) . . . . ? C49 C48 P C54 142.2(9) . . . . ? C53 C48 P C54 -36.7(9) . . . . ? Si6 O7 Si1 O3 -109.7(12) . . . . ? Si6 O7 Si1 O6 9.6(14) . . . . ? Si6 O7 Si1 C1 128.4(13) . . . . ? V O3 Si1 O7 48.3(10) . . . . ? V O3 Si1 O6 -70.4(9) . . . . ? V O3 Si1 C1 169.7(8) . . . . ? Si4 O6 Si1 O7 -69.3(7) . . . . ? Si4 O6 Si1 O3 51.8(7) . . . . ? Si4 O6 Si1 C1 172.1(6) . . . . ? C5 C1 Si1 O7 -171.9(5) . . . . ? C2 C1 Si1 O7 71.0(6) . . . . ? C5 C1 Si1 O3 65.3(6) . . . . ? C2 C1 Si1 O3 -51.8(6) . . . . ? C5 C1 Si1 O6 -54.1(6) . . . . ? C2 C1 Si1 O6 -171.2(5) . . . . ? Si5 O9 Si2 O4 65.4(8) . . . . ? Si5 O9 Si2 O8 -53.5(8) . . . . ? Si5 O9 Si2 C6 -174.8(7) . . . . ? V O4 Si2 O9 -98.6(7) . . . . ? V O4 Si2 O8 21.2(8) . . . . ? V O4 Si2 C6 140.1(7) . . . . ? Si4 O8 Si2 O9 34.5(9) . . . . ? Si4 O8 Si2 O4 -84.9(9) . . . . ? Si4 O8 Si2 C6 156.7(8) . . . . ? C10 C6 Si2 O9 -44.0(11) . . . . ? C7 C6 Si2 O9 86.2(8) . . . . ? C10 C6 Si2 O4 76.1(11) . . . . ? C7 C6 Si2 O4 -153.6(7) . . . . ? C10 C6 Si2 O8 -165.5(10) . . . . ? C7 C6 Si2 O8 -35.3(9) . . . . ? Si6 O11 Si3 O5 88.8(12) . . . . ? Si6 O11 Si3 O10 -32.6(13) . . . . ? Si6 O11 Si3 C11 -152.7(11) . . . . ? Si5 O10 Si3 O11 -26.1(8) . . . . ? Si5 O10 Si3 O5 -148.4(7) . . . . ? Si5 O10 Si3 C11 92.9(8) . . . . ? C15 C11 Si3 O11 -52.9(8) . . . . ? C12 C11 Si3 O11 -170.5(6) . . . . ? C15 C11 Si3 O5 67.5(7) . . . . ? C12 C11 Si3 O5 -50.1(6) . . . . ? C15 C11 Si3 O10 -173.1(6) . . . . ? C12 C11 Si3 O10 69.3(6) . . . . ? Si1 O6 Si4 O8 -39.2(7) . . . . ? Si1 O6 Si4 O12 81.2(7) . . . . ? Si1 O6 Si4 C16 -161.4(7) . . . . ? Si2 O8 Si4 O6 77.2(9) . . . . ? Si2 O8 Si4 O12 -42.9(9) . . . . ? Si2 O8 Si4 C16 -163.2(8) . . . . ? Si7 O12 Si4 O6 -52.0(9) . . . . ? Si7 O12 Si4 O8 69.0(9) . . . . ? Si7 O12 Si4 C16 -168.7(8) . . . . ? C17 C16 Si4 O6 58.0(11) . . . . ? C20 C16 Si4 O6 -159.4(10) . . . . ? C17 C16 Si4 O8 -63.4(11) . . . . ? C20 C16 Si4 O8 79.2(11) . . . . ? C17 C16 Si4 O12 175.8(10) . . . . ? C20 C16 Si4 O12 -41.7(11) . . . . ? Si3 O10 Si5 O13 6.2(8) . . . . ? Si3 O10 Si5 O9 125.1(7) . . . . ? Si3 O10 Si5 C21 -113.8(7) . . . . ? Si7 O13 Si5 O10 70.2(8) . . . . ? Si7 O13 Si5 O9 -48.0(8) . . . . ? Si7 O13 Si5 C21 -168.1(7) . . . . ? Si2 O9 Si5 O10 -57.8(8) . . . . ? Si2 O9 Si5 O13 60.7(8) . . . . ? Si2 O9 Si5 C21 180.0(7) . . . . ? C22 C21 Si5 O10 171.6(5) . . . . ? C25 C21 Si5 O10 53.9(6) . . . . ? C22 C21 Si5 O13 51.6(6) . . . . ? C25 C21 Si5 O13 -66.1(6) . . . . ? C22 C21 Si5 O9 -68.1(6) . . . . ? C25 C21 Si5 O9 174.2(5) . . . . ? Si3 O11 Si6 O7 -54.7(13) . . . . ? Si3 O11 Si6 O14 65.1(13) . . . . ? Si3 O11 Si6 C26 -170.2(11) . . . . ? Si1 O7 Si6 O11 110.5(13) . . . . ? Si1 O7 Si6 O14 -9.3(14) . . . . ? Si1 O7 Si6 C26 -136.9(13) . . . . ? Si7 O14 Si6 O11 -50.6(8) . . . . ? Si7 O14 Si6 O7 68.0(8) . . . . ? Si7 O14 Si6 C26 -168.5(6) . . . . ? C30 C26 Si6 O11 -155.4(7) . . . . ? C27 C26 Si6 O11 -44.9(9) . . . . ? C30 C26 Si6 O7 89.7(7) . . . . ? C27 C26 Si6 O7 -159.7(8) . . . . ? C30 C26 Si6 O14 -34.4(8) . . . . ? C27 C26 Si6 O14 76.1(9) . . . . ? Si6 O14 Si7 O13 40.3(8) . . . . ? Si6 O14 Si7 O12 -80.0(8) . . . . ? Si6 O14 Si7 C31 159.1(7) . . . . ? Si5 O13 Si7 O14 -70.4(8) . . . . ? Si5 O13 Si7 O12 48.5(8) . . . . ? Si5 O13 Si7 C31 163.2(8) . . . . ? Si4 O12 Si7 O14 52.3(9) . . . . ? Si4 O12 Si7 O13 -67.8(9) . . . . ? Si4 O12 Si7 C31 179.4(9) . . . . ? C35 C31 Si7 O14 -49.2(12) . . . . ? C32 C31 Si7 O14 72.6(15) . . . . ? C35 C31 Si7 O13 72.6(12) . . . . ? C32 C31 Si7 O13 -165.6(13) . . . . ? C35 C31 Si7 O12 -170.6(10) . . . . ? C32 C31 Si7 O12 -48.8(15) . . . . ? Si1 O3 V O1 -78.3(9) . . . . ? Si1 O3 V O2 162.6(8) . . . . ? Si1 O3 V O4 44.8(10) . . . . ? Si2 O4 V O1 114.6(7) . . . . ? Si2 O4 V O2 -123.2(7) . . . . ? Si2 O4 V O3 -3.7(8) . . . . ? Cl3 C60 Cl1 C61 -150.7(11) . . . . ? Cl2 C61 Cl1 C60 162.5(10) . . . . ? Cl1 C60 Cl3 C62 124.0(14) . . . 2_566 ? Cl5S C64 Cl4 C63 -31(2) . . . . ? Cl4S C64 Cl4 C63 108(3) . . . . ? Cl5 C64 Cl4 C63 35(2) . . . . ? Cl5S C63 Cl4 C64 43(4) . . . . ? Cl5 C63 Cl4 C64 -54(3) . . . . ? Cl5S C63 Cl5 C62 -97(3) . . . . ? C64 C63 Cl5 C62 -42(3) . . . . ? Cl4 C63 Cl5 C62 -6(3) . . . . ? Cl5S C63 Cl5 C64 -55(3) . . . . ? Cl4 C63 Cl5 C64 36(2) . . . . ? Cl3 C62 Cl5 C63 150(6) 2_566 . . . ? Cl3 C62 Cl5 C64 114(6) 2_566 . . . ? Cl4 C64 Cl5 C63 -50(3) . . . . ? Cl5S C64 Cl5 C63 42(2) . . . . ? Cl4S C64 Cl5 C63 -79(3) . . . . ? Cl4 C64 Cl5 C62 85(3) . . . . ? Cl5S C64 Cl5 C62 177(3) . . . . ? C63 C64 Cl5 C62 135(3) . . . . ? Cl4S C64 Cl5 C62 56(2) . . . . ? Cl5 C63 Cl5S C64 75(3) . . . . ? Cl4 C63 Cl5S C64 -36(3) . . . . ? Cl4 C64 Cl5S C63 52(4) . . . . ? Cl4S C64 Cl5S C63 29(5) . . . . ? Cl5 C64 Cl5S C63 -51(3) . . . . ? O5-H5 0.924 1.793 153.61 2.653 O1 . . . . _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 24.16 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.597 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.097 # Attachment 'complex_4.CIF' data_d:\x-data\ohde11 _database_code_depnum_ccdc_archive 'CCDC 662556' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H92 O14 P Si8 V' _chemical_formula_weight 1367.99 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' P P 0.1023 0.0942 '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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2305(8) _cell_length_b 13.1509(9) _cell_length_c 22.7799(17) _cell_angle_alpha 91.236(6) _cell_angle_beta 96.081(6) _cell_angle_gamma 110.382(5) _cell_volume 3408.