Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' # 1. Submission Details _journal_coden_Cambridge 0222 #============================================================================== _audit_creation_method SHELXL-97 _publ_contact_author_name 'Jun Okuda' _publ_contact_author_address ; Institut fur Anorganische Chemie Aachen University of Technology (RWTH) Prof.-Pirlet-Str. 1 D-52056 Aachen Germany ; _publ_contact_author_phone '0049 241 8094645' _publ_contact_author_fax '0049 241 8092644' _publ_contact_author_email jun.okuda@ac.rwth-aachen.de _publ_requested_category ? _publ_section_title ; Synthesis, Structure and Hydrosilylation Activity of Neutral and Cationic Rare-Earth Metal Silanolate Complexes ; _publ_requested_coeditor_name ? # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address B.Elvidge ; Institute of Inorganic Chemistry Aachen University of Technology (RWTH) Prof.-Pirlet-Str. 1 D-52056 Aachen Germany ; S.Arndt ; Institute of Inorganic Chemistry Aachen University of Technology (RWTH) Prof.-Pirlet-Str. 1 D-52056 Aachen Germany ; T.P.Spaniol ; Institute of Inorganic Chemistry Aachen University of Technology (RWTH) Prof.-Pirlet-Str. 1 D-52056 Aachen Germany ; J.Okuda ; Institute of Inorganic Chemistry Aachen University of Technology (RWTH) Prof.-Pirlet-Str. 1 D-52056 Aachen Germany ; #============================================================================ # 3. Chemical Data data_be6 _database_code_depnum_ccdc_archive 'CCDC 282721' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H98 O8 Si6 Y2' _chemical_formula_weight 1053.54 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2(1)/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.406(3) _cell_length_b 20.736(4) _cell_length_c 19.089(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.003(4) _cell_angle_gamma 90.00 _cell_volume 5942(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 956 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.51 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 2.103 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4720 _exptl_absorpt_correction_T_max 0.6005 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40280 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_sigmaI/netI 0.1765 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.38 _reflns_number_total 14697 _reflns_number_gt 6991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _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^)+(0.0578P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14697 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _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 Y1 Y 0.96277(3) 0.35361(2) 0.73061(2) 0.02396(13) Uani 1 1 d . . . Y2 Y 0.97421(3) 0.18396(3) 0.68788(3) 0.02836(14) Uani 1 1 d . . . Si1 Si 1.09826(9) 0.50852(7) 0.79638(8) 0.0275(3) Uani 1 1 d . . . Si2 Si 0.77914(13) 0.39416(10) 0.56595(9) 0.0600(6) Uani 1 1 d . . . Si3 Si 0.84748(9) 0.26761(7) 0.80849(7) 0.0234(3) Uani 1 1 d . . . Si4 Si 0.76832(10) 0.11883(8) 0.53497(8) 0.0341(4) Uani 1 1 d . . . Si5 Si 1.01697(10) 0.01531(8) 0.77156(9) 0.0393(4) Uani 1 1 d . . . Si6 Si 1.11129(9) 0.27259(7) 0.63379(7) 0.0274(4) Uani 1 1 d . . . O1 O 0.8622(2) 0.34758(16) 0.80655(16) 0.0239(8) Uani 1 1 d . . . O2 O 0.9159(2) 0.24978(16) 0.75875(16) 0.0256(8) Uani 1 1 d . . . O3 O 0.7450(2) 0.25381(16) 0.77155(16) 0.0282(8) Uani 1 1 d . . . O4 O 0.8693(2) 0.24023(16) 0.88953(16) 0.0247(8) Uani 1 1 d . . . O5 O 1.0747(2) 0.19828(17) 0.60865(17) 0.0324(9) Uani 1 1 d . . . O6 O 1.0465(2) 0.28352(17) 0.68848(17) 0.0290(8) Uani 1 1 d . . . O7 O 1.0910(2) 0.31691(17) 0.56276(17) 0.0326(9) Uani 1 1 d . . . O8 O 1.2161(2) 0.27588(16) 0.66866(16) 0.0266(8) Uani 1 1 d . . . C1 C 1.0757(3) 0.4211(2) 0.7997(3) 0.0314(13) Uani 1 1 d . . . H1A H 1.0714 0.4135 0.8501 0.038 Uiso 1 1 calc R . . H1B H 1.1321 0.4006 0.7952 0.038 Uiso 1 1 calc R . . C2 C 1.0774(4) 0.5510(3) 0.8777(3) 0.0381(14) Uani 1 1 d . . . H2A H 1.0157 0.5436 0.8813 0.057 Uiso 1 1 calc R . . H2B H 1.0875 0.5974 0.8735 0.057 Uiso 1 1 calc R . . H2C H 1.1181 0.5343 0.9209 0.057 Uiso 1 1 calc R . . C3 C 1.2170(4) 0.5239(3) 0.7911(3) 0.0473(16) Uani 1 1 d . . . H3A H 1.2574 0.5051 0.8332 0.071 Uiso 1 1 calc R . . H3B H 1.2274 0.5705 0.7900 0.071 Uiso 1 1 calc R . . H3C H 1.2282 0.5042 0.7473 0.071 Uiso 1 1 calc R . . C4 C 1.0277(4) 0.5503(3) 0.7160(3) 0.0429(15) Uani 1 1 d . . . H4A H 1.0409 0.5325 0.6720 0.064 Uiso 1 1 calc R . . H4B H 1.0408 0.5965 0.7187 0.064 Uiso 1 1 calc R . . H4C H 0.9646 0.5435 0.7154 0.064 Uiso 1 1 calc R . . C5 C 0.8881(4) 0.4012(4) 0.6209(3) 0.064(2) Uani 1 1 d . . . H5A H 0.8949 0.4481 0.6305 0.076 Uiso 1 1 calc R . . H5B H 0.9273 0.3914 0.5877 0.076 Uiso 1 1 calc R . . C6 C 0.7032(4) 0.3410(3) 0.6040(3) 0.060(2) Uani 1 1 d . . . H6A H 0.7375 0.3055 0.6307 0.089 Uiso 1 1 calc R . . H6B H 0.6569 0.3235 0.5648 0.089 Uiso 1 1 calc R . . H6C H 0.6753 0.3662 0.6365 0.089 Uiso 1 1 calc R . . C7 C 0.7588(7) 0.3878(7) 0.4721(4) 0.200(7) Uani 1 1 d . . . H7A H 0.7760 0.4281 0.4520 0.300 Uiso 1 1 calc R . . H7B H 0.6953 0.3797 0.4526 0.300 Uiso 1 1 calc R . . H7C H 0.7938 0.3521 0.4591 0.300 Uiso 1 1 calc R . . C8 C 0.7276(7) 0.4814(5) 0.5716(7) 0.193(7) Uani 1 1 d . . . H8A H 0.7058 0.4850 0.6159 0.290 Uiso 1 1 calc R . . H8B H 0.6780 0.4882 0.5300 0.290 Uiso 1 1 calc R . . H8C H 0.7735 0.5142 0.5717 0.290 Uiso 1 1 calc R . . C9 C 0.8261(3) 0.4018(3) 0.8426(3) 0.0288(12) Uani 1 1 d . . . C10 C 0.8313(3) 0.4604(2) 0.7968(3) 0.0340(13) Uani 1 1 d . . . H10A H 0.8934 0.4680 0.7946 0.051 Uiso 1 1 calc R . . H10B H 0.8085 0.4981 0.8179 0.051 Uiso 1 1 calc R . . H10C H 0.7953 0.4532 0.7481 0.051 Uiso 1 1 calc R . . C11 C 0.8841(4) 0.4090(3) 0.9171(3) 0.0523(18) Uani 1 1 d . . . H11A H 0.8817 0.3693 0.9444 0.078 Uiso 1 1 calc R . . H11B H 0.8626 0.4452 0.9415 0.078 Uiso 1 1 calc R . . H11C H 0.9457 0.4172 0.9137 0.078 Uiso 1 1 calc R . . C12 C 0.7302(4) 0.3872(3) 0.8449(3) 0.0479(16) Uani 1 1 d . . . H12A H 0.6952 0.3800 0.7959 0.072 Uiso 1 1 calc R . . H12B H 0.7053 0.4237 0.8663 0.072 Uiso 1 1 calc R . . H12C H 0.7283 0.3484 0.8739 0.072 Uiso 1 1 calc R . . C13 C 0.6774(3) 0.2058(3) 0.7772(3) 0.0314(13) Uani 1 1 d . . . C14 C 0.6297(4) 0.2281(3) 0.8339(3) 0.0440(16) Uani 1 1 d . . . H14A H 0.6723 0.2311 0.8803 0.066 Uiso 1 1 calc R . . H14B H 0.5829 0.1970 0.8374 0.066 Uiso 1 1 calc R . . H14C H 0.6029 0.2705 0.8206 0.066 Uiso 1 1 calc R . . C15 C 0.6139(3) 0.2047(3) 0.7040(3) 0.0427(16) Uani 1 1 d . . . H15A H 0.5881 0.2477 0.6928 0.064 Uiso 1 1 calc R . . H15B H 0.5661 0.1735 0.7044 0.064 Uiso 1 1 calc R . . H15C H 0.6463 0.1921 0.6675 0.064 Uiso 1 1 calc R . . C16 C 0.7202(3) 0.1404(3) 0.7960(3) 0.0454(16) Uani 1 1 d . . . H16A H 0.7548 0.1286 0.7607 0.068 Uiso 1 1 calc R . . H16B H 0.6737 0.1080 0.7956 0.068 Uiso 1 1 calc R . . H16C H 0.7597 0.1422 0.8440 0.068 Uiso 1 1 calc R . . C17 C 0.9487(3) 0.2198(3) 0.9419(3) 0.0287(12) Uani 1 1 d . . . C18 C 0.9356(4) 0.2397(3) 1.0160(3) 0.0411(15) Uani 1 1 d . . . H18A H 0.9365 0.2868 1.0197 0.062 Uiso 1 1 calc R . . H18B H 0.9838 0.2216 1.0533 0.062 Uiso 1 1 calc R . . H18C H 0.8783 0.2233 1.0225 0.062 Uiso 1 1 calc R . . C19 C 0.9529(4) 0.1470(3) 0.9366(3) 0.0430(15) Uani 1 1 d . . . H19A H 0.9000 0.1281 0.9491 0.064 Uiso 1 1 calc R . . H19B H 1.0065 0.1312 0.9700 0.064 Uiso 1 1 calc R . . H19C H 0.9547 0.1347 0.8874 0.064 Uiso 1 1 calc R . . C20 C 1.0324(3) 0.2502(3) 0.9257(3) 0.0359(14) Uani 1 1 d . . . H20A H 1.0411 0.2341 0.8795 0.054 Uiso 1 1 calc R . . H20B H 1.0841 0.2388 0.9639 0.054 Uiso 1 1 calc R . . H20C H 1.0256 0.2972 0.9234 0.054 Uiso 1 1 calc R . . C21 C 0.8358(3) 0.1447(3) 0.6212(3) 0.0429(15) Uani 1 1 d . . . H21A H 0.8287 0.1068 0.6509 0.051 Uiso 1 1 calc R . . H21B H 0.7955 0.1775 0.6343 0.051 Uiso 1 1 calc R . . C22 C 0.7634(5) 0.1827(5) 0.4644(4) 0.145(5) Uani 1 1 d . . . H22A H 0.8196 0.2068 0.4740 0.217 Uiso 1 1 calc R . . H22B H 0.7141 0.2123 0.4655 0.217 Uiso 1 1 calc R . . H22C H 0.7539 0.1624 0.4169 0.217 Uiso 1 1 calc R . . C23 C 0.8128(5) 0.0421(4) 0.5058(5) 0.141(5) Uani 1 1 d . . . H23A H 0.8653 0.0515 0.4865 0.212 Uiso 1 1 calc R . . H23B H 0.7670 0.0216 0.4685 0.212 Uiso 1 1 calc R . . H23C H 0.8297 0.0130 0.5471 0.212 Uiso 1 1 calc R . . C24 C 0.6492(3) 0.1018(3) 0.5372(3) 0.0406(15) Uani 1 1 d . . . H24A H 0.6474 0.0714 0.5762 0.061 Uiso 1 1 calc R . . H24B H 0.6184 0.0829 0.4913 0.061 Uiso 1 1 calc R . . H24C H 0.6197 0.1420 0.5454 0.061 Uiso 1 1 calc R . . C25 C 1.0498(3) 0.1006(2) 0.7621(3) 0.0361(14) Uani 1 1 d . . . H25A H 1.1089 0.0979 0.7499 0.043 Uiso 1 1 calc R . . H25B H 1.0611 0.1184 0.8115 0.043 Uiso 1 1 calc R . . C26 C 0.9040(4) 0.0101(3) 0.7918(4) 0.061(2) Uani 1 1 d . . . H26A H 0.9042 0.0331 0.8367 0.091 Uiso 1 1 calc R . . H26B H 0.8887 -0.0353 0.7969 0.091 Uiso 1 1 calc R . . H26C H 0.8600 0.0297 0.7524 0.091 Uiso 1 1 calc R . . C27 C 1.0928(4) -0.0290(3) 0.8473(3) 0.0589(19) Uani 1 1 d . . . H27A H 1.1535 -0.0293 0.8394 0.088 Uiso 1 1 calc R . . H27B H 1.0718 -0.0735 0.8490 0.088 Uiso 1 1 calc R . . H27C H 1.0925 -0.0074 0.8929 0.088 Uiso 1 1 calc R . . C28 C 1.0131(4) -0.0319(3) 0.6867(3) 0.0481(16) Uani 1 1 d . . . H28A H 0.9950 -0.0764 0.6934 0.072 Uiso 1 1 calc R . . H28B H 1.0722 -0.0318 0.6757 0.072 Uiso 1 1 calc R . . H28C H 0.9699 -0.0120 0.6469 0.072 Uiso 1 1 calc R . . C29 C 1.0899(4) 0.1576(3) 0.5484(3) 0.0429(16) Uani 1 1 d . . . C30 C 1.1883(4) 0.1597(3) 0.5479(3) 0.0497(17) Uani 1 1 d . . . H30A H 1.2056 0.2041 0.5400 0.075 Uiso 1 1 calc R . . H30B H 1.1995 0.1320 0.5092 0.075 Uiso 1 1 calc R . . H30C H 1.2234 0.1442 0.5942 0.075 Uiso 1 1 calc R . . C31 C 1.0610(4) 0.0898(3) 0.5656(3) 0.0505(18) Uani 1 1 d . . . H31A H 1.0984 0.0752 0.6114 0.076 Uiso 1 1 calc R . . H31B H 1.0677 0.0600 0.5272 0.076 Uiso 1 1 calc R . . H31C H 0.9986 0.0907 0.5691 0.076 Uiso 1 1 calc R . . C32 C 1.0322(4) 0.1833(3) 0.4791(3) 0.0558(19) Uani 1 1 d . . . H32A H 0.9698 0.1839 0.4828 0.084 Uiso 1 1 calc R . . H32B H 1.0384 0.1555 0.4390 0.084 Uiso 1 1 calc R . . H32C H 1.0511 0.2272 0.4706 0.084 Uiso 1 1 calc R . . C33 C 1.1306(3) 0.3767(3) 0.5457(3) 0.0342(14) Uani 1 1 d . . . C34 C 1.2199(3) 0.3618(3) 0.5280(3) 0.0440(16) Uani 1 1 d . . . H34A H 1.2603 0.3434 0.5704 0.066 Uiso 1 1 calc R . . H34B H 1.2457 0.4016 0.5138 0.066 Uiso 1 1 calc R . . H34C H 1.2113 0.3307 0.4884 0.066 Uiso 1 1 calc R . . C35 C 1.0647(4) 0.4038(3) 0.4797(3) 0.0544(19) Uani 1 1 d . . . H35A H 1.0539 0.3715 0.4413 0.082 Uiso 1 1 calc R . . H35B H 1.0897 0.4428 0.4630 0.082 Uiso 1 1 calc R . . H35C H 1.0083 0.4144 0.4928 0.082 Uiso 1 1 calc R . . C36 C 1.1410(4) 0.4233(3) 0.6082(3) 0.0385(14) Uani 1 1 d . . . H36A H 1.0834 0.4290 0.6211 0.058 Uiso 1 1 calc R . . H36B H 1.1619 0.4650 0.5943 0.058 Uiso 1 1 calc R . . H36C H 1.1843 0.4061 0.6496 0.058 Uiso 1 1 calc R . . C37 C 1.2797(3) 0.2636(2) 0.7359(3) 0.0284(12) Uani 1 1 d . . . C38 C 1.2394(4) 0.2216(3) 0.7848(3) 0.0523(18) Uani 1 1 d . . . H38A H 1.1897 0.2445 0.7979 0.078 Uiso 1 1 calc R . . H38B H 1.2847 0.2116 0.8284 0.078 Uiso 1 1 calc R . . H38C H 1.2176 0.1814 0.7599 0.078 Uiso 1 1 calc R . . C39 C 1.3085(4) 0.3289(3) 0.7693(3) 0.0469(16) Uani 1 1 d . . . H39A H 1.3316 0.3553 0.7350 0.070 Uiso 1 1 calc R . . H39B H 1.3552 0.3228 0.8131 0.070 Uiso 1 1 calc R . . H39C H 1.2573 0.3505 0.7814 0.070 Uiso 1 1 calc R . . C40 C 1.3578(4) 0.2296(3) 0.7154(3) 0.0495(17) Uani 1 1 d . . . H40A H 1.3380 0.1880 0.6931 0.074 Uiso 1 1 calc R . . H40B H 1.4049 0.2225 0.7586 0.074 Uiso 1 1 calc R . . H40C H 1.3807 0.2564 0.6813 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0163(3) 0.0352(3) 0.0199(2) -0.0009(2) 0.00302(19) 0.0024(2) Y2 0.0181(3) 0.0394(3) 0.0281(3) -0.0154(3) 0.0065(2) -0.0068(2) Si1 0.0245(8) 0.0289(9) 0.0283(8) 0.0011(7) 0.0047(6) 0.0043(7) Si2 0.0531(12) 0.0828(15) 0.0314(9) 0.0221(10) -0.0175(8) -0.0397(11) Si3 0.0146(7) 0.0361(9) 0.0192(7) -0.0051(6) 0.0032(6) -0.0005(6) Si4 0.0240(8) 0.0476(10) 0.0262(8) -0.0083(7) -0.0039(6) 0.0029(7) Si5 0.0227(9) 0.0389(10) 0.0538(11) -0.0128(9) 0.0036(8) -0.0031(7) Si6 0.0178(8) 0.0408(10) 0.0235(8) -0.0099(7) 0.0048(6) -0.0037(7) O1 0.0196(18) 0.033(2) 0.0186(17) -0.0016(16) 0.0036(14) 0.0039(15) O2 0.0186(18) 0.041(2) 0.0169(17) -0.0051(16) 0.0043(14) -0.0033(16) O3 0.0139(18) 0.048(2) 0.0212(18) 0.0028(17) 0.0006(14) -0.0050(16) O4 0.0134(17) 0.039(2) 0.0200(18) -0.0010(16) 0.0000(14) -0.0014(15) O5 0.022(2) 0.046(2) 0.032(2) -0.0165(18) 0.0114(16) -0.0059(17) O6 0.0173(18) 0.041(2) 0.0289(19) -0.0121(17) 0.0068(15) -0.0055(16) O7 0.023(2) 0.046(2) 0.0268(19) -0.0048(18) 0.0012(15) -0.0017(18) O8 0.0175(18) 0.039(2) 0.0217(18) -0.0028(16) 0.0013(14) -0.0023(16) C1 0.024(3) 0.034(3) 0.033(3) 0.002(3) -0.002(2) 0.002(2) C2 0.043(4) 0.037(3) 0.035(3) -0.002(3) 0.009(3) 0.000(3) C3 0.040(4) 0.044(4) 0.062(4) 0.000(3) 0.021(3) -0.002(3) C4 0.040(4) 0.045(4) 0.041(3) 0.004(3) 0.004(3) 0.013(3) C5 0.035(4) 0.115(6) 0.037(4) 0.036(4) -0.001(3) -0.002(4) C6 0.051(4) 0.077(5) 0.044(4) 0.008(4) -0.004(3) -0.033(4) C7 0.173(11) 0.369(19) 0.041(5) 0.040(8) -0.010(6) -0.160(12) C8 0.128(10) 0.172(11) 0.311(17) 0.168(12) 0.115(10) 0.086(8) C9 0.031(3) 0.036(3) 0.022(3) 0.000(2) 0.011(2) 0.013(3) C10 0.023(3) 0.037(3) 0.042(3) 0.003(3) 0.007(2) 0.006(2) C11 0.077(5) 0.054(4) 0.024(3) -0.014(3) 0.006(3) 0.027(4) C12 0.044(4) 0.048(4) 0.063(4) 0.008(3) 0.036(3) 0.010(3) C13 0.019(3) 0.052(4) 0.022(3) -0.002(3) 0.003(2) -0.010(3) C14 0.034(3) 0.071(5) 0.030(3) -0.002(3) 0.014(3) -0.014(3) C15 0.023(3) 0.073(5) 0.030(3) -0.004(3) 0.002(2) -0.017(3) C16 0.026(3) 0.049(4) 0.058(4) -0.001(3) 0.002(3) -0.008(3) C17 0.023(3) 0.036(3) 0.024(3) 0.001(3) -0.002(2) -0.002(2) C18 0.037(3) 0.063(4) 0.019(3) 0.000(3) -0.003(2) 0.001(3) C19 0.037(3) 0.041(4) 0.044(4) 0.001(3) -0.006(3) 0.000(3) C20 0.021(3) 0.051(4) 0.031(3) -0.002(3) -0.004(2) 0.001(3) C21 0.028(3) 0.070(4) 0.029(3) -0.014(3) 0.004(2) -0.012(3) C22 0.034(5) 0.304(15) 0.098(7) 0.130(8) 0.019(4) 0.013(6) C23 0.035(5) 0.135(8) 0.237(12) -0.147(8) -0.006(6) 0.005(5) C24 0.032(3) 0.044(4) 0.041(3) -0.012(3) -0.001(3) -0.004(3) C25 0.024(3) 0.040(4) 0.044(3) -0.021(3) 0.006(3) -0.003(3) C26 0.032(4) 0.052(4) 0.102(6) -0.032(4) 0.021(4) -0.017(3) C27 0.045(4) 0.071(5) 0.054(4) 0.005(4) -0.001(3) -0.009(4) C28 0.049(4) 0.038(4) 0.053(4) -0.011(3) 0.002(3) -0.001(3) C29 0.027(3) 0.066(4) 0.036(3) -0.033(3) 0.007(3) -0.005(3) C30 0.036(4) 0.063(5) 0.056(4) -0.030(3) 0.024(3) -0.010(3) C31 0.042(4) 0.056(4) 0.061(4) -0.045(4) 0.026(3) -0.014(3) C32 0.038(4) 0.088(5) 0.042(4) -0.032(4) 0.009(3) -0.015(4) C33 0.024(3) 0.052(4) 0.027(3) 0.005(3) 0.005(2) 0.004(3) C34 0.037(4) 0.065(4) 0.034(3) 0.007(3) 0.018(3) 0.010(3) C35 0.040(4) 0.092(6) 0.030(3) 0.014(3) 0.005(3) 0.016(4) C36 0.032(3) 0.045(4) 0.040(3) 0.003(3) 0.011(3) 0.008(3) C37 0.021(3) 0.033(3) 0.029(3) -0.003(2) -0.001(2) -0.005(2) C38 0.043(4) 0.072(5) 0.035(3) 0.013(3) -0.005(3) -0.025(3) C39 0.033(4) 0.045(4) 0.055(4) -0.008(3) -0.008(3) 0.001(3) C40 0.034(4) 0.060(4) 0.049(4) -0.008(3) -0.001(3) 0.013(3) _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 Y1 O6 2.211(3) . ? Y1 O1 2.352(3) . ? Y1 C5 2.366(5) . ? Y1 O2 2.370(3) . ? Y1 C1 2.386(5) . ? Y1 Si3 3.1198(15) . ? Y1 Y2 3.6245(10) . ? Y2 O2 2.246(3) . ? Y2 O6 2.344(3) . ? Y2 C21 2.367(5) . ? Y2 C25 2.369(5) . ? Y2 O5 2.413(3) . ? Y2 Si6 3.1441(16) . ? Si1 C1 1.849(5) . ? Si1 C2 1.875(5) . ? Si1 C4 1.880(5) . ? Si1 C3 1.882(5) . ? Si2 C7 1.754(8) . ? Si2 C5 1.774(6) . ? Si2 C6 1.869(6) . ? Si2 C8 1.989(10) . ? Si3 O3 1.603(3) . ? Si3 O4 1.611(3) . ? Si3 O2 1.613(3) . ? Si3 O1 1.675(4) . ? Si4 C21 1.819(5) . ? Si4 C23 1.866(7) . ? Si4 C22 1.878(8) . ? Si4 C24 1.879(5) . ? Si5 C25 1.859(5) . ? Si5 C26 1.869(5) . ? Si5 C27 1.881(6) . ? Si5 C28 1.881(6) . ? Si6 O8 1.603(3) . ? Si6 O7 1.609(4) . ? Si6 O6 1.615(3) . ? Si6 O5 1.674(4) . ? O1 C9 1.489(6) . ? O3 C13 1.462(6) . ? O4 C17 1.458(5) . ? O5 C29 1.487(6) . ? O7 C33 1.450(6) . ? O8 C37 1.451(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.507(7) . ? C9 C10 1.511(7) . ? C9 C12 1.518(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.511(7) . ? C13 C15 