# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1793 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Edelmann, Frank T. (Prof.) Chemisches Institut Otto-von-Guericke-Universit\"at Magdeburg Universit\"atsplatz 2 D-39106 Magdeburg Germany ; _publ_contact_author_phone '049 391 67-18327' _publ_contact_author_fax '049 391 67-11933' _publ_contact_author_email frank.edelmann@vst.uni-magdeburg.de _publ_requested_journal 'J. Organomet. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in 'J. Organomet. Chem.' ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'Silsesquioxane Chemistry 4. Silsesquioxane Complexes of Titanium(III) and Titanium(IV).' ; loop_ _publ_author_name _publ_author_address 'Giessmann, Stephan' ; Chemisches Institut Otto-von-Guericke-Universit\"at Magdeburg Universit\"atsplatz 2 D-39106 Magdeburg Germany ; 'Fischer, Axel K.' ; Chemisches Institut Otto-von-Guericke-Universit\"at Magdeburg Universit\"atsplatz 2 D-39106 Magdeburg Germany ; 'Edelmann, Frank T.' ; Chemisches Institut Otto-von-Guericke-Universit\"at Magdeburg Universit\"atsplatz 2 D-39106 Magdeburg Germany ; #============================================================================== data_fulti _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71.50 H129 O12 Si9 Ti' _chemical_formula_weight 1481.46 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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0870(6) _cell_length_b 26.1626(3) _cell_length_c 24.4490(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.616(3) _cell_angle_gamma 90.00 _cell_volume 8297.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 28.3 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.88 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker AXS SMART CCD System' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54689 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.34 _reflns_number_total 20363 _reflns_number_gt 14323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART CCD System' _computing_cell_refinement 'Bruker AXS SMART CCD System' _computing_data_reduction 'Bruker AXS SMART CCD System' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP5' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+1.1511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20363 _refine_ls_number_parameters 844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1532 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _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 Ti Ti 0.25038(3) 0.870670(16) 0.485225(15) 0.02364(10) Uani 1 1 d . . . Si1 Si 0.07268(5) 0.84922(2) 0.36615(2) 0.02227(13) Uani 1 1 d . . . Si2 Si 0.09071(5) 0.75834(2) 0.28387(2) 0.02155(13) Uani 1 1 d . . . Si3 Si -0.01407(5) 0.82720(2) 0.18665(2) 0.02126(13) Uani 1 1 d . . . Si4 Si 0.04551(5) 0.92077(2) 0.26070(2) 0.02125(13) Uani 1 1 d . . . Si5 Si 0.47660(5) 0.72925(3) 0.29974(3) 0.03262(16) Uani 1 1 d . . . Si6 Si 0.27765(5) 0.74841(2) 0.21795(2) 0.02224(13) Uani 1 1 d . . . Si7 Si 0.19472(5) 0.83727(2) 0.13896(2) 0.02282(13) Uani 1 1 d . . . Si8 Si 0.22052(5) 0.94724(2) 0.18811(2) 0.02425(14) Uani 1 1 d . . . Si9 Si 0.45754(6) 0.95252(3) 0.22521(3) 0.04186(19) Uani 1 1 d . . . O1 O 