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9163 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16343 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 28.00 _reflns_number_total 16343 _reflns_number_gt 9495 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^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 16343 _refine_ls_number_parameters 778 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8211(3) 0.7612(3) 0.32200(14) 0.0369(8) Uani 1 1 d . . . H1 H 0.7373 0.7567 0.3180 0.044 Uiso 1 1 calc R . . C2 C 0.8275(4) 0.6611(3) 0.28899(17) 0.0470(10) Uani 1 1 d . . . H2A H 0.7743 0.6434 0.2514 0.056 Uiso 1 1 calc R . . H2B H 0.9086 0.6741 0.2801 0.056 Uiso 1 1 calc R . . C3 C 0.7899(4) 0.5697(4) 0.3300(2) 0.0614(12) Uani 1 1 d . . . H3A H 0.7037 0.5319 0.3237 0.074 Uiso 1 1 calc R . . H3B H 0.8286 0.5162 0.3236 0.074 Uiso 1 1 calc R . . C4 C 0.8289(6) 0.6251(5) 0.3912(2) 0.088(2) Uani 1 1 d . . . H4A H 0.7654 0.5966 0.4166 0.106 Uiso 1 1 calc R . . H4B H 0.8989 0.6106 0.4093 0.106 Uiso 1 1 calc R . . C5 C 0.8580(4) 0.7451(4) 0.38652(18) 0.0636(13) Uani 1 1 d . . . H5A H 0.9433 0.7845 0.3973 0.076 Uiso 1 1 calc R . . H5B H 0.8147 0.7729 0.4133 0.076 Uiso 1 1 calc R . . C6 C 1.2950(3) 1.1415(3) 0.14637(14) 0.0353(8) Uani 1 1 d . . . H6 H 1.3681 1.1897 0.1710 0.042 Uiso 1 1 calc R . . C7 C 1.2669(4) 1.2058(4) 0.09456(17) 0.0508(10) Uani 1 1 d . . . H7A H 1.1812 1.1808 0.0822 0.061 Uiso 1 1 calc R . . H7B H 1.2953 1.2845 0.1063 0.061 Uiso 1 1 calc R . . C8 C 1.3286(7) 1.1847(5) 0.0460(2) 0.102(2) Uani 1 1 d . . . H8A H 1.2735 1.1630 0.0090 0.122 Uiso 1 1 calc R . . H8B H 1.3939 1.2520 0.0396 0.122 Uiso 1 1 calc R . . C9 C 1.3749(5) 1.0986(4) 0.06005(18) 0.0620(12) Uani 1 1 d . . . H9A H 1.4618 1.1287 0.0675 0.074 Uiso 1 1 calc R . . H9B H 1.3514 1.0424 0.0269 0.074 Uiso 1 1 calc R . . C10 C 1.3232(4) 1.0500(3) 0.11540(16) 0.0463(9) Uani 1 1 d . . . H10A H 1.3807 1.0283 0.1412 0.056 Uiso 1 1 calc R . . H10B H 1.2511 0.9855 0.1049 0.056 Uiso 1 1 calc R . . C11 C 1.0033(3) 1.4200(3) 0.37959(14) 0.0335(7) Uani 1 1 d . . . H11 H 0.9330 1.4268 0.3956 0.040 Uiso 1 1 calc R . . C12 C 1.0708(3) 1.5290(3) 0.35511(16) 0.0404(8) Uani 1 1 d . . . H12A H 1.0157 1.5627 0.3369 0.048 Uiso 1 1 calc R . . H12B H 1.1192 1.5185 0.3249 0.048 Uiso 1 1 calc R . . C13 C 1.1493(4) 1.6006(3) 0.40846(18) 0.0539(11) Uani 1 1 d . . . H13A H 1.2305 1.6359 0.3988 0.065 Uiso 1 1 calc R . . H13B H 1.1188 1.6579 0.4196 0.065 Uiso 1 1 calc R . . C14 C 1.1477(4) 1.5272(3) 0.45848(17) 0.0545(11) Uani 1 1 d . . . H14A H 1.1031 1.5419 0.4894 0.065 Uiso 1 1 calc R . . H14B H 1.2287 1.5388 0.4765 0.065 Uiso 1 1 calc R . . C15 C 1.0885(3) 1.4116(3) 0.43166(15) 0.0431(9) Uani 1 1 d . . . H15A H 1.0459 1.3632 0.4608 0.052 Uiso 1 1 calc R . . H15B H 1.1471 1.3831 0.4180 0.052 Uiso 1 1 calc R . . C16 C 1.2683(3) 0.8728(3) 0.31836(14) 0.0326(7) Uani 1 1 d . . . H16 H 1.2499 0.8377 0.3564 0.039 Uiso 1 1 calc R . . C17 C 1.4032(3) 0.9288(3) 0.3223(2) 0.0501(10) Uani 1 1 d . . . H17A H 1.4239 0.9916 0.2971 0.060 Uiso 1 1 calc R . . H17B H 1.4377 0.9544 0.3636 0.060 Uiso 1 1 calc R . . C18 C 1.4463(3) 0.8429(4) 0.3004(2) 0.0542(11) Uani 1 1 d . . . H18A H 1.4485 0.7912 0.3311 0.065 Uiso 1 1 calc R . . H18B H 1.5255 0.8754 0.2877 0.065 Uiso 1 1 calc R . . C19 C 1.3550(4) 0.7882(4) 0.24851(18) 0.0548(11) Uani 1 1 d . . . H19A H 1.3552 0.7147 0.2385 0.066 Uiso 1 1 calc R . . H19B H 1.3698 0.8316 0.2133 0.066 Uiso 1 1 calc R . . C20 C 1.2389(3) 0.7819(3) 0.26924(15) 0.0389(8) Uani 1 1 d . . . H20A H 1.2001 0.7101 0.2847 0.047 Uiso 1 1 calc R . . H20B H 1.1856 0.7928 0.2361 0.047 Uiso 1 1 calc R . . C21 C 1.2908(3) 1.4196(3) 0.26190(16) 0.0400(8) Uani 1 1 d . . . H21 H 1.2504 1.4539 0.2323 0.048 Uiso 1 1 calc R . . C22 C 1.3945(4) 1.4078(4) 0.23548(19) 0.0590(12) Uani 1 1 d . . . H22A H 1.4173 1.3492 0.2535 0.071 Uiso 1 1 calc R . . H22B H 1.3761 1.3915 0.1922 0.071 Uiso 1 1 calc R . . C23 C 1.4912(4) 1.5172(4) 0.2500(2) 0.0598(12) Uani 1 1 d . . . H23A H 1.5696 1.5125 0.2472 0.072 Uiso 1 1 calc R . . H23B H 1.4799 1.5723 0.2234 0.072 Uiso 1 1 calc R . . C24 C 1.4765(4) 1.5428(4) 0.3129(2) 0.0714(15) Uani 1 1 d . . . H24A H 1.5145 1.5049 0.3407 0.086 Uiso 1 1 calc R . . H24B H 1.5120 1.6220 0.3231 0.086 Uiso 1 1 calc R . . C25 C 1.3469(4) 1.5035(3) 0.31557(19) 0.0507(10) Uani 1 1 d . . . H25A H 1.3175 1.5647 0.3128 0.061 Uiso 1 1 calc R . . H25B H 1.3278 1.4688 0.3531 0.061 Uiso 1 1 calc R . . C26 C 0.8432(3) 1.0382(3) 0.44185(14) 0.0335(7) Uani 1 1 d . . . H26 H 0.8645 0.9782 0.4602 0.040 Uiso 1 1 calc R . . C27 C 0.8565(4) 1.1269(4) 0.49112(18) 0.0627(14) Uani 1 1 d . . . H27A H 0.8939 1.1112 0.5288 0.075 Uiso 1 1 calc R . . H27B H 0.9058 1.1993 0.4798 0.075 Uiso 1 1 calc R . . C28 C 0.7445(6) 1.1249(8) 0.4973(3) 0.168(5) Uani 1 1 d . . . H28A H 0.7400 1.1964 0.4874 0.201 Uiso 1 1 calc R . . H28B H 0.7317 1.1154 0.5393 0.201 Uiso 1 1 calc R . . C29 C 0.6520(4) 1.0426(4) 0.46196(19) 0.0570(11) Uani 1 1 d . . . H29A H 0.5979 1.0740 0.4403 0.068 Uiso 1 1 calc R . . H29B H 0.6067 0.9862 0.4869 0.068 Uiso 1 1 calc R . . C30 C 0.7104(3) 0.9943(3) 0.41886(15) 0.0349(8) Uani 1 1 d . . . H30A H 0.6968 1.0172 0.3784 0.042 Uiso 1 1 calc R . . H30B H 0.6786 0.9139 