1.515(6) . ? C13 C16 1.517(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.514(7) . ? C17 C20 1.527(7) . ? C17 C18 1.530(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.515(8) . ? C29 C30 1.519(7) . ? C29 C31 1.533(8) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.515(7) . ? C33 C34 1.521(7) . ? C33 C35 1.537(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.509(7) . ? C37 C40 1.518(7) . ? C37 C39 1.520(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Y1 O1 135.11(12) . . ? O6 Y1 C5 99.18(19) . . ? O1 Y1 C5 108.13(17) . . ? O6 Y1 O2 73.59(12) . . ? O1 Y1 O2 62.33(11) . . ? C5 Y1 O2 117.85(18) . . ? O6 Y1 C1 100.05(15) . . ? O1 Y1 C1 100.94(15) . . ? C5 Y1 C1 113.2(2) . . ? O2 Y1 C1 128.96(14) . . ? O6 Y1 Si3 103.81(9) . . ? O1 Y1 Si3 31.90(8) . . ? C5 Y1 Si3 116.39(15) . . ? O2 Y1 Si3 30.44(8) . . ? C1 Y1 Si3 119.62(13) . . ? O6 Y1 Y2 38.58(9) . . ? O1 Y1 Y2 99.16(8) . . ? C5 Y1 Y2 104.13(19) . . ? O2 Y1 Y2 37.07(7) . . ? C1 Y1 Y2 128.88(12) . . ? Si3 Y1 Y2 67.30(3) . . ? O2 Y2 O6 73.48(11) . . ? O2 Y2 C21 95.69(16) . . ? O6 Y2 C21 132.41(17) . . ? O2 Y2 C25 107.02(15) . . ? O6 Y2 C25 118.07(15) . . ? C21 Y2 C25 109.46(19) . . ? O2 Y2 O5 134.61(12) . . ? O6 Y2 O5 61.57(11) . . ? C21 Y2 O5 109.40(15) . . ? C25 Y2 O5 99.56(15) . . ? O2 Y2 Si6 103.39(9) . . ? O6 Y2 Si6 29.94(8) . . ? C21 Y2 Si6 127.91(14) . . ? C25 Y2 Si6 110.28(13) . . ? O5 Y2 Si6 31.73(8) . . ? O2 Y2 Y1 39.50(8) . . ? O6 Y2 Y1 36.03(8) . . ? C21 Y2 Y1 111.78(15) . . ? C25 Y2 Y1 128.03(12) . . ? O5 Y2 Y1 95.29(8) . . ? Si6 Y2 Y1 64.96(3) . . ? C1 Si1 C2 111.3(2) . . ? C1 Si1 C4 113.6(2) . . ? C2 Si1 C4 106.5(2) . . ? C1 Si1 C3 111.2(2) . . ? C2 Si1 C3 108.3(3) . . ? C4 Si1 C3 105.6(3) . . ? C7 Si2 C5 122.6(4) . . ? C7 Si2 C6 111.7(4) . . ? C5 Si2 C6 114.2(3) . . ? C7 Si2 C8 98.1(6) . . ? C5 Si2 C8 103.3(5) . . ? C6 Si2 C8 102.9(4) . . ? O3 Si3 O4 109.37(17) . . ? O3 Si3 O2 114.19(18) . . ? O4 Si3 O2 117.50(18) . . ? O3 Si3 O1 106.96(18) . . ? O4 Si3 O1 111.72(17) . . ? O2 Si3 O1 95.99(17) . . ? O3 Si3 Y1 120.15(13) . . ? O4 Si3 Y1 129.86(13) . . ? O2 Si3 Y1 48.14(12) . . ? O1 Si3 Y1 47.88(11) . . ? C21 Si4 C23 110.4(3) . . ? C21 Si4 C22 111.3(4) . . ? C23 Si4 C22 110.2(5) . . ? C21 Si4 C24 113.4(2) . . ? C23 Si4 C24 105.8(3) . . ? C22 Si4 C24 105.5(3) . . ? C25 Si5 C26 111.2(3) . . ? C25 Si5 C27 113.8(3) . . ? C26 Si5 C27 105.0(3) . . ? C25 Si5 C28 111.6(3) . . ? C26 Si5 C28 107.3(3) . . ? C27 Si5 C28 107.5(3) . . ? O8 Si6 O7 108.16(18) . . ? O8 Si6 O6 115.90(18) . . ? O7 Si6 O6 115.71(19) . . ? O8 Si6 O5 113.66(18) . . ? O7 Si6 O5 107.17(18) . . ? O6 Si6 O5 95.56(18) . . ? O8 Si6 Y2 125.21(14) . . ? O7 Si6 Y2 126.39(13) . . ? O6 Si6 Y2 46.45(13) . . ? O5 Si6 Y2 49.30(11) . . ? C9 O1 Si3 132.1(3) . . ? C9 O1 Y1 127.6(3) . . ? Si3 O1 Y1 100.21(15) . . ? Si3 O2 Y2 153.7(2) . . ? Si3 O2 Y1 101.42(16) . . ? Y2 O2 Y1 103.43(12) . . ? C13 O3 Si3 137.5(3) . . ? C17 O4 Si3 136.3(3) . . ? C29 O5 Si6 130.0(3) . . ? C29 O5 Y2 130.6(3) . . ? Si6 O5 Y2 98.98(15) . . ? Si6 O6 Y1 145.4(2) . . ? Si6 O6 Y2 103.61(17) . . ? Y1 O6 Y2 105.38(12) . . ? C33 O7 Si6 131.7(3) . . ? C37 O8 Si6 140.9(3) . . ? Si1 C1 Y1 132.5(2) . . ? Si1 C1 H1A 104.1 . . ? Y1 C1 H1A 104.1 . . ? Si1 C1 H1B 104.1 . . ? Y1 C1 H1B 104.1 . . ? H1A C1 H1B 105.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 Y1 134.1(3) . . ? Si2 C5 H5A 103.7 . . ? Y1 C5 H5A 103.7 . . ? Si2 C5 H5B 103.7 . . ? Y1 C5 H5B 103.7 . . ? H5A C5 H5B 105.3 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 C11 107.9(4) . . ? O1 C9 C10 105.5(4) . . ? C11 C9 C10 111.7(5) . . ? O1 C9 C12 109.2(4) . . ? C11 C9 C12 111.5(5) . . ? C10 C9 C12 110.8(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 C14 108.3(4) . . ? O3 C13 C15 105.5(4) . . ? C14 C13 C15 110.4(4) . . ? O3 C13 C16 110.3(4) . . ? C14 C13 C16 111.0(5) . . ? C15 C13 C16 111.2(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 C19 106.6(4) . . ? O4 C17 C20 111.0(4) . . ? C19 C17 C20 110.4(4) . . ? O4 C17 C18 106.9(4) . . ? C19 C17 C18 110.3(4) . . ? C20 C17 C18 111.6(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si4 C21 Y2 148.2(3) . . ? Si4 C21 H21A 99.7 . . ? Y2 C21 H21A 99.7 . . ? Si4 C21 H21B 99.7 . . ? Y2 C21 H21B 99.7 . . ? H21A C21 H21B 104.1 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si5 C25 Y2 130.1(3) . . ? Si5 C25 H25A 104.7 . . ? Y2 C25 H25A 104.7 . . ? Si5 C25 H25B 104.7 . . ? Y2 C25 H25B 104.7 . . ? H25A C25 H25B 105.7 . . ? Si5 C26 H26A 109.5 . . ? Si5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si5 C27 H27A 109.5 . . ? Si5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si5 C28 H28A 109.5 . . ? Si5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 C32 108.2(5) . . ? O5 C29 C30 108.7(4) . . ? C32 C29 C30 112.0(5) . . ? O5 C29 C31 104.5(4) . . ? C32 C29 C31 111.6(5) . . ? C30 C29 C31 111.4(5) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O7 C33 C36 110.1(4) . . ? O7 C33 C34 108.8(4) . . ? C36 C33 C34 111.4(4) . . ? O7 C33 C35 105.2(4) . . ? C36 C33 C35 110.2(5) . . ? C34 C33 C35 110.9(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O8 C37 C38 111.0(4) . . ? O8 C37 C40 105.7(4) . . ? C38 C37 C40 110.6(5) . . ? O8 C37 C39 106.8(4) . . ? C38 C37 C39 112.1(5) . . ? C40 C37 C39 110.4(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Y1 Y2 O2 155.20(18) . . . . ? O1 Y1 Y2 O2 -6.33(14) . . . . ? C5 Y1 Y2 O2 -117.77(19) . . . . ? C1 Y1 Y2 O2 105.8(2) . . . . ? Si3 Y1 Y2 O2 -4.72(12) . . . . ? O1 Y1 Y2 O6 -161.53(15) . . . . ? C5 Y1 Y2 O6 87.0(2) . . . . ? O2 Y1 Y2 O6 -155.20(18) . . . . ? C1 Y1 Y2 O6 -49.4(2) . . . . ? Si3 Y1 Y2 O6 -159.92(14) . . . . ? O6 Y1 Y2 C21 -133.3(2) . . . . ? O1 Y1 Y2 C21 65.20(16) . . . . ? C5 Y1 Y2 C21 -46.2(2) . . . . ? O2 Y1 Y2 C21 71.53(19) . . . . ? C1 Y1 Y2 C21 177.4(2) . . . . ? Si3 Y1 Y2 C21 66.81(14) . . . . ? O6 Y1 Y2 C25 86.6(2) . . . . ? O1 Y1 Y2 C25 -74.95(18) . . . . ? C5 Y1 Y2 C25 173.6(2) . . . . ? O2 Y1 Y2 C25 -68.6(2) . . . . ? C1 Y1 Y2 C25 37.2(2) . . . . ? Si3 Y1 Y2 C25 -73.34(17) . . . . ? O6 Y1 Y2 O5 -19.93(15) . . . . ? O1 Y1 Y2 O5 178.54(11) . . . . ? C5 Y1 Y2 O5 67.09(17) . . . . ? O2 Y1 Y2 O5 -175.13(15) . . . . ? C1 Y1 Y2 O5 -69.31(18) . . . . ? Si3 Y1 Y2 O5 -179.85(9) . . . . ? O6 Y1 Y2 Si6 -10.34(14) . . . . ? O1 Y1 Y2 Si6 -171.87(8) . . . . ? C5 Y1 Y2 Si6 76.69(15) . . . . ? O2 Y1 Y2 Si6 -165.54(12) . . . . ? C1 Y1 Y2 Si6 -59.72(17) . . . . ? Si3 Y1 Y2 Si6 -170.26(4) . . . . ? O6 Y1 Si3 O3 -103.77(18) . . . . ? O1 Y1 Si3 O3 86.0(2) . . . . ? C5 Y1 Si3 O3 4.0(3) . . . . ? O2 Y1 Si3 O3 -96.7(2) . . . . ? C1 Y1 Si3 O3 146.0(2) . . . . ? Y2 Y1 Si3 O3 -91.03(16) . . . . ? O6 Y1 Si3 O4 86.29(19) . . . . ? O1 Y1 Si3 O4 -84.0(2) . . . . ? C5 Y1 Si3 O4 -165.9(3) . . . . ? O2 Y1 Si3 O4 93.4(2) . . . . ? C1 Y1 Si3 O4 -24.0(2) . . . . ? Y2 Y1 Si3 O4 99.03(17) . . . . ? O6 Y1 Si3 O2 -7.12(17) . . . . ? O1 Y1 Si3 O2 -177.4(2) . . . . ? C5 Y1 Si3 O2 100.7(3) . . . . ? C1 Y1 Si3 O2 -117.4(2) . . . . ? Y2 Y1 Si3 O2 5.62(15) . . . . ? O6 Y1 Si3 O1 170.27(16) . . . . ? C5 Y1 Si3 O1 -82.0(3) . . . . ? O2 Y1 Si3 O1 177.4(2) . . . . ? C1 Y1 Si3 O1 60.0(2) . . . . ? Y2 Y1 Si3 O1 -176.99(14) . . . . ? O2 Y2 Si6 O8 96.65(18) . . . . ? O6 Y2 Si6 O8 93.8(2) . . . . ? C21 Y2 Si6 O8 -155.0(2) . . . . ? C25 Y2 Si6 O8 -17.5(2) . . . . ? O5 Y2 Si6 O8 -92.3(2) . . . . ? Y1 Y2 Si6 O8 106.05(16) . . . . ? O2 Y2 Si6 O7 -89.64(19) . . . . ? O6 Y2 Si6 O7 -92.5(2) . . . . ? C21 Y2 Si6 O7 18.7(3) . . . . ? C25 Y2 Si6 O7 156.2(2) . . . . ? O5 Y2 Si6 O7 81.4(2) . . . . ? Y1 Y2 Si6 O7 -80.25(17) . . . . ? O2 Y2 Si6 O6 2.82(19) . . . . ? C21 Y2 Si6 O6 111.1(2) . . . . ? C25 Y2 Si6 O6 -111.3(2) . . . . ? O5 Y2 Si6 O6 173.8(2) . . . . ? Y1 Y2 Si6 O6 12.21(16) . . . . ? O2 Y2 Si6 O5 -171.00(18) . . . . ? O6 Y2 Si6 O5 -173.8(2) . . . . ? C21 Y2 Si6 O5 -62.7(2) . . . . ? C25 Y2 Si6 O5 74.9(2) . . . . ? Y1 Y2 Si6 O5 -161.61(16) . . . . ? O3 Si3 O1 C9 65.8(4) . . . . ? O4 Si3 O1 C9 -53.8(4) . . . . ? O2 Si3 O1 C9 -176.6(4) . . . . ? Y1 Si3 O1 C9 -178.5(4) . . . . ? O3 Si3 O1 Y1 -115.61(16) . . . . ? O4 Si3 O1 Y1 124.74(15) . . . . ? O2 Si3 O1 Y1 1.95(16) . . . . ? O6 Y1 O1 C9 165.2(3) . . . . ? C5 Y1 O1 C9 -70.3(4) . . . . ? O2 Y1 O1 C9 177.1(4) . . . . ? C1 Y1 O1 C9 48.7(3) . . . . ? Si3 Y1 O1 C9 178.6(4) . . . . ? Y2 Y1 O1 C9 -178.6(3) . . . . ? O6 Y1 O1 Si3 -13.4(2) . . . . ? C5 Y1 O1 Si3 111.1(2) . . . . ? O2 Y1 O1 Si3 -1.49(12) . . . . ? C1 Y1 O1 Si3 -129.94(17) . . . . ? Y2 Y1 O1 Si3 2.81(13) . . . . ? O3 Si3 O2 Y2 -51.1(5) . . . . ? O4 Si3 O2 Y2 79.0(4) . . . . ? O1 Si3 O2 Y2 -162.7(4) . . . . ? Y1 Si3 O2 Y2 -160.8(5) . . . . ? O3 Si3 O2 Y1 109.68(18) . . . . ? O4 Si3 O2 Y1 -120.25(17) . . . . ? O1 Si3 O2 Y1 -1.95(16) . . . . ? O6 Y2 O2 Si3 175.5(4) . . . . ? C21 Y2 O2 Si3 42.9(4) . . . . ? C25 Y2 O2 Si3 -69.5(4) . . . . ? O5 Y2 O2 Si3 167.4(4) . . . . ? Si6 Y2 O2 Si3 174.1(4) . . . . ? Y1 Y2 O2 Si3 160.6(5) . . . . ? O6 Y2 O2 Y1 14.91(11) . . . . ? C21 Y2 O2 Y1 -117.73(17) . . . . ? C25 Y2 O2 Y1 129.90(15) . . . . ? O5 Y2 O2 Y1 6.8(2) . . . . ? Si6 Y2 O2 Y1 13.45(11) . . . . ? O6 Y1 O2 Si3 172.79(17) . . . . ? O1 Y1 O2 Si3 1.56(13) . . . . ? C5 Y1 O2 Si3 -95.3(2) . . . . ? C1 Y1 O2 Si3 83.0(2) . . . . ? Y2 Y1 O2 Si3 -171.4(2) . . . . ? O6 Y1 O2 Y2 -15.82(11) . . . . ? O1 Y1 O2 Y2 172.94(16) . . . . ? C5 Y1 O2 Y2 76.0(2) . . . . ? C1 Y1 O2 Y2 -105.59(19) . . . . ? Si3 Y1 O2 Y2 171.4(2) . . . . ? O4 Si3 O3 C13 -29.3(5) . . . . ? O2 Si3 O3 C13 104.7(5) . . . . ? O1 Si3 O3 C13 -150.4(4) . . . . ? Y1 Si3 O3 C13 158.9(4) . . . . ? O3 Si3 O4 C17 157.2(4) . . . . ? O2 Si3 O4 C17 25.0(5) . . . . ? O1 Si3 O4 C17 -84.6(5) . . . . ? Y1 Si3 O4 C17 -32.0(5) . . . . ? O8 Si6 O5 C29 -70.7(4) . . . . ? O7 Si6 O5 C29 48.7(4) . . . . ? O6 Si6 O5 C29 167.8(4) . . . . ? Y2 Si6 O5 C29 172.3(5) . . . . ? O8 Si6 O5 Y2 116.96(17) . . . . ? O7 Si6 O5 Y2 -123.59(16) . . . . ? O6 Si6 O5 Y2 -4.50(18) . . . . ? O2 Y2 O5 C29 -159.9(4) . . . . ? O6 Y2 O5 C29 -168.8(4) . . . . ? C21 Y2 O5 C29 -40.3(4) . . . . ? C25 Y2 O5 C29 74.4(4) . . . . ? Si6 Y2 O5 C29 -172.3(5) . . . . ? Y1 Y2 O5 C29 -155.6(4) . . . . ? O2 Y2 O5 Si6 12.3(2) . . . . ? O6 Y2 O5 Si6 3.50(14) . . . . ? C21 Y2 O5 Si6 132.0(2) . . . . ? C25 Y2 O5 Si6 -113.33(18) . . . . ? Y1 Y2 O5 Si6 16.69(15) . . . . ? O8 Si6 O6 Y1 98.6(3) . . . . ? O7 Si6 O6 Y1 -29.6(4) . . . . ? O5 Si6 O6 Y1 -141.7(3) . . . . ? Y2 Si6 O6 Y1 -146.4(4) . . . . ? O8 Si6 O6 Y2 -115.00(18) . . . . ? O7 Si6 O6 Y2 116.80(18) . . . . ? O5 Si6 O6 Y2 4.71(18) . . . . ? O1 Y1 O6 Si6 172.4(3) . . . . ? C5 Y1 O6 Si6 44.9(4) . . . . ? O2 Y1 O6 Si6 161.4(4) . . . . ? C1 Y1 O6 Si6 -70.8(3) . . . . ? Si3 Y1 O6 Si6 165.1(3) . . . . ? Y2 Y1 O6 Si6 146.1(4) . . . . ? O1 Y1 O6 Y2 26.3(2) . . . . ? C5 Y1 O6 Y2 -101.19(19) . . . . ? O2 Y1 O6 Y2 15.28(11) . . . . ? C1 Y1 O6 Y2 143.12(16) . . . . ? Si3 Y1 O6 Y2 19.04(13) . . . . ? O2 Y2 O6 Si6 -177.14(19) . . . . ? C21 Y2 O6 Si6 -94.7(2) . . . . ? C25 Y2 O6 Si6 82.0(2) . . . . ? O5 Y2 O6 Si6 -3.69(14) . . . . ? Y1 Y2 O6 Si6 -161.0(2) . . . . ? O2 Y2 O6 Y1 -16.16(12) . . . . ? C21 Y2 O6 Y1 66.3(2) . . . . ? C25 Y2 O6 Y1 -116.99(17) . . . . ? O5 Y2 O6 Y1 157.29(17) . . . . ? Si6 Y2 O6 Y1 161.0(2) . . . . ? O8 Si6 O7 C33 -34.4(5) . . . . ? O6 Si6 O7 C33 97.5(4) . . . . ? O5 Si6 O7 C33 -157.3(4) . . . . ? Y2 Si6 O7 C33 151.0(4) . . . . ? O7 Si6 O8 C37 161.4(5) . . . . ? O6 Si6 O8 C37 29.6(6) . . . . ? O5 Si6 O8 C37 -79.7(5) . . . . ? Y2 Si6 O8 C37 -23.9(6) . . . . ? C2 Si1 C1 Y1 111.2(4) . . . . ? C4 Si1 C1 Y1 -9.0(5) . . . . ? C3 Si1 C1 Y1 -127.9(4) . . . . ? O6 Y1 C1 Si1 121.9(4) . . . . ? O1 Y1 C1 Si1 -98.0(4) . . . . ? C5 Y1 C1 Si1 17.3(4) . . . . ? O2 Y1 C1 Si1 -161.1(3) . . . . ? Si3 Y1 C1 Si1 -125.8(3) . . . . ? Y2 Y1 C1 Si1 150.7(3) . . . . ? C7 Si2 C5 Y1 -136.4(7) . . . . ? C6 Si2 C5 Y1 3.8(7) . . . . ? C8 Si2 C5 Y1 114.7(6) . . . . ? O6 Y1 C5 Si2 104.0(5) . . . . ? O1 Y1 C5 Si2 -39.9(6) . . . . ? O2 Y1 C5 Si2 27.8(6) . . . . ? C1 Y1 C5 Si2 -150.8(5) . . . . ? Si3 Y1 C5 Si2 -6.5(6) . . . . ? Y2 Y1 C5 Si2 64.9(5) . . . . ? Si3 O1 C9 C11 84.0(5) . . . . ? Y1 O1 C9 C11 -94.2(4) . . . . ? Si3 O1 C9 C10 -156.6(3) . . . . ? Y1 O1 C9 C10 25.2(5) . . . . ? Si3 O1 C9 C12 -37.4(6) . . . . ? Y1 O1 C9 C12 144.4(3) . . . . ? Si3 O3 C13 C14 88.9(6) . . . . ? Si3 O3 C13 C15 -152.9(4) . . . . ? Si3 O3 C13 C16 -32.8(6) . . . . ? Si3 O4 C17 C19 -97.3(5) . . . . ? Si3 O4 C17 C20 23.0(6) . . . . ? Si3 O4 C17 C18 144.8(4) . . . . ? C23 Si4 C21 Y2 67.4(7) . . . . ? C22 Si4 C21 Y2 -55.3(7) . . . . ? C24 Si4 C21 Y2 -174.0(6) . . . . ? O2 Y2 C21 Si4 142.5(6) . . . . ? O6 Y2 C21 Si4 69.7(7) . . . . ? C25 Y2 C21 Si4 -107.2(6) . . . . ? O5 Y2 C21 Si4 0.9(7) . . . . ? Si6 Y2 C21 Si4 30.6(7) . . . . ? Y1 Y2 C21 Si4 105.2(6) . . . . ? C26 Si5 C25 Y2 -53.6(4) . . . . ? C27 Si5 C25 Y2 -172.0(3) . . . . ? C28 Si5 C25 Y2 66.1(4) . . . . ? O2 Y2 C25 Si5 104.0(3) . . . . ? O6 Y2 C25 Si5 -176.0(3) . . . . ? C21 Y2 C25 Si5 1.4(4) . . . . ? O5 Y2 C25 Si5 -113.3(3) . . . . ? Si6 Y2 C25 Si5 -144.2(3) . . . . ? Y1 Y2 C25 Si5 142.2(3) . . . . ? Si6 O5 C29 C32 -75.7(5) . . . . ? Y2 O5 C29 C32 94.4(5) . . . . ? Si6 O5 C29 C30 46.2(6) . . . . ? Y2 O5 C29 C30 -143.8(4) . . . . ? Si6 O5 C29 C31 165.3(4) . . . . ? Y2 O5 C29 C31 -24.7(6) . . . . ? Si6 O7 C33 C36 -45.2(6) . . . . ? Si6 O7 C33 C34 77.2(5) . . . . ? Si6 O7 C33 C35 -164.0(4) . . . . ? Si6 O8 C37 C38 17.2(7) . . . . ? Si6 O8 C37 C40 137.2(5) . . . . ? Si6 O8 C37 C39 -105.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.380 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.106 #===END #=============================================================== data_be8 _database_code_depnum_ccdc_archive 'CCDC 282722' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H98 O8 Sc2 Si6' _chemical_formula_weight 965.64 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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2(1)/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.337(3) _cell_length_b 20.339(3) _cell_length_c 19.066(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.614(5) _cell_angle_gamma 90.00 _cell_volume 5780.