0.09892(13) 0.79502(7) 0.33712(6) 0.0315(4) Uani 1 1 d . . . O2 O 0.01598(12) 0.78276(6) 0.23217(6) 0.0277(3) Uani 1 1 d . . . O3 O -0.02004(12) 0.88165(6) 0.21768(6) 0.0261(3) Uani 1 1 d . . . O4 O 0.07720(13) 0.89363(7) 0.31953(6) 0.0318(4) Uani 1 1 d . . . O5 O 0.20584(12) 0.75105(6) 0.26723(6) 0.0260(3) Uani 1 1 d . . . O6 O 0.07411(12) 0.82988(7) 0.14607(6) 0.0297(4) Uani 1 1 d . . . O7 O 0.15042(13) 0.93574(7) 0.23651(6) 0.0296(4) Uani 1 1 d . . . O8 O 0.39662(12) 0.74408(7) 0.24482(6) 0.0308(4) Uani 1 1 d . . . O9 O 0.26539(13) 0.80088(6) 0.18238(6) 0.0287(4) Uani 1 1 d . . . O10 O 0.22910(13) 0.89599(6) 0.15135(6) 0.0306(4) Uani 1 1 d . . . O11 O 0.33368(13) 0.96385(7) 0.21677(7) 0.0369(4) Uani 1 1 d . . . O12 O 0.15452(12) 0.85968(6) 0.41935(6) 0.0261(3) Uani 1 1 d . . . C11 C -0.06336(17) 0.84456(9) 0.38174(8) 0.0235(4) Uani 1 1 d . . . H11 H -0.0694 0.8107 0.4001 0.028 Uiso 1 1 calc R . . C12 C -0.09373(19) 0.88523(10) 0.42202(9) 0.0308(5) Uani 1 1 d . . . H12A H -0.0458 0.8834 0.4569 0.037 Uiso 1 1 calc R . . H12B H -0.0873 0.9196 0.4059 0.037 Uiso 1 1 calc R . . C13 C -0.2046(2) 0.87752(12) 0.43444(10) 0.0391(6) Uani 1 1 d . . . H13A H -0.2092 0.8448 0.4543 0.047 Uiso 1 1 calc R . . H13B H -0.2229 0.9054 0.4587 0.047 Uiso 1 1 calc R . . C14 C -0.2810(2) 0.87693(12) 0.38154(12) 0.0433(7) Uani 1 1 d . . . H14A H -0.2817 0.9109 0.3636 0.052 Uiso 1 1 calc R . . H14B H -0.3511 0.8700 0.3907 0.052 Uiso 1 1 calc R . . C15 C -0.2518(2) 0.83605(11) 0.34157(11) 0.0372(6) Uani 1 1 d . . . H15A H -0.2578 0.8018 0.3580 0.045 Uiso 1 1 calc R . . H15B H -0.3000 0.8376 0.3068 0.045 Uiso 1 1 calc R . . C16 C -0.14217(18) 0.84402(10) 0.32913(9) 0.0280(5) Uani 1 1 d . . . H16A H -0.1383 0.8769 0.3094 0.034 Uiso 1 1 calc R . . H16B H -0.1242 0.8163 0.3045 0.034 Uiso 1 1 calc R . . C21 C 0.03518(18) 0.69523(9) 0.29799(10) 0.0284(5) Uani 1 1 d . . . H21 H 0.0399 0.6737 0.2646 0.034 Uiso 1 1 calc R . . C22 C -0.0800(2) 0.69791(11) 0.30495(12) 0.0410(6) Uani 1 1 d . . . H22A H -0.0887 0.7192 0.3375 0.049 Uiso 1 1 calc R . . H22B H -0.1187 0.7143 0.2720 0.049 Uiso 1 1 calc R . . C23 C -0.1241(2) 0.64481(11) 0.31247(14) 0.0498(8) Uani 1 1 d . . . H23A H -0.1971 0.6479 0.3186 0.060 Uiso 1 1 calc R . . H23B H -0.1217 0.6246 0.2785 0.060 Uiso 1 1 calc R . . C24 C -0.0641(2) 0.61741(12) 0.36082(14) 0.0516(8) Uani 1 1 d . . . H24A H -0.0922 0.5825 0.3634 0.062 Uiso 1 1 calc R . . H24B H -0.0727 0.6358 0.3953 0.062 Uiso 1 1 calc R . . C25 C 0.0494(2) 0.61398(11) 0.35535(13) 0.0455(7) Uani 1 1 d . . . H25A H 0.0589 0.5918 0.3236 0.055 Uiso 1 1 calc R . . H25B H 0.0866 0.5981 0.3890 0.055 Uiso 1 1 calc R . . C26 C 0.0955(2) 0.66684(10) 0.34697(11) 0.0350(6) Uani 1 1 d . . . H26A H 0.1681 0.6629 0.3405 0.042 Uiso 1 1 calc R . . H26B H 0.0947 0.6874 0.3809 0.042 Uiso 1 1 calc R . . C31 C -0.14026(18) 0.81408(9) 0.14540(9) 0.0252(5) Uani 1 1 d . . . H31 H -0.1347 0.7800 0.1275 0.030 Uiso 1 1 calc R . . C32 C -0.22914(19) 0.81051(11) 0.18020(10) 0.0339(6) Uani 1 1 d . . . H32A H -0.2147 0.7827 0.2076 0.041 Uiso 1 1 calc R . . H32B H -0.2338 0.8429 0.2006 0.041 Uiso 1 1 calc R . . C33 C -0.3324(2) 0.80011(12) 0.14464(12) 0.0438(7) Uani 1 1 d . . . H33A H -0.3305 0.7658 