0.4180 0.042 Uiso 1 1 calc R . . C31 C 1.3155(3) 1.2128(3) 0.45502(13) 0.0299(7) Uani 1 1 d . . . H31 H 1.2907 1.1606 0.4865 0.036 Uiso 1 1 calc R . . C32 C 1.3372(4) 1.3261(3) 0.48230(16) 0.0443(9) Uani 1 1 d . . . H32A H 1.3484 1.3800 0.4517 0.053 Uiso 1 1 calc R . . H32B H 1.2713 1.3268 0.5039 0.053 Uiso 1 1 calc R . . C33 C 1.4495(4) 1.3489(4) 0.5244(2) 0.0644(13) Uani 1 1 d . . . H33A H 1.4925 1.4281 0.5312 0.077 Uiso 1 1 calc R . . H33B H 1.4313 1.3178 0.5630 0.077 Uiso 1 1 calc R . . C34 C 1.5206(4) 1.2958(5) 0.4947(3) 0.093(2) Uani 1 1 d . . . H34A H 1.5525 1.2543 0.5232 0.112 Uiso 1 1 calc R . . H34B H 1.5871 1.3513 0.4791 0.112 Uiso 1 1 calc R . . C35 C 1.4389(3) 1.2195(4) 0.44410(17) 0.0499(10) Uani 1 1 d . . . H35A H 1.4576 1.2492 0.4053 0.060 Uiso 1 1 calc R . . H35B H 1.4460 1.1468 0.4449 0.060 Uiso 1 1 calc R . . C36 C 0.6177(4) 1.2489(3) 0.31420(18) 0.0503(10) Uani 1 1 d . . . H36A H 0.5345 1.2112 0.2998 0.060 Uiso 1 1 calc R . . H36B H 0.6301 1.3238 0.3277 0.060 Uiso 1 1 calc R . . H36C H 0.6408 1.2111 0.3472 0.060 Uiso 1 1 calc R . . C37 C 0.6728(4) 1.3285(4) 0.19216(17) 0.0547(11) Uani 1 1 d . . . H37A H 0.6845 1.4024 0.2074 0.066 Uiso 1 1 calc R . . H37B H 0.5908 1.2927 0.1750 0.066 Uiso 1 1 calc R . . H37C H 0.7246 1.3320 0.1617 0.066 Uiso 1 1 calc R . . C38 C 0.6843(4) 1.1095(3) 0.22759(19) 0.0590(12) Uani 1 1 d . . . H38C H 0.7352 1.1106 0.1970 0.071 Uiso 1 1 calc R . . H38B H 0.6020 1.0731 0.2111 0.071 Uiso 1 1 calc R . . H38A H 0.7034 1.0701 0.2608 0.071 Uiso 1 1 calc R . . C39 C 1.1621(3) 1.5690(3) 0.08903(13) 0.0297(7) Uani 1 1 d . . . C40 C 1.1306(3) 1.4562(3) 0.08241(14) 0.0340(7) Uani 1 1 d . . . H40 H 1.1548 1.4243 0.0508 0.041 Uiso 1 1 calc R . . C41 C 1.0642(3) 1.3912(3) 0.12183(15) 0.0384(8) Uani 1 1 d . . . H41 H 1.0437 1.3146 0.1176 0.046 Uiso 1 1 calc R . . C42 C 1.0274(3) 1.4372(3) 0.16736(15) 0.0378(8) Uani 1 1 d . . . H42 H 0.9788 1.3918 0.1934 0.045 Uiso 1 1 calc R . . C43 C 1.0607(3) 1.5489(3) 0.17534(15) 0.0386(8) Uani 1 1 d . . . H43 H 1.0359 1.5801 0.2071 0.046 Uiso 1 1 calc R . . C44 C 1.1301(3) 1.6151(3) 0.13721(13) 0.0315(7) Uani 1 1 d . . . H44 H 1.1559 1.6919 0.1437 0.038 Uiso 1 1 calc R . . C45 C 1.3851(3) 1.7393(3) 0.07810(14) 0.0306(7) Uani 1 1 d . . . C46 C 1.4423(3) 1.6935(3) 0.11968(15) 0.0372(8) Uani 1 1 d . . . H46 H 1.4062 1.6196 0.1280 0.045 Uiso 1 1 calc R . . C47 C 1.5514(3) 1.7547(3) 0.14905(15) 0.0388(8) Uani 1 1 d . . . H47 H 1.5899 1.7229 0.1776 0.047 Uiso 1 1 calc R . . C48 C 1.6039(3) 1.8612(3) 0.13696(16) 0.0400(9) Uani 1 1 d . . . H48 H 1.6794 1.9028 0.1566 0.048 Uiso 1 1 calc R . . C49 C 1.5472(3) 1.9081(3) 0.09632(16) 0.0430(9) Uani 1 1 d . . . H49 H 1.5834 1.9824 0.0886 0.052 Uiso 1 1 calc R . . C50 C 1.4378(3) 1.8476(3) 0.06667(15) 0.0394(8) Uani 1 1 d . . . H50 H 1.3992 1.8802 0.0387 0.047 Uiso 1 1 calc R . . C51 C 1.1734(3) 1.7411(3) 0.00524(13) 0.0288(7) Uani 1 1 d . . . C52 C 1.0838(3) 1.7623(3) 0.02966(14) 0.0330(7) Uani 1 1 d . . . H52 H 1.0555 1.7274 0.0639 0.040 Uiso 1 1 calc R . . C53 C 1.0355(3) 1.8339(3) 0.00437(14) 0.0385(8) Uani 1 1 d . . . H53 H 0.9733 1.8471 0.0210 0.046 Uiso 1 1 calc R . . C54 C 1.0770(3) 1.8865(3) -0.04499(15) 0.0392(8) Uani 1 1 d . . . H54 H 1.0446 1.9369 -0.0617 0.047 Uiso 1 1 calc R . . C55 C 1.1657(3) 1.8654(3) -0.06989(16) 0.0407(8) Uani 1 1 d . . . H55 H 1.1939 1.9011 -0.1040 0.049 Uiso 1 1 calc R . . C56 C 1.2137(3) 1.7927(3) -0.04562(14) 0.0359(8) Uani 1 1 d . . . H56 H 1.2738 1.7778 -0.0633 0.043 Uiso 1 1 calc R . . C57 C 1.2729(3) 1.5742(3) -0.01848(14) 0.0308(7) Uani 1 1 d . . . C58 C 1.1766(3) 1.5034(3) -0.05532(14) 0.0345(8) Uani 1 1 d . . . H58 H 1.1001 1.5048 -0.0528 0.041 Uiso 1 1 calc R . . C59 C 1.1931(3) 1.4313(3) -0.09555(15) 0.0395(8) Uani 1 1 d . . . H59 H 1.1276 1.3812 -0.1197 0.047 Uiso 1 1 calc R . . C60 C 1.3044(4) 1.4325(3) -0.10043(16) 0.0498(10) Uani 1 1 d . . . H60 H 1.3155 1.3824 -0.1277 0.060 Uiso 1 1 calc R . . C61 C 1.4006(4) 1.5059(4) -0.06603(17) 0.0533(11) Uani 1 1 d . . . H61 H 1.4776 1.5077 -0.0706 0.064 Uiso 1 1 calc R . . C62 C 1.3846(3) 1.5770(3) -0.02475(15) 0.0426(9) Uani 1 1 d . . . H62 H 1.4504 1.6274 -0.0009 0.051 Uiso 1 1 calc R . . O1 O 0.8500(2) 0.8626(2) 0.10000(10) 0.0405(6) Uani 1 1 d . . . O2 O 0.9995(2) 0.7925(2) 0.16311(10) 0.0398(6) Uani 1 1 d . . . O3 O 0.86682(19) 0.89290(18) 0.22394(9) 0.0323(5) Uani 1 1 d . . . O4 O 1.0568(2) 1.02066(19) 0.15622(9) 0.0353(5) Uani 1 1 d . . . O5 O 1.04611(19) 0.89630(18) 0.30219(10) 0.0331(5) Uani 1 1 d . . . O6 O 0.9025(2) 0.99497(19) 0.32894(9) 0.0347(5) Uani 1 1 d . . . O7 O 1.2172(2) 1.02855(18) 0.24740(9) 0.0340(5) Uani 1 1 d . . . O8 O 1.1573(2) 1.19955(19) 0.22489(9) 0.0346(5) Uani 1 1 d . . . O9 O 0.9031(2) 1.18931(18) 0.35531(10) 0.0350(5) Uani 1 1 d . . . O10 O 1.0576(2) 1.30438(18) 0.28728(9) 0.0342(5) Uani 1 1 d . . . O11 O 0.8472(2) 1.31275(19) 0.27715(10) 0.0355(5) Uani 1 1 d . . . O12 O 1.22181(19) 1.05181(18) 0.36286(9) 0.0317(5) Uani 1 1 d . . . O13 O 1.22979(19) 1.24936(17) 0.33956(9) 0.0308(5) Uani 1 1 d . . . O14 O 1.07311(19) 1.12956(18) 0.40593(9) 0.0337(5) Uani 1 1 d . . . P P 1.24710(7) 1.65670(7) 0.03847(4) 0.02867(18) Uani 1 1 d . . . Si1 Si 0.90994(8) 0.89023(7) 0.29292(4) 0.02791(19) Uani 1 1 d . . . Si2 Si 1.17713(8) 1.09478(7) 0.19478(4) 0.0295(2) Uani 1 1 d . . . Si3 Si 0.95151(8) 1.30315(7) 