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 941 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 20.67 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.399 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8076 _exptl_absorpt_correction_T_max 0.9390 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78058 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.19 _reflns_number_total 14152 _reflns_number_gt 11129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution ; isotypic replacement using the coordinates of C40 H98 O8 Si6 Y2 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _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^)+(0.0754P)^2^+3.1599P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14152 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.1748 _refine_ls_wR_factor_gt 0.1591 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sc1 Sc 0.96538(3) 0.34655(3) 0.73280(3) 0.01571(13) Uani 1 1 d . . . Sc2 Sc 0.97489(4) 0.18934(3) 0.68550(3) 0.01996(14) Uani 1 1 d . . . Si1 Si 1.09543(6) 0.50223(4) 0.79607(5) 0.02126(19) Uani 1 1 d . . . Si2 Si 0.78174(6) 0.39672(5) 0.57533(5) 0.0272(2) Uani 1 1 d . . . Si3 Si 0.85253(5) 0.26531(4) 0.80572(4) 0.01764(18) Uani 1 1 d . . . Si4 Si 0.77522(6) 0.12321(5) 0.53640(5) 0.0284(2) Uani 1 1 d . . . Si5 Si 1.01525(6) 0.02127(5) 0.76516(6) 0.0296(2) Uani 1 1 d . . . Si6 Si 1.10939(5) 0.27310(4) 0.63626(4) 0.01867(18) Uani 1 1 d . . . O1 O 0.87130(13) 0.34665(10) 0.80438(11) 0.0201(4) Uani 1 1 d . . . O2 O 0.92094(13) 0.24696(10) 0.75570(10) 0.0181(4) Uani 1 1 d . . . O3 O 0.74886(13) 0.25323(11) 0.76853(11) 0.0221(5) Uani 1 1 d . . . O4 O 0.87398(14) 0.23654(11) 0.88636(11) 0.0241(5) Uani 1 1 d . . . O5 O 1.07064(14) 0.19808(11) 0.61023(12) 0.0240(5) Uani 1 1 d . . . O6 O 1.04488(13) 0.28260(10) 0.69133(11) 0.0192(4) Uani 1 1 d . . . O7 O 1.08736(14) 0.31955(11) 0.56625(12) 0.0251(5) Uani 1 1 d . . . O8 O 1.21481(13) 0.27641(11) 0.67046(11) 0.0219(5) Uani 1 1 d . . . C1 C 1.0721(2) 0.41258(15) 0.79414(17) 0.0213(6) Uani 1 1 d . . . H1A H 1.0731 0.4024 0.8451 0.026 Uiso 1 1 calc R . . H1B H 1.1278 0.3930 0.7857 0.026 Uiso 1 1 calc R . . C2 C 1.0739(2) 0.54262(18) 0.87874(19) 0.0326(8) Uani 1 1 d . . . H2A H 1.0095 0.5413 0.8769 0.049 Uiso 1 1 calc R . . H2B H 1.0940 0.5885 0.8807 0.049 Uiso 1 1 calc R . . H2C H 1.1069 0.5192 0.9218 0.049 Uiso 1 1 calc R . . C3 C 1.2159(2) 0.51799(18) 0.7952(2) 0.0334(8) Uani 1 1 d . . . H3A H 1.2550 0.4991 0.8387 0.050 Uiso 1 1 calc R . . H3B H 1.2263 0.5655 0.7942 0.050 Uiso 1 1 calc R . . H3C H 1.2292 0.4976 0.7523 0.050 Uiso 1 1 calc R . . C4 C 1.0276(2) 0.54904(16) 0.71709(19) 0.0296(7) Uani 1 1 d . . . H4A H 1.0429 0.5338 0.6727 0.044 Uiso 1 1 calc R . . H4B H 1.0410 0.5961 0.7236 0.044 Uiso 1 1 calc R . . H4C H 0.9636 0.5417 0.7137 0.044 Uiso 1 1 calc R . . C5 C 0.8956(2) 0.39412(19) 0.63206(18) 0.0301(8) Uani 1 1 d . . . H5A H 0.9099 0.4412 0.6418 0.036 Uiso 1 1 calc R . . H5B H 0.9316 0.3805 0.5978 0.036 Uiso 1 1 calc R . . C6 C 0.7020(2) 0.3421(2) 0.6078(2) 0.0393(9) Uani 1 1 d . . . H6A H 0.7196 0.2961 0.6042 0.059 Uiso 1 1 calc R . . H6B H 0.6413 0.3489 0.5780 0.059 Uiso 1 1 calc R . . H6C H 0.7033 0.3526 0.6582 0.059 Uiso 1 1 calc R . . C7 C 0.7792(4) 0.3768(4) 0.4799(2) 0.091(2) Uani 1 1 d . . . H7A H 0.8144 0.4095 0.4607 0.136 Uiso 1 1 calc R . . H7B H 0.7170 0.3775 0.4515 0.136 Uiso 1 1 calc R . . H7C H 0.8048 0.3330 0.4773 0.136 Uiso 1 1 calc R . . C8 C 0.7340(4) 0.4819(2) 0.5754(4) 0.082(2) Uani 1 1 d . . . H8A H 0.7243 0.4918 0.6233 0.123 Uiso 1 1 calc R . . H8B H 0.6767 0.4845 0.5394 0.123 Uiso 1 1 calc R . . H8C H 0.7761 0.5139 0.5634 0.123 Uiso 1 1 calc R . . C9 C 0.8369(2) 0.40104(16) 0.84178(17) 0.0249(7) Uani 1 1 d . . . C10 C 0.8345(2) 0.46047(16) 0.79427(18) 0.0269(7) Uani 1 1 d . . . H10A H 0.8951 0.4698 0.7885 0.040 Uiso 1 1 calc R . . H10B H 0.8122 0.4984 0.8165 0.040 Uiso 1 1 calc R . . H10C H 0.7947 0.4519 0.7469 0.040 Uiso 1 1 calc R . . C11 C 0.9028(3) 0.41135(19) 0.91427(18) 0.0390(9) Uani 1 1 d . . . H11A H 0.9013 0.3731 0.9453 0.059 Uiso 1 1 calc R . . H11B H 0.8860 0.4509 0.9374 0.059 Uiso 1 1 calc R . . H11C H 0.9634 0.4167 0.9068 0.059 Uiso 1 1 calc R . . C12 C 0.7439(3) 0.3843(2) 0.8509(2) 0.0433(10) Uani 1 1 d . . . H12A H 0.7050 0.3732 0.8039 0.065 Uiso 1 1 calc R . . H12B H 0.7190 0.4223 0.8712 0.065 Uiso 1 1 calc R . . H12C H 0.7476 0.3467 0.8836 0.065 Uiso 1 1 calc R . . C13 C 0.6810(2) 0.20576(18) 0.77517(18) 0.0273(7) Uani 1 1 d . . . C14 C 0.6393(3) 0.2269(2) 0.8362(2) 0.0453(10) Uani 1 1 d . . . H14A H 0.6854 0.2274 0.8816 0.068 Uiso 1 1 calc R . . H14B H 0.5917 0.1960 0.8402 0.068 Uiso 1 1 calc R . . H14C H 0.6139 0.2711 0.8263 0.068 Uiso 1 1 calc R . . C15 C 0.6108(2) 0.2096(2) 0.7042(2) 0.0386(9) Uani 1 1 d . . . H15A H 0.5879 0.2547 0.6967 0.058 Uiso 1 1 calc R . . H15B H 0.5612 0.1797 0.7058 0.058 Uiso 1 1 calc R . . H15C H 0.6379 0.1970 0.6645 0.058 Uiso 1 1 calc R . . C16 C 0.7214(3) 0.13813(19) 0.7875(3) 0.0514(12) Uani 1 1 d . . . H16A H 0.7504 0.1272 0.7483 0.077 Uiso 1 1 calc R . . H16B H 0.6741 0.1060 0.7885 0.077 Uiso 1 1 calc R . . H16C H 0.7660 0.1372 0.8337 0.077 Uiso 1 1 calc R . . C17 C 0.9530(2) 0.21510(17) 0.93985(17) 0.0258(7) Uani 1 1 d . . . C18 C 0.9377(2) 0.2356(2) 1.01266(18) 0.0360(9) Uani 1 1 d . . . H18A H 0.9373 0.2837 1.0157 0.054 Uiso 1 1 calc R . . H18B H 0.9860 0.2181 1.0512 0.054 Uiso 1 1 calc R . . H18C H 0.8800 0.2183 1.0180 0.054 Uiso 1 1 calc R . . C19 C 0.9573(3) 0.14087(18) 0.9349(2) 0.0363(9) Uani 1 1 d . . . H19A H 0.9019 0.1217 0.9431 0.055 Uiso 1 1 calc R . . H19B H 1.0087 0.1245 0.9716 0.055 Uiso 1 1 calc R . . H19C H 0.9642 0.1283 0.8869 0.055 Uiso 1 1 calc R . . C20 C 1.0372(2) 0.24675(18) 0.92639(18) 0.0296(7) Uani 1 1 d . . . H20A H 1.0468 0.2315 0.8800 0.044 Uiso 1 1 calc R . . H20B H 1.0888 0.2345 0.9652 0.044 Uiso 1 1 calc R . . H20C H 1.0303 0.2947 0.9253 0.044 Uiso 1 1 calc R . . C21 C 0.8451(2) 0.1576(2) 0.6191(2) 0.0420(10) Uani 1 1 d . . . H21A H 0.8270 0.1279 0.6543 0.050 Uiso 1 1 calc R . . H21B H 0.8105 0.1983 0.6216 0.050 Uiso 1 1 calc R . . C22 C 0.7665(3) 0.1794(5) 0.4592(3) 0.136(4) Uani 1 1 d . . . H22A H 0.8215 0.1767 0.4415 0.203 Uiso 1 1 calc R . . H22B H 0.7584 0.2245 0.4744 0.203 Uiso 1 1 calc R . . H22C H 0.7150 0.1667 0.4204 0.203 Uiso 1 1 calc R . . C23 C 0.8175(3) 0.0430(3) 0.5135(5) 0.145(4) Uani 1 1 d . . . H23A H 0.8712 0.0497 0.4949 0.217 Uiso 1 1 calc R . . H23B H 0.7711 0.0212 0.4766 0.217 Uiso 1 1 calc R . . H23C H 0.8326 0.0154 0.5568 0.217 Uiso 1 1 calc R . . C24 C 0.6565(2) 0.10861(19) 0.5427(2) 0.0356(8) Uani 1 1 d . . . H24A H 0.6563 0.0809 0.5847 0.053 Uiso 1 1 calc R . . H24B H 0.6235 0.0864 0.4988 0.053 Uiso 1 1 calc R . . H24C H 0.6278 0.1508 0.5478 0.053 Uiso 1 1 calc R . . C25 C 1.0456(2) 0.10763(16) 0.75243(19) 0.0279(7) Uani 1 1 d . . . H25A H 1.1034 0.1043 0.7380 0.034 Uiso 1 1 calc R . . H25B H 1.0607 0.1259 0.8020 0.034 Uiso 1 1 calc R . . C26 C 0.9003(3) 0.0128(2) 0.7805(3) 0.0486(11) Uani 1 1 d . . . H26A H 0.8954 0.0394 0.8223 0.073 Uiso 1 1 calc R . . H26B H 0.8888 -0.0335 0.7897 0.073 Uiso 1 1 calc R . . H26C H 0.8562 0.0279 0.7376 0.073 Uiso 1 1 calc R . . C27 C 1.0928(3) -0.0168(2) 0.8456(2) 0.0485(11) Uani 1 1 d . . . H27A H 1.1546 -0.0144 0.8400 0.073 Uiso 1 1 calc R . . H27B H 1.0762 -0.0630 0.8496 0.073 Uiso 1 1 calc R . . H27C H 1.0883 0.0069 0.8893 0.073 Uiso 1 1 calc R . . C28 C 1.0181(3) -0.03178(18) 0.6855(2) 0.0390(9) Uani 1 1 d . . . H28A H 0.9994 -0.0765 0.6943 0.059 Uiso 1 1 calc R . . H28B H 1.0793 -0.0328 0.6782 0.059 Uiso 1 1 calc R . . H28C H 0.9772 -0.0138 0.6424 0.059 Uiso 1 1 calc R . . C29 C 1.0853(2) 0.15820(18) 0.54872(19) 0.0320(8) Uani 1 1 d . . . C30 C 1.1836(2) 0.1615(2) 0.5471(2) 0.0385(9) Uani 1 1 d . . . H30A H 1.1997 0.2070 0.5389 0.058 Uiso 1 1 calc R . . H30B H 1.1942 0.1336 0.5080 0.058 Uiso 1 1 calc R . . H30C H 1.2205 0.1460 0.5933 0.058 Uiso 1 1 calc R . . C31 C 1.0595(3) 0.08892(19) 0.5647(2) 0.0458(11) Uani 1 1 d . . . H31A H 1.0999 0.0734 0.6094 0.069 Uiso 1 1 calc R . . H31B H 1.0643 0.0599 0.5248 0.069 Uiso 1 1 calc R . . H31C H 0.9976 0.0886 0.5704 0.069 Uiso 1 1 calc R . . C32 C 1.0260(3) 0.1855(2) 0.4807(2) 0.0467(11) Uani 1 1 d . . . H32A H 0.9635 0.1854 0.4848 0.070 Uiso 1 1 calc R . . H32B H 1.0314 0.1582 0.4395 0.070 Uiso 1 1 calc R . . H32C H 1.0444 0.2306 0.4733 0.070 Uiso 1 1 calc R . . C33 C 1.1286(2) 0.37958(17) 0.54774(18) 0.0276(7) Uani 1 1 d . . . C34 C 1.2170(2) 0.3620(2) 0.5295(2) 0.0353(8) Uani 1 1 d . . . H34A H 1.2577 0.3428 0.5720 0.053 Uiso 1 1 calc R . . H34B H 1.2442 0.4018 0.5149 0.053 Uiso 1 1 calc R . . H34C H 1.2061 0.3301 0.4899 0.053 Uiso 1 1 calc R . . C35 C 1.0612(3) 0.4066(2) 0.4815(2) 0.0413(10) Uani 1 1 d . . . H35A H 1.0510 0.3737 0.4428 0.062 Uiso 1 1 calc R . . H35B H 1.0852 0.4468 0.4650 0.062 Uiso 1 1 calc R . . H35C H 1.0044 0.4164 0.4944 0.062 Uiso 1 1 calc R . . C36 C 1.1426(2) 0.42733(17) 0.6100(2) 0.0316(8) Uani 1 1 d . . . H36A H 1.0852 0.4357 0.6225 0.047 Uiso 1 1 calc R . . H36B H 1.1667 0.4687 0.5961 0.047 Uiso 1 1 calc R . . H36C H 1.1850 0.4086 0.6518 0.047 Uiso 1 1 calc R . . C37 C 1.2818(2) 0.26379(16) 0.73643(17) 0.0237(7) Uani 1 1 d . . . C38 C 1.2438(3) 0.2211(2) 0.7865(2) 0.0457(11) Uani 1 1 d . . . H38A H 1.1957 0.2449 0.8016 0.069 Uiso 1 1 calc R . . H38B H 1.2912 0.2101 0.8290 0.069 Uiso 1 1 calc R . . H38C H 1.2196 0.1807 0.7614 0.069 Uiso 1 1 calc R . . C39 C 1.3131(2) 0.32934(18) 0.7696(2) 0.0362(9) Uani 1 1 d . . . H39A H 1.3339 0.3565 0.7343 0.054 Uiso 1 1 calc R . . H39B H 1.3625 0.3227 0.8121 0.054 Uiso 1 1 calc R . . H39C H 1.2633 0.3516 0.7840 0.054 Uiso 1 1 calc R . . C40 C 1.3590(3) 0.2296(2) 0.7132(2) 0.0471(11) Uani 1 1 d . . . H40A H 1.3386 0.1870 0.6915 0.071 Uiso 1 1 calc R . . H40B H 1.4088 0.2229 0.7554 0.071 Uiso 1 1 calc R . . H40C H 1.3791 0.2570 0.6778 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sc1 0.0132(3) 0.0180(3) 0.0157(3) 0.0000(2) 0.0031(2) 0.0007(2) Sc2 0.0174(3) 0.0203(3) 0.0218(3) -0.0050(2) 0.0039(2) -0.0036(2) Si1 0.0183(4) 0.0200(4) 0.0239(4) -0.0020(3) 0.0018(3) 0.0007(3) Si2 0.0244(5) 0.0332(5) 0.0207(4) 0.0061(4) -0.0014(4) -0.0031(4) Si3 0.0131(4) 0.0244(4) 0.0145(4) 0.0004(3) 0.0015(3) -0.0022(3) Si4 0.0226(4) 0.0336(5) 0.0248(5) -0.0079(4) -0.0031(4) 0.0024(4) Si5 0.0195(4) 0.0240(5) 0.0421(6) 0.0005(4) 0.0007(4) -0.0011(4) Si6 0.0157(4) 0.0217(4) 0.0192(4) -0.0028(3) 0.0052(3) -0.0011(3) O1 0.0189(10) 0.0248(11) 0.0179(10) -0.0029(9) 0.0067(8) 0.0000(9) O2 0.0143(9) 0.0224(10) 0.0171(10) -0.0004(8) 0.0026(8) -0.0022(8) O3 0.0126(10) 0.0321(12) 0.0197(11) 0.0025(9) -0.0003(8) -0.0054(9) O4 0.0174(10) 0.0362(13) 0.0171(10) 0.0053(9) 0.0006(8) -0.0031(9) O5 0.0221(11) 0.0269(12) 0.0243(11) -0.0086(9) 0.0077(9) -0.0040(9) O6 0.0177(10) 0.0195(10) 0.0211(11) -0.0030(8) 0.0058(8) -0.0027(8) O7 0.0209(11) 0.0322(12) 0.0213(11) 0.0032(9) 0.0035(9) -0.0019(9) O8 0.0169(10) 0.0278(12) 0.0206(11) -0.0004(9) 0.0035(8) -0.0011(9) C1 0.0199(15) 0.0192(15) 0.0234(15) 0.0007(12) 0.0022(12) 0.0012(12) C2 0.038(2) 0.0288(18) 0.0301(19) -0.0064(14) 0.0055(15) 0.0011(15) C3 0.0251(17) 0.0301(18) 0.045(2) -0.0033(16) 0.0077(15) -0.0063(14) C4 0.0304(18) 0.0226(16) 0.0334(18) 0.0029(14) 0.0030(14) 0.0052(14) C5 0.0207(16) 0.044(2) 0.0236(17) 0.0083(15) 0.0020(13) 0.0001(14) C6 0.0313(19) 0.046(2) 0.034(2) 0.0129(17) -0.0061(15) -0.0137(17) C7 0.079(4) 0.161(7) 0.029(2) -0.016(3) 0.006(2) -0.054(4) C8 0.054(3) 0.054(3) 0.148(6) 0.048(4) 0.041(4) 0.025(2) C9 0.0293(17) 0.0255(16) 0.0223(16) -0.0022(13) 0.0108(13) 0.0056(13) C10 0.0239(16) 0.0285(17) 0.0279(17) -0.0021(14) 0.0054(13) 0.0075(13) C11 0.061(3) 0.033(2) 0.0206(17) -0.0051(15) 0.0031(17) 0.0142(18) C12 0.043(2) 0.039(2) 0.060(3) -0.0025(19) 0.036(2) 0.0034(18) C13 0.0167(15) 0.0385(19) 0.0262(17) 0.0019(14) 0.0038(13) -0.0074(13) C14 0.039(2) 0.069(3) 0.032(2) -0.0001(19) 0.0167(17) -0.022(2) C15 0.0221(17) 0.061(3) 0.0300(19) 0.0037(18) 0.0014(14) -0.0173(17) C16 0.0232(19) 0.035(2) 0.092(4) 0.012(2) 0.004(2) -0.0086(16) C17 0.0218(15) 0.0305(17) 0.0212(15) 0.0060(13) -0.0028(12) -0.0028(13) C18 0.0346(19) 0.050(2) 0.0209(17) 0.0060(16) 0.0006(14) -0.0045(17) C19 0.037(2) 0.034(2) 0.033(2) 0.0042(16) -0.0022(16) -0.0044(16) C20 0.0208(16) 0.0381(19) 0.0267(17) 0.0024(15) -0.0010(13) -0.0021(14) C21 0.0268(18) 0.062(3) 0.034(2) -0.0200(19) 0.0014(15) -0.0073(18) C22 0.035(3) 0.300(11) 0.064(4) 0.100(6) -0.004(3) -0.029(5) C23 0.033(3) 0.101(5) 0.271(10) -0.138(6) -0.023(4) 0.012(3) C24 0.0295(18) 0.039(2) 0.033(2) 0.0032(16) -0.0022(15) -0.0063(16) C25 0.0220(16) 0.0236(16) 0.0366(19) -0.0029(14) 0.0038(14) -0.0031(13) C26 0.034(2) 0.033(2) 0.081(3) -0.007(2) 0.017(2) -0.0097(17) C27 0.045(2) 0.044(2) 0.049(3) 0.013(2) -0.004(2) 0.0011(19) C28 0.040(2) 0.0233(18) 0.049(2) 0.0005(16) 0.0018(18) 0.0005(15) C29 0.0290(18) 0.039(2) 0.0313(18) -0.0216(16) 0.0137(15) -0.0071(15) C30 0.0327(19) 0.043(2) 0.045(2) -0.0197(18) 0.0195(17) -0.0031(17) C31 0.049(2) 0.036(2) 0.061(3) -0.029(2) 0.030(2) -0.0142(18) C32 0.037(2) 0.073(3) 0.029(2) -0.022(2) 0.0059(16) -0.005(2) C33 0.0238(16) 0.0332(18) 0.0272(17) 0.0093(14) 0.0090(13) 0.0010(14) C34 0.0288(18) 0.048(2) 0.033(2) 0.0104(17) 0.0152(15) 0.0028(16) C35 0.033(2) 0.056(3) 0.035(2) 0.0204(18) 0.0076(16) 0.0082(18) C36 0.0305(18) 0.0281(18) 0.038(2) 0.0025(15) 0.0106(15) -0.0002(14) C37 0.0174(14) 0.0268(16) 0.0244(16) 0.0000(13) 0.0000(12) -0.0012(12) C38 0.041(2) 0.059(3) 0.0289(19) 0.0172(19) -0.0072(16) -0.018(2) C39 0.0330(19) 0.0275(18) 0.041(2) -0.0047(16) -0.0058(16) -0.0029(15) C40 0.033(2) 0.057(3) 0.046(2) -0.005(2) -0.0007(18) 0.0216(19) _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 Sc1 O6 2.063(2) . ? Sc1 C5 2.192(3) . ? Sc1 O1 2.207(2) . ? Sc1 O2 2.213(2) . ? Sc1 C1 2.225(3) . ? Sc1 Si3 2.9651(10) . ? Sc1 Sc2 3.3347(9) . ? Sc2 O2 2.091(2) . ? Sc2 O6 2.170(2) . ? Sc2 C21 2.190(3) . ? Sc2 C25 2.217(3) . ? Sc2 O5 2.289(2) . ? Sc2 Si6 2.9919(11) . ? Si1 C1 1.857(3) . ? Si1 C2 1.874(3) . ? Si1 C4 1.876(3) . ? Si1 C3 1.879(3) . ? Si2 C5 1.825(3) . ? Si2 C7 1.855(5) . ? Si2 C6 1.862(4) . ? Si2 C8 1.882(5) . ? Si3 O3 1.600(2) . ? Si3 O4 1.605(2) . ? Si3 O2 1.619(2) . ? Si3 O1 1.681(2) . ? Si4 C21 1.824(4) . ? Si4 C22 1.844(6) . ? Si4 C23 1.846(5) . ? Si4 C24 1.876(4) . ? Si5 C25 1.848(3) . ? Si5 C26 1.862(4) . ? Si5 C28 1.872(4) . ? Si5 C27 1.874(4) . ? Si6 O8 1.596(2) . ? Si6 O7 1.605(2) . ? Si6 O6 1.615(2) . ? Si6 O5 1.670(2) . ? O1 C9 1.479(4) . ? O3 C13 1.447(4) . ? O4 C17 1.455(4) . ? O5 C29 1.486(4) . ? O7 C33 1.456(4) . ? O8 C37 1.447(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.506(5) . ? C9 C12 1.515(5) . ? C9 C11 1.522(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.504(5) . ? C13 C14 1.516(5) . ? C13 C15 1.520(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.515(5) . ? C17 C20 1.517(5) . ? C17 C18 1.520(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.504(6) . ? C29 C31 1.514(5) . ? C29 C30 1.518(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.509(5) . ? C33 C34 1.519(5) . ? C33 C35 1.533(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.505(5) . ? C37 C39 1.505(5) . ? C37 C40 1.525(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Sc1 C5 98.82(12) . . ? O6 Sc1 O1 140.25(8) . . ? C5 Sc1 O1 106.61(11) . . ? O6 Sc1 O2 74.69(8) . . ? C5 Sc1 O2 117.86(11) . . ? O1 Sc1 O2 66.57(8) . . ? O6 Sc1 C1 98.86(10) . . ? C5 Sc1 C1 109.96(13) . . ? O1 Sc1 C1 100.46(10) . . ? O2 Sc1 C1 132.18(10) . . ? O6 Sc1 Si3 106.93(6) . . ? C5 Sc1 Si3 115.99(9) . . ? O1 Sc1 Si3 34.10(6) . . ? O2 Sc1 Si3 32.50(5) . . ? C1 Sc1 Si3 121.90(9) . . ? O6 Sc1 Sc2 39.16(6) . . ? C5 Sc1 Sc2 103.28(10) . . ? O1 Sc1 Sc2 104.16(6) . . ? O2 Sc1 Sc2 37.90(5) . . ? C1 Sc1 Sc2 130.35(8) . . ? Si3 Sc1 Sc2 70.12(2) . . ? O2 Sc2 O6 75.09(8) . . ? O2 Sc2 C21 95.30(12) . . ? O6 Sc2 C21 131.20(14) . . ? O2 Sc2 C25 105.40(11) . . ? O6 Sc2 C25 117.18(10) . . ? C21 Sc2 C25 111.54(15) . . ? O2 Sc2 O5 140.06(8) . . ? O6 Sc2 O5 65.26(8) . . ? C21 Sc2 O5 106.89(12) . . ? C25 Sc2 O5 96.88(11) . . ? O2 Sc2 Si6 106.72(6) . . ? O6 Sc2 Si6 31.65(6) . . ? C21 Sc2 Si6 125.90(12) . . ? C25 Sc2 Si6 109.11(9) . . ? O5 Sc2 Si6 33.65(6) . . ? O2 Sc2 Sc1 40.56(6) . . ? O6 Sc2 Sc1 36.91(5) . . ? C21 Sc2 Sc1 110.31(12) . . ? C25 Sc2 Sc1 127.57(9) . . ? O5 Sc2 Sc1 99.81(6) . . ? Si6 Sc2 Sc1 67.42(2) . . ? C1 Si1 C2 112.07(16) . . ? C1 Si1 C4 114.50(15) . . ? C2 Si1 C4 106.17(16) . . ? C1 Si1 C3 110.64(15) . . ? C2 Si1 C3 107.50(17) . . ? C4 Si1 C3 105.48(17) . . ? C5 Si2 C7 111.8(2) . . ? C5 Si2 C6 113.40(16) . . ? C7 Si2 C6 109.4(2) . . ? C5 Si2 C8 110.1(2) . . ? C7 Si2 C8 106.4(3) . . ? C6 Si2 C8 105.3(2) . . ? O3 Si3 O4 109.07(11) . . ? O3 Si3 O2 114.70(11) . . ? O4 Si3 O2 117.72(12) . . ? O3 Si3 O1 107.48(11) . . ? O4 Si3 O1 112.10(12) . . ? O2 Si3 O1 94.64(11) . . ? O3 Si3 Sc1 120.44(8) . . ? O4 Si3 Sc1 129.91(9) . . ? O2 Si3 Sc1 47.26(8) . . ? O1 Si3 Sc1 47.41(7) . . ? C21 Si4 C22 111.7(3) . . ? C21 Si4 C23 112.1(2) . . ? C22 Si4 C23 108.8(4) . . ? C21 Si4 C24 112.78(18) . . ? C22 Si4 C24 105.1(2) . . ? C23 Si4 C24 106.0(2) . . ? C25 Si5 C26 112.71(17) . . ? C25 Si5 C28 112.75(17) . . ? C26 Si5 C28 106.14(19) . . ? C25 Si5 C27 111.69(18) . . ? C26 Si5 C27 106.0(2) . . ? C28 Si5 C27 107.09(19) . . ? O8 Si6 O7 108.04(12) . . ? O8 Si6 O6 116.50(11) . . ? O7 Si6 O6 115.40(12) . . ? O8 Si6 O5 114.54(12) . . ? O7 Si6 O5 107.47(12) . . ? O6 Si6 O5 94.18(11) . . ? O8 Si6 Sc2 127.07(9) . . ? O7 Si6 Sc2 124.78(9) . . ? O6 Si6 Sc2 44.84(8) . . ? O5 Si6 Sc2 49.42(8) . . ? C9 O1 Si3 130.32(19) . . ? C9 O1 Sc1 131.17(18) . . ? Si3 O1 Sc1 98.49(10) . . ? Si3 O2 Sc2 156.26(13) . . ? Si3 O2 Sc1 100.24(10) . . ? Sc2 O2 Sc1 101.54(8) . . ? C13 O3 Si3 136.4(2) . . ? C17 O4 Si3 136.9(2) . . ? C29 O5 Si6 128.6(2) . . ? C29 O5 Sc2 133.69(19) . . ? Si6 O5 Sc2 96.93(10) . . ? Si6 O6 Sc1 146.34(13) . . ? Si6 O6 Sc2 103.51(10) . . ? Sc1 O6 Sc2 103.94(9) . . ? C33 O7 Si6 132.6(2) . . ? C37 O8 Si6 142.3(2) . . ? Si1 C1 Sc1 135.86(16) . . ? Si1 C1 H1A 103.2 . . ? Sc1 C1 H1A 103.2 . . ? Si1 C1 H1B 103.2 . . ? Sc1 C1 H1B 103.2 . . ? H1A C1 H1B 105.2 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 Sc1 137.21(19) . . ? Si2 C5 H5A 102.8 . . ? Sc1 C5 H5A 102.8 . . ? Si2 C5 H5B 