0.1276 0.053 Uiso 1 1 calc R . . H33B H -0.3881 0.8002 0.1683 0.053 Uiso 1 1 calc R . . C34 C -0.3556(2) 0.83997(12) 0.09962(11) 0.0450(7) Uani 1 1 d . . . H34A H -0.3641 0.8738 0.1165 0.054 Uiso 1 1 calc R . . H34B H -0.4211 0.8313 0.0763 0.054 Uiso 1 1 calc R . . C35 C -0.2687(2) 0.84241(12) 0.06396(10) 0.0409(6) Uani 1 1 d . . . H35A H -0.2838 0.8695 0.0358 0.049 Uiso 1 1 calc R . . H35B H -0.2645 0.8095 0.0445 0.049 Uiso 1 1 calc R . . C36 C -0.1655(2) 0.85346(11) 0.09875(10) 0.0361(6) Uani 1 1 d . . . H36A H -0.1673 0.8881 0.1150 0.043 Uiso 1 1 calc R . . H36B H -0.1102 0.8530 0.0747 0.043 Uiso 1 1 calc R . . C41 C -0.0345(2) 0.97793(10) 0.27131(14) 0.0471(7) Uani 1 1 d . . . H41 H -0.0535 0.9716 0.3090 0.057 Uiso 1 1 calc R . . C42 C -0.1391(2) 0.98120(11) 0.23668(13) 0.0430(7) Uani 1 1 d . . . H42A H -0.1783 0.9497 0.2421 0.052 Uiso 1 1 calc R . . H42B H -0.1294 0.9829 0.1972 0.052 Uiso 1 1 calc R . . C43 C -0.2019(2) 1.02720(12) 0.25059(17) 0.0591(9) Uani 1 1 d . . . H43A H -0.2579 1.0328 0.2198 0.071 Uiso 1 1 calc R . . H43B H -0.2345 1.0189 0.2838 0.071 Uiso 1 1 calc R . . C44 C -0.1447(3) 1.07494(12) 0.26074(18) 0.0673(11) Uani 1 1 d . . . H44A H -0.1371 1.0905 0.2246 0.081 Uiso 1 1 calc R . . H44B H -0.1870 1.0986 0.2800 0.081 Uiso 1 1 calc R . . C45 C -0.0427(2) 1.07181(11) 0.29280(14) 0.0510(8) Uani 1 1 d . . . H45A H -0.0511 1.0700 0.3324 0.061 Uiso 1 1 calc R . . H45B H -0.0049 1.1037 0.2871 0.061 Uiso 1 1 calc R . . C46 C 0.0224(2) 1.02693(10) 0.27914(14) 0.0474(7) Uani 1 1 d . . . H46A H 0.0523 1.0349 0.2450 0.057 Uiso 1 1 calc R . . H46B H 0.0803 1.0227 0.3093 0.057 Uiso 1 1 calc R . . C51 C 0.4275(3) 0.67127(13) 0.33193(14) 0.0671(11) Uani 1 1 d . . . H51A H 0.3566 0.6773 0.3391 0.080 Uiso 1 1 calc R . . H51B H 0.4713 0.6639 0.3668 0.080 Uiso 1 1 calc R . . H51C H 0.4289 0.6421 0.3069 0.080 Uiso 1 1 calc R . . C52 C 0.6032(2) 0.71743(13) 0.27655(15) 0.0587(9) Uani 1 1 d . . . H52A H 0.5974 0.6888 0.2504 0.070 Uiso 1 1 calc R . . H52B H 0.6539 0.7091 0.3085 0.070 Uiso 1 1 calc R . . H52C H 0.6254 0.7481 0.2584 0.070 Uiso 1 1 calc R . . C53 C 0.4851(2) 0.78228(12) 0.34968(11) 0.0473(7) Uani 1 1 d . . . H53A H 0.5159 0.8121 0.3340 0.057 Uiso 1 1 calc R . . H53B H 0.5282 0.7719 0.3838 0.057 Uiso 1 1 calc R . . H53C H 0.4159 0.7910 0.3578 0.057 Uiso 1 1 calc R . . C61 C 0.2401(2) 0.69242(10) 0.17295(10) 0.0323(5) Uani 1 1 d . . . H61 H 0.1679 0.6986 0.1552 0.039 Uiso 1 1 calc R . . C62 C 0.3068(3) 0.68609(11) 0.12602(10) 0.0445(7) Uani 1 1 d . . . H62A H 0.3065 0.7184 0.1049 0.053 Uiso 1 1 calc R . . H62B H 0.3788 0.6787 0.1419 0.053 Uiso 1 1 calc R . . C63 C 0.2661(3) 0.64260(13) 0.08706(12) 0.0621(10) Uani 1 1 d . . . H63A H 0.1968 0.6518 0.0683 0.075 Uiso 1 1 calc R . . H63B H 0.3123 0.6383 0.0585 0.075 Uiso 1 1 calc R . . C64 C 0.2594(3) 0.59258(12) 0.11749(12) 0.0559(9) Uani 1 1 d . . . H64A H 0.3299 0.5805 0.1309 0.067 Uiso 1 1 calc R . . H64B H 0.2259 0.5666 0.0916 0.067 Uiso 1 1 calc R . . C65 C 0.1988(2) 0.59763(12) 0.16615(14) 0.0526(8) Uani 1 1 d . . . H65A H 0.2038 0.5653 0.1874 0.063 Uiso 1 1 calc R . . H65B H 0.1252 0.6036 0.1523 0.063 Uiso 1 1 calc R . . C66 C 0.2394(2) 0.64168(10) 0.20412(11) 0.0360(6) Uani 1 1 d . . . H66A H 0.3103 0.6337 0.2214 0.043 Uiso 1 1 calc R . . H66B H 0.1956 0.6452 0.2340 0.043 Uiso 1 1 calc R . . C71 C 0.20911(19) 0.81890(10) 0.06737(9) 0.0304(5) Uani 1 1 d . . . H71 H 0.1937 0.7815 0.0645 0.036 Uiso 1 1 calc R . . C72 C 0.1315(2) 0.84464(14) 0.02414(10) 0.0495(8) Uani 1 1 d . . . H72A H 0.1446 0.8819 0.0245 0.059 Uiso 1 1 calc R . . H72B H 0.0610 0.8390 0.0335 0.059 Uiso 1 1 calc R . . C73 C 0.1385(3) 0.82362(17) -0.03360(11) 0.0671(11) Uani 1 1 d . . . H73A H 0.1176 0.7872 -0.0351 0.081 Uiso 1 1 calc R . . H73B H 0.0902 0.8426 -0.0609 0.081 Uiso 1 1 calc R . . C74 C 0.2463(3) 0.82819(17) -0.04864(12) 0.0673(10) Uani 1 1 d . . . H74A H 0.2630 0.8648 -0.0528 0.081 Uiso 1 1 calc R . . H74B H 0.2492 0.8112 -0.0846 0.081 Uiso 1 1 calc R . . C75 C 0.3258(3) 0.80440(17) -0.00569(12) 0.0669(11) Uani 1 1 d . . . H75A H 0.3955 0.8113 -0.0155 0.080 Uiso 1 1 calc R . . H75B H 0.3158 0.7669 -0.0058 0.080 Uiso 1 1 calc R . . C76 C 0.3190(2) 0.82517(13) 0.05249(10) 0.0422(7) Uani 1 1 d . . . H76A H 0.3382 0.8618 0.0541 0.051 Uiso 1 1 calc R . . H76B H 0.3682 0.8065 0.0796 0.051 Uiso 1 1 calc R . . C81 C 0.16399(19) 1.00023(9) 0.14348(9) 0.0276(5) Uani 1 1 d . . . H81 H 0.1567 1.0298 0.1686 0.033 Uiso 1 1 calc R . . C82 C 0.2343(2) 1.01849(11) 0.10189(11) 0.0393(6) Uani 1 1 d . . . H82A H 0.3037 1.0262 0.1216 0.047 Uiso 1 1 calc R . . H82B H 0.2415 0.9909 0.0749 0.047 Uiso 1 1 calc R . . C83 C 0.1904(3) 1.06621(12) 0.07134(12) 0.0495(8) Uani 1 1 d . . . H83A H 0.1900 1.0948 0.0979 0.059 Uiso 1 1 calc R . . H83B H 0.2352 1.0761 0.0435 0.059 Uiso 1 1 calc R . . C84 C 0.0811(3) 1.05732(13) 0.04271(12) 0.0564(9) Uani 1 1 d . . . H84A H 0.0529 1.0898 0.0264 0.068 Uiso 1 1 calc R . . H84B H 0.0828 1.0324 0.0124 0.068 Uiso 1 1 calc R . . C85 C 0.0114(2) 1.03739(12) 0.08246(12) 0.0491(7) Uani 1 1 d . . . H85A H -0.0569 1.0291 0.0619 0.059 Uiso 1 1 calc R . . H85B H 0.0015 1.0644 0.1096 0.059 Uiso 1 1 calc R . . C86 C 0.0559(2) 0.98971(11) 0.11299(11) 0.0385(6) Uani 1 1 d . . . H86A H 0.0595 0.9616 0.0863 0.046 Uiso 1 1 calc R . . H86B H 0.0098 0.9788 0.1398 0.046 Uiso 1 1 calc R . . C91 C 0.5155(3) 0.9971(2) 0.28039(15) 0.0957(17) Uani 1 1 d . . . H91A H 0.5005 1.0325 0.2688 0.115 Uiso 1 1 calc R . . H91B H 0.5903 0.9920 0.2869 0.115 Uiso 1 1 calc R . . H91C H 0.4862 0.9903 0.3145 0.115 Uiso 1 1 calc R . . C92 C 0.4800(4) 0.88595(19) 0.2457(3) 0.122(2) Uani 1 1 d . . . H92A H 0.4416 0.8780 0.2764 0.146 Uiso 1 1 calc R . . H92B H 0.5538 0.8805 0.2572 0.146 Uiso 1 1 calc R . . H92C H 0.4565 0.8636 0.2143 0.146 Uiso 1 1 calc R . . C93 C 0.5112(3) 0.96580(14) 0.16071(13) 0.0569(9) Uani 1 1 d . . . H93A H 0.4799 0.9427 0.1317 0.068 Uiso 1 1 calc R . . H93B H 0.5860 0.9605 0.1666 0.068 Uiso 1 1 calc R . . H93C H 0.4964 1.0013 0.1495 0.068 Uiso 1 1 calc R . . C101 C 0.29944(19) 0.94352(10) 0.43433(10) 0.0310(5) Uani 1 1 d . . . C102 C 0.3884(2) 0.92684(10) 0.46941(11) 0.0359(6) Uani 1 1 d . . . C103 C 0.3710(2) 0.93586(10) 0.52445(11) 0.0398(6) Uani 1 1 d . . . C104 C 0.2698(2) 0.95493(10) 0.52355(10) 0.0372(6) Uani 1 1 d . . . C105 C 0.22557(19) 0.96010(9) 0.46758(10) 0.0299(5) Uani 1 1 d . . . C106 C 0.2901(2) 0.94499(12) 0.37226(10) 0.0444(7) Uani 