0.32401(4) 0.0301(2) Uani 1 1 d . . . Si4 Si 1.18516(8) 0.96416(7) 0.30674(4) 0.02759(19) Uani 1 1 d . . . Si5 Si 1.18064(8) 1.28900(7) 0.27866(4) 0.0289(2) Uani 1 1 d . . . Si6 Si 0.93387(8) 1.08781(7) 0.38163(4) 0.02781(19) Uani 1 1 d . . . Si7 Si 1.20584(8) 1.16015(7) 0.38910(4) 0.02667(19) Uani 1 1 d . . . Si8 Si 0.70765(9) 1.25008(8) 0.25366(4) 0.0358(2) Uani 1 1 d . . . V V 0.94301(5) 0.88685(5) 0.15913(2) 0.03032(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0273(18) 0.042(2) 0.0330(17) 0.0041(15) -0.0008(14) 0.0030(15) C2 0.047(2) 0.034(2) 0.047(2) -0.0012(16) -0.0039(17) 0.0010(17) C3 0.041(2) 0.053(3) 0.091(3) 0.022(2) 0.014(2) 0.013(2) C4 0.150(6) 0.106(4) 0.061(3) 0.035(3) 0.055(3) 0.097(4) C5 0.060(3) 0.074(3) 0.036(2) 0.016(2) 0.0008(19) -0.002(2) C6 0.0339(19) 0.0378(19) 0.0316(16) -0.0017(14) 0.0053(14) 0.0091(15) C7 0.056(3) 0.060(3) 0.040(2) 0.0140(18) 0.0163(18) 0.021(2) C8 0.183(7) 0.111(5) 0.054(3) 0.030(3) 0.056(4) 0.092(5) C9 0.074(3) 0.081(3) 0.039(2) 0.000(2) 0.021(2) 0.032(3) C10 0.050(2) 0.050(2) 0.042(2) -0.0038(17) 0.0144(17) 0.0201(19) C11 0.0323(18) 0.0303(17) 0.0357(17) -0.0032(14) 0.0010(14) 0.0095(14) C12 0.039(2) 0.040(2) 0.0414(19) -0.0030(16) 0.0016(16) 0.0144(17) C13 0.063(3) 0.039(2) 0.052(2) -0.0122(18) -0.005(2) 0.014(2) C14 0.060(3) 0.045(2) 0.041(2) -0.0091(17) -0.0084(19) 0.001(2) C15 0.047(2) 0.043(2) 0.0340(18) -0.0036(15) -0.0022(16) 0.0116(18) C16 0.0318(18) 0.0362(18) 0.0310(16) -0.0045(14) 0.0018(13) 0.0145(15) C17 0.031(2) 0.046(2) 0.070(3) -0.0177(19) -0.0123(18) 0.0159(17) C18 0.031(2) 0.060(3) 0.069(3) -0.015(2) -0.0008(19) 0.0166(19) C19 0.051(3) 0.065(3) 0.049(2) -0.011(2) 0.0076(19) 0.021(2) C20 0.039(2) 0.043(2) 0.0344(18) -0.0104(15) -0.0027(15) 0.0161(16) C21 0.036(2) 0.039(2) 0.0396(19) 0.0050(15) 0.0013(15) 0.0063(16) C22 0.043(2) 0.066(3) 0.054(2) -0.012(2) 0.0189(19) -0.001(2) C23 0.034(2) 0.070(3) 0.060(3) -0.003(2) 0.0061(19) -0.001(2) C24 0.041(3) 0.085(4) 0.073(3) -0.036(3) 0.002(2) 0.008(2) C25 0.045(2) 0.040(2) 0.059(2) -0.0057(18) 0.0118(19) 0.0034(18) C26 0.0283(17) 0.0369(18) 0.0295(16) -0.0040(14) 0.0046(13) 0.0043(14) C27 0.070(3) 0.058(3) 0.037(2) -0.0194(18) 0.023(2) -0.010(2) C28 0.094(5) 0.272(10) 0.157(7) -0.173(7) -0.063(5) 0.123(6) C29 0.051(3) 0.073(3) 0.056(2) -0.002(2) 0.022(2) 0.030(2) C30 0.0263(17) 0.0400(19) 0.0343(17) 0.0001(14) 0.0063(13) 0.0061(15) C31 0.0320(18) 0.0310(17) 0.0251(15) -0.0020(12) -0.0003(13) 0.0103(14) C32 0.049(2) 0.044(2) 0.0341(18) -0.0114(16) -0.0075(16) 0.0134(18) C33 0.070(3) 0.051(3) 0.052(2) -0.015(2) -0.031(2) 0.008(2) C34 0.039(3) 0.138(5) 0.083(4) -0.048(4) -0.024(3) 0.018(3) C35 0.029(2) 0.069(3) 0.046(2) -0.0108(19) -0.0027(16) 0.0131(19) C36 0.047(2) 0.049(2) 0.056(2) 0.0023(19) 0.0131(19) 0.0169(19) C37 0.045(2) 0.076(3) 0.041(2) 0.008(2) -0.0034(18) 0.021(2) C38 0.063(3) 0.051(3) 0.052(2) -0.018(2) 0.005(2) 0.008(2) C39 0.0246(16) 0.0339(17) 0.0266(15) -0.0031(13) -0.0008(12) 0.0067(14) C40 0.0320(18) 0.0347(18) 0.0326(17) -0.0031(14) -0.0023(14) 0.0107(15) C41 0.036(2) 0.0327(18) 0.0409(19) -0.0005(15) -0.0061(15) 0.0079(15) C42 0.0290(18) 0.048(2) 0.0316(17) 0.0099(15) -0.0003(14) 0.0079(16) C43 0.038(2) 0.047(2) 0.0301(17) -0.0010(15) -0.0012(15) 0.0151(17) C44 0.0300(18) 0.0359(18) 0.0263(15) -0.0027(13) -0.0029(13) 0.0107(14) C45 0.0293(17) 0.0320(17) 0.0295(16) -0.0098(13) 0.0020(13) 0.0106(14) C46 0.0328(19) 0.0375(19) 0.0401(18) -0.0050(15) 0.0006(15) 0.0122(15) C47 0.0324(19) 0.047(2) 0.0374(18) -0.0122(15) -0.0047(15) 0.0175(17) C48 0.0231(17) 0.048(2) 0.0429(19) -0.0163(16) 0.0022(15) 0.0071(16) C49 0.0318(19) 0.038(2) 0.047(2) -0.0030(16) 0.0001(16) -0.0017(16) C50 0.0337(19) 0.042(2) 0.0362(18) -0.0044(15) 0.0000(15) 0.0064(16) C51 0.0250(16) 0.0313(17) 0.0258(15) -0.0076(12) -0.0018(12) 0.0065(13) C52 0.0340(19) 0.0360(18) 0.0276(15) -0.0060(13) 0.0014(13) 0.0117(15) C53 0.043(2) 0.046(2) 0.0301(17) -0.0046(15) -0.0002(15) 0.0215(17) C54 0.040(2) 0.0359(19) 0.0387(19) -0.0015(15) -0.0036(16) 0.0128(16) C55 0.040(2) 0.038(2) 0.0369(18) 0.0070(15) 0.0018(15) 0.0051(16) C56 0.0302(18) 0.0403(19) 0.0324(17) -0.0023(14) 0.0054(14) 0.0062(15) C57 0.0292(17) 0.0337(17) 0.0276(15) -0.0030(13) -0.0017(13) 0.0104(14) C58 0.0316(18) 0.0371(19) 0.0327(17) -0.0085(14) -0.0025(14) 0.0122(15) C59 0.045(2) 0.0380(19) 0.0348(18) -0.0104(15) -0.0054(15) 0.0167(17) C60 0.058(3) 0.062(3) 0.0359(19) -0.0203(18) -0.0073(17) 0.036(2) C61 0.045(2) 0.080(3) 0.042(2) -0.020(2) -0.0027(17) 0.034(2) C62 0.035(2) 0.054(2) 0.0365(18) -0.0135(16) -0.0041(15) 0.0163(18) O1 0.0340(13) 0.0556(16) 0.0272(11) -0.0087(11) -0.0023(10) 0.0122(12) O2 0.0414(14) 0.0426(14) 0.0341(12) -0.0119(10) 0.0014(10) 0.0149(11) O3 0.0322(13) 0.0390(13) 0.0246(10) -0.0055(9) 0.0004(9) 0.0122(10) O4 0.0328(13) 0.0414(13) 0.0260(11) -0.0013(10) 0.0013(9) 0.0070(11) O5 0.0290(12) 0.0336(12) 0.0336(12) -0.0074(10) 0.0030(9) 0.0081(10) O6 0.0304(12) 0.0432(14) 0.0302(11) -0.0076(10) 0.0030(9) 0.0133(11) O7 0.0326(13) 0.0396(13) 0.0279(11) -0.0013(10) 0.0027(9) 0.0108(11) O8 0.0343(13) 0.0410(13) 0.0286(11) -0.0004(10) 0.0045(10) 0.0134(11) O9 0.0346(13) 0.0332(12) 0.0353(12) -0.0019(10) 0.0037(10) 0.0098(10) O10 0.0331(13) 0.0391(13) 0.0317(12) 0.0003(10) 0.0026(10) 0.0148(11) O11 0.0343(13) 0.0384(13) 0.0335(12) -0.0015(10) -0.0005(10) 