102.8 . . ? Sc1 C5 H5B 102.8 . . ? H5A C5 H5B 105.0 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 C10 105.7(2) . . ? O1 C9 C12 109.9(3) . . ? C10 C9 C12 111.0(3) . . ? O1 C9 C11 107.7(3) . . ? C10 C9 C11 110.6(3) . . ? C12 C9 C11 111.6(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 C16 110.2(3) . . ? O3 C13 C14 108.6(3) . . ? C16 C13 C14 111.9(3) . . ? O3 C13 C15 105.2(3) . . ? C16 C13 C15 111.4(3) . . ? C14 C13 C15 109.3(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 C19 107.2(3) . . ? O4 C17 C20 110.8(3) . . ? C19 C17 C20 111.2(3) . . ? O4 C17 C18 106.0(3) . . ? C19 C17 C18 110.4(3) . . ? C20 C17 C18 111.0(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si4 C21 Sc2 151.8(2) . . ? Si4 C21 H21A 98.6 . . ? Sc2 C21 H21A 98.6 . . ? Si4 C21 H21B 98.6 . . ? Sc2 C21 H21B 98.6 . . ? H21A C21 H21B 103.8 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si5 C25 Sc2 133.14(17) . . ? Si5 C25 H25A 103.9 . . ? Sc2 C25 H25A 103.9 . . ? Si5 C25 H25B 103.9 . . ? Sc2 C25 H25B 103.9 . . ? H25A C25 H25B 105.4 . . ? Si5 C26 H26A 109.5 . . ? Si5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si5 C27 H27A 109.5 . . ? Si5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si5 C28 H28A 109.5 . . ? Si5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 C32 107.9(3) . . ? O5 C29 C31 104.7(3) . . ? C32 C29 C31 112.6(3) . . ? O5 C29 C30 109.1(3) . . ? C32 C29 C30 111.6(3) . . ? C31 C29 C30 110.6(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O7 C33 C36 109.8(3) . . ? O7 C33 C34 108.7(3) . . ? C36 C33 C34 111.2(3) . . ? O7 C33 C35 104.6(3) . . ? C36 C33 C35 111.2(3) . . ? C34 C33 C35 111.2(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O8 C37 C38 110.6(3) . . ? O8 C37 C39 107.4(3) . . ? C38 C37 C39 112.2(3) . . ? O8 C37 C40 105.6(3) . . ? C38 C37 C40 111.4(3) . . ? C39 C37 C40 109.4(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Sc1 Sc2 O2 153.74(13) . . . . ? C5 Sc1 Sc2 O2 -118.58(12) . . . . ? O1 Sc1 Sc2 O2 -7.33(10) . . . . ? C1 Sc1 Sc2 O2 110.06(14) . . . . ? Si3 Sc1 Sc2 O2 -5.41(8) . . . . ? C5 Sc1 Sc2 O6 87.68(13) . . . . ? O1 Sc1 Sc2 O6 -161.07(11) . . . . ? O2 Sc1 Sc2 O6 -153.74(13) . . . . ? C1 Sc1 Sc2 O6 -43.68(14) . . . . ? Si3 Sc1 Sc2 O6 -159.15(9) . . . . ? O6 Sc1 Sc2 C21 -132.58(15) . . . . ? C5 Sc1 Sc2 C21 -44.90(15) . . . . ? O1 Sc1 Sc2 C21 66.35(13) . . . . ? O2 Sc1 Sc2 C21 73.68(15) . . . . ? C1 Sc1 Sc2 C21 -176.26(16) . . . . ? Si3 Sc1 Sc2 C21 68.27(12) . . . . ? O6 Sc1 Sc2 C25 86.29(15) . . . . ? C5 Sc1 Sc2 C25 173.97(15) . . . . ? O1 Sc1 Sc2 C25 -74.78(13) . . . . ? O2 Sc1 Sc2 C25 -67.45(14) . . . . ? C1 Sc1 Sc2 C25 42.61(16) . . . . ? Si3 Sc1 Sc2 C25 -72.86(12) . . . . ? O6 Sc1 Sc2 O5 -20.35(11) . . . . ? C5 Sc1 Sc2 O5 67.33(11) . . . . ? O1 Sc1 Sc2 O5 178.58(8) . . . . ? O2 Sc1 Sc2 O5 -174.09(10) . . . . ? C1 Sc1 Sc2 O5 -64.03(13) . . . . ? Si3 Sc1 Sc2 O5 -179.51(6) . . . . ? O6 Sc1 Sc2 Si6 -11.03(9) . . . . ? C5 Sc1 Sc2 Si6 76.65(9) . . . . ? O1 Sc1 Sc2 Si6 -172.10(6) . . . . ? O2 Sc1 Sc2 Si6 -164.77(9) . . . . ? C1 Sc1 Sc2 Si6 -54.71(11) . . . . ? Si3 Sc1 Sc2 Si6 -170.18(3) . . . . ? O6 Sc1 Si3 O3 -104.11(12) . . . . ? C5 Sc1 Si3 O3 4.96(16) . . . . ? O1 Sc1 Si3 O3 86.16(14) . . . . ? O2 Sc1 Si3 O3 -96.71(14) . . . . ? C1 Sc1 Si3 O3 143.61(14) . . . . ? Sc2 Sc1 Si3 O3 -90.52(10) . . . . ? O6 Sc1 Si3 O4 85.63(14) . . . . ? C5 Sc1 Si3 O4 -165.30(16) . . . . ? O1 Sc1 Si3 O4 -84.10(15) . . . . ? O2 Sc1 Si3 O4 93.03(16) . . . . ? C1 Sc1 Si3 O4 -26.65(16) . . . . ? Sc2 Sc1 Si3 O4 99.22(12) . . . . ? O6 Sc1 Si3 O2 -7.40(11) . . . . ? C5 Sc1 Si3 O2 101.67(15) . . . . ? O1 Sc1 Si3 O2 -177.13(14) . . . . ? C1 Sc1 Si3 O2 -119.67(14) . . . . ? Sc2 Sc1 Si3 O2 6.19(10) . . . . ? O6 Sc1 Si3 O1 169.73(12) . . . . ? C5 Sc1 Si3 O1 -81.20(15) . . . . ? O2 Sc1 Si3 O1 177.13(14) . . . . ? C1 Sc1 Si3 O1 57.45(14) . . . . ? Sc2 Sc1 Si3 O1 -176.68(10) . . . . ? O2 Sc2 Si6 O8 94.27(12) . . . . ? O6 Sc2 Si6 O8 91.90(15) . . . . ? C21 Sc2 Si6 O8 -156.07(17) . . . . ? C25 Sc2 Si6 O8 -19.15(15) . . . . ? O5 Sc2 Si6 O8 -92.20(15) . . . . ? Sc1 Sc2 Si6 O8 104.55(11) . . . . ? O2 Sc2 Si6 O7 -90.05(13) . . . . ? O6 Sc2 Si6 O7 -92.42(15) . . . . ? C21 Sc2 Si6 O7 19.61(18) . . . . ? C25 Sc2 Si6 O7 156.53(14) . . . . ? O5 Sc2 Si6 O7 83.48(15) . . . . ? Sc1 Sc2 Si6 O7 -79.78(11) . . . . ? O2 Sc2 Si6 O6 2.37(12) . . . . ? C21 Sc2 Si6 O6 112.03(18) . . . . ? C25 Sc2 Si6 O6 -111.05(14) . . . . ? O5 Sc2 Si6 O6 175.90(15) . . . . ? Sc1 Sc2 Si6 O6 12.65(10) . . . . ? O2 Sc2 Si6 O5 -173.53(12) . . . . ? O6 Sc2 Si6 O5 -175.90(15) . . . . ? C21 Sc2 Si6 O5 -63.87(18) . . . . ? C25 Sc2 Si6 O5 73.05(14) . . . . ? Sc1 Sc2 Si6 O5 -163.25(11) . . . . ? O3 Si3 O1 C9 66.0(3) . . . . ? O4 Si3 O1 C9 -53.9(3) . . . . ? O2 Si3 O1 C9 -176.3(2) . . . . ? Sc1 Si3 O1 C9 -178.4(3) . . . . ? O3 Si3 O1 Sc1 -115.59(11) . . . . ? O4 Si3 O1 Sc1 124.57(11) . . . . ? O2 Si3 O1 Sc1 2.12(10) . . . . ? O6 Sc1 O1 C9 162.9(2) . . . . ? C5 Sc1 O1 C9 -69.6(3) . . . . ? O2 Sc1 O1 C9 176.7(2) . . . . ? C1 Sc1 O1 C9 45.1(2) . . . . ? Si3 Sc1 O1 C9 178.4(3) . . . . ? Sc2 Sc1 O1 C9 -178.4(2) . . . . ? O6 Sc1 O1 Si3 -15.47(17) . . . . ? C5 Sc1 O1 Si3 112.03(13) . . . . ? O2 Sc1 O1 Si3 -1.68(8) . . . . ? C1 Sc1 O1 Si3 -133.30(11) . . . . ? Sc2 Sc1 O1 Si3 3.22(10) . . . . ? O3 Si3 O2 Sc2 -46.8(3) . . . . ? O4 Si3 O2 Sc2 83.6(3) . . . . ? O1 Si3 O2 Sc2 -158.4(3) . . . . ? Sc1 Si3 O2 Sc2 -156.3(4) . . . . ? O3 Si3 O2 Sc1 109.53(12) . . . . ? O4 Si3 O2 Sc1 -120.09(12) . . . . ? O1 Si3 O2 Sc1 -2.12(10) . . . . ? O6 Sc2 O2 Si3 172.2(3) . . . . ? C21 Sc2 O2 Si3 40.9(3) . . . . ? C25 Sc2 O2 Si3 -73.2(3) . . . . ? O5 Sc2 O2 Si3 165.3(3) . . . . ? Si6 Sc2 O2 Si3 170.9(3) . . . . ? Sc1 Sc2 O2 Si3 156.2(4) . . . . ? O6 Sc2 O2 Sc1 15.96(8) . . . . ? C21 Sc2 O2 Sc1 -115.33(14) . . . . ? C25 Sc2 O2 Sc1 130.60(10) . . . . ? O5 Sc2 O2 Sc1 9.09(16) . . . . ? Si6 Sc2 O2 Sc1 14.67(8) . . . . ? O6 Sc1 O2 Si3 172.66(11) . . . . ? C5 Sc1 O2 Si3 -95.32(14) . . . . ? O1 Sc1 O2 Si3 1.75(9) . . . . ? C1 Sc1 O2 Si3 84.53(15) . . . . ? Sc2 Sc1 O2 Si3 -170.50(15) . . . . ? O6 Sc1 O2 Sc2 -16.84(8) . . . . ? C5 Sc1 O2 Sc2 75.17(13) . . . . ? O1 Sc1 O2 Sc2 172.25(10) . . . . ? C1 Sc1 O2 Sc2 -104.97(13) . . . . ? Si3 Sc1 O2 Sc2 170.50(15) . . . . ? O4 Si3 O3 C13 -28.3(3) . . . . ? O2 Si3 O3 C13 106.2(3) . . . . ? O1 Si3 O3 C13 -150.0(3) . . . . ? Sc1 Si3 O3 C13 159.6(3) . . . . ? O3 Si3 O4 C17 158.9(3) . . . . ? O2 Si3 O4 C17 26.0(3) . . . . ? O1 Si3 O4 C17 -82.2(3) . . . . ? Sc1 Si3 O4 C17 -30.0(4) . . . . ? O8 Si6 O5 C29 -70.2(3) . . . . ? O7 Si6 O5 C29 49.8(3) . . . . ? O6 Si6 O5 C29 168.1(3) . . . . ? Sc2 Si6 O5 C29 171.0(3) . . . . ? O8 Si6 O5 Sc2 118.78(11) . . . . ? O7 Si6 O5 Sc2 -121.19(11) . . . . ? O6 Si6 O5 Sc2 -2.90(11) . . . . ? O2 Sc2 O5 C29 -160.6(3) . . . . ? O6 Sc2 O5 C29 -167.9(3) . . . . ? C21 Sc2 O5 C29 -39.7(3) . . . . ? C25 Sc2 O5 C29 75.3(3) . . . . ? Si6 Sc2 O5 C29 -170.2(3) . . . . ? Sc1 Sc2 O5 C29 -154.6(3) . . . . ? O2 Sc2 O5 Si6 9.68(18) . . . . ? O6 Sc2 O5 Si6 2.37(9) . . . . ? C21 Sc2 O5 Si6 130.54(15) . . . . ? C25 Sc2 O5 Si6 -114.43(12) . . . . ? Sc1 Sc2 O5 Si6 15.67(10) . . . . ? O8 Si6 O6 Sc1 99.1(2) . . . . ? O7 Si6 O6 Sc1 -29.2(3) . . . . ? O5 Si6 O6 Sc1 -140.8(2) . . . . ? Sc2 Si6 O6 Sc1 -143.9(3) . . . . ? O8 Si6 O6 Sc2 -117.00(12) . . . . ? O7 Si6 O6 Sc2 114.71(12) . . . . ? O5 Si6 O6 Sc2 3.12(12) . . . . ? C5 Sc1 O6 Si6 43.6(2) . . . . ? O1 Sc1 O6 Si6 173.28(17) . . . . ? O2 Sc1 O6 Si6 160.2(2) . . . . ? C1 Sc1 O6 Si6 -68.4(2) . . . . ? Si3 Sc1 O6 Si6 164.3(2) . . . . ? Sc2 Sc1 O6 Si6 143.8(3) . . . . ? C5 Sc1 O6 Sc2 -100.24(12) . . . . ? O1 Sc1 O6 Sc2 29.47(16) . . . . ? O2 Sc1 O6 Sc2 16.37(8) . . . . ? C1 Sc1 O6 Sc2 147.81(10) . . . . ? Si3 Sc1 O6 Sc2 20.48(9) . . . . ? O2 Sc2 O6 Si6 -177.65(12) . . . . ? C21 Sc2 O6 Si6 -93.74(17) . . . . ? C25 Sc2 O6 Si6 82.43(15) . . . . ? O5 Sc2 O6 Si6 -2.50(9) . . . . ? Sc1 Sc2 O6 Si6 -160.33(16) . . . . ? O2 Sc2 O6 Sc1 -17.32(8) . . . . ? C21 Sc2 O6 Sc1 66.59(17) . . . . ? C25 Sc2 O6 Sc1 -117.24(13) . . . . ? O5 Sc2 O6 Sc1 157.83(11) . . . . ? Si6 Sc2 O6 Sc1 160.33(16) . . . . ? O8 Si6 O7 C33 -30.7(3) . . . . ? O6 Si6 O7 C33 101.7(3) . . . . ? O5 Si6 O7 C33 -154.8(3) . . . . ? Sc2 Si6 O7 C33 152.9(2) . . . . ? O7 Si6 O8 C37 160.9(3) . . . . ? O6 Si6 O8 C37 29.1(4) . . . . ? O5 Si6 O8 C37 -79.4(3) . . . . ? Sc2 Si6 O8 C37 -22.9(4) . . . . ? C2 Si1 C1 Sc1 106.5(2) . . . . ? C4 Si1 C1 Sc1 -14.5(3) . . . . ? C3 Si1 C1 Sc1 -133.5(2) . . . . ? O6 Sc1 C1 Si1 124.3(2) . . . . ? C5 Sc1 C1 Si1 21.5(3) . . . . ? O1 Sc1 C1 Si1 -90.6(2) . . . . ? O2 Sc1 C1 Si1 -158.38(18) . . . . ? Si3 Sc1 C1 Si1 -119.3(2) . . . . ? Sc2 Sc1 C1 Si1 150.48(17) . . . . ? C7 Si2 C5 Sc1 -127.5(4) . . . . ? C6 Si2 C5 Sc1 -3.3(4) . . . . ? C8 Si2 C5 Sc1 114.4(3) . . . . ? O6 Sc1 C5 Si2 111.7(3) . . . . ? O1 Sc1 C5 Si2 -37.5(3) . . . . ? O2 Sc1 C5 Si2 34.4(3) . . . . ? C1 Sc1 C5 Si2 -145.5(3) . . . . ? Si3 Sc1 C5 Si2 -2.1(3) . . . . ? Sc2 Sc1 C5 Si2 72.0(3) . . . . ? Si3 O1 C9 C10 -151.3(2) . . . . ? Sc1 O1 C9 C10 30.7(3) . . . . ? Si3 O1 C9 C12 -31.4(4) . . . . ? Sc1 O1 C9 C12 150.6(2) . . . . ? Si3 O1 C9 C11 90.3(3) . . . . ? Sc1 O1 C9 C11 -87.6(3) . . . . ? Si3 O3 C13 C16 -38.2(4) . . . . ? Si3 O3 C13 C14 84.7(4) . . . . ? Si3 O3 C13 C15 -158.4(3) . . . . ? Si3 O4 C17 C19 -97.9(3) . . . . ? Si3 O4 C17 C20 23.6(4) . . . . ? Si3 O4 C17 C18 144.2(3) . . . . ? C22 Si4 C21 Sc2 -68.3(6) . . . . ? C23 Si4 C21 Sc2 54.1(7) . . . . ? C24 Si4 C21 Sc2 173.6(5) . . . . ? O2 Sc2 C21 Si4 161.9(5) . . . . ? O6 Sc2 C21 Si4 87.1(6) . . . . ? C25 Sc2 C21 Si4 -89.3(6) . . . . ? O5 Sc2 C21 Si4 15.5(6) . . . . ? Si6 Sc2 C21 Si4 46.8(6) . . . . ? Sc1 Sc2 C21 Si4 123.0(5) . . . . ? C26 Si5 C25 Sc2 -47.2(3) . . . . ? C28 Si5 C25 Sc2 72.9(3) . . . . ? C27 Si5 C25 Sc2 -166.4(2) . . . . ? O2 Sc2 C25 Si5 99.6(2) . . . . ? O6 Sc2 C25 Si5 -179.5(2) . . . . ? C21 Sc2 C25 Si5 -2.6(3) . . . . ? O5 Sc2 C25 Si5 -113.9(2) . . . . ? Si6 Sc2 C25 Si5 -146.1(2) . . . . ? Sc1 Sc2 C25 Si5 138.1(2) . . . . ? Si6 O5 C29 C32 -76.7(3) . . . . ? Sc2 O5 C29 C32 90.9(4) . . . . ? Si6 O5 C29 C31 163.2(2) . . . . ? Sc2 O5 C29 C31 -29.2(4) . . . . ? Si6 O5 C29 C30 44.7(4) . . . . ? Sc2 O5 C29 C30 -147.7(3) . . . . ? Si6 O7 C33 C36 -47.6(4) . . . . ? Si6 O7 C33 C34 74.2(4) . . . . ? Si6 O7 C33 C35 -166.9(2) . . . . ? Si6 O8 C37 C38 16.3(5) . . . . ? Si6 O8 C37 C39 -106.4(4) . . . . ? Si6 O8 C37 C40 136.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.19 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.783 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.142 #===END data_be11 _database_code_depnum_ccdc_archive 'CCDC 282723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H81 Lu O12 Si3' _chemical_formula_weight 965.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0820 0.0700 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8580 '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 11.9494(7) _cell_length_b 13.9573(9) _cell_length_c 14.4939(9) _cell_angle_alpha 86.7120(10) _cell_angle_beta 76.0020(10) _cell_angle_gamma 88.5490(10) _cell_volume 2341.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6669 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 25.24 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 2.237 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3726 _exptl_absorpt_correction_T_max 0.4327 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23138 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.06 _reflns_number_total 10229 _reflns_number_gt 9181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _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^)+(0.0619P)^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 geom _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10229 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu Lu 0.085573(14) 0.122323(12) 0.293510(12) 0.01662(8) Uani 1 1 d . . . Si1 Si 0.24347(12) -0.10480(10) 0.18872(10) 0.0290(3) Uani 1 1 d . . . Si2 Si 0.08792(12) 0.28123(9) 0.49761(9) 0.0246(3) Uani 1 1 d . . . Si3 Si 0.22829(10) 0.29782(8) 0.11136(8) 0.0176(2) Uani 1 1 d . . . O1 O -0.0945(3) 0.2155(2) 0.3271(2) 0.0225(6) Uani 1 1 d . . . O2 O -0.0769(3) 0.0318(2) 0.3757(2) 0.0277(7) Uani 1 1 d . . . O3 O -0.0223(3) 0.0636(2) 0.1824(2) 0.0270(7) Uani 1 1 d . . . O4 O -0.1735(3) 0.2180(2) 0.1593(2) 0.0304(8) Uani 1 1 d . . . O5 O 0.5330(3) 1.1234(2) 0.4231(2) 0.0294(7) Uani 1 1 d . . . O6 O 0.5971(3) 0.9219(2) 0.3766(2) 0.0304(7) Uani 1 1 d . . . O7 O 0.3550(4) 0.5792(3) 0.6073(3) 0.0540(11) Uani 1 1 d . . . O8 O 0.4808(4) 0.5923(3) 0.4035(3) 0.0490(10) Uani 1 1 d . . . O9 O 0.1725(3) 0.2176(3) 0.1883(3) 0.0369(9) Uani 1 1 d . . . O10 O 0.3634(3) 0.3185(3) 0.1003(3) 0.0365(9) Uani 1 1 d . . . O11A O 0.1556(4) 0.3919(4) 0.1585(4) 0.0223(17) Uiso 0.594(13) 1 d P . . O11B O 0.1588(6) 0.3957(5) 0.1011(6) 0.022(3) Uiso 0.406(13) 1 d P . . O12A O 0.2002(5) 0.2943(4) 0.0066(4) 0.0268(17) Uiso 0.620(11) 1 d P . . O12B O 0.2294(6) 0.2378(6) 0.0188(5) 0.015(2) Uiso 0.380(11) 1 d P . . C1 C -0.2010(4) 0.1730(4) 0.3804(4) 0.0305(11) Uani 1 1 d . . . H1A H -0.2479 0.1541 0.3369 0.037 Uiso 1 1 calc R . . H1B H -0.2463 0.2190 0.4247 0.037 Uiso 1 1 calc R . . C2 C -0.1677(4) 0.0857(4) 0.4352(4) 0.0343(12) Uani 1 1 d . . . H2A H -0.1417 0.1064 0.4907 0.041 Uiso 1 1 calc R . . H2B H -0.2359 0.0444 0.4591 0.041 Uiso 1 1 calc R . . C3 C -0.1118(5) -0.0368(4) 0.3178(4) 0.0366(12) Uani 1 1 d . . . H3A H -0.1865 -0.0646 0.3526 0.044 Uiso 1 1 calc R . . H3B H -0.0540 -0.0896 0.3064 0.044 Uiso 1 1 calc R . . C4 C -0.1238(4) 0.0080(4) 0.2234(4) 0.0333(11) Uani 1 1 d . . . H4A H -0.1317 -0.0426 0.1803 0.040 Uiso 1 1 calc R . . H4B H -0.1933 0.0499 0.2328 0.040 Uiso 1 1 calc R . . C5 C -0.0233(4) 0.1082(4) 0.0905(3) 0.0305(11) Uani 1 1 d . . . H5A H -0.0759 0.0725 0.0620 0.037 Uiso 1 1 calc R . . H5B H 0.0551 0.1040 0.0482 0.037 Uiso 1 1 calc R . . C6 C -0.0613(4) 0.2122(4) 0.0953(4) 0.0347(12) Uani 1 1 d . . . H6A H -0.0056 0.2500 0.1185 0.042 Uiso 1 1 calc R . . H6B H -0.0643 0.2389 0.0312 0.042 Uiso 1 1 calc R . . C7 C -0.1896(5) 0.2996(4) 0.2119(4) 0.0365(12) Uani 1 1 d . . . H7A H -0.2705 0.3015 0.2497 0.044 Uiso 1 1 calc R . . H7B H -0.1777 0.3569 0.1673 0.044 Uiso 1 1 calc R . . C8 C -0.1101(4) 0.3060(3) 0.2794(3) 0.0252(10) Uani 1 1 d . . . H8A H -0.0340 0.3298 0.2428 0.030 Uiso 1 1 calc R . . H8B H -0.1429 0.3531 0.3276 0.030 Uiso 1 1 calc R . . C9 C 0.1975(4) -0.0214(3) 0.2834(3) 0.0253(10) Uani 1 1 d . . . H9A H 0.2702 -0.0024 0.2983 0.030 Uiso 1 1 calc R . . H9B H 0.1572 -0.0622 0.3390 0.030 Uiso 1 1 calc R . . C10 C 0.3425(6) -0.2033(5) 0.2141(5) 0.0571(19) Uani 1 1 d . . . H10A H 0.4148 -0.1758 0.2201 0.086 Uiso 1 1 calc R . . H10B H 0.3586 -0.2471 0.1618 0.086 Uiso 1 1 calc R . . H10C H 0.3059 -0.2388 0.2736 0.086 Uiso 1 1 calc R . . C11 C 0.1190(5) -0.1688(4) 0.1624(4) 0.0448(15) Uani 1 1 d . . . H11A H 0.0745 -0.2015 0.2209 0.067 Uiso 1 1 calc R . . H11B H 0.1483 -0.2161 0.1147 0.067 Uiso 1 1 calc R . . H11C H 0.0692 -0.1221 0.1379 0.067 Uiso 1 1 calc R . . C12 C 0.3167(8) -0.0414(5) 0.0744(5) 0.092(3) Uani 1 1 d . . . H12A H 0.2680 0.0123 0.0601 0.138 Uiso 1 1 calc R . . H12B H 0.3297 -0.0861 0.0230 0.138 Uiso 1 1 calc R . . H12C H 0.3909 -0.0169 0.0798 0.138 Uiso 1 1 calc R . . C13 C 0.1241(4) 0.1673(3) 0.4381(3) 0.0237(9) Uani 1 1 d . . . H13A H 0.0888 0.1168 0.4863 0.028 Uiso 1 1 calc R . . H13B H 0.2085 0.1593 0.4292 0.028 Uiso 1 1 calc R . . C14 C 0.1547(5) 0.2975(4) 0.6011(3) 0.0332(11) Uani 1 1 d . . . H14A H 0.1260 0.2480 0.6515 0.050 Uiso 1 1 calc R . . H14B H 0.1339 0.3611 0.6258 0.050 Uiso 1 1 calc R . . H14C H 0.2388 0.2917 0.5797 0.050 Uiso 1 1 calc R . . C15 C -0.0709(5) 0.2951(4) 0.5480(4) 0.0397(13) Uani 1 1 d . . . H15A H -0.1101 0.3024 0.4959 0.060 Uiso 1 1 calc R . . H15B H -0.0858 0.3520 0.5859 0.060 Uiso 1 1 calc R . . H15C H -0.0998 0.2381 0.5886 0.060 Uiso 1 1 calc R . . C16 C 0.1358(6) 0.3869(4) 0.4122(4) 0.0413(14) Uani 1 1 d . . . H16A H 0.2199 0.3919 0.3983 0.062 Uiso 1 1 calc R . . H16B H 0.1003 0.4457 0.4407 0.062 Uiso 1 1 calc R . . H16C H 0.1121 0.3784 0.3530 0.062 Uiso 1 1 calc R . . C17 C 0.4509(4) 0.2804(4) 0.1432(3) 0.0295(11) Uani 1 1 d . . . C18 C 0.4180(6) 0.2980(5) 0.2477(4) 0.0490(16) Uani 1 1 d . . . H18A H 0.4078 0.3671 0.2563 0.074 Uiso 1 1 calc R . . H18B H 0.4791 0.2732 0.2774 0.074 Uiso 1 1 calc R . . H18C H 0.3457 0.2652 0.2776 0.074 Uiso 1 1 calc R . . C19 C 0.5582(5) 0.3344(6) 0.0922(4) 0.0575(19) Uani 1 1 d . . . H19A H 0.5732 0.3257 0.0237 0.086 Uiso 1 1 calc R . . H19B H 0.6240 0.3097 0.1160 0.086 Uiso 1 1 calc R . . H19C H 0.5470 0.4028 0.1040 0.086 Uiso 1 1 calc R . . C20 C 0.4664(6) 0.1742(5) 0.1267(5) 0.0581(18) Uani 1 1 d . . . H20A H 0.3964 0.1402 0.1606 0.087 Uiso 1 1 calc R . . H20B H 0.5321 0.1492 0.1504 0.087 Uiso 1 1 calc R . . H20C H 0.4806 0.1645 0.0584 0.087 Uiso 1 1 calc R . . C21 C 0.1599(5) 0.4944(3) 0.1284(4) 0.0335(11) Uani 1 1 d . . . C22 C 0.0472(5) 0.5284(4) 0.1900(4) 0.0468(15) Uani 1 1 d . . . H22A H -0.0165 0.5090 0.1637 0.070 Uiso 1 1 calc R . . H22B H 0.0474 0.5984 0.1916 0.070 Uiso 1 1 calc R . . H22C H 0.0375 0.4997 0.2548 0.070 Uiso 1 1 calc R . . C23 C 0.2619(6) 0.5282(4) 0.1622(5) 0.0570(18) Uani 1 1 d . . . H23A H 0.2602 0.4984 0.2254 0.086 Uiso 1 1 calc R . . H23B H 0.2577 0.5982 0.1658 0.086 Uiso 1 1 calc R . . H23C H 0.3336 0.5101 0.1174 0.086 Uiso 1 1 calc R . . C24 C 0.1687(6) 0.5318(6) 0.0277(5) 0.068(2) Uani 1 1 d . . . H24A H 0.2441 0.5141 -0.0122 0.101 Uiso 1 1 calc R . . H24B H 0.1599 0.6018 0.0259 0.101 Uiso 1 1 calc R . . H24C H 0.1077 0.5037 0.0035 0.101 Uiso 1 1 calc R . . C25 C 0.2663(4) 0.2639(4) -0.0840(3) 0.0304(11) Uani 1 1 d . . . C26 C 0.3643(5) 0.3334(4) -0.1174(4) 0.0476(15) Uani 1 1 d . . . H26A H 0.3331 0.3987 -0.1211 0.071 Uiso 1 1 calc R . . H26B H 0.4095 0.3169 -0.1806 0.071 Uiso 1 1 calc R . . H26C H 0.4139 0.3297 -0.0725 0.071 Uiso 1 1 calc R . . C27 C 0.1745(7) 0.2805(7) -0.1361(6) 0.085(3) Uani 1 1 d . . . H27A H 0.1122 0.2347 -0.1113 0.128 Uiso 1 1 calc R . . H27B H 0.2066 0.2717 -0.2040 0.128 Uiso 1 1 calc R . . H27C H 0.1441 0.3461 -0.1275 0.128 Uiso 1 1 calc R . . C28 C 0.3116(7) 0.1638(5) -0.0973(8) 0.104(4) Uani 1 1 d . . . H28A H 0.3667 0.1501 -0.0578 0.157 Uiso 1 1 calc R . . H28B H 0.3504 0.1568 -0.1644 0.157 Uiso 1 1 calc R . . H28C H 0.2476 0.1187 -0.0784 0.157 Uiso 1 1 calc R . . C29 C 0.4681(4) 1.1891(4) 0.4874(4) 0.0318(11) Uani 1 1 d . . . H29A H 0.3873 1.1909 0.4815 0.038 Uiso 1 1 calc R . . H29B H 0.5001 1.2543 0.4702 0.038 Uiso 1 1 calc R . . C30 C 0.4644(4) 1.0581(3) 0.3889(3) 0.0253(10) Uani 1 1 d . . . H30A H 0.4147 1.0939 0.3529 0.030 Uiso 1 1 calc R . . H30B H 0.4141 1.0216 0.4432 0.030 Uiso 1 1 calc R . . C31 C 0.5422(4) 0.9908(3) 0.3259(3) 0.0279(10) Uani 1 1 d . . . H31A H 0.4967 0.9570 0.2893 0.033 Uiso 1 1 calc R . . H31B H 0.6020 1.0284 0.2797 0.033 Uiso 1 1 calc R . . C32 C 0.5299(5) 0.8381(4) 0.4108(4) 0.0334(11) Uani 1 1 d . . . H32A H 0.5611 0.7842 0.3703 0.040 Uiso 1 1 calc R . . H32B H 0.4493 0.8504 0.4065 0.040 Uiso 1 1 calc R . . C33 C 0.3703(6) 0.5085(5) 0.6785(4) 0.0562(18) Uani 1 1 d . . . H33A H 0.3223 0.4521 0.6774 0.067 Uiso 1 1 calc R . . H33B H 0.3456 0.5352 0.7422 0.067 Uiso 1 1 calc R . . C34 C 0.3186(6) 0.5408(6) 0.5334(4) 0.069(3) Uani 1 1 d . . . H34A H 0.2334 0.5372 0.5502 0.083 Uiso 1 1 calc R . . H34B H 0.3500 0.4747 0.5242 0.083 Uiso 1 1 calc R . . C35 C 0.3588(4) 0.6023(4) 0.4402(4) 0.0389(13) Uani 1 1 d . . . H35A H 0.3184 0.5821 0.3926 0.047 Uiso 1 1 calc R . . H35B H 0.3390 0.6705 0.4521 0.047 Uiso 1 1 calc R . . C36 C 0.4992(6) 0.5227(4) 0.3409(5) 0.0476(15) Uani 1 1 d . . . H36A H 0.4804 0.5468 0.2808 0.057 Uiso 1 1 calc R . . H36B H 0.4494 0.4672 0.3672 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu 0.01481(11) 0.01570(11) 0.01948(11) 0.00214(6) -0.00483(7) -0.00276(7) Si1 0.0295(7) 0.0233(7) 0.0324(7) -0.0097(5) -0.0020(6) -0.0009(5) Si2 0.0310(7) 0.0219(6) 0.0205(6) -0.0023(5) -0.0055(5) 0.0043(5) Si3 0.0174(6) 0.0181(6) 0.0176(5) 0.0019(4) -0.0053(4) -0.0037(5) O1 0.0149(15) 0.0261(17) 0.0256(15) 0.0014(13) -0.0037(12) 0.0000(12) O2 0.0221(17) 0.0225(16) 0.0352(18) 0.0039(13) -0.0013(14) -0.0050(13) O3 0.0225(17) 0.0290(18) 0.0324(17) -0.0035(14) -0.0116(14) -0.0036(14) O4 0.0189(17) 0.038(2) 0.0385(19) -0.0078(15) -0.0132(14) 0.0015(14) O5 0.0189(16) 0.0293(18) 0.0426(19) -0.0072(15) -0.0109(14) -0.0048(14) O6 0.0221(17) 0.0277(18) 0.043(2) -0.0020(15) -0.0109(15) -0.0007(14) O7 0.061(3) 0.044(3) 0.057(3) -0.007(2) -0.014(2) 0.003(2) O8 0.057(3) 0.040(2) 0.050(2) -0.0043(19) -0.012(2) -0.002(2) O9 0.0268(19) 0.044(2) 0.043(2) 0.0257(17) -0.0192(16) -0.0175(16) O10 0.0208(17) 0.035(2) 0.055(2) 0.0236(17) -0.0168(16) -0.0102(15) C1 0.019(2) 0.034(3) 0.034(3) -0.001(2) 0.001(2) -0.001(2) C2 0.024(3) 0.035(3) 0.036(3) 0.006(2) 0.007(2) -0.003(2) C3 0.030(3) 0.024(3) 0.054(3) 0.002(2) -0.007(2) -0.010(2) C4 0.020(2) 0.030(3) 0.054(3) -0.008(2) -0.014(2) -0.009(2) C5 0.028(3) 0.037(3) 0.030(2) -0.011(2) -0.013(2) 0.004(2) C6 0.030(3) 0.044(3) 0.030(3) 0.000(2) -0.009(2) 0.005(2) C7 0.033(3) 0.040(3) 0.039(3) 0.000(2) -0.015(2) 0.006(2) C8 0.025(2) 0.023(2) 0.028(2) -0.0030(18) -0.0074(19) 0.0021(19) C9 0.024(2) 0.024(2) 0.030(2) -0.0051(18) -0.0098(19) 0.0005(19) C10 0.044(4) 0.051(4) 0.087(5) -0.043(4) -0.032(4) 0.023(3) C11 0.049(4) 0.039(3) 0.056(4) -0.024(3) -0.029(3) 0.006(3) C12 0.128(8) 0.050(4) 0.062(5) -0.023(4) 0.055(5) -0.018(5) C13 0.022(2) 0.023(2) 0.027(2) -0.0031(18) -0.0074(18) 0.0047(18) C14 0.050(3) 0.026(3) 0.024(2) -0.0046(19) -0.011(2) 0.004(2) C15 0.034(3) 0.045(3) 0.039(3) -0.014(2) -0.005(2) 0.007(2) C16 0.072(4) 0.024(3) 0.030(3) 0.000(2) -0.015(3) -0.008(3) C17 0.018(2) 0.042(3) 0.030(2) 0.003(2) -0.0100(19) -0.001(2) C18 0.053(4) 0.062(4) 0.034(3) -0.006(3) -0.010(3) -0.027(3) C19 0.027(3) 0.101(6) 0.045(3) 0.021(3) -0.015(3) -0.021(3) C20 0.062(4) 0.049(4) 0.055(4) 0.001(3) -0.001(3) 0.024(3) C21 0.035(3) 0.017(2) 0.047(3) 0.001(2) -0.007(2) -0.002(2) C22 0.053(4) 0.033(3) 0.046(3) 0.005(2) 0.000(3) 0.007(3) C23 0.062(4) 0.035(3) 0.083(5) 0.014(3) -0.038(4) -0.013(3) C24 0.055(4) 0.108(7) 0.040(3) -0.013(4) -0.009(3) -0.011(4) C25 0.032(3) 0.043(3) 0.017(2) -0.0009(19) -0.0058(19) -0.002(2) C26 0.044(3) 0.038(3) 0.050(3) -0.007(3) 0.010(3) -0.006(3) C27 0.063(5) 0.120(7) 0.080(5) 0.053(5) -0.042(4) -0.020(5) C28 0.050(5) 0.037(4) 0.206(12) 0.006(5) 0.006(6) -0.005(3) C29 0.029(3) 0.027(3) 0.043(3) -0.003(2) -0.017(2) 0.001(2) C30 0.019(2) 0.027(2) 0.032(2) -0.0005(19) -0.0101(19) -0.0073(19) C31 0.023(2) 0.033(3) 0.029(2) -0.002(2) -0.0083(19) 0.000(2) C32 0.031(3) 0.029(3) 0.044(3) -0.006(2) -0.015(2) -0.005(2) C33 0.063(4) 0.054(4) 0.040(3) 0.010(3) 0.005(3) 0.018(3) C34 0.054(4) 0.119(6) 0.047(4) -0.052(4) -0.035(3) 0.065(4) C35 0.027(3) 0.025(3) 0.065(4) 0.001(2) -0.014(3) 0.001(2) C36 0.058(4) 0.033(3) 0.060(4) 0.005(3) -0.031(3) -0.016(3) _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 Lu O9 2.060(3) . ? Lu O2 2.370(3) . ? Lu C13 2.373(4) . ? Lu C9 2.374(4) . ? Lu O1 2.445(3) . ? Lu O3 2.477(3) . ? Si1 C9 1.824(5) . ? Si1 C12 1.862(7) . ? Si1 C10 1.870(6) . ? Si1 C11 1.881(6) . ? Si2 C13 1.844(4) . ? Si2 C15 1.870(6) . ? Si2 C16 1.878(5) . ? Si2 C14 1.888(5) . ? Si3 O9 1.574(3) . ? Si3 O11B 1.599(8) . ? Si3 O10 1.616(3) . ? Si3 O12B 1.618(7) . ? Si3 O12A 1.636(5) . ? Si3 O11A 1.645(5) . ? O1 C8 1.435(5) . ? O1 C1 1.442(5) . ? O2 C2 1.438(6) . ? O2 C3 1.440(6) . ? O3 C4 1.440(6) . ? O3 C5 1.441(6) . ? O4 C7 1.391(6) . ? O4 C6 1.438(6) . ? O5 C29 1.422(6) . ? O5 C30 1.427(5) . ? O6 C31 1.420(6) . ? O6 C32 1.430(6) . ? O7 C34 1.389(7) . ? O7 C33 1.427(7) . ? O8 C36 1.345(7) . ? O8 C35 1.431(7) . ? O10 C17 1.417(6) . ? O11A O11B 0.822(8) . ? O11A C21 1.470(7) . ? O11B C21 1.456(9) . ? O12A O12B 0.880(8) . ? O12A C25 1.439(7) . ? O12B C25 1.475(8) . ? C1 C2 1.512(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.510(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.527(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.503(7) . ? C17 C19 1.512(7) . ? C17 C20 1.515(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.502(8) . ? C21 C22 1.506(8) . ? C21 C23 1.514(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.482(8) . ? C25 C28 1.491(9) . ? C25 C26 1.508(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.508(7) 2_676 ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.492(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C29 1.508(7) 2_676 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C36 1.571(9) 2_666 ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.539(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C33 1.571(9) 2_666 ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Lu O2 154.19(13) . . ? O9 Lu C13 106.51(15) . . ? O2 Lu C13 92.01(14) . . ? O9 Lu C9 106.97(16) . . ? O2 Lu C9 88.50(14) . . ? C13 Lu C9 95.48(15) . . ? O9 Lu O1 95.11(12) . . ? O2 Lu O1 66.37(11) . . ? C13 Lu O1 90.34(13) . . ? C9 Lu O1 154.41(14) . . ? O9 Lu O3 90.19(12) . . ? O2 Lu O3 68.56(11) . . ? C13 Lu O3 159.42(14) . . ? C9 Lu O3 90.88(13) . . ? O1 Lu O3 75.97(10) . . ? C9 Si1 C12 111.4(3) . . ? C9 Si1 C10 114.8(3) . . ? C12 Si1 C10 107.4(4) . . ? C9 Si1 C11 112.6(2) . . ? C12 Si1 C11 105.4(4) . . ? C10 Si1 C11 104.4(3) . . ? C13 Si2 C15 111.8(2) . . ? C13 Si2 C16 111.1(2) . . ? C15 Si2 C16 107.5(3) . . ? C13 Si2 C14 115.5(2) . . ? C15 Si2 C14 104.8(2) . . ? C16 Si2 C14 105.6(2) . . ? O9 Si3 O11B 119.7(3) . . ? O9 Si3 O10 116.62(18) . . ? O11B Si3 O10 110.7(3) . . ? O9 Si3 O12B 96.8(3) . . ? O11B Si3 O12B 107.2(4) . . ? O10 Si3 O12B 102.8(3) . . ? O9 Si3 O12A 116.7(2) . . ? O11B Si3 O12A 76.2(4) . . ? O10 Si3 O12A 110.4(2) . . ? O12B Si3 O12A 31.4(3) . . ? O9 Si3 O11A 99.6(3) . . ? O11B Si3 O11A 29.3(3) . . ? O10 Si3 O11A 107.2(2) . . ? O12B Si3 O11A 134.3(4) . . ? O12A Si3 O11A 104.5(3) . . ? C8 O1 C1 113.5(3) . . ? C8 O1 Lu 123.9(3) . . ? C1 O1 Lu 121.1(3) . . ? C2 O2 C3 116.5(4) . . ? C2 O2 Lu 115.2(3) . . ? C3 O2 Lu 113.3(3) . . ? C4 O3 C5 113.0(4) . . ? C4 O3 Lu 117.1(3) . . ? C5 O3 Lu 125.2(3) . . ? C7 O4 C6 113.3(4) . . ? C29 O5 C30 114.1(4) . . ? C31 O6 C32 113.9(4) . . ? C34 O7 C33 113.0(6) . . ? C36 O8 C35 107.9(5) . . ? Si3 O9 Lu 174.1(3) . . ? C17 O10 Si3 135.6(3) . . ? O11B O11A C21 72.7(7) . . ? O11B O11A Si3 72.3(7) . . ? C21 O11A Si3 132.4(4) . . ? O11A O11B C21 74.6(7) . . ? O11A O11B Si3 78.4(7) . . ? C21 O11B Si3 137.8(6) . . ? O12B O12A C25 74.6(6) . . ? O12B O12A Si3 73.2(6) . . ? C25 O12A Si3 133.1(4) . . ? O12A O12B C25 70.2(6) . . ? O12A O12B Si3 75.4(6) . . ? C25 O12B Si3 131.7(6) . . ? O1 C1 C2 106.3(4) . . ? O1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? O1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? O2 C2 C1 110.9(4) . . ? O2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? O2 C3 C4 112.1(4) . . ? O2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? O2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 108.2(4) . . ? O3 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O3 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? O3 C5 C6 112.9(4) . . ? O3 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? O3 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? O4 C6 C5 108.7(4) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? O4 C7 C8 114.8(4) . . ? O4 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? O4 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? O1 C8 C7 112.7(4) . . ? O1 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? O1 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? Si1 C9 Lu 132.2(2) . . ? Si1 C9 H9A 104.2 . . ? Lu C9 H9A 104.2 . . ? Si1 C9 H9B 104.2 . . ? Lu C9 H9B 104.2 . . ? H9A C9 H9B 105.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 Lu 128.4(2) . . ? Si2 C13 H13A 105.2 . . ? Lu C13 H13A 105.2 . . ? Si2 C13 H13B 105.2 . . ? Lu C13 H13B 105.2 . . ? H13A C13 H13B 105.9 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O10 C17 C18 109.2(5) . . ? O10 C17 C19 104.6(4) . . ? C18 C17 C19 111.8(5) . . ? O10 C17 C20 109.4(5) . . ? C18 C17 C20 111.2(5) . . ? C19 C17 C20 110.5(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O11B C21 O11A 32.6(3) . . ? O11B C21 C24 91.3(6) . . ? O11A C21 C24 123.9(5) . . ? O11B C21 C22 114.1(5) . . ? O11A C21 C22 100.0(4) . . ? C24 C21 C22 108.8(5) . . ? O11B C21 C23 119.1(5) . . ? O11A C21 C23 102.4(5) . . ? C24 C21 C23 109.7(5) . . ? C22 C21 C23 111.6(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O12A C25 O12B 35.1(3) . . ? O12A C25 C27 96.7(5) . . ? O12B C25 C27 117.2(6) . . ? O12A C25 C28 122.1(6) . . ? O12B C25 C28 87.6(6) . . ? C27 C25 C28 109.0(7) . . ? O12A C25 C26 106.9(4) . . ? O12B C25 C26 118.1(5) . . ? C27 C25 C26 112.2(5) . . ? C28 C25 C26 109.4(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 C32 112.0(4) . 2_676 ? O5 C29 H29A 109.2 . . ? C32 C29 H29A 109.2 2_676 . ? O5 C29 H29B 109.2 . . ? C32 C29 H29B 109.2 2_676 . ? H29A C29 H29B 107.9 . . ? O5 C30 C31 108.9(4) . . ? O5 C30 H30A 109.9 . . ? C31 C30 H30A 109.9 . . ? O5 C30 H30B 109.9 . . ? C31 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? O6 C31 C30 113.2(4) . . ? O6 C31 H31A 108.9 . . ? C30 C31 H31A 108.9 . . ? O6 C31 H31B 108.9 . . ? C30 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? O6 C32 C29 110.9(4) . 2_676 ? O6 C32 H32A 109.5 . . ? C29 C32 H32A 109.5 2_676 . ? O6 C32 H32B 109.5 . . ? C29 C32 H32B 109.5 2_676 . ? H32A C32 H32B 108.0 . . ? O7 C33 C36 109.6(5) . 2_666 ? O7 C33 H33A 109.8 . . ? C36 C33 H33A 109.8 2_666 . ? O7 C33 H33B 109.8 . . ? C36 C33 H33B 109.8 2_666 . ? H33A C33 H33B 108.2 . . ? O7 C34 C35 111.1(7) . . ? O7 C34 H34A 109.4 . . ? C35 C34 H34A 109.4 . . ? O7 C34 H34B 109.4 . . ? C35 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? O8 C35 C34 110.6(4) . . ? O8 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? O8 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? O8 C36 C33 108.3(5) . 2_666 ? O8 C36 H36A 110.0 . . ? C33 C36 H36A 110.0 2_666 . ? O8 C36 H36B 110.0 . . ? C33 C36 H36B 110.0 2_666 . ? H36A C36 H36B 108.