1 1 d . . . H10A H 0.2225 0.9588 0.3573 0.053 Uiso 1 1 calc R . . H10B H 0.2972 0.9103 0.3581 0.053 Uiso 1 1 calc R . . H10C H 0.3445 0.9668 0.3610 0.053 Uiso 1 1 calc R . . C107 C 0.4886(2) 0.91074(13) 0.45052(15) 0.0556(8) Uani 1 1 d . . . H10D H 0.5272 0.9411 0.4419 0.067 Uiso 1 1 calc R . . H10E H 0.4743 0.8894 0.4175 0.067 Uiso 1 1 calc R . . H10F H 0.5295 0.8913 0.4799 0.067 Uiso 1 1 calc R . . C108 C 0.4559(3) 0.93635(13) 0.57271(14) 0.0652(10) Uani 1 1 d . . . H10G H 0.5050 0.9636 0.5676 0.078 Uiso 1 1 calc R . . H10H H 0.4916 0.9033 0.5750 0.078 Uiso 1 1 calc R . . H10I H 0.4261 0.9424 0.6069 0.078 Uiso 1 1 calc R . . C109 C 0.2203(3) 0.97321(12) 0.57229(12) 0.0630(10) Uani 1 1 d . . . H10J H 0.2509 0.9552 0.6056 0.076 Uiso 1 1 calc R . . H10K H 0.1460 0.9663 0.5658 0.076 Uiso 1 1 calc R . . H10L H 0.2316 1.0100 0.5772 0.076 Uiso 1 1 calc R . . C110 C 0.1204(2) 0.98135(11) 0.44805(13) 0.0450(7) Uani 1 1 d . . . H11A H 0.1240 1.0187 0.4469 0.054 Uiso 1 1 calc R . . H11B H 0.0724 0.9709 0.4735 0.054 Uiso 1 1 calc R . . H11C H 0.0963 0.9682 0.4110 0.054 Uiso 1 1 calc R . . C111 C 0.17864(19) 0.79103(9) 0.50968(9) 0.0292(5) Uani 1 1 d . . . C112 C 0.27845(19) 0.78060(9) 0.49690(9) 0.0284(5) Uani 1 1 d . . . C113 C 0.3511(2) 0.80404(10) 0.53746(10) 0.0346(6) Uani 1 1 d . . . C114 C 0.2943(2) 0.82915(10) 0.57538(10) 0.0388(6) Uani 1 1 d . . . C115 C 0.1881(2) 0.82272(10) 0.55720(10) 0.0356(6) Uani 1 1 d . . . C116 C 0.0811(2) 0.76816(11) 0.48191(12) 0.0440(7) Uani 1 1 d . . . H11D H 0.0679 0.7358 0.5000 0.053 Uiso 1 1 calc R . . H11E H 0.0874 0.7618 0.4430 0.053 Uiso 1 1 calc R . . H11F H 0.0238 0.7918 0.4845 0.053 Uiso 1 1 calc R . . C117 C 0.3028(2) 0.74737(10) 0.44996(11) 0.0418(7) Uani 1 1 d . . . H11G H 0.2887 0.7116 0.4580 0.050 Uiso 1 1 calc R . . H11H H 0.3757 0.7512 0.4455 0.050 Uiso 1 1 calc R . . H11I H 0.2599 0.7577 0.4158 0.050 Uiso 1 1 calc R . . C118 C 0.4663(2) 0.79607(13) 0.54332(14) 0.0540(8) Uani 1 1 d . . . H11J H 0.4828 0.7612 0.5562 0.065 Uiso 1 1 calc R . . H11K H 0.5004 0.8206 0.5701 0.065 Uiso 1 1 calc R . . H11L H 0.4905 0.8013 0.5075 0.065 Uiso 1 1 calc R . . C119 C 0.3372(3) 0.84876(13) 0.63248(11) 0.0647(10) Uani 1 1 d . . . H11M H 0.3182 0.8252 0.6606 0.078 Uiso 1 1 calc R . . H11N H 0.3086 0.8827 0.6382 0.078 Uiso 1 1 calc R . . H11O H 0.4125 0.8511 0.6354 0.078 Uiso 1 1 calc R . . C120 C 0.1002(3) 0.83961(13) 0.58743(13) 0.0572(9) Uani 1 1 d . . . H12C H 0.0373 0.8430 0.5611 0.069 Uiso 1 1 calc R . . H12D H 0.1171 0.8726 0.6053 0.069 Uiso 1 1 calc R . . H12E H 0.0893 0.8141 0.6154 0.069 Uiso 1 1 calc R . . C200 C 0.2916(9) 1.0031(4) -0.0558(5) 0.106(3) Uiso 0.50 1 d P . . C201 C 0.3989(4) 1.00189(17) -0.02452(18) 0.0794(12) Uiso 1 1 d . . . C202 C 0.4552(4) 1.04608(18) -0.01279(19) 0.0843(12) Uiso 1 1 d . . . C203 C 0.4422(4) 0.95543(18) -0.01215(18) 0.0841(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0282(2) 0.0247(2) 0.01695(18) -0.00085(15) -0.00088(15) 0.00093(16) Si1 0.0253(3) 0.0254(3) 0.0159(3) -0.0013(2) 0.0016(2) -0.0017(2) Si2 0.0243(3) 0.0208(3) 0.0195(3) -0.0001(2) 0.0028(2) 0.0009(2) Si3 0.0215(3) 0.0232(3) 0.0183(3) -0.0012(2) -0.0001(2) 0.0012(2) Si4 0.0242(3) 0.0201(3) 0.0190(3) 