0.0139(11) O12 0.0318(12) 0.0335(12) 0.0268(11) -0.0050(9) -0.0022(9) 0.0096(10) O13 0.0297(12) 0.0321(12) 0.0284(11) -0.0026(9) 0.0005(9) 0.0091(10) O14 0.0297(12) 0.0403(13) 0.0275(11) -0.0040(10) 0.0026(9) 0.0084(10) P 0.0260(4) 0.0292(4) 0.0276(4) -0.0065(3) -0.0008(3) 0.0073(3) Si1 0.0247(5) 0.0299(5) 0.0256(4) -0.0049(3) 0.0013(3) 0.0060(4) Si2 0.0284(5) 0.0339(5) 0.0241(4) -0.0026(3) 0.0032(3) 0.0085(4) Si3 0.0291(5) 0.0314(5) 0.0287(4) -0.0031(4) -0.0001(4) 0.0106(4) Si4 0.0269(5) 0.0284(4) 0.0263(4) -0.0044(3) 0.0014(3) 0.0092(4) Si5 0.0285(5) 0.0288(5) 0.0277(4) -0.0004(3) 0.0042(4) 0.0080(4) Si6 0.0251(5) 0.0309(5) 0.0256(4) -0.0040(3) 0.0032(3) 0.0078(4) Si7 0.0241(4) 0.0284(4) 0.0243(4) -0.0042(3) 0.0002(3) 0.0062(4) Si8 0.0315(5) 0.0418(6) 0.0310(5) -0.0056(4) 0.0000(4) 0.0107(4) V 0.0278(3) 0.0362(3) 0.0236(3) -0.0075(2) -0.0008(2) 0.0088(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.532(5) . ? C1 C2 1.533(5) . ? C1 Si1 1.848(3) . ? C1 H1 1.0000 . ? C2 C3 1.511(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.510(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.501(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C10 1.540(5) . ? C6 C7 1.544(5) . ? C6 Si2 1.849(3) . ? C6 H6 1.0000 . ? C7 C8 1.477(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.459(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.523(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C15 1.526(5) . ? C11 C12 1.534(5) . ? C11 Si3 1.853(3) . ? C11 H11 1.0000 . ? C12 C13 1.536(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.507(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.519(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C20 1.538(4) . ? C16 C17 1.547(5) . ? C16 Si4 1.832(3) . ? C16 H16 1.0000 . ? C17 C18 1.499(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.512(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.519(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.514(6) . ? C21 C25 1.556(5) . ? C21 Si5 1.853(4) . ? C21 H21 1.0000 . ? C22 C23 1.513(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.508(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.495(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C30 1.549(5) . ? C26 C27 1.555(5) . ? C26 Si6 1.843(3) . ? C26 H26 1.0000 . ? C27 C28 1.382(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.419(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.522(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.525(5) . ? C31 C35 1.529(5) . ? C31 Si7 1.848(3) . ? C31 H31 1.0000 . ? C32 C33 1.523(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.493(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.531(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 Si8 1.850(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 Si8 1.858(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 Si8 1.844(4) . ? C38 H38C 0.9800 . ? C38 H38B 0.9800 . ? C38 H38A 0.9800 . ? C39 C40 1.396(5) . ? C39 C44 1.398(4) . ? C39 P 1.793(3) . ? C40 C41 1.378(5) . ? C40 H40 0.9500 . ? C41 C42 1.381(5) . ? C41 H41 0.9500 . ? C42 C43 1.383(5) . ? C42 H42 0.9500 . ? C43 C44 1.381(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.388(5) . ? C45 C46 1.388(5) . ? C45 P 1.789(3) . ? C46 C47 1.385(5) . ? C46 H46 0.9500 . ? C47 C48 1.370(5) . ? C47 H47 0.9500 . ? C48 C49 1.381(5) . ? C48 H48 0.9500 . ? C49 C50 1.386(5) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.388(5) . ? C51 C56 1.403(5) . ? C51 P 1.790(3) . ? C52 C53 1.380(5) . ? C52 H52 0.9500 . ? C53 C54 1.382(5) . ? C53 H53 0.9500 . ? C54 C55 1.382(5) . ? C54 H54 0.9500 . ? C55 C56 1.381(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C62 1.377(5) . ? C57 C58 1.397(4) . ? C57 P 1.795(3) . ? C58 C59 1.383(4) . ? C58 H58 0.9500 . ? C59 C60 1.373(5) . ? C59 H59 0.9500 . ? C60 C61 1.383(5) . ? C60 H60 0.9500 . ? C61 C62 1.388(5) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? O1 V 1.617(2) . ? O2 V 1.616(3) . ? O3 Si1 1.609(2) . ? O3 V 1.842(2) . ? O4 Si2 1.605(2) . ? O4 V 1.832(2) . ? O5 Si4 1.613(2) . ? O5 Si1 1.630(2) . ? O6 Si6 1.610(2) . ? O6 Si1 1.623(2) . ? O7 Si4 1.621(2) . ? O7 Si2 1.629(2) . ? O8 Si5 1.611(2) . ? O8 Si2 1.629(2) . ? O9 Si3 1.618(2) . ? O9 Si6 1.619(3) . ? O10 Si3 1.612(2) . ? O10 Si5 1.618(2) . ? O11 Si3 1.616(2) . ? O11 Si8 1.639(2) . ? O12 Si7 1.615(2) . ? O12 Si4 1.618(2) . ? O13 Si7 1.620(2) . ? O13 Si5 1.622(2) . ? O14 Si7 1.621(2) . ? O14 Si6 1.626(2) . ? 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 C5 C1 C2 102.7(3) . . ? C5 C1 Si1 115.6(2) . . ? C2 C1 Si1 112.8(3) . . ? C5 C1 H1 108.5 . . ? C2 C1 H1 108.5 . . ? Si1 C1 H1 108.5 . . ? C3 C2 C1 105.8(3) . . ? C3 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? C3 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? C4 C3 C2 104.3(4) . . ? C4 C3 H3A 110.9 . . ? C2 C3 H3A 110.9 . . ? C4 C3 H3B 110.9 . . ? C2 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? C5 C4 C3 108.7(4) . . ? C5 C4 H4A 110.0 . . ? C3 C4 H4A 109.9 . . ? C5 C4 H4B 109.9 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? C4 C5 C1 106.5(4) . . ? C4 C5 H5A 110.4 . . ? C1 C5 H5A 110.4 . . ? C4 C5 H5B 110.4 . . ? C1 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? C10 C6 C7 103.4(3) . . ? C10 C6 Si2 114.8(2) . . ? C7 C6 Si2 113.8(3) . . ? C10 C6 H6 108.2 . . ? C7 C6 H6 108.2 . . ? Si2 C6 H6 