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Lu O1 C8 -1.0(3) . . . . ? O2 Lu O1 C8 -162.3(3) . . . . ? C13 Lu O1 C8 105.6(3) . . . . ? C9 Lu O1 C8 -150.9(3) . . . . ? O3 Lu O1 C8 -89.9(3) . . . . ? O9 Lu O1 C1 164.2(3) . . . . ? O2 Lu O1 C1 2.9(3) . . . . ? C13 Lu O1 C1 -89.2(3) . . . . ? C9 Lu O1 C1 14.3(5) . . . . ? O3 Lu O1 C1 75.3(3) . . . . ? O9 Lu O2 C2 -75.4(5) . . . . ? C13 Lu O2 C2 61.1(3) . . . . ? C9 Lu O2 C2 156.6(3) . . . . ? O1 Lu O2 C2 -28.4(3) . . . . ? O3 Lu O2 C2 -111.9(3) . . . . ? O9 Lu O2 C3 62.2(5) . . . . ? C13 Lu O2 C3 -161.3(3) . . . . ? C9 Lu O2 C3 -65.8(3) . . . . ? O1 Lu O2 C3 109.3(3) . . . . ? O3 Lu O2 C3 25.7(3) . . . . ? O9 Lu O3 C4 -164.5(3) . . . . ? O2 Lu O3 C4 0.5(3) . . . . ? C13 Lu O3 C4 -19.7(5) . . . . ? C9 Lu O3 C4 88.5(3) . . . . ? O1 Lu O3 C4 -69.3(3) . . . . ? O9 Lu O3 C5 -10.8(3) . . . . ? O2 Lu O3 C5 154.2(4) . . . . ? C13 Lu O3 C5 134.0(4) . . . . ? C9 Lu O3 C5 -117.7(3) . . . . ? O1 Lu O3 C5 84.4(3) . . . . ? O11B Si3 O9 Lu -4(2) . . . . ? O10 Si3 O9 Lu 134(2) . . . . ? O12B Si3 O9 Lu -118(2) . . . . ? O12A Si3 O9 Lu -93(2) . . . . ? O11A Si3 O9 Lu 19(2) . . . . ? O2 Lu O9 Si3 54(2) . . . . ? C13 Lu O9 Si3 -80(2) . . . . ? C9 Lu O9 Si3 178(100) . . . . ? O1 Lu O9 Si3 11(2) . . . . ? O3 Lu O9 Si3 87(2) . . . . ? O9 Si3 O10 C17 1.1(6) . . . . ? O11B Si3 O10 C17 142.5(6) . . . . ? O12B Si3 O10 C17 -103.3(6) . . . . ? O12A Si3 O10 C17 -135.1(5) . . . . ? O11A Si3 O10 C17 111.6(5) . . . . ? O9 Si3 O11A O11B -136.4(7) . . . . ? O10 Si3 O11A O11B 101.8(7) . . . . ? O12B Si3 O11A O11B -27.0(9) . . . . ? O12A Si3 O11A O11B -15.4(7) . . . . ? O9 Si3 O11A C21 179.1(5) . . . . ? O11B Si3 O11A C21 -44.5(7) . . . . ? O10 Si3 O11A C21 57.3(6) . . . . ? O12B Si3 O11A C21 -71.5(7) . . . . ? O12A Si3 O11A C21 -59.9(6) . . . . ? Si3 O11A O11B C21 -147.1(4) . . . . ? C21 O11A O11B Si3 147.1(4) . . . . ? O9 Si3 O11B O11A 51.5(7) . . . . ? O10 Si3 O11B O11A -88.5(7) . . . . ? O12B Si3 O11B O11A 160.1(6) . . . . ? O12A Si3 O11B O11A 164.6(7) . . . . ? O9 Si3 O11B C21 102.6(8) . . . . ? O10 Si3 O11B C21 -37.4(10) . . . . ? O12B Si3 O11B C21 -148.8(8) . . . . ? O12A Si3 O11B C21 -144.3(9) . . . . ? O11A Si3 O11B C21 51.1(8) . . . . ? O9 Si3 O12A O12B -55.2(7) . . . . ? O11B Si3 O12A O12B -171.8(7) . . . . ? O10 Si3 O12A O12B 81.0(6) . . . . ? O11A Si3 O12A O12B -164.1(6) . . . . ? O9 Si3 O12A C25 -103.8(6) . . . . ? O11B Si3 O12A C25 139.7(7) . . . . ? O10 Si3 O12A C25 32.4(7) . . . . ? O12B Si3 O12A C25 -48.5(7) . . . . ? O11A Si3 O12A C25 147.4(6) . . . . ? Si3 O12A O12B C25 -145.4(4) . . . . ? C25 O12A O12B Si3 145.4(4) . . . . ? O9 Si3 O12B O12A 132.3(6) . . . . ? O11B Si3 O12B O12A 8.4(7) . . . . ? O10 Si3 O12B O12A -108.3(6) . . . . ? O11A Si3 O12B O12A 21.8(8) . . . . ? O9 Si3 O12B C25 178.0(7) . . . . ? O11B Si3 O12B C25 54.0(8) . . . . ? O10 Si3 O12B C25 -62.7(8) . . . . ? O12A Si3 O12B C25 45.7(7) . . . . ? O11A Si3 O12B C25 67.5(9) . . . . ? C8 O1 C1 C2 -173.1(4) . . . . ? Lu O1 C1 C2 20.3(5) . . . . ? C3 O2 C2 C1 -85.2(5) . . . . ? Lu O2 C2 C1 51.1(5) . . . . ? O1 C1 C2 O2 -44.1(5) . . . . ? C2 O2 C3 C4 87.1(5) . . . . ? Lu O2 C3 C4 -50.0(5) . . . . ? C5 O3 C4 C3 178.7(4) . . . . ? Lu O3 C4 C3 -24.4(5) . . . . ? O2 C3 C4 O3 48.0(6) . . . . ? C4 O3 C5 C6 98.7(5) . . . . ? Lu O3 C5 C6 -56.0(5) . . . . ? C7 O4 C6 C5 144.6(4) . . . . ? O3 C5 C6 O4 -56.8(5) . . . . ? C6 O4 C7 C8 -63.3(6) . . . . ? C1 O1 C8 C7 -57.0(5) . . . . ? Lu O1 C8 C7 109.2(4) . . . . ? O4 C7 C8 O1 -40.7(6) . . . . ? C12 Si1 C9 Lu 52.7(5) . . . . ? C10 Si1 C9 Lu 175.2(3) . . . . ? C11 Si1 C9 Lu -65.5(4) . . . . ? O9 Lu C9 Si1 -61.0(3) . . . . ? O2 Lu C9 Si1 98.0(3) . . . . ? C13 Lu C9 Si1 -170.2(3) . . . . ? O1 Lu C9 Si1 87.5(4) . . . . ? O3 Lu C9 Si1 29.4(3) . . . . ? C15 Si2 C13 Lu 70.0(4) . . . . ? C16 Si2 C13 Lu -50.1(4) . . . . ? C14 Si2 C13 Lu -170.3(3) . . . . ? O9 Lu C13 Si2 61.8(3) . . . . ? O2 Lu C13 Si2 -100.0(3) . . . . ? C9 Lu C13 Si2 171.3(3) . . . . ? O1 Lu C13 Si2 -33.6(3) . . . . ? O3 Lu C13 Si2 -81.3(5) . . . . ? Si3 O10 C17 C18 -62.6(6) . . . . ? Si3 O10 C17 C19 177.7(5) . . . . ? Si3 O10 C17 C20 59.3(6) . . . . ? Si3 O11B C21 O11A -52.2(8) . . . . ? O11A O11B C21 C24 179.0(7) . . . . ? Si3 O11B C21 C24 126.8(9) . . . . ? O11A O11B C21 C22 -69.7(8) . . . . ? Si3 O11B C21 C22 -121.9(8) . . . . ? O11A O11B C21 C23 65.5(8) . . . . ? Si3 O11B C21 C23 13.3(12) . . . . ? Si3 O11A C21 O11B 44.4(7) . . . . ? O11B O11A C21 C24 -1.2(9) . . . . ? Si3 O11A C21 C24 43.2(9) . . . . ? O11B O11A C21 C22 119.6(8) . . . . ? Si3 O11A C21 C22 164.0(5) . . . . ? O11B O11A C21 C23 -125.5(8) . . . . ? Si3 O11A C21 C23 -81.1(7) . . . . ? Si3 O12A C25 O12B 48.1(7) . . . . ? O12B O12A C25 C27 129.3(7) . . . . ? Si3 O12A C25 C27 177.3(6) . . . . ? O12B O12A C25 C28 11.8(9) . . . . ? Si3 O12A C25 C28 59.9(9) . . . . ? O12B O12A C25 C26 -115.0(7) . . . . ? Si3 O12A C25 C26 -67.0(7) . . . . ? Si3 O12B C25 O12A -47.4(7) . . . . ? O12A O12B C25 C27 -59.8(8) . . . . ? Si3 O12B C25 C27 -107.2(8) . . . . ? O12A O12B C25 C28 -170.0(7) . . . . ? Si3 O12B C25 C28 142.6(8) . . . . ? O12A O12B C25 C26 79.3(8) . . . . ? Si3 O12B C25 C26 31.9(10) . . . . ? C30 O5 C29 C32 103.6(5) . . . 2_676 ? C29 O5 C30 C31 -177.6(4) . . . . ? C32 O6 C31 C30 86.0(5) . . . . ? O5 C30 C31 O6 73.1(5) . . . . ? C31 O6 C32 C29 -134.8(4) . . . 2_676 ? C34 O7 C33 C36 96.5(6) . . . 2_666 ? C33 O7 C34 C35 -152.0(5) . . . . ? C36 O8 C35 C34 93.7(6) . . . . ? O7 C34 C35 O8 71.3(6) . . . . ? C35 O8 C36 C33 -164.7(5) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.630 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.227 #===END data_be9 _database_code_depnum_ccdc_archive 'CCDC 282724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H123 B2 O11 Si Y' _chemical_formula_weight 1495.48 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' B B 0.0013 0.0007 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0500(12) _cell_length_b 25.186(2) _cell_length_c 25.083(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.606(2) _cell_angle_gamma 90.00 _cell_volume 8217.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4887 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 21.27 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6511 _exptl_absorpt_correction_T_max 0.6958 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112659 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 28.61 _reflns_number_total 20811 _reflns_number_gt 13255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _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^)+(0.0475P)^2^+2.2639P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20811 _refine_ls_number_parameters 937 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 Y Y 1.246626(16) 0.169081(8) 1.318383(8) 0.01730(6) Uani 1 1 d . . . Si Si 1.06477(5) 0.14996(2) 1.20207(2) 0.01846(13) Uani 1 1 d . . . O1 O 1.13441(11) 0.16780(6) 1.25516(6) 0.0201(3) Uani 1 1 d . . . O2 O 0.96786(11) 0.18908(6) 1.18675(6) 0.0220(3) Uani 1 1 d . . . O3 O 1.02907(12) 0.08932(6) 1.21379(6) 0.0220(3) Uani 1 1 d . . . O4 O 1.13075(12) 0.14917(6) 1.14967(6) 0.0260(4) Uani 1 1 d . . . O5 O 1.27709(12) 0.26270(6) 1.30333(6) 0.0225(4) Uani 1 1 d . . . O6 O 1.38930(11) 0.17841(6) 1.26567(6) 0.0211(3) Uani 1 1 d . . . O7 O 1.30536(12) 0.08293(6) 1.29513(6) 0.0216(3) Uani 1 1 d . . . O8 O 1.15285(12) 0.10741(6) 1.36691(6) 0.0230(4) Uani 1 1 d . . . O9 O 1.15250(12) 0.22019(6) 1.38006(6) 0.0248(4) Uani 1 1 d . . . O10 O 1.37751(12) 0.16845(6) 1.39186(6) 0.0230(3) Uani 1 1 d . . . O11 O 1.49505(16) 0.10794(8) 1.13768(8) 0.0489(5) Uani 1 1 d . . . B1 B 1.2711(2) 0.05924(10) 1.59831(10) 0.0189(5) Uani 1 1 d . . . B2 B 0.6903(2) 0.14277(11) 0.90814(10) 0.0214(6) Uani 1 1 d . . . C1 C 0.88947(17) 0.21293(9) 1.21613(9) 0.0233(5) Uani 1 1 d . . . C2 C 0.85428(19) 0.17447(10) 1.25769(10) 0.0282(5) Uani 1 1 d . . . H2A H 0.8212 0.1437 1.2397 0.042 Uiso 1 1 calc R . . H2B H 0.8052 0.1923 1.2792 0.042 Uiso 1 1 calc R . . H2C H 0.9138 0.1626 1.2810 0.042 Uiso 1 1 calc R . . C3 C 0.9326(2) 0.26304(10) 1.24284(11) 0.0343(6) Uani 1 1 d . . . H3A H 0.9919 0.2540 1.2676 0.051 Uiso 1 1 calc R . . H3B H 0.8797 0.2800 1.2626 0.051 Uiso 1 1 calc R . . H3C H 0.9542 0.2876 1.2155 0.051 Uiso 1 1 calc R . . C4 C 0.80175(19) 0.22630(11) 1.17441(11) 0.0334(6) Uani 1 1 d . . . H4A H 0.8269 0.2502 1.1475 0.050 Uiso 1 1 calc R . . H4B H 0.7463 0.2438 1.1919 0.050 Uiso 1 1 calc R . . H4C H 0.7757 0.1936 1.1571 0.050 Uiso 1 1 calc R . . C5 C 0.97880(18) 0.04784(9) 1.18077(10) 0.0258(5) Uani 1 1 d . . . C6 C 0.9445(2) 0.00686(10) 1.22015(11) 0.0357(6) Uani 1 1 d . . . H6A H 1.0047 -0.0068 1.2418 0.054 Uiso 1 1 calc R . . H6B H 0.9097 -0.0225 1.2005 0.054 Uiso 1 1 calc R . . H6C H 0.8971 0.0234 1.2436 0.054 Uiso 1 1 calc R . . C7 C 1.0549(2) 0.02425(10) 1.14478(10) 0.0337(6) Uani 1 1 d . . . H7A H 1.0790 0.0520 1.1214 0.051 Uiso 1 1 calc R . . H7B H 1.0213 -0.0040 1.1229 0.051 Uiso 1 1 calc R . . H7C H 1.1135 0.0095 1.1668 0.051 Uiso 1 1 calc R . . C8 C 0.88536(19) 0.07008(10) 1.14762(10) 0.0320(6) Uani 1 1 d . . . H8A H 0.8368 0.0848 1.1715 0.048 Uiso 1 1 calc R . . H8B H 0.8519 0.0416 1.1260 0.048 Uiso 1 1 calc R . . H8C H 0.9074 0.0981 1.1240 0.048 Uiso 1 1 calc R . . C9 C 1.13267(19) 0.18334(11) 1.10342(10) 0.0323(6) Uani 1 1 d . . . C10 C 1.2220(2) 0.16272(14) 1.07344(11) 0.0503(9) Uani 1 1 d . . . H10A H 1.2856 0.1643 1.0970 0.075 Uiso 1 1 calc R . . H10B H 1.2292 0.1848 1.0418 0.075 Uiso 1 1 calc R . . H10C H 1.2084 0.1259 1.0624 0.075 Uiso 1 1 calc R . . C11 C 1.1503(2) 0.24026(11) 1.12105(12) 0.0428(7) Uani 1 1 d . . . H11A H 1.0945 0.2516 1.1424 0.064 Uiso 1 1 calc R . . H11B H 1.1518 0.2631 1.0895 0.064 Uiso 1 1 calc R . . H11C H 1.2160 0.2430 1.1427 0.064 Uiso 1 1 calc R . . C12 C 1.0318(2) 0.17840(13) 1.06867(11) 0.0454(8) Uani 1 1 d . . . H12A H 1.0216 0.1414 1.0575 0.068 Uiso 1 1 calc R . . H12B H 1.0342 0.2010 1.0370 0.068 Uiso 1 1 calc R . . H12C H 0.9748 0.1896 1.0892 0.068 Uiso 1 1 calc R . . C13 C 1.37140(17) 0.29490(9) 1.30817(10) 0.0242(5) Uani 1 1 d . . . H13A H 1.4314 0.2736 1.2992 0.029 Uiso 1 1 calc R . . H13B H 1.3845 0.3089 1.3450 0.029 Uiso 1 1 calc R . . C14 C 1.35145(19) 0.33972(9) 1.26860(10) 0.0291(6) Uani 1 1 d . . . H14A H 1.3645 0.3286 1.2319 0.035 Uiso 1 1 calc R . . H14B H 1.3941 0.3712 1.2787 0.035 Uiso 1 1 calc R . . C15 C 1.23740(19) 0.35083(10) 1.27329(11) 0.0340(6) Uani 1 1 d . . . H15A H 1.2269 0.3725 1.3053 0.041 Uiso 1 1 calc R . . H15B H 1.2061 0.3692 1.2411 0.041 Uiso 1 1 calc R . . C16 C 1.19356(18) 0.29560(9) 1.27823(10) 0.0253(5) Uani 1 1 d . . . H16A H 1.1345 0.2962 1.3006 0.030 Uiso 1 1 calc R . . H16B H 1.1700 0.2814 1.2425 0.030 Uiso 1 1 calc R . . C17 C 1.48603(16) 0.14924(9) 1.27037(9) 0.0223(5) Uani 1 1 d . . . H17A H 1.4818 0.1170 1.2477 0.027 Uiso 1 1 calc R . . H17B H 1.5050 0.1388 1.3079 0.027 Uiso 1 1 calc R . . C18 C 1.56280(18) 0.18884(10) 1.25079(10) 0.0282(6) Uani 1 1 d . . . H18A H 1.6195 0.1703 1.2345 0.034 Uiso 1 1 calc R . . H18B H 1.5921 0.2114 1.2805 0.034 Uiso 1 1 calc R . . C19 C 1.49921(19) 0.22212(10) 1.20892(11) 0.0315(6) Uani 1 1 d . . . H19A H 1.5073 0.2605 1.2167 0.038 Uiso 1 1 calc R . . H19B H 1.5205 0.2150 1.1726 0.038 Uiso 1 1 calc R . . C20 C 1.38805(19) 0.20442(10) 1.21361(9) 0.0265(5) Uani 1 1 d . . . H20A H 1.3411 0.2354 1.2119 0.032 Uiso 1 1 calc R . . H20B H 1.3656 0.1794 1.1845 0.032 Uiso 1 1 calc R . . C21 C 1.35836(19) 0.04215(9) 1.32847(10) 0.0273(5) Uani 1 1 d . . . H21A H 1.3249 0.0374 1.3622 0.033 Uiso 1 1 calc R . . H21B H 1.4312 0.0520 1.3373 0.033 Uiso 1 1 calc R . . C22 C 1.3506(2) -0.00801(10) 1.29541(10) 0.0363(6) Uani 1 1 d . . . H22A H 1.2864 -0.0275 1.3007 0.044 Uiso 1 1 calc R . . H22B H 1.4101 -0.0317 1.3044 0.044 Uiso 1 1 calc R . . C23 C 1.35069(19) 0.01257(10) 1.23860(10) 0.0298(6) Uani 1 1 d . . . H23A H 1.4213 0.0208 1.2293 0.036 Uiso 1 1 calc R . . H23B H 1.3192 -0.0134 1.2126 0.036 Uiso 1 1 calc R . . C24 C 1.28632(18) 0.06231(9) 1.24021(9) 0.0256(5) Uani 1 1 d . . . H24A H 1.3073 0.0886 1.2139 0.031 Uiso 1 1 calc R . . H24B H 1.2126 0.0540 1.2322 0.031 Uiso 1 1 calc R . . C25 C 1.13354(18) 0.10293(10) 1.42328(9) 0.0251(5) Uani 1 1 d . . . H25A H 1.1430 0.1377 1.4414 0.030 Uiso 1 1 calc R . . H25B H 1.1810 0.0769 1.4417 0.030 Uiso 1 1 calc R . . C26 C 1.02245(19) 0.08425(10) 1.42379(10) 0.0295(6) Uani 1 1 d . . . H26A H 0.9766 0.1142 1.4314 0.035 Uiso 1 1 calc R . . H26B H 1.0162 0.0563 1.4511 0.035 Uiso 1 1 calc R . . C27 C 0.9957(2) 0.06234(12) 1.36754(10) 0.0373(7) Uani 1 1 d . . . H27A H 0.9688 0.0257 1.3692 0.045 Uiso 1 1 calc R . . H27B H 0.9433 0.0848 1.3478 0.045 Uiso 1 1 calc R . . C28 C 1.09527(18) 0.06328(9) 1.34084(9) 0.0258(5) Uani 1 1 d . . . H28A H 1.1330 0.0294 1.3466 0.031 Uiso 1 1 calc R . . H28B H 1.0825 0.0696 1.3019 0.031 Uiso 1 1 calc R . . C29 C 1.1964(2) 0.25860(10) 1.41887(10) 0.0323(6) Uani 1 1 d . . . H29A H 1.2624 0.2725 1.4078 0.039 Uiso 1 1 calc R . . H29B H 1.2086 0.2421 1.4546 0.039 Uiso 1 1 calc R . . C30 C 1.1180(2) 0.30243(13) 1.41987(13) 0.0482(8) Uani 1 1 d . . . H30A H 1.1168 0.3174 1.4563 0.058 Uiso 1 1 calc R . . H30B H 1.1333 0.3313 1.3949 0.058 Uiso 1 1 calc R . . C31 C 1.0170(2) 0.27629(14) 1.40256(16) 0.0696(12) Uani 1 1 d . . . H31A H 0.9728 0.2745 1.4328 0.083 Uiso 1 1 calc R . . H31B H 0.9804 0.2966 1.3731 0.083 Uiso 1 1 calc R . . C32 C 1.04151(18) 0.22212(10) 1.38436(11) 0.0316(6) Uani 1 1 d . . . H32A H 1.0211 0.1954 1.4104 0.038 Uiso 1 1 calc R . . H32B H 1.0042 0.2146 1.3492 0.038 Uiso 1 1 calc R . . C33 C 1.46433(18) 0.20569(10) 1.40105(9) 0.0268(5) Uani 1 1 d . . . H33A H 1.4391 0.2428 1.4009 0.032 Uiso 1 1 calc R . . H33B H 1.5124 0.2018 1.3727 0.032 Uiso 1 1 calc R . . C34 C 1.5174(2) 0.19216(11) 1.45464(11) 0.0386(7) Uani 1 1 d . . . H34A H 1.4900 0.2134 1.4835 0.046 Uiso 1 1 calc R . . H34B H 1.5926 0.1979 1.4551 0.046 Uiso 1 1 calc R . . C35 C 1.4917(2) 0.13295(11) 1.46015(11) 0.0365(6) Uani 1 1 d . . . H35A H 1.5348 0.1104 1.4386 0.044 Uiso 1 1 calc R . . H35B H 1.4996 0.1212 1.4979 0.044 Uiso 1 1 calc R . . C36 C 1.38113(19) 0.13239(10) 1.43841(10) 0.0296(6) Uani 1 1 d . . . H36A H 1.3594 0.0961 1.4274 0.036 Uiso 1 1 calc R . . H36B H 1.3359 0.1454 1.4655 0.036 Uiso 1 1 calc R . . C37 C 1.36216(17) 0.10474(9) 1.59910(8) 0.0206(5) Uani 1 1 d . . . C38 C 1.46622(18) 0.09103(9) 1.60931(9) 0.0233(5) Uani 1 1 d . . . H38 H 1.4829 0.0548 1.6159 0.028 Uiso 1 1 calc R . . C39 C 1.54591(19) 0.12742(10) 1.61025(9) 0.0284(6) Uani 1 1 d . . . H39 H 1.6150 0.1157 1.6169 0.034 Uiso 1 1 calc R . . C40 C 1.5253(2) 0.18079(10) 1.60148(10) 0.0312(6) Uani 1 1 d . . . H40 H 1.5794 0.2061 1.6021 0.037 Uiso 1 1 calc R . . C41 C 1.4238(2) 0.19628(10) 1.59175(10) 0.0315(6) Uani 1 1 d . . . H41 H 1.4079 0.2327 1.5859 0.038 Uiso 1 1 calc R . . C42 C 1.34491(18) 0.15912(9) 1.59051(10) 0.0254(5) Uani 1 1 d . . . H42 H 1.2761 0.1711 1.5835 0.031 Uiso 1 1 calc R . . C43 C 1.26303(17) 0.02552(8) 1.54179(8) 0.0188(5) Uani 1 1 d . . . C44 C 1.17140(18) 0.00009(9) 1.52344(9) 0.0225(5) Uani 1 1 d . . . H44 H 1.1127 0.0049 1.5430 0.027 Uiso 1 1 calc R . . C45 C 1.16209(19) -0.03190(9) 1.47802(9) 0.0254(5) Uani 1 1 d . . . H45 H 1.0983 -0.0485 1.4673 0.031 Uiso 1 1 calc R . . C46 C 1.24604(19) -0.03944(9) 1.44858(9) 0.0268(5) Uani 1 1 d . . . H46 H 1.2405 -0.0609 1.4174 0.032 Uiso 1 1 calc R . . C47 C 1.33828(19) -0.01520(9) 1.46529(9) 0.0247(5) Uani 1 1 d . . . H47 H 1.3967 -0.0203 1.4456 0.030 Uiso 1 1 calc R . . C48 C 1.34605(18) 0.01670(9) 1.51086(9) 0.0214(5) Uani 1 1 d . . . H48 H 1.4101 0.0331 1.5213 0.026 Uiso 1 1 calc R . . C49 C 1.15845(17) 0.08671(8) 1.60541(9) 0.0191(5) Uani 1 1 d . . . C50 C 1.11027(18) 0.11817(9) 1.56444(9) 0.0229(5) Uani 1 1 d . . . H50 H 1.1443 0.1231 1.5327 0.028 Uiso 1 1 calc R . . C51 C 1.01537(18) 0.14253(9) 1.56789(10) 0.0261(5) Uani 1 1 d . . . H51 H 0.9864 0.1637 1.5391 0.031 Uiso 1 1 calc R . . C52 C 0.96324(19) 0.13583(10) 1.61337(10) 0.0297(6) Uani 1 1 d . . . H52 H 0.8984 0.1522 1.6163 0.036 Uiso 1 1 calc R . . C53 C 1.00736(19) 0.10488(10) 1.65434(10) 0.0300(6) Uani 1 1 d . . . H53 H 0.9722 0.0998 1.6857 0.036 Uiso 1 1 calc R . . C54 C 1.10276(18) 0.08101(9) 1.65052(9) 0.0244(5) Uani 1 1 d . . . H54 H 1.1311 0.0601 1.6796 0.029 Uiso 1 1 calc R . . C55 C 1.30009(17) 0.01775(9) 1.64799(9) 0.0200(5) Uani 1 1 d . . . C56 C 1.28757(17) -0.03733(9) 1.64504(9) 0.0236(5) Uani 1 1 d . . . H56 H 1.2653 -0.0529 1.6116 0.028 Uiso 1 1 calc R . . C57 C 1.30659(18) -0.07031(10) 1.68948(10) 0.0278(6) Uani 1 1 d . . . H57 H 1.2968 -0.1075 1.6858 0.033 Uiso 1 1 calc R . . C58 C 1.33960(18) -0.04933(10) 1.73894(10) 0.0289(6) Uani 1 1 d . . . H58 H 1.3517 -0.0717 1.7693 0.035 Uiso 1 1 calc R . . C59 C 1.35447(19) 0.00493(10) 1.74309(9) 0.0285(6) Uani 1 1 d . . . H59 H 1.3778 0.0202 1.7765 0.034 Uiso 1 1 calc R . . C60 C 1.33545(19) 0.03718(10) 1.69861(9) 0.0261(5) Uani 1 1 d . . . H60 H 1.3469 0.0743 1.7026 0.031 Uiso 1 1 calc R . . C61 C 0.74822(18) 0.09505(9) 0.94428(9) 0.0230(5) Uani 1 1 d . . . C62 C 0.7009(2) 0.04640(10) 0.95216(10) 0.0297(6) Uani 1 1 d . . . H62 H 0.6323 0.0414 0.9373 0.036 Uiso 1 1 calc R . . C63 C 0.7493(2) 0.00463(11) 0.98086(10) 0.0360(6) Uani 1 1 d . . . H63 H 0.7137 -0.0278 0.9850 0.043 Uiso 1 1 calc R . . C64 C 0.8486(2) 0.01056(11) 1.00313(10) 0.0377(7) Uani 1 1 d . . . H64 H 0.8817 -0.0174 1.0232 0.045 Uiso 1 1 calc R . . C65 C 0.8991(2) 0.05752(11) 0.99588(10) 0.0383(7) Uani 1 1 d . . . H65 H 0.9680 0.0618 1.0105 0.046 Uiso 1 1 calc R . . C66 C 0.84965(19) 0.09905(11) 0.96702(10) 0.0310(6) Uani 1 1 d . . . H66 H 0.8862 0.1312 0.9627 0.037 Uiso 1 1 calc R . . C67 C 0.73205(17) 0.20226(9) 0.92795(9) 0.0219(5) Uani 1 1 d . . . C68 C 0.75634(18) 0.21469(10) 0.98237(10) 0.0262(5) Uani 1 1 d . . . H68 H 0.7505 0.1876 1.0083 0.031 Uiso 1 1 calc R . . C69 C 0.78852(19) 0.26496(10) 0.99958(10) 0.0307(6) Uani 1 1 d . . . H69 H 0.8036 0.2715 1.0367 0.037 Uiso 1 1 calc R . . C70 C 0.79887(19) 0.30556(11) 0.96322(11) 0.0327(6) Uani 1 1 d . . . H70 H 0.8209 0.3399 0.9749 0.039 Uiso 1 1 calc R . . C71 C 0.77637(19) 0.29491(10) 0.90928(10) 0.0292(6) Uani 1 1 d . . . H71 H 0.7828 0.3222 0.8836 0.035 Uiso 1 1 calc R . . C72 C 0.74444(18) 0.24450(9) 0.89256(10) 0.0255(5) Uani 1 1 d . . . H72 H 0.7303 0.2384 0.8553 0.031 Uiso 1 1 calc R . . C73 C 0.56603(18) 0.13778(9) 0.91496(9) 0.0225(5) Uani 1 1 d . . . C74 C 0.51707(18) 0.16570(10) 0.95419(10) 0.0266(5) Uani 1 1 d . . . H74 H 