0.0001(2) 0.0011(2) 0.0006(2) Si5 0.0277(4) 0.0324(4) 0.0346(4) 0.0072(3) -0.0079(3) -0.0027(3) Si6 0.0219(3) 0.0243(3) 0.0198(3) 0.0005(2) 0.0002(2) 0.0032(2) Si7 0.0241(3) 0.0266(3) 0.0177(3) 0.0020(2) 0.0021(2) 0.0032(2) Si8 0.0247(3) 0.0266(3) 0.0212(3) 0.0035(2) 0.0020(2) -0.0030(3) Si9 0.0273(4) 0.0573(5) 0.0394(4) 0.0098(4) -0.0014(3) -0.0070(3) O1 0.0338(9) 0.0350(10) 0.0252(8) -0.0097(7) 0.0019(7) 0.0049(7) O2 0.0279(9) 0.0276(9) 0.0260(8) 0.0037(7) -0.0021(6) 0.0005(7) O3 0.0291(9) 0.0248(8) 0.0231(7) -0.0032(6) -0.0014(6) 0.0002(7) O4 0.0379(10) 0.0376(10) 0.0188(7) 0.0058(7) -0.0002(7) -0.0102(8) O5 0.0263(8) 0.0281(9) 0.0237(7) 0.0001(6) 0.0040(6) 0.0026(7) O6 0.0254(9) 0.0407(10) 0.0230(8) -0.0012(7) 0.0039(6) 0.0011(7) O7 0.0290(9) 0.0371(10) 0.0229(8) 0.0032(7) 0.0042(7) -0.0053(7) O8 0.0230(8) 0.0395(10) 0.0290(8) 0.0078(7) -0.0004(7) 0.0030(7) O9 0.0306(9) 0.0289(9) 0.0259(8) 0.0077(7) 0.0007(7) 0.0045(7) O10 0.0379(10) 0.0263(9) 0.0290(8) 0.0020(7) 0.0096(7) 0.0003(7) O11 0.0282(9) 0.0481(11) 0.0330(9) 0.0043(8) -0.0012(7) -0.0087(8) O12 0.0307(9) 0.0296(9) 0.0171(7) 0.0005(6) 0.0000(6) -0.0022(7) C11 0.0269(12) 0.0249(11) 0.0184(9) -0.0007(9) 0.0024(8) -0.0014(9) C12 0.0325(13) 0.0373(14) 0.0231(11) -0.0068(10) 0.0051(10) 0.0004(11) C13 0.0386(15) 0.0484(17) 0.0327(13) -0.0083(12) 0.0139(11) -0.0009(12) C14 0.0288(14) 0.0550(18) 0.0482(16) -0.0111(14) 0.0127(12) 0.0010(12) C15 0.0289(13) 0.0457(16) 0.0368(13) -0.0050(12) 0.0030(11) -0.0047(11) C16 0.0273(12) 0.0349(13) 0.0211(10) -0.0041(9) 0.0008(9) -0.0002(10) C21 0.0306(13) 0.0253(12) 0.0293(11) 0.0024(10) 0.0038(10) -0.0002(10) C22 0.0326(14) 0.0384(15) 0.0515(16) 0.0076(13) 0.0037(12) 0.0008(11) C23 0.0329(15) 0.0435(17) 0.074(2) 0.0051(16) 0.0108(14) -0.0093(13) C24 0.056(2) 0.0366(16) 0.067(2) 0.0169(15) 0.0242(16) -0.0021(14) C25 0.0508(18) 0.0329(15) 0.0537(17) 0.0113(13) 0.0103(14) 0.0061(13) C26 0.0343(14) 0.0319(14) 0.0378(13) 0.0084(11) 0.0014(11) 0.0027(11) C31 0.0263(12) 0.0235(11) 0.0248(10) -0.0052(9) 0.0000(9) 0.0013(9) C32 0.0250(13) 0.0442(15) 0.0316(12) -0.0004(11) -0.0001(10) -0.0013(11) C33 0.0267(14) 0.0569(19) 0.0465(15) -0.0015(14) -0.0002(12) -0.0059(13) C34 0.0282(14) 0.0608(19) 0.0424(15) -0.0094(14) -0.0093(11) 0.0084(13) C35 0.0383(15) 0.0525(17) 0.0284(12) -0.0022(12) -0.0084(11) 0.0073(13) C36 0.0337(14) 0.0418(15) 0.0308(12) 0.0034(11) -0.0033(10) 0.0001(11) C41 0.0336(15) 0.0312(14) 0.073(2) -0.0115(14) -0.0048(14) 0.0076(11) C42 0.0323(15) 0.0346(15) 0.0592(17) -0.0049(13) -0.0048(13) 0.0035(11) C43 0.0323(16) 0.0436(18) 0.098(3) -0.0090(18) -0.0035(16) 0.0086(13) C44 0.049(2) 0.0372(17) 0.111(3) -0.0155(19) -0.0081(19) 0.0201(15) C45 0.0472(18) 0.0326(15) 0.071(2) -0.0177(15) -0.0005(15) 0.0062(13) C46 0.0395(16) 0.0324(15) 0.0666(19) -0.0124(14) -0.0061(14) 0.0055(12) C51 0.082(3) 0.053(2) 0.0554(19) 0.0267(16) -0.0319(18) -0.0271(18) C52 0.0300(16) 0.058(2) 0.085(2) -0.0120(19) -0.0054(15) 0.0111(14) C53 0.0540(19) 0.0540(19) 0.0342(14) 0.0002(13) 0.0065(13) -0.0132(15) C61 0.0322(13) 0.0353(14) 0.0272(11) -0.0063(10) -0.0036(10) 0.0085(11) C62 0.066(2) 0.0423(16) 0.0259(12) 0.0002(11) 0.0093(12) 0.0212(14) C63 0.087(3) 0.065(2) 