108.2 . . ? C8 C7 C6 105.9(4) . . ? C8 C7 H7A 110.6 . . ? C6 C7 H7A 110.6 . . ? C8 C7 H7B 110.6 . . ? C6 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? C9 C8 C7 110.5(4) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 106.4(4) . . ? C8 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? C8 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.6 . . ? C9 C10 C6 104.7(3) . . ? C9 C10 H10A 110.8 . . ? C6 C10 H10A 110.8 . . ? C9 C10 H10B 110.8 . . ? C6 C10 H10B 110.8 . . ? H10A C10 H10B 108.9 . . ? C15 C11 C12 103.0(3) . . ? C15 C11 Si3 115.2(2) . . ? C12 C11 Si3 114.2(2) . . ? C15 C11 H11 108.0 . . ? C12 C11 H11 108.0 . . ? Si3 C11 H11 108.0 . . ? C11 C12 C13 105.7(3) . . ? C11 C12 H12A 110.6 . . ? C13 C12 H12A 110.6 . . ? C11 C12 H12B 110.6 . . ? C13 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C14 C13 C12 106.9(3) . . ? C14 C13 H13A 110.3 . . ? C12 C13 H13A 110.3 . . ? C14 C13 H13B 110.3 . . ? C12 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? C13 C14 C15 106.3(3) . . ? C13 C14 H14A 110.5 . . ? C15 C14 H14A 110.5 . . ? C13 C14 H14B 110.5 . . ? C15 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? C14 C15 C11 104.8(3) . . ? C14 C15 H15A 110.8 . . ? C11 C15 H15A 110.8 . . ? C14 C15 H15B 110.8 . . ? C11 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? C20 C16 C17 104.0(3) . . ? C20 C16 Si4 114.2(2) . . ? C17 C16 Si4 114.8(2) . . ? C20 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? Si4 C16 H16 107.8 . . ? C18 C17 C16 105.0(3) . . ? C18 C17 H17A 110.7 . . ? C16 C17 H17A 110.7 . . ? C18 C17 H17B 110.7 . . ? C16 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C17 C18 C19 102.1(3) . . ? C17 C18 H18A 111.4 . . ? C19 C18 H18A 111.4 . . ? C17 C18 H18B 111.4 . . ? C19 C18 H18B 111.4 . . ? H18A C18 H18B 109.2 . . ? C18 C19 C20 104.7(3) . . ? C18 C19 H19A 110.8 . . ? C20 C19 H19A 110.8 . . ? C18 C19 H19B 110.8 . . ? C20 C19 H19B 110.8 . . ? H19A C19 H19B 108.9 . . ? C19 C20 C16 106.4(3) . . ? C19 C20 H20A 110.5 . . ? C16 C20 H20A 110.5 . . ? C19 C20 H20B 110.5 . . ? C16 C20 H20B 110.5 . . ? H20A C20 H20B 108.6 . . ? C22 C21 C25 104.5(3) . . ? C22 C21 Si5 114.1(3) . . ? C25 C21 Si5 115.5(3) . . ? C22 C21 H21 107.4 . . ? C25 C21 H21 107.4 . . ? Si5 C21 H21 107.4 . . ? C23 C22 C21 104.1(3) . . ? C23 C22 H22A 110.9 . . ? C21 C22 H22A 110.9 . . ? C23 C22 H22B 110.9 . . ? C21 C22 H22B 110.9 . . ? H22A C22 H22B 109.0 . . ? C24 C23 C22 102.0(4) . . ? C24 C23 H23A 111.4 . . ? C22 C23 H23A 111.4 . . ? C24 C23 H23B 111.4 . . ? C22 C23 H23B 111.4 . . ? H23A C23 H23B 109.2 . . ? C25 C24 C23 105.7(4) . . ? C25 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? C25 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? C24 C25 C21 105.9(3) . . ? C24 C25 H25A 110.6 . . ? C21 C25 H25A 110.6 . . ? C24 C25 H25B 110.6 . . ? C21 C25 H25B 110.6 . . ? H25A C25 H25B 108.7 . . ? C30 C26 C27 104.5(3) . . ? C30 C26 Si6 111.6(2) . . ? C27 C26 Si6 114.2(2) . . ? C30 C26 H26 108.8 . . ? C27 C26 H26 108.8 . . ? Si6 C26 H26 108.8 . . ? C28 C27 C26 106.7(4) . . ? C28 C27 H27A 110.4 . . ? C26 C27 H27A 110.4 . . ? C28 C27 H27B 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C27 C28 C29 115.4(4) . . ? C27 C28 H28A 108.4 . . ? C29 C28 H28A 108.4 . . ? C27 C28 H28B 108.4 . . ? C29 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? C28 C29 C30 106.0(4) . . ? C28 C29 H29A 110.5 . . ? C30 C29 H29A 110.5 . . ? C28 C29 H29B 110.5 . . ? C30 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C29 C30 C26 105.8(3) . . ? C29 C30 H30A 110.6 . . ? C26 C30 H30A 110.6 . . ? C29 C30 H30B 110.6 . . ? C26 C30 H30B 110.6 . . ? H30A C30 H30B 108.7 . . ? C32 C31 C35 102.4(3) . . ? C32 C31 Si7 119.2(2) . . ? C35 C31 Si7 113.0(2) . . ? C32 C31 H31 107.2 . . ? C35 C31 H31 107.2 . . ? Si7 C31 H31 107.2 . . ? C33 C32 C31 102.8(3) . . ? C33 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? C33 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? C34 C33 C32 105.5(3) . . ? C34 C33 H33A 110.6 . . ? C32 C33 H33A 110.6 . . ? C34 C33 H33B 110.6 . . ? C32 C33 H33B 110.6 . . ? H33A C33 H33B 108.8 . . ? C33 C34 C35 107.2(4) . . ? C33 C34 H34A 110.3 . . ? C35 C34 H34A 110.3 . . ? C33 C34 H34B 110.3 . . ? C35 C34 H34B 110.3 . . ? H34A C34 H34B 108.5 . . ? C31 C35 C34 104.7(3) . . ? C31 C35 H35A 110.8 . . ? C34 C35 H35A 110.8 . . ? C31 C35 H35B 110.8 . . ? C34 C35 H35B 110.8 . . ? H35A C35 H35B 108.9 . . ? Si8 C36 H36A 109.5 . . ? Si8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si8 C37 H37A 109.5 . . ? Si8 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si8 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si8 C38 H38C 109.5 . . ? Si8 C38 H38B 109.5 . . ? H38C C38 H38B 109.5 . . ? Si8 C38 H38A 109.5 . . ? H38C C38 H38A 109.5 . . ? H38B C38 H38A 109.5 . . ? C40 C39 C44 119.4(3) . . ? C40 C39 P 121.6(2) . . ? C44 C39 P 119.0(2) . . ? C41 C40 C39 120.0(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.2(3) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C43 120.4(3) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 120.0(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C39 119.8(3) . . ? C43 C44 H44 120.1 . . ? C39 C44 H44 120.1 . . ? C50 C45 C46 119.3(3) . . ? C50 C45 P 121.1(3) . . ? C46 C45 P 119.5(3) . . ? C47 C46 C45 120.5(3) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C48 C47 C46 