0.5551 0.1918 0.9747 0.032 Uiso 1 1 calc R . . C75 C 0.41499(19) 0.15668(10) 0.96436(11) 0.0317(6) Uani 1 1 d . . . H75 H 0.3850 0.1768 0.9912 0.038 Uiso 1 1 calc R . . C76 C 0.3570(2) 0.11871(11) 0.93574(11) 0.0350(7) Uani 1 1 d . . . H76 H 0.2878 0.1122 0.9430 0.042 Uiso 1 1 calc R . . C77 C 0.40156(19) 0.09044(10) 0.89632(11) 0.0335(6) Uani 1 1 d . . . H77 H 0.3628 0.0643 0.8763 0.040 Uiso 1 1 calc R . . C78 C 0.50325(18) 0.10023(9) 0.88599(10) 0.0268(5) Uani 1 1 d . . . H78 H 0.5316 0.0808 0.8582 0.032 Uiso 1 1 calc R . . C79 C 0.71414(17) 0.13490(9) 0.84516(9) 0.0213(5) Uani 1 1 d . . . C80 C 0.80583(18) 0.11186(9) 0.83053(9) 0.0244(5) Uani 1 1 d . . . H80 H 0.8535 0.0984 0.8578 0.029 Uiso 1 1 calc R . . C81 C 0.82938(19) 0.10798(9) 0.77776(10) 0.0281(6) Uani 1 1 d . . . H81 H 0.8925 0.0922 0.7697 0.034 Uiso 1 1 calc R . . C82 C 0.76212(19) 0.12676(9) 0.73683(10) 0.0267(5) Uani 1 1 d . . . H82 H 0.7785 0.1240 0.7007 0.032 Uiso 1 1 calc R . . C83 C 0.67092(19) 0.14948(10) 0.74903(10) 0.0275(6) Uani 1 1 d . . . H83 H 0.6236 0.1624 0.7213 0.033 Uiso 1 1 calc R . . C84 C 0.64840(18) 0.15345(9) 0.80220(9) 0.0252(5) Uani 1 1 d . . . H84 H 0.5853 0.1695 0.8098 0.030 Uiso 1 1 calc R . . C85 C 1.4612(3) 0.05921(12) 1.11285(13) 0.0521(8) Uani 1 1 d . . . H85A H 1.3864 0.0606 1.1025 0.063 Uiso 1 1 calc R . . H85B H 1.4750 0.0292 1.1378 0.063 Uiso 1 1 calc R . . C86 C 1.5202(2) 0.05209(11) 1.06373(10) 0.0360(6) Uani 1 1 d . . . H86A H 1.5339 0.0142 1.0568 0.043 Uiso 1 1 calc R . . H86B H 1.4832 0.0680 1.0316 0.043 Uiso 1 1 calc R . . C87 C 1.6172(2) 0.08169(15) 1.08013(14) 0.0647(11) Uani 1 1 d . . . H87A H 1.6659 0.0593 1.1026 0.078 Uiso 1 1 calc R . . H87B H 1.6512 0.0943 1.0486 0.078 Uiso 1 1 calc R . . C88 C 1.5791(3) 0.12704(15) 1.11133(13) 0.0653(11) Uani 1 1 d . . . H88A H 1.6340 0.1400 1.1377 0.078 Uiso 1 1 calc R . . H88B H 1.5572 0.1567 1.0871 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y 0.01641(11) 0.01664(11) 0.01854(11) 0.00074(9) -0.00052(8) -0.00260(9) Si 0.0169(3) 0.0181(3) 0.0200(3) 0.0009(3) -0.0004(3) -0.0001(2) O1 0.0179(8) 0.0194(8) 0.0227(8) 0.0003(7) 0.0008(6) -0.0007(7) O2 0.0193(8) 0.0231(8) 0.0236(9) 0.0024(7) 0.0011(7) 0.0027(7) O3 0.0232(9) 0.0192(8) 0.0228(8) -0.0013(7) -0.0035(7) -0.0016(7) O4 0.0268(9) 0.0273(9) 0.0243(9) 0.0034(7) 0.0057(7) 0.0032(7) O5 0.0190(8) 0.0181(8) 0.0298(9) 0.0032(7) -0.0020(7) -0.0015(7) O6 0.0175(8) 0.0212(9) 0.0247(8) 0.0062(7) 0.0019(7) 0.0006(6) O7 0.0243(9) 0.0174(8) 0.0226(8) 0.0021(7) -0.0018(7) -0.0002(7) O8 0.0282(9) 0.0246(9) 0.0163(8) -0.0006(7) 0.0018(7) -0.0079(7) O9 0.0202(8) 0.0258(9) 0.0286(9) -0.0066(7) 0.0027(7) -0.0061(7) O10 0.0220(8) 0.0247(8) 0.0216(8) 0.0045(7) -0.0025(7) -0.0057(7) O11 0.0506(13) 0.0549(13) 0.0425(12) -0.0179(10) 0.0119(10) -0.0077(11) B1 0.0209(13) 0.0204(13) 0.0155(12) -0.0016(10) 0.0025(10) 0.0009(11) B2 0.0185(13) 0.0253(14) 0.0204(13) -0.0024(11) 0.0013(11) 0.0022(11) C1 0.0184(12) 0.0215(12) 0.0297(13) -0.0002(10) 0.0011(10) 0.0011(10) C2 0.0270(13) 0.0296(14) 0.0283(13) -0.0008(11) 0.0046(10) -0.0005(11) C3 0.0280(14) 0.0269(14) 0.0474(17) -0.0042(12) -0.0002(12) 0.0018(11) C4 0.0227(13) 0.0370(15) 0.0395(16) 0.0041(12) -0.0033(11) 0.0052(12) C5 0.0275(13) 0.0189(12) 0.0296(13) -0.0066(10) -0.0062(11) -0.0027(10) C6 0.0415(16) 0.0231(13) 0.0415(16) -0.0020(12) -0.0037(13) -0.0094(12) C7 0.0335(15) 0.0303(14) 0.0362(15) -0.0117(12) -0.0037(12) 0.0049(12) C8 0.0286(14) 0.0301(14) 0.0353(15) -0.0104(11) -0.0088(11) -0.0005(11) C9 0.0250(13) 0.0497(17) 0.0221(13) 0.0117(12) 0.0005(11) -0.0059(12) C10 0.0303(15) 0.095(3) 0.0264(15) 0.0094(16) 0.0058(12) 0.0015(16) C11 0.0315(15) 0.0422(17) 0.0532(18) 0.0239(14) -0.0049(13) -0.0089(13) C12 0.0321(16) 0.079(2) 0.0248(14) 0.0064(14) -0.0021(12) -0.0074(15) C13 0.0208(12) 0.0199(12) 0.0310(13) 0.0035(10) -0.0047(10) -0.0073(10) C14 0.0291(14) 0.0207(13) 0.0360(15) 0.0083(10) -0.0060(11) -0.0064(10) C15 0.0323(15) 0.0253(13) 0.0427(16) 0.0073(12) -0.0065(12) 0.0034(11) C16 0.0216(12) 0.0254(13) 0.0280(13) 0.0036(10) -0.0028(10) 0.0025(10) C17 0.0182(12) 0.0228(12) 0.0259(12) 0.0025(10) 0.0021(10) 0.0023(10) C18 0.0219(13) 0.0290(13) 0.0342(14) 0.0043(11) 0.0051(11) -0.0031(11) C19 0.0301(14) 0.0297(14) 0.0356(15) 0.0087(11) 0.0088(12) -0.0015(11) C20 0.0303(14) 0.0270(13) 0.0222(12) 0.0059(10) 0.0023(10) -0.0008(11) C21 0.0310(14) 0.0210(12) 0.0291(13) 0.0060(10) -0.0035(11) 0.0018(11) C22 0.0461(17) 0.0226(13) 0.0389(16) 0.0008(11) -0.0041(13) 0.0025(12) C23 0.0297(14) 0.0254(13) 0.0339(14) -0.0064(11) 0.0000(11) 0.0034(11) C24 0.0259(13) 0.0250(13) 0.0251(13) -0.0019(10) -0.0033(10) 0.0013(10) C25 0.0305(14) 0.0269(13) 0.0183(12) 0.0029(10) 0.0052(10) -0.0055(11) C26 0.0283(14) 0.0313(14) 0.0298(14) 0.0007(11) 0.0079(11) -0.0061(11) C27 0.0318(15) 0.0499(18) 0.0301(15) 0.0036(13) 0.0005(12) -0.0123(13) C28 0.0325(14) 0.0218(12) 0.0227(12) -0.0010(10) 0.0010(10) -0.0121(10) C29 0.0312(15) 0.0344(15) 0.0305(14) -0.0108(12) -0.0025(11) -0.0076(12) C30 0.0379(17) 0.0527(19) 0.0536(19) -0.0297(16) 0.0022(14) -0.0021(15) C31 0.0358(18) 0.078(3) 0.096(3) -0.055(2) 0.0102(18) -0.0073(17) C32 0.0202(13) 0.0331(15) 0.0415(16) -0.0019(12) 0.0023(11) -0.0039(11) C33 0.0251(13) 0.0280(13) 0.0264(13) 0.0026(10) -0.0034(10) -0.0072(11) C34 0.0339(15) 0.0460(17) 0.0338(15) 0.0117(13) -0.0091(12) -0.0148(13) C35 0.0325(15) 0.0392(16) 0.0361(15) 0.0120(12) -0.0080(12) 0.0006(12) C36 0.0345(15) 0.0295(14) 0.0237(13) 0.0060(11) -0.0045(11) -0.0093(11) C37 0.0237(12) 0.0234(12) 0.0149(11) -0.0048(9) 0.0027(9) 0.0019(10) C38 0.0279(13) 0.0230(12) 0.0189(12) -0.0042(9) 0.0005(10) 0.0034(10) C39 0.0208(12) 0.0392(15) 0.0251(13) -0.0102(11) 0.0018(10) 0.0009(11) C40 0.0306(14) 0.0310(15) 0.0325(14) -0.0116(11) 0.0058(11) -0.0108(11) C41 0.0342(15) 0.0191(13) 0.0417(16) -0.0059(11) 0.0060(12) -0.0013(11) C42 0.0215(12) 0.0228(13) 0.0323(14) -0.0039(10) 0.0035(10) 0.0009(10) C43 0.0226(12) 0.0152(11) 0.0186(11) 0.0012(9) 0.0020(9) 0.0000(9) C44 0.0263(13) 0.0204(12) 0.0219(12) -0.0020(9) 0.0079(10) -0.0031(10) C45 0.0264(13) 0.0227(12) 0.0274(13) -0.0026(10) 0.0026(10) -0.0055(10) C46 0.0350(15) 0.0232(13) 0.0222(12) -0.0061(10) 0.0026(11) 0.0006(11) C47 0.0276(13) 0.0253(13) 0.0219(12) -0.0040(10) 0.0070(10) 0.0030(10) C48 0.0230(12) 0.0206(12) 0.0205(12) -0.0005(9) 0.0015(10) 0.0012(10) C49 0.0213(12) 0.0159(11) 0.0197(11) -0.0043(9) -0.0001(9) -0.0025(9) C50 0.0268(13) 0.0209(12) 0.0213(12) -0.0037(9) 0.0028(10) -0.0007(10) C51 0.0273(13) 0.0208(13) 0.0289(13) -0.0042(10) -0.0050(11) 0.0030(10) C52 0.0219(13) 0.0282(14) 0.0390(15) -0.0103(11) 0.0032(11) 0.0038(11) C53 0.0267(14) 0.0367(15) 0.0277(14) -0.0034(11) 0.0087(11) 0.0009(11) C54 0.0257(13) 0.0265(13) 0.0213(12) -0.0031(10) 0.0037(10) 0.0001(10) C55 0.0182(11) 0.0203(12) 0.0219(12) 0.0004(9) 0.0044(9) 0.0034(9) C56 0.0223(12) 0.0252(13) 0.0231(12) -0.0002(10) 0.0012(10) -0.0005(10) C57 0.0273(14) 0.0216(13) 0.0344(14) 0.0055(11) 0.0014(11) 0.0024(10) C58 0.0269(13) 0.0332(15) 0.0267(13) 0.0103(11) 0.0037(11) 0.0070(11) C59 0.0324(14) 0.0347(15) 0.0182(12) -0.0022(10) 0.0011(10) 0.0082(11) C60 0.0330(14) 0.0235(13) 0.0218(12) -0.0009(10) 0.0027(10) 0.0070(11) C61 0.0232(13) 0.0264(13) 0.0196(12) -0.0029(10) 0.0036(10) 0.0067(10) C62 0.0297(14) 0.0296(14) 0.0294(14) 0.0016(11) -0.0008(11) 0.0087(11) C63 0.0423(17) 0.0278(14) 0.0372(15) 0.0071(12) -0.0004(13) 0.0082(12) C64 0.0472(18) 0.0353(16) 0.0295(14) 0.0015(12) -0.0048(13) 0.0201(14) C65 0.0328(15) 0.0463(18) 0.0337(15) -0.0065(13) -0.0109(12) 0.0170(13) C66 0.0273(14) 0.0339(15) 0.0314(14) -0.0019(11) -0.0004(11) 0.0061(11) C67 0.0141(11) 0.0276(13) 0.0241(12) -0.0015(10) 0.0023(9) 0.0038(10) C68 0.0253(13) 0.0287(13) 0.0244(13) -0.0008(10) 0.0015(10) 0.0016(11) C69 0.0296(14) 0.0362(15) 0.0253(13) -0.0063(11) -0.0038(11) 0.0010(12) C70 0.0283(14) 0.0291(14) 0.0402(16) -0.0062(12) -0.0009(12) -0.0043(11) C71 0.0295(14) 0.0260(13) 0.0320(14) 0.0025(11) 0.0020(11) -0.0004(11) C72 0.0250(13) 0.0286(13) 0.0229(13) -0.0026(10) 0.0017(10) 0.0018(10) C73 0.0227(12) 0.0195(12) 0.0250(12) 0.0054(10) -0.0001(10) 0.0036(10) C74 0.0248(13) 0.0266(13) 0.0284(13) 0.0064(11) 0.0027(10) 0.0039(11) C75 0.0271(14) 0.0322(15) 0.0374(15) 0.0127(12) 0.0118(12) 0.0086(11) C76 0.0217(13) 0.0359(15) 0.0479(17) 0.0211(13) 0.0063(12) 0.0045(12) C77 0.0267(14) 0.0262(14) 0.0462(17) 0.0130(12) -0.0059(12) -0.0018(11) C78 0.0249(13) 0.0231(13) 0.0317(14) 0.0037(10) -0.0022(11) 0.0044(10) C79 0.0215(12) 0.0173(11) 0.0250(12) -0.0012(9) 0.0004(10) -0.0011(9) C80 0.0230(13) 0.0242(13) 0.0260(13) 0.0006(10) 0.0015(10) 0.0019(10) C81 0.0288(14) 0.0242(13) 0.0326(14) -0.0018(11) 0.0105(11) 0.0035(11) C82 0.0350(14) 0.0228(13) 0.0230(13) -0.0018(10) 0.0065(11) -0.0036(11) C83 0.0314(14) 0.0266(13) 0.0238(13) 0.0006(10) -0.0028(11) 0.0000(11) C84 0.0211(12) 0.0293(13) 0.0248(13) -0.0022(10) -0.0004(10) 0.0052(10) C85 0.058(2) 0.0431(18) 0.057(2) -0.0138(16) 0.0177(17) -0.0088(16) C86 0.0482(17) 0.0293(15) 0.0299(14) 0.0019(12) -0.0012(13) 0.0015(13) C87 0.0433(19) 0.100(3) 0.052(2) -0.032(2) 0.0144(16) -0.0197(19) C88 0.077(3) 0.074(2) 0.048(2) -0.0262(18) 0.0177(18) -0.039(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 Y O1 2.0705(15) . ? Y O8 2.3730(15) . ? Y O6 2.3802(15) . ? Y O7 2.3892(15) . ? Y O10 2.4102(15) . ? Y O9 2.4216(16) . ? Y O5 2.4257(15) . ? Si O1 1.6146(16) . ? Si O2 1.6247(16) . ? Si O4 1.6281(17) . ? Si O3 1.6304(16) . ? O2 C1 1.439(3) . ? O3 C5 1.456(3) . ? O4 C9 1.446(3) . ? O5 C16 1.470(3) . ? O5 C13 1.471(3) . ? O6 C17 1.457(3) . ? O6 C20 1.460(3) . ? O7 C21 1.463(3) . ? O7 C24 1.474(3) . ? O8 C25 1.460(3) . ? O8 C28 1.466(3) . ? O9 C29 1.457(3) . ? O9 C32 1.462(3) . ? O10 C33 1.475(3) . ? O10 C36 1.477(3) . ? O11 C88 1.410(4) . ? O11 C85 1.430(3) . ? B1 C55 1.647(3) . ? B1 C49 1.647(3) . ? B1 C43 1.649(3) . ? B1 C37 1.650(3) . ? B2 C79 1.646(3) . ? B2 C73 1.649(3) . ? B2 C61 1.651(3) . ? B2 C67 1.657(4) . ? C1 C3 1.516(3) . ? C1 C2 1.521(3) . ? C1 C4 1.525(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.516(3) . ? C5 C6 1.521(3) . ? C5 C8 1.526(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.512(4) . ? C9 C12 1.524(3) . ? C9 C10 1.528(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.512(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.528(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.513(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.523(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.534(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.531(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.510(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.516(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.510(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.525(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.529(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.509(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.507(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.505(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.482(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.501(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.537(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.501(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.402(3) . ? C37 C38 1.405(3) . ? C38 C39 1.385(3) . ? C38 H38 0.9500 . ? C39 C40 1.385(4) . ? C39 H39 0.9500 . ? C40 C41 1.384(4) . ? C40 H40 0.9500 . ? C41 C42 1.390(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.400(3) . ? C43 C44 1.401(3) . ? C44 C45 1.393(3) . ? C44 H44 0.9500 . ? C45 C46 1.382(3) . ? C45 H45 0.9500 . ? C46 C47 1.384(3) . ? C46 H46 0.9500 . ? C47 C48 1.394(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.400(3) . ? C49 C50 1.406(3) . ? C50 C51 1.391(3) . ? C50 H50 0.9500 . ? C51 C52 1.385(3) . ? C51 H51 0.9500 . ? C52 C53 1.379(3) . ? C52 H52 0.9500 . ? C53 C54 1.393(3) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.398(3) . ? C55 C60 1.404(3) . ? C56 C57 1.396(3) . ? C56 H56 0.9500 . ? C57 C58 1.385(3) . ? C57 H57 0.9500 . ? C58 C59 1.383(4) . ? C58 H58 0.9500 . ? C59 C60 1.386(3) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.394(3) . ? C61 C66 1.402(3) . ? C62 C63 1.397(3) . ? C62 H62 0.9500 . ? C63 C64 1.378(4) . ? C63 H63 0.9500 . ? C64 C65 1.373(4) . ? C64 H64 0.9500 . ? C65 C66 1.400(3) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C72 1.403(3) . ? C67 C68 1.411(3) . ? C68 C69 1.392(3) . ? C68 H68 0.9500 . ? C69 C70 1.384(4) . ? C69 H69 0.9500 . ? C70 C71 1.387(3) . ? C70 H70 0.9500 . ? C71 C72 1.390(3) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.404(3) . ? C73 C78 1.414(3) . ? C74 C75 1.395(3) . ? C74 H74 0.9500 . ? C75 C76 1.384(4) . ? C75 H75 0.9500 . ? C76 C77 1.384(4) . ? C76 H76 0.9500 . ? C77 C78 1.394(3) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C84 1.402(3) . ? C79 C80 1.405(3) . ? C80 C81 1.386(3) . ? C80 H80 0.9500 . ? C81 C82 1.380(3) . ? C81 H81 0.9500 . ? C82 C83 1.377(3) . ? C82 H82 0.9500 . ? C83 C84 1.392(3) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C86 1.515(4) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.498(4) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.492(5) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Y O8 91.17(6) . . ? O1 Y O6 96.48(6) . . ? O8 Y O6 143.92(5) . . ? O1 Y O7 91.14(6) . . ? O8 Y O7 73.71(5) . . ? O6 Y O7 70.94(5) . . ? O1 Y O10 178.72(6) . . ? O8 Y O10 88.08(5) . . ? O6 Y O10 83.54(5) . . ? O7 Y O10 87.66(5) . . ? O1 Y O9 97.69(6) . . ? O8 Y O9 73.22(5) . . ? O6 Y O9 139.64(5) . . ? O7 Y O9 145.88(5) . . ? O10 Y O9 83.09(5) . . ? O1 Y O5 90.61(5) . . ? O8 Y O5 144.47(5) . . ? O6 Y O5 70.87(5) . . ? O7 Y O5 141.72(5) . . ? O10 Y O5 90.60(5) . . ? O9 Y O5 71.38(5) . . ? O1 Si O2 113.72(8) . . ? O1 Si O4 111.72(9) . . ? O2 Si O4 105.58(8) . . ? O1 Si O3 105.19(8) . . ? O2 Si O3 112.48(9) . . ? O4 Si O3 108.14(9) . . ? Si O1 Y 162.30(9) . . ? C1 O2 Si 134.73(14) . . ? C5 O3 Si 133.77(14) . . ? C9 O4 Si 133.21(16) . . ? C16 O5 C13 108.13(16) . . ? C16 O5 Y 119.30(12) . . ? C13 O5 Y 132.04(13) . . ? C17 O6 C20 104.24(16) . . ? C17 O6 Y 128.06(12) . . ? C20 O6 Y 126.02(13) . . ? C21 O7 C24 108.87(16) . . ? C21 O7 Y 130.11(13) . . ? C24 O7 Y 120.98(12) . . ? C25 O8 C28 104.55(16) . . ? C25 O8 Y 133.11(13) . . ? C28 O8 Y 122.31(12) . . ? C29 O9 C32 105.52(18) . . ? C29 O9 Y 125.97(14) . . ? C32 O9 Y 128.40(13) . . ? C33 O10 C36 106.98(16) . . ? C33 O10 Y 127.14(12) . . ? C36 O10 Y 125.75(13) . . ? C88 O11 C85 108.2(2) . . ? C55 B1 C49 109.73(18) . . ? C55 B1 C43 108.58(18) . . ? C49 B1 C43 108.27(18) . . ? C55 B1 C37 108.06(18) . . ? C49 B1 C37 110.81(18) . . ? C43 B1 C37 111.35(18) . . ? C79 B2 C73 110.72(19) . . ? C79 B2 C61 109.00(18) . . ? C73 B2 C61 107.36(19) . . ? C79 B2 C67 108.27(19) . . ? C73 B2 C67 109.89(18) . . ? C61 B2 C67 111.61(19) . . ? O2 C1 C3 108.63(19) . . ? O2 C1 C2 110.57(19) . . ? C3 C1 C2 110.4(2) . . ? O2 C1 C4 105.43(19) . . ? C3 C1 C4 110.6(2) . . ? C2 C1 C4 111.1(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C7 109.46(19) . . ? O3 C5 C6 105.08(19) . . ? C7 C5 C6 111.2(2) . . ? O3 C5 C8 110.51(18) . . ? C7 C5 C8 110.6(2) . . ? C6 C5 C8 109.8(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 C11 110.0(2) . . ? O4 C9 C12 109.9(2) . . ? C11 C9 C12 110.4(2) . . ? O4 C9 C10 104.8(2) . . ? C11 C9 C10 111.2(2) . . ? C12 C9 C10 110.4(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 C14 104.99(17) . . ? O5 C13 H13A 110.7 . . ? C14 C13 H13A 110.7 . . ? O5 C13 H13B 110.7 . . ? C14 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C13 C14 C15 101.8(2) . . ? C13 C14 H14A 111.4 . . ? C15 C14 H14A 111.4 . . ? C13 C14 H14B 111.4 . . ? C15 C14 H14B 111.4 . . ? H14A C14 H14B 109.3 . . ? C16 C15 C14 102.42(19) . . ? C16 C15 H15A 111.3 . . ? C14 C15 H15A 111.3 . . ? C16 C15 H15B 111.3 . . ? C14 C15 H15B 111.3 . . ? H15A C15 H15B 109.2 . . ? O5 C16 C15 106.33(18) . . ? O5 C16 H16A 110.5 . . ? C15 C16 H16A 110.5 . . ? O5 C16 H16B 110.5 . . ? C15 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? O6 C17 C18 103.40(18) . . ? O6 C17 H17A 111.1 . . ? C18 C17 H17A 111.1 . . ? O6 C17 H17B 111.1 . . ? C18 C17 H17B 111.1 . . ? H17A C17 H17B 109.0 . . ? C17 C18 C19 104.18(19) . . ? C17 C18 H18A 110.9 . . ? C19 C18 H18A 110.9 . . ? C17 C18 H18B 110.9 . . ? C19 C18 H18B 110.9 . . ? H18A C18 H18B 108.9 . . ? C20 C19 C18 104.60(19) . . ? C20 C19 H19A 110.8 . . ? C18 C19 H19A 110.8 . . ? C20 C19 H19B 110.8 . . ? C18 C19 H19B 110.8 . . ? H19A C19 H19B 108.9 . . ? O6 C20 C19 104.88(19) . . ? O6 C20 H20A 110.8 . . ? C19 C20 H20A 110.8 . . ? O6 C20 H20B 110.8 . . ? C19 C20 H20B 110.8 . . ? H20A C20 H20B 108.8 . . ? O7 C21 C22 105.40(19) . . ? O7 C21 H21A 110.7 . . ? C22 C21 H21A 110.7 . . ? O7 C21 H21B 110.7 . . ? C22 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C21 C22 C23 103.0(2) . . ? C21 C22 H22A 111.2 . . ? C23 C22 H22A 111.2 . . ? C21 C22 H22B 111.2 . . ? C23 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? C24 C23 C22 102.5(2) . . ? C24 C23 H23A 111.3 . . ? C22 C23 H23A 111.3 . . ? C24 C23 H23B 111.3 . . ? C22 C23 H23B 111.3 . . ? H23A C23 H23B 109.2 . . ? O7 C24 C23 105.35(18) . . ? O7 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? O7 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? O8 C25 C26 105.66(18) . . ? O8 C25 H25A 110.6 . . ? C26 C25 H25A 110.6 . . ? O8 C25 H25B 110.6 . . ? C26 C25 H25B 110.6 . . ? H25A C25 H25B 108.7 . . ? C25 C26 C27 104.5(2) . . ? C25 C26 H26A 110.9 . . ? C27 C26 H26A 110.9 . . ? C25 C26 H26B 110.9 . . ? C27 C26 H26B 110.9 . . ? H26A C26 H26B 108.9 . . ? C28 C27 C26 105.2(2) . . ? C28 C27 H27A 110.7 . . ? C26 C27 H27A 110.7 . . ? C28 C27 H27B 110.7 . . ? C26 C27 H27B 110.7 . . ? H27A C27 H27B 108.8 . . ? O8 C28 C27 104.06(19) . . ? O8 C28 H28A 110.9 . . ? C27 C28 H28A 110.9 . . ? O8 C28 H28B 110.9 . . ? C27 C28 H28B 110.9 . . ? H28A C28 H28B 109.0 . . ? O9 C29 C30 105.4(2) . . ? O9 C29 H29A 110.7 . . ? C30 C29 H29A 110.7 . . ? O9 C29 H29B 110.7 . . ? C30 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C31 C30 C29 104.8(2) . . ? C31 C30 H30A 110.8 . . ? C29 C30 H30A 110.8 . . ? C31 C30 H30B 110.8 . . ? C29 C30 H30B 110.8 . . ? H30A C30 H30B 108.9 . . ? C32 C31 C30 106.6(2) . . ? C32 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? C32 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? O9 C32 C31 107.0(2) . . ? O9 C32 H32A 110.3 . . ? C31 C32 H32A 110.3 . . ? O9 C32 H32B 110.3 . . ? C31 C32 H32B 110.3 . . ? H32A C32 H32B 108.6 . . ? O10 C33 C34 106.82(19) . . ? O10 C33 H33A 110.4 . . ? C34 C33 H33A 110.4 . . ? O10 C33 H33B 110.4 . . ? C34 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? C33 C34 C35 102.2(2) . . ? C33 C34 H34A 111.3 . . ? C35 C34 H34A 111.3 . . ? C33 C34 H34B 111.3 . . ? C35 C34 H34B 111.3 . . ? H34A C34 H34B 109.2 . . ? C36 C35 C34 100.8(2) . . ? C36 C35 H35A 111.6 . . ? C34 C35 H35A 111.6 . . ? C36 C35 H35B 111.6 . . ? C34 C35 H35B 111.6 . . ? H35A C35 H35B 109.4 . . ? O10 C36 C35 104.49(19) . . ? O10 C36 H36A 110.9 . . ? C35 C36 H36A 110.9 . . ? O10 C36 H36B 110.9 . . ? C35 C36 H36B 110.9 . . ? H36A C36 H36B 108.9 . . ? C42 C37 C38 114.1(2) . . ? C42 C37 B1 124.8(2) . . ? C38 C37 B1 121.1(2) . . ? C39 C38 C37 123.7(2) . . ? C39 C38 H38 118.2 . . ? C37 C38 H38 118.2 . . ? C40 C39 C38 120.3(2) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 118.2(2) . . ? C41 C40 H40 120.9 . . ? C39 C40 H40 120.9 . . ? C40 C41 C42 120.7(2) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C41 C42 C37 123.0(2) . . ? C41 C42 H42 118.5 . . ? C37 C42 H42 118.5 . . ? C48 C43 C44 115.1(2) . . ? C48 C43 B1 124.0(2) . . ? C44 C43 B1 120.77(19) . . ? C45 C44 C43 123.3(2) . . ? C45 C44 H44 118.3 . . ? C43 C44 H44 118.3 . . ? C46 C45 C44 119.7(2) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 119.0(2) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C46 C47 C48 120.4(2) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C47 C48 C43 122.5(2) . . ? C47 C48 H48 118.8 . . ? C43 C48 H48 118.8 . . ? C54 C49 C50 114.7(2) . . ? C54 C49 B1 124.7(2) . . ? C50 C49 B1 120.6(2) . . ? C51 C50 C49 123.5(2) . . ? C51 C50 H50 118.3 . . ? C49 C50 H50 118.3 . . ? C52 C51 C50 119.8(2) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C53 C52 C51 118.7(2) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? C52 C53 C54 121.0(2) . . ? C52 C53 H53 119.5 . . ? C54 C53 H53 119.5 . . ? C53 C54 C49 122.4(2) . . ? C53 C54 H54 118.8 . . ? C49 C54 H54 118.8 . . ? C56 C55 C60 115.0(2) . . ? C56 C55 B1 124.8(2) . . ? C60 C55 B1 120.1(2) . . ? C57 C56 C55 122.4(2) . . ? C57 C56 H56 118.8 . . ? C55 C56 H56 118.8 . . ? C58 C57 C56 120.7(2) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? C59 C58 C57 118.4(2) . . ? C59 C58 H58 120.8 . . ? C57 C58 H58 120.8 . . ? C58 C59 C60 120.2(2) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C59 C60 C55 123.3(2) . . ? C59 C60 H60 118.4 . . ? C55 C60 H60 118.4 . . ? C62 C61 C66 114.9(2) . . ? C62 C61 B2 121.9(2) . . ? C66 C61 B2 123.1(2) . . ? C61 C62 C63 123.2(2) . . ? C61 C62 H62 118.4 . . ? C63 C62 H62 118.4 . . ? C64 C63 C62 119.9(3) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C65 C64 C63 119.1(2) . . ? C65 C64 H64 120.5 . . ? C63 C64 H64 120.5 . . ? C64 C65 C66 120.4(3) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C65 C66 C61 122.5(3) . . ? C65 C66 H66 118.7 . . ? C61 C66 H66 118.7 . . ? C72 C67 C68 114.5(2) . . ? C72 C67 B2 123.2(2) . . ? C68 C67 B2 122.2(2) . . ? C69 C68 C67 122.7(2) . . ? C69 C68 H68 118.6 . . ? C67 C68 H68 118.6 . . ? C70 C69 C68 120.7(2) . . ? C70 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? C69 C70 C71 118.4(2) . . ? C69 C70 H70 120.8 . . ? C71 C70 H70 120.8 . . ? C70 C71 C72 120.4(2) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C71 C72 C67 123.3(2) . . ? C71 C72 H72 118.4 . . ? C67 C72 H72 118.4 . . ? C74 C73 C78 114.7(2) . . ? C74 C73 B2 122.8(2) . . ? C78 C73 B2 122.1(2) . . ? C75 C74 C73 122.8(2) . . ? C75 C74 H74 118.6 . . ? C73 C74 H74 118.6 . . ? C76 C75 C74 120.5(2) . . ? C76 C75 H75 119.7 . . ? C74 C75 H75 119.7 . . ? C77 C76 C75 118.9(2) . . ? C77 C76 H76 120.6 . . ? C75 C76 H76 120.6 . . ? C76 C77 C78 120.2(3) . . ? C76 C77 H77 119.9 . . ? C78 C77 H77 119.9 . . ? C77 C78 C73 122.9(2) . . ? C77 C78 H78 118.5 . . ? C73 C78 H78 118.5 . . ? C84 C79 C80 114.7(2) . . ? C84 C79 B2 123.1(2) . . ? C80 C79 B2 122.1(2) . . ? C81 C80 C79 122.5(2) . . ? C81 C80 H80 118.7 . . ? C79 C80 H80 118.7 . . ? C82 C81 C80 120.7(2) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? C83 C82 C81 119.1(2) . . ? C83 C82 H82 120.4 . . ? C81 C82 H82 120.4 . . ? C82 C83 C84 119.7(2) . . ? C82 C83 H83 120.2 . . ? C84 C83 H83 120.2 . . ? C83 C84 C79 123.3(2) . . ? C83 C84 H84 118.4 . . ? C79 C84 H84 118.4 . . ? O11 C85 C86 107.3(2) . . ? O11 C85 H85A 110.3 . . ? C86 C85 H85A 110.3 . . ? O11 C85 H85B 110.3 . . ? C86 C85 H85B 110.3 . . ? H85A C85 H85B 108.5 . . ? C87 C86 C85 101.0(2) . . ? C87 C86 H86A 111.6 . . ? C85 C86 H86A 111.6 . . ? C87 C86 H86B 111.6 . . ? C85 C86 H86B 111.6 . . ? H86A C86 H86B 109.4 . . ? C88 C87 C86 102.4(3) . . ? C88 C87 H87A 111.3 . . ? C86 C87 H87A 111.3 . . ? C88 C87 H87B 111.3 . . ? C86 C87 H87B 111.3 . . ? H87A C87 H87B 109.2 . . ? O11 C88 C87 106.8(3) . . ? O11 C88 H88A 110.4 . . ? C87 C88 H88A 110.4 . . ? O11 C88 H88B 110.4 . . ? C87 C88 H88B 110.4 . . ? H88A C88 H88B 108.6 . . ? 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 O2 Si O1 Y 176.1(3) . . . . ? O4 Si O1 Y -64.5(3) . . . . ? O3 Si O1 Y 52.6(3) . . . . ? O8 Y O1 Si -79.0(3) . . . . ? O6 Y O1 Si 65.6(3) . . . . ? O7 Y O1 Si -5.3(3) . . . . ? O10 Y O1 Si -25(3) . . . . ? O9 Y O1 Si -152.3(3) . . . . ? O5 Y O1 Si 136.5(3) . . . . ? O1 Si O2 C1 -46.8(2) . . . . ? O4 Si O2 C1 -169.61(19) . . . . ? O3 Si O2 C1 72.7(2) . . . . ? O1 Si O3 C5 -169.63(19) . . . . ? O2 Si O3 C5 66.1(2) . . . . ? O4 Si O3 C5 -50.1(2) . . . . ? O1 Si O4 C9 -107.0(2) . . . . ? O2 Si O4 C9 17.1(2) . . . . ? O3 Si O4 C9 137.7(2) . . . . ? O1 Y O5 C16 26.71(15) . . . . ? O8 Y O5 C16 -66.16(18) . . . . ? O6 Y O5 C16 123.36(15) . . . . ? O7 Y O5 C16 119.32(15) . . . . ? O10 Y O5 C16 -153.70(15) . . . . ? O9 Y O5 C16 -71.20(15) . . . . ? O1 Y O5 C13 -143.94(18) . . . . ? O8 Y O5 C13 123.18(18) . . . . ? O6 Y O5 C13 -47.30(17) . . . . ? O7 Y O5 C13 -51.3(2) . . . . ? O10 Y O5 C13 35.65(18) . . . . ? O9 Y O5 C13 118.15(18) . . . . ? O1 Y O6 C17 -133.59(16) . . . . ? O8 Y O6 C17 -32.6(2) . . . . ? O7 Y O6 C17 -44.63(16) . . . . ? O10 Y O6 C17 45.13(16) . . . . ? O9 Y O6 C17 116.45(16) . . . . ? O5 Y O6 C17 138.02(17) . . . . ? O1 Y O6 C20 29.30(17) . . . . ? O8 Y O6 C20 130.31(16) . . . . ? O7 Y O6 C20 118.27(17) . . . . ? O10 Y O6 C20 -151.98(17) . . . . ? O9 Y O6 C20 -80.66(18) . . . . ? O5 Y O6 C20 -59.09(16) . . . . ? O1 Y O7 C21 -153.96(18) . . . . ? O8 Y O7 C21 -63.07(18) . . . . ? O6 Y O7 C21 109.58(18) . . . . ? O10 Y O7 C21 25.61(18) . . . . ? O9 Y O7 C21 -48.4(2) . . . . ? O5 Y O7 C21 113.61(18) . . . . ? O1 Y O7 C24 23.36(15) . . . . ? O8 Y O7 C24 114.25(15) . . . . ? O6 Y O7 C24 -73.11(15) . . . . ? O10 Y O7 C24 -157.07(15) . . . . ? O9 Y O7 C24 128.89(15) . . . . ? O5 Y O7 C24 -69.07(17) . . . . ? O1 Y O8 C25 -140.09(19) . . . . ? O6 Y O8 C25 117.21(18) . . . . ? O7 Y O8 C25 129.06(19) . . . . ? O10 Y O8 C25 40.94(19) . . . . ? O9 Y O8 C25 -42.42(18) . . . . ? O5 Y O8 C25 -47.4(2) . . . . ? O1 Y O8 C28 37.53(16) . . . . ? O6 Y O8 C28 -65.17(19) . . . . ? O7 Y O8 C28 -53.32(16) . . . . ? O10 Y O8 C28 -141.44(16) . . . . ? O9 Y O8 C28 135.20(16) . . . . ? O5 Y O8 C28 130.22(15) . . . . ? O1 Y O9 C29 -145.33(18) . . . . ? O8 Y O9 C29 125.76(18) . . . . ? O6 Y O9 C29 -35.8(2) . . . . ? O7 Y O9 C29 111.08(18) . . . . ? O10 Y O9 C29 35.69(17) . . . . ? O5 Y O9 C29 -57.29(17) . . . . ? O1 Y O9 C32 30.36(18) . . . . ? O8 Y O9 C32 -58.55(18) . . . . ? O6 Y O9 C32 139.90(17) . . . . ? O7 Y O9 C32 -73.2(2) . . . . ? O10 Y O9 C32 -148.62(18) . . . . ? O5 Y O9 C32 118.40(18) . . . . ? O1 Y O10 C33 138(2) . . . . ? O8 Y O10 C33 -167.49(17) . . . . ? O6 Y O10 C33 47.66(17) . . . . ? O7 Y O10 C33 118.74(17) . . . . ? O9 Y O10 C33 -94.17(17) . . . . ? O5 Y O10 C33 -23.01(17) . . . . ? O1 Y O10 C36 -46(3) . . . . ? O8 Y O10 C36 7.95(17) . . . . ? O6 Y O10 C36 -136.90(17) . . . . ? O7 Y O10 C36 -65.82(17) . . . . ? O9 Y O10 C36 81.27(17) . . . . ? O5 Y O10 C36 152.43(17) . . . . ? Si O2 C1 C3 83.2(2) . . . . ? Si O2 C1 C2 -38.1(3) . . . . ? Si O2 C1 C4 -158.23(17) . . . . ? Si O3 C5 C7 74.6(3) . . . . ? Si O3 C5 C6 -165.90(17) . . . . ? Si O3 C5 C8 -47.5(3) . . . . ? Si O4 C9 C11 53.9(3) . . . . ? Si O4 C9 C12 -67.8(3) . . . . ? Si O4 C9 C10 173.54(18) . . . . ? C16 O5 C13 C14 -19.5(2) . . . . ? Y O5 C13 C14 151.93(15) . . . . ? O5 C13 C14 C15 36.6(2) . . . . ? C13 C14 C15 C16 -39.5(2) . . . . ? C13 O5 C16 C15 -5.9(2) . . . . ? Y O5 C16 C15 -178.62(15) . . . . ? C14 C15 C16 O5 28.5(2) . . . . ? C20 O6 C17 C18 43.9(2) . . . . ? Y O6 C17 C18 -150.29(15) . . . . ? O6 C17 C18 C19 -31.4(2) . . . . ? C17 C18 C19 C20 8.0(3) . . . . ? C17 O6 C20 C19 -38.8(2) . . . . ? Y O6 C20 C19 155.04(15) . . . . ? C18 C19 C20 O6 18.2(3) . . . . ? C24 O7 C21 C22 -12.0(2) . . . . ? Y O7 C21 C22 165.59(15) . . . . ? O7 C21 C22 C23 31.5(3) . . . . ? C21 C22 C23 C24 -38.5(3) . . . . ? C21 O7 C24 C23 -12.5(2) . . . . ? Y O7 C24 C23 169.69(14) . . . . ? C22 C23 C24 O7 31.6(2) . . . . ? C28 O8 C25 C26 -36.3(2) . . . . ? Y O8 C25 C26 141.66(16) . . . . ? O8 C25 C26 C27 17.6(3) . . . . ? C25 C26 C27 C28 6.9(3) . . . . ? C25 O8 C28 C27 40.5(2) . . . . ? Y O8 C28 C27 -137.66(16) . . . . ? C26 C27 C28 O8 -28.8(3) . . . . ? C32 O9 C29 C30 -33.4(3) . . . . ? Y O9 C29 C30 143.07(18) . . . . ? O9 C29 C30 C31 25.8(3) . . . . ? C29 C30 C31 C32 -8.6(4) . . . . ? C29 O9 C32 C31 28.1(3) . . . . ? Y O9 C32 C31 -148.3(2) . . . . ? C30 C31 C32 O9 -11.6(4) . . . . ? C36 O10 C33 C34 -1.7(3) . . . . ? Y O10 C33 C34 174.38(16) . . . . ? O10 C33 C34 C35 26.8(3) . . . . ? C33 C34 C35 C36 -41.0(3) . . . . ? C33 O10 C36 C35 -24.9(2) . . . . ? Y O10 C36 C35 158.91(16) . . . . ? C34 C35 C36 O10 40.7(3) . . . . ? C55 B1 C37 C42 -138.4(2) . . . . ? C49 B1 C37 C42 -18.1(3) . . . . ? C43 B1 C37 C42 102.5(2) . . . . ? C55 B1 C37 C38 41.0(3) . . . . ? C49 B1 C37 C38 161.28(19) . . . . ? C43 B1 C37 C38 -78.1(3) . . . . ? C42 C37 C38 C39 -0.8(3) . . . . ? B1 C37 C38 C39 179.7(2) . . . . ? C37 C38 C39 C40 0.8(4) . . . . ? C38 C39 C40 C41 -0.2(4) . . . . ? C39 C40 C41 C42 -0.4(4) . . . . ? C40 C41 C42 C37 0.4(4) . . . . ? C38 C37 C42 C41 0.2(3) . . . . ? B1 C37 C42 C41 179.7(2) . . . . ? C55 B1 C43 C48 -89.9(2) . . . . ? C49 B1 C43 C48 151.0(2) . . . . ? C37 B1 C43 C48 28.9(3) . . . . ? C55 B1 C43 C44 85.3(2) . . . . ? C49 B1 C43 C44 -33.8(3) . . . . ? C37 B1 C43 C44 -155.8(2) . . . . ? C48 C43 C44 C45 0.2(3) . . . . ? B1 C43 C44 C45 -175.4(2) . . . . ? C43 C44 C45 C46 -0.4(4) . . . . ? C44 C45 C46 C47 0.5(4) . . . . ? C45 C46 C47 C48 -0.6(4) . . . . ? C46 C47 C48 C43 0.4(4) . . . . ? C44 C43 C48 C47 -0.2(3) . . . . ? B1 C43 C48 C47 175.3(2) . . . . ? C55 B1 C49 C54 7.9(3) . . . . ? C43 B1 C49 C54 126.3(2) . . . . ? C37 B1 C49 C54 -111.3(2) . . . . ? C55 B1 C49 C50 -171.40(19) . . . . ? C43 B1 C49 C50 -53.0(3) . . . . ? C37 B1 C49 C50 69.3(3) . . . . ? C54 C49 C50 C51 0.7(3) . . . . ? B1 C49 C50 C51 -179.9(2) . . . . ? C49 C50 C51 C52 -0.6(4) . . . . ? C50 C51 C52 C53 0.0(4) . . . . ? C51 C52 C53 C54 0.5(4) . . . . ? C52 C53 C54 C49 -0.3(4) . . . . ? C50 C49 C54 C53 -0.2(3) . . . . ? B1 C49 C54 C53 -179.6(2) . . . . ? C49 B1 C55 C56 99.6(2) . . . . ? C43 B1 C55 C56 -18.6(3) . . . . ? C37 B1 C55 C56 -139.5(2) . . . . ? C49 B1 C55 C60 -77.1(3) . . . . ? C43 B1 C55 C60 164.8(2) . . . . ? C37 B1 C55 C60 43.9(3) . . . . ? C60 C55 C56 C57 1.4(3) . . . . ? B1 C55 C56 C57 -175.3(2) . . . . ? C55 C56 C57 C58 -0.3(4) . . . . ? C56 C57 C58 C59 -0.8(4) . . . . ? C57 C58 C59 C60 0.7(4) . . . . ? C58 C59 C60 C55 0.5(4) . . . . ? C56 C55 C60 C59 -1.5(3) . . . . ? B1 C55 C60 C59 175.4(2) . . . . ? C79 B2 C61 C62 -88.5(3) . . . . ? C73 B2 C61 C62 31.5(3) . . . . ? C67 B2 C61 C62 152.0(2) . . . . ? C79 B2 C61 C66 88.3(3) . . . . ? C73 B2 C61 C66 -151.8(2) . . . . ? C67 B2 C61 C66 -31.3(3) . . . . ? C66 C61 C62 C63 0.6(4) . . . . ? B2 C61 C62 C63 177.6(2) . . . . ? C61 C62 C63 C64 0.2(4) . . . . ? C62 C63 C64 C65 -1.1(4) . . . . ? C63 C64 C65 C66 1.1(4) . . . . ? C64 C65 C66 C61 -0.2(4) . . . . ? C62 C61 C66 C65 -0.6(4) . . . . ? B2 C61 C66 C65 -177.5(2) . . . . ? C79 B2 C67 C72 23.6(3) . . . . ? C73 B2 C67 C72 -97.4(2) . . . . ? C61 B2 C67 C72 143.6(2) . . . . ? C79 B2 C67 C68 -157.5(2) . . . . ? C73 B2 C67 C68 81.4(3) . . . . ? C61 B2 C67 C68 -37.6(3) . . . . ? C72 C67 C68 C69 0.9(3) . . . . ? B2 C67 C68 C69 -178.0(2) . . . . ? C67 C68 C69 C70 -0.4(4) . . . . ? C68 C69 C70 C71 0.0(4) . . . . ? C69 C70 C71 C72 -0.1(4) . . . . ? C70 C71 C72 C67 0.6(4) . . . . ? C68 C67 C72 C71 -1.0(3) . . . . ? B2 C67 C72 C71 177.9(2) . . . . ? C79 B2 C73 C74 -148.8(2) . . . . ? C61 B2 C73 C74 92.3(3) . . . . ? C67 B2 C73 C74 -29.3(3) . . . . ? C79 B2 C73 C78 39.0(3) . . . . ? C61 B2 C73 C78 -79.9(3) . . . . ? C67 B2 C73 C78 158.6(2) . . . . ? C78 C73 C74 C75 0.8(3) . . . . ? B2 C73 C74 C75 -171.9(2) . . . . ? C73 C74 C75 C76 0.5(4) . . . . ? C74 C75 C76 C77 -1.0(4) . . . . ? C75 C76 C77 C78 0.2(4) . . . . ? C76 C77 C78 C73 1.2(4) . . . . ? C74 C73 C78 C77 -1.7(3) . . . . ? B2 C73 C78 C77 171.1(2) . . . . ? C73 B2 C79 C84 36.0(3) . . . . ? C61 B2 C79 C84 153.9(2) . . . . ? C67 B2 C79 C84 -84.5(3) . . . . ? C73 B2 C79 C80 -148.1(2) . . . . ? C61 B2 C79 C80 -30.3(3) . . . . ? C67 B2 C79 C80 91.3(2) . . . . ? C84 C79 C80 C81 0.2(3) . . . . ? B2 C79 C80 C81 -176.0(2) . . . . ? C79 C80 C81 C82 -0.3(4) . . . . ? C80 C81 C82 C83 0.0(4) . . . . ? C81 C82 C83 C84 0.4(4) . . . . ? C82 C83 C84 C79 -0.5(4) . . . . ? C80 C79 C84 C83 0.2(3) . . . . ? B2 C79 C84 C83 176.4(2) . . . . ? C88 O11 C85 C86 -7.6(4) . . . . ? O11 C85 C86 C87 28.0(3) . . . . ? C85 C86 C87 C88 -36.5(3) . . . . ? C85 O11 C88 C87 -16.5(4) . . . . ? C86 C87 C88 O11 34.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.61 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.994 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.066 #===END #===============================================================