0.0308(14) -0.0159(14) -0.0072(15) 0.0358(19) C64 0.068(2) 0.0447(18) 0.0487(17) -0.0239(15) -0.0141(15) 0.0184(15) C65 0.0456(18) 0.0384(16) 0.070(2) -0.0220(15) -0.0057(15) 0.0012(13) C66 0.0362(14) 0.0322(14) 0.0391(13) -0.0099(11) 0.0030(11) -0.0019(11) C71 0.0299(13) 0.0374(14) 0.0236(11) -0.0018(10) 0.0026(9) 0.0050(10) C72 0.0419(17) 0.080(2) 0.0257(12) 0.0062(14) -0.0001(11) 0.0093(15) C73 0.062(2) 0.116(3) 0.0222(13) -0.0046(17) -0.0008(13) -0.007(2) C74 0.076(3) 0.102(3) 0.0257(14) -0.0026(16) 0.0140(15) -0.005(2) C75 0.060(2) 0.108(3) 0.0374(16) 0.0036(18) 0.0259(15) 0.024(2) C76 0.0329(15) 0.065(2) 0.0301(13) 0.0044(13) 0.0086(11) 0.0073(13) C81 0.0333(13) 0.0255(12) 0.0238(10) 0.0024(9) 0.0036(9) 0.0004(10) C82 0.0427(16) 0.0379(15) 0.0385(14) 0.0123(12) 0.0102(12) 0.0003(12) C83 0.062(2) 0.0446(17) 0.0429(16) 0.0212(14) 0.0100(14) 0.0024(15) C84 0.075(2) 0.0519(19) 0.0394(15) 0.0197(14) -0.0051(15) 0.0134(17) C85 0.0468(18) 0.0509(18) 0.0462(16) 0.0045(14) -0.0067(13) 0.0115(14) C86 0.0341(14) 0.0436(16) 0.0359(13) 0.0035(12) -0.0025(11) -0.0009(12) C91 0.044(2) 0.188(5) 0.055(2) -0.037(3) 0.0059(17) -0.044(3) C92 0.061(3) 0.093(3) 0.204(6) 0.090(4) -0.009(3) 0.012(2) C93 0.056(2) 0.062(2) 0.0587(19) 0.0000(17) 0.0271(16) 0.0083(16) C101 0.0328(13) 0.0313(13) 0.0283(11) 0.0012(10) 0.0014(10) -0.0094(10) C102 0.0314(14) 0.0323(14) 0.0422(14) -0.0018(11) -0.0013(11) -0.0049(11) C103 0.0498(17) 0.0283(14) 0.0355(13) -0.0037(11) -0.0152(12) -0.0023(12) C104 0.0597(18) 0.0235(13) 0.0277(12) -0.0043(10) 0.0037(12) 0.0022(12) C105 0.0335(13) 0.0218(12) 0.0334(12) 0.0040(10) 0.0012(10) -0.0009(10) C106 0.0523(18) 0.0515(18) 0.0295(13) 0.0049(12) 0.0064(12) -0.0207(14) C107 0.0326(16) 0.0522(19) 0.083(2) -0.0047(18) 0.0116(16) -0.0054(13) C108 0.080(3) 0.0477(19) 0.0561(19) -0.0009(16) -0.0360(18) -0.0072(17) C109 0.114(3) 0.0380(17) 0.0399(16) -0.0093(14) 0.0223(18) 0.0113(18) C110 0.0385(16) 0.0350(15) 0.0610(18) 0.0132(14) 0.0049(13) 0.0041(12) C111 0.0335(13) 0.0288(13) 0.0251(11) 0.0089(10) 0.0039(9) 0.0006(10) C112 0.0356(13) 0.0250(12) 0.0248(11) 0.0025(9) 0.0049(10) 0.0023(10) C113 0.0367(14) 0.0303(13) 0.0349(13) 0.0076(11) -0.0016(11) 0.0027(11) C114 0.0594(18) 0.0347(14) 0.0196(11) 0.0036(10) -0.0049(11) 0.0050(13) C115 0.0499(17) 0.0332(14) 0.0254(11) 0.0075(10) 0.0117(11) 0.0108(12) C116 0.0382(16) 0.0420(16) 0.0492(16) 0.0208(13) -0.0036(12) -0.0064(12) C117 0.0576(19) 0.0340(15) 0.0369(14) -0.0005(12) 0.0178(13) 0.0040(13) C118 0.0376(17) 0.0517(19) 0.069(2) 0.0123(16) -0.0070(15) 0.0045(14) C119 0.111(3) 0.052(2) 0.0246(13) 0.0012(13) -0.0143(16) -0.002(2) C120 0.075(2) 0.055(2) 0.0490(17) 0.0111(15) 0.0338(17) 0.0232(17) _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 Ti O12 1.9274(15) . ? Ti C115 2.390(2) . ? Ti C105 2.393(2) . ? Ti C111 2.394(2) . ? Ti C104 2.396(3) . ? Ti C112 2.396(2) . ? Ti C102 2.399(3) . ? Ti C101 2.409(2) . ? Ti C103 2.433(3) . ? Ti C113 2.442(2) . ? Ti C114 2.456(2) . ? Si1 O12 1.5951(16) . ? Si1 O4 1.6342(17) . ? Si1 O1 1.6424(17) . ? Si1 C11 1.873(2) . ? Si2 O1 1.6093(16) . ? Si2 O5 1.6232(17) . ? Si2 O2 1.6233(16) . ? Si2 C21 1.855(2) . ? Si3 O6 1.6200(16) . ? Si3 O3 1.6208(16) . ? Si3 O2 