119.9(3) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 120.1(3) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C48 C49 C50 120.4(4) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C49 C50 C45 119.7(3) . . ? C49 C50 H50 120.2 . . ? C45 C50 H50 120.2 . . ? C52 C51 C56 119.1(3) . . ? C52 C51 P 122.8(3) . . ? C56 C51 P 118.0(3) . . ? C53 C52 C51 120.3(3) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 120.4(3) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C55 C54 C53 119.7(3) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C56 C55 C54 120.5(3) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C55 C56 C51 119.8(3) . . ? C55 C56 H56 120.1 . . ? C51 C56 H56 120.1 . . ? C62 C57 C58 120.1(3) . . ? C62 C57 P 121.2(2) . . ? C58 C57 P 118.7(3) . . ? C59 C58 C57 119.7(3) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? C60 C59 C58 119.8(3) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C61 120.7(3) . . ? C59 C60 H60 119.6 . . ? C61 C60 H60 119.6 . . ? C60 C61 C62 119.8(4) . . ? C60 C61 H61 120.1 . . ? C62 C61 H61 120.1 . . ? C57 C62 C61 119.8(3) . . ? C57 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? Si1 O3 V 129.15(14) . . ? Si2 O4 V 137.84(15) . . ? Si4 O5 Si1 151.03(16) . . ? Si6 O6 Si1 157.17(16) . . ? Si4 O7 Si2 147.10(16) . . ? Si5 O8 Si2 151.71(16) . . ? Si3 O9 Si6 146.05(16) . . ? Si3 O10 Si5 154.44(16) . . ? Si3 O11 Si8 141.41(16) . . ? Si7 O12 Si4 144.17(15) . . ? Si7 O13 Si5 147.37(15) . . ? Si7 O14 Si6 146.50(15) . . ? C45 P C51 109.97(15) . . ? C45 P C39 108.29(15) . . ? C51 P C39 111.88(16) . . ? C45 P C57 109.00(15) . . ? C51 P C57 109.13(14) . . ? C39 P C57 108.52(15) . . ? O3 Si1 O6 109.29(12) . . ? O3 Si1 O5 110.58(12) . . ? O6 Si1 O5 107.94(12) . . ? O3 Si1 C1 110.23(14) . . ? O6 Si1 C1 111.84(15) . . ? O5 Si1 C1 106.93(15) . . ? O4 Si2 O8 108.75(13) . . ? O4 Si2 O7 111.63(13) . . ? O8 Si2 O7 108.30(12) . . ? O4 Si2 C6 109.61(14) . . ? O8 Si2 C6 109.53(14) . . ? O7 Si2 C6 108.99(15) . . ? O10 Si3 O11 107.26(12) . . ? O10 Si3 O9 109.89(13) . . ? O11 Si3 O9 108.75(13) . . ? O10 Si3 C11 109.57(14) . . ? O11 Si3 C11 110.26(14) . . ? O9 Si3 C11 111.04(14) . . ? O5 Si4 O12 108.75(12) . . ? O5 Si4 O7 110.67(12) . . ? O12 Si4 O7 108.78(12) . . ? O5 Si4 C16 110.16(14) . . ? O12 Si4 C16 108.39(13) . . ? O7 Si4 C16 110.03(14) . . ? O8 Si5 O10 108.45(12) . . ? O8 Si5 O13 110.65(12) . . ? O10 Si5 O13 108.87(12) . . ? O8 Si5 C21 109.87(15) . . ? O10 Si5 C21 110.37(15) . . ? O13 Si5 C21 108.62(15) . . ? O6 Si6 O9 107.90(12) . . ? O6 Si6 O14 110.63(12) . . ? O9 Si6 O14 108.58(13) . . ? O6 Si6 C26 110.73(14) . . ? O9 Si6 C26 107.74(15) . . ? O14 Si6 C26 111.14(14) . . ? O12 Si7 O13 109.02(12) . . ? O12 Si7 O14 109.07(12) . . ? O13 Si7 O14 110.08(13) . . ? O12 Si7 C31 107.46(13) . . ? O13 Si7 C31 109.83(14) . . ? O14 Si7 C31 111.32(13) . . ? O11 Si8 C38 109.16(18) . . ? O11 Si8 C36 110.04(16) . . ? C38 Si8 C36 109.9(2) . . ? O11 Si8 C37 105.77(17) . . ? C38 Si8 C37 111.2(2) . . ? C36 Si8 C37 110.7(2) . . ? O2 V O1 109.03(12) . . ? O2 V O4 111.03(12) . . ? O1 V O4 108.97(12) . . ? O2 V O3 111.48(12) . . ? O1 V O3 109.00(11) . . ? O4 V O3 107.29(10) . . ? 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 C5 C1 C2 C3 35.0(4) . . . . ? Si1 C1 C2 C3 160.1(3) . . . . ? C1 C2 C3 C4 -30.9(5) . . . . ? C2 C3 C4 C5 14.6(6) . . . . ? C3 C4 C5 C1 7.1(6) . . . . ? C2 C1 C5 C4 -25.5(5) . . . . ? Si1 C1 C5 C4 -148.7(3) . . . . ? C10 C6 C7 C8 -24.7(5) . . . . ? Si2 C6 C7 C8 -149.9(4) . . . . ? C6 C7 C8 C9 9.8(7) . . . . ? C7 C8 C9 C10 9.5(7) . . . . ? C8 C9 C10 C6 -25.0(5) . . . . ? C7 C6 C10 C9 30.2(4) . . . . ? Si2 C6 C10 C9 154.7(3) . . . . ? C15 C11 C12 C13 -30.2(4) . . . . ? Si3 C11 C12 C13 -155.9(3) . . . . ? C11 C12 C13 C14 12.5(4) . . . . ? C12 C13 C14 C15 10.4(5) . . . . ? C13 C14 C15 C11 -29.6(4) . . . . ? C12 C11 C15 C14 36.7(4) . . . . ? Si3 C11 C15 C14 161.8(3) . . . . ? C20 C16 C17 C18 -26.0(4) . . . . ? Si4 C16 C17 C18 -151.5(3) . . . . ? C16 C17 C18 C19 41.0(4) . . . . ? C17 C18 C19 C20 -40.2(5) . . . . ? C18 C19 C20 C16 24.1(4) . . . . ? C17 C16 C20 C19 1.0(4) . . . . ? Si4 C16 C20 C19 126.8(3) . . . . ? C25 C21 C22 C23 -29.4(4) . . . . ? Si5 C21 C22 C23 -156.5(3) . . . . ? C21 C22 C23 C24 41.9(5) . . . . ? C22 C23 C24 C25 -38.4(5) . . . . ? C23 C24 C25 C21 20.2(5) . . . . ? C22 C21 C25 C24 5.8(5) . . . . ? Si5 C21 C25 C24 131.9(4) . . . . ? C30 C26 C27 C28 4.3(6) . . . . ? Si6 C26 C27 C28 126.6(6) . . . . ? C26 C27 C28 C29 3.8(10) . . . . ? C27 C28 C29 C30 -10.4(10) . . . . ? C28 C29 C30 C26 12.2(6) . . . . ? C27 C26 C30 C29 -10.0(4) . . . . ? Si6 C26 C30 C29 -134.0(3) . . . . ? C35 C31 C32 C33 -41.7(4) . . . . ? Si7 C31 C32 C33 -167.2(3) . . . . ? C31 C32 C33 C34 34.7(5) . . . . ? C32 C33 C34 C35 -14.0(6) . . . . ? C32 C31 C35 C34 33.2(5) . . . . ? Si7 C31 C35 C34 162.6(4) . . . . ? C33 C34 C35 C31 -12.1(6) . . . . ? C44 C39 C40 C41 2.7(5) . . . . ? P C39 C40 C41 -179.4(3) . . . . ? C39 C40 C41 C42 0.9(5) . . . . ? C40 C41 C42 C43 -2.7(5) . . . . ? C41 C42 C43 C44 0.8(5) . . . . ? C42 C43 C44 C39 2.8(5) . . . . ? C40 C39 C44 C43 -4.5(5) . . . . ? P C39 C44 C43 177.4(3) . . . . ? C50 C45 C46 C47 -0.7(5) . . . . ? P C45 C46 C47 177.3(3) . . . . ? C45 C46 C47 C48 -0.2(5) . . . . ? C46 C47 C48 C49 1.1(5) . . . . ? C47 C48 C49 C50 -1.1(5) . . . . ? C48 C49 C50 C45 0.2(5) . . . . ? C46 C45 C50 C49 0.8(5) . . . . ? P C45 C50 C49 -177.2(3) . . . . ? C56 C51 C52 C53 -0.4(5) . . . . ? P C51 C52 C53 175.5(2) . . . . ? C51 C52 C53 C54 -1.0(5) . . . . ? C52 C53 C54 C55 1.4(5) . . . . ? C53 C54 C55 C56 -0.4(5) . . . . ? C54 C55 C56 C51 -1.0(5) . . . . ? C52 C51 C56 C55 1.4(5) . . . . ? P C51 C56 C55 -174.8(3) . . . . ? C62 C57 C58 C59 4.1(5) . . . . ? P C57 C58 C59 -173.5(3) . . . . ? C57 C58 C59 C60 -2.3(6) . . . . ? C58 C59 C60 C61 -0.8(6) . . . . ? C59 C60 C61 C62 2.1(7) . . . . ? C58 C57 C62 C61 -2.8(6) . . . . ? P C57 C62 C61 174.8(3) . . . . ? C60 C61 C62 C57 -0.2(6) . . . . ? C50 C45 P C51 -19.1(3) . . . . ? C46 C45 P C51 162.9(3) . . . . ? C50 C45 P C39 -141.6(3) . . . . ? C46 C45 P C39 40.4(3) . . . . ? C50 C45 P C57 100.5(3) . . . . ? C46 C45 P C57 -77.5(3) . . . . ? C52 C51 P C45 -100.2(3) . . . . ? C56 C51 P C45 75.7(3) . . . . ? C52 C51 P C39 20.2(3) . . . . ? C56 C51 P C39 -163.9(2) . . . . ? C52 C51 P C57 140.3(3) . . . . ? C56 C51 P C57 -43.8(3) . . . . ? C40 C39 P C45 -115.6(3) . . . . ? C44 C39 P C45 62.4(3) . . . . ? C40 C39 P C51 123.0(3) . . . . ? C44 C39 P C51 -59.0(3) . . . . ? C40 C39 P C57 2.6(3) . . . . ? C44 C39 P C57 -179.4(2) . . . . ? C62 C57 P C45 2.8(4) . . . . ? C58 C57 P C45 -179.6(3) . . . . ? C62 C57 P C51 122.9(3) . . . . ? C58 C57 P C51 -59.5(3) . . . . ? C62 C57 P C39 -115.0(3) . . . . ? C58 C57 P C39 62.6(3) . . . . ? V O3 Si1 O6 125.87(17) . . . . ? V O3 Si1 O5 7.2(2) . . . . ? V O3 Si1 C1 -110.8(2) . . . . ? Si6 O6 Si1 O3 -155.9(4) . . . . ? Si6 O6 Si1 O5 -35.6(5) . . . . ? Si6 O6 Si1 C1 81.7(4) . . . . ? Si4 O5 Si1 O3 78.6(3) . . . . ? Si4 O5 Si1 O6 -40.8(3) . . . . ? Si4 O5 Si1 C1 -161.3(3) . . . . ? C5 C1 Si1 O3 176.4(3) . . . . ? C2 C1 Si1 O3 58.7(3) . . . . ? C5 C1 Si1 O6 -61.8(3) . . . . ? C2 C1 Si1 O6 -179.5(2) . . . . ? C5 C1 Si1 O5 56.2(3) . . . . ? C2 C1 Si1 O5 -61.6(3) . . . . ? V O4 Si2 O8 -111.1(2) . . . . ? V O4 Si2 O7 8.3(3) . . . . ? V O4 Si2 C6 129.1(2) . . . . ? Si5 O8 Si2 O4 144.5(3) . . . . ? Si5 O8 Si2 O7 23.0(4) . . . . ? Si5 O8 Si2 C6 -95.7(4) . . . . ? Si4 O7 Si2 O4 -60.8(3) . . . . ? Si4 O7 Si2 O8 58.9(3) . . . . ? Si4 O7 Si2 C6 178.0(3) . . . . ? C10 C6 Si2 O4 -61.2(3) . . . . ? C7 C6 Si2 O4 57.6(3) . . . . ? C10 C6 Si2 O8 179.5(2) . . . . ? C7 C6 Si2 O8 -61.6(3) . . . . ? C10 C6 Si2 O7 61.2(3) . . . . ? C7 C6 Si2 O7 -179.9(3) . . . . ? Si5 O10 Si3 O11 -167.7(3) . . . . ? Si5 O10 Si3 O9 -49.6(4) . . . . ? Si5 O10 Si3 C11 72.7(4) . . . . ? Si8 O11 Si3 O10 123.9(2) . . . . ? Si8 O11 Si3 O9 5.1(3) . . . . ? Si8 O11 Si3 C11 -116.9(3) . . . . ? Si6 O9 Si3 O10 26.2(3) . . . . ? Si6 O9 Si3 O11 143.3(3) . . . . ? Si6 O9 Si3 C11 -95.2(3) . . . . ? C15 C11 Si3 O10 -71.1(3) . . . . ? C12 C11 Si3 O10 47.9(3) . . . . ? C15 C11 Si3 O11 171.1(3) . . . . ? C12 C11 Si3 O11 -69.9(3) . . . . ? C15 C11 Si3 O9 50.5(3) . . . . ? C12 C11 Si3 O9 169.5(2) . . . . ? Si1 O5 Si4 O12 62.6(3) . . . . ? Si1 O5 Si4 O7 -56.9(3) . . . . ? Si1 O5 Si4 C16 -178.8(3) . . . . ? Si7 O12 Si4 O5 -66.3(3) . . . . ? Si7 O12 Si4 O7 54.3(3) . . . . ? Si7 O12 Si4 C16 174.0(3) . . . . ? Si2 O7 Si4 O5 36.0(3) . . . . ? Si2 O7 Si4 O12 -83.5(3) . . . . ? Si2 O7 Si4 C16 157.9(3) . . . . ? C20 C16 Si4 O5 59.0(3) . . . . ? C17 C16 Si4 O5 178.9(2) . . . . ? C20 C16 Si4 O12 177.8(2) . . . . ? C17 C16 Si4 O12 -62.2(3) . . . . ? C20 C16 Si4 O7 -63.3(3) . . . . ? C17 C16 Si4 O7 56.6(3) . . . . ? Si2 O8 Si5 O10 -138.5(3) . . . . ? Si2 O8 Si5 O13 -19.2(4) . . . . ? Si2 O8 Si5 C21 100.7(4) . . . . ? Si3 O10 Si5 O8 121.2(4) . . . . ? Si3 O10 Si5 O13 0.7(4) . . . . ? Si3 O10 Si5 C21 -118.4(4) . . . . ? Si7 O13 Si5 O8 -62.2(3) . . . . ? Si7 O13 Si5 O10 56.9(3) . . . . ? Si7 O13 Si5 C21 177.1(3) . . . . ? C22 C21 Si5 O8 -43.2(3) . . . . ? C25 C21 Si5 O8 -164.3(3) . . . . ? C22 C21 Si5 O10 -162.7(3) . . . . ? C25 C21 Si5 O10 76.2(3) . . . . ? C22 C21 Si5 O13 78.0(3) . . . . ? C25 C21 Si5 O13 -43.1(3) . . . . ? Si1 O6 Si6 O9 155.2(4) . . . . ? Si1 O6 Si6 O14 36.6(5) . . . . ? Si1 O6 Si6 C26 -87.1(4) . . . . ? Si3 O9 Si6 O6 -90.7(3) . . . . ? Si3 O9 Si6 O14 29.3(3) . . . . ? Si3 O9 Si6 C26 149.7(3) . . . . ? Si7 O14 Si6 O6 38.9(3) . . . . ? Si7 O14 Si6 O9 -79.3(3) . . . . ? Si7 O14 Si6 C26 162.4(3) . . . . ? C30 C26 Si6 O6 -54.6(3) . . . . ? C27 C26 Si6 O6 -172.8(3) . . . . ? C30 C26 Si6 O9 63.2(3) . . . . ? C27 C26 Si6 O9 -55.1(3) . . . . ? C30 C26 Si6 O14 -177.9(2) . . . . ? C27 C26 Si6 O14 63.8(3) . . . . ? Si4 O12 Si7 O13 -49.5(3) . . . . ? Si4 O12 Si7 O14 70.7(3) . . . . ? Si4 O12 Si7 C31 -168.5(3) . . . . ? Si5 O13 Si7 O12 76.6(3) . . . . ? Si5 O13 Si7 O14 -43.0(3) . . . . ? Si5 O13 Si7 C31 -165.9(3) . . . . ? Si6 O14 Si7 O12 -65.5(3) . . . . ? Si6 O14 Si7 O13 54.1(3) . . . . ? Si6 O14 Si7 C31 176.1(3) . . . . ? C32 C31 Si7 O12 168.4(3) . . . . ? C35 C31 Si7 O12 48.2(3) . . . . ? C32 C31 Si7 O13 50.0(3) . . . . ? C35 C31 Si7 O13 -70.3(3) . . . . ? C32 C31 Si7 O14 -72.2(3) . . . . ? C35 C31 Si7 O14 167.6(3) . . . . ? Si3 O11 Si8 C38 -56.8(3) . . . . ? Si3 O11 Si8 C36 63.9(3) . . . . ? Si3 O11 Si8 C37 -176.5(3) . . . . ? Si2 O4 V O2 -55.5(2) . . . . ? Si2 O4 V O1 -175.6(2) . . . . ? Si2 O4 V O3 66.6(2) . . . . ? Si1 O3 V O2 45.7(2) . . . . ? Si1 O3 V O1 166.13(17) . . . . ? Si1 O3 V O4 -76.02(19) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.558 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.070