1.6214(16) . ? Si3 C31 1.849(2) . ? Si4 O4 1.6084(16) . ? Si4 O7 1.6135(17) . ? Si4 O3 1.6281(16) . ? Si4 C41 1.863(3) . ? Si5 O8 1.6361(17) . ? Si5 C53 1.842(3) . ? Si5 C52 1.847(3) . ? Si5 C51 1.862(3) . ? Si6 O8 1.6117(17) . ? Si6 O9 1.6215(16) . ? Si6 O5 1.6248(16) . ? Si6 C61 1.859(3) . ? Si7 O10 1.6182(18) . ? Si7 O9 1.6212(16) . ? Si7 O6 1.6223(17) . ? Si7 C71 1.849(2) . ? Si8 O11 1.6117(18) . ? Si8 O7 1.6187(16) . ? Si8 O10 1.6263(17) . ? Si8 C81 1.856(2) . ? Si9 O11 1.6338(19) . ? Si9 C92 1.825(4) . ? Si9 C93 1.842(3) . ? Si9 C91 1.867(4) . ? C11 C12 1.537(3) . ? C11 C16 1.538(3) . ? C12 C13 1.535(3) . ? C13 C14 1.526(4) . ? C14 C15 1.531(4) . ? C15 C16 1.519(3) . ? C21 C26 1.536(3) . ? C21 C22 1.541(4) . ? C22 C23 1.525(4) . ? C23 C24 1.511(4) . ? C24 C25 1.512(4) . ? C25 C26 1.533(4) . ? C31 C32 1.532(3) . ? C31 C36 1.540(3) . ? C32 C33 1.531(3) . ? C33 C34 1.518(4) . ? C34 C35 1.524(4) . ? C35 C36 1.526(3) . ? C41 C46 1.482(4) . ? C41 C42 1.513(4) . ? C42 C43 1.521(4) . ? C43 C44 1.460(5) . ? C44 C45 1.458(4) . ? C45 C46 1.514(4) . ? C61 C66 1.531(4) . ? C61 C62 1.540(4) . ? C62 C63 1.533(4) . ? C63 C64 1.513(5) . ? C64 C65 1.520(5) . ? C65 C66 1.530(4) . ? C71 C72 1.522(3) . ? C71 C76 1.538(4) . ? C72 C73 1.529(4) . ? C73 C74 1.508(5) . ? C74 C75 1.511(5) . ? C75 C76 1.536(4) . ? C81 C86 1.534(3) . ? C81 C82 1.536(3) . ? C82 C83 1.528(4) . ? C83 C84 1.525(5) . ? C84 C85 1.511(4) . ? C85 C86 1.529(4) . ? C101 C105 1.411(3) . ? C101 C102 1.420(4) . ? C101 C106 1.507(3) . ? C102 C103 1.414(4) . ? C102 C107 1.507(4) . ? C103 C104 1.412(4) . ? C103 C108 1.510(4) . ? C104 C105 1.420(3) . ? C104 C109 1.508(4) . ? C105 C110 1.502(4) . ? C111 C112 1.409(3) . ? C111 C115 1.419(3) . ? C111 C116 1.490(4) . ? C112 C113 1.419(3) . ? C112 C117 1.507(3) . ? C113 C114 1.424(4) . ? C113 C118 1.510(4) . ? C114 C115 1.411(4) . ? C114 C119 1.523(4) . ? C115 C120 1.513(4) . ? C200 C201 1.508(12) . ? C201 C203 1.358(6) . ? C201 C202 1.380(6) . ? C202 C203 1.400(6) 3_675 ? C203 C202 1.400(6) 3_675 ? 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 O12 Ti C115 106.82(9) . . ? O12 Ti C105 86.42(8) . . ? C115 Ti C105 126.47(9) . . ? O12 Ti C111 81.11(7) . . ? C115 Ti C111 34.52(8) . . ? C105 Ti C111 147.96(9) . . ? O12 Ti C104 119.20(8) . . ? C115 Ti C104 102.93(9) . . ? C105 Ti C104 34.50(8) . . ? C111 Ti C104 136.73(9) . . ? O12 Ti C112 91.45(7) . . ? C115 Ti C112 57.18(8) . . ? C105 Ti C112 176.22(8) . . ? C111 Ti C112 34.23(8) . . ? C104 Ti C112 148.39(8) . . ? O12 Ti C102 112.16(8) . . ? C115 Ti C102 141.02(10) . . ? C105 Ti C102 57.26(9) . . ? C111 Ti C102 154.43(9) . . ? C104 Ti C102 57.06(10) . . ? C112 Ti C102 120.98(9) . . ? O12 Ti C101 82.82(7) . . ? C115 Ti C101 159.31(9) . . ? C105 Ti C101 34.18(8) . . ? C111 Ti C101 163.30(8) . . ? C104 Ti C101 56.80(8) . . ? C112 Ti C101 142.40(9) . . ? C102 Ti C101 34.35(8) . . ? O12 Ti C103 138.63(8) . . ? C115 Ti C103 110.14(10) . . ? C105 Ti C103 56.71(9) . . ? C111 Ti C103 140.11(9) . . ? C104 Ti C103 34.00(10) . . ? C112 Ti C103 124.14(9) . . ? C102 Ti C103 34.02(9) . . ? C101 Ti C103 56.33(9) . . ? O12 Ti C113 125.24(8) . . ? C115 Ti C113 56.86(9) . . ? C105 Ti C113 147.47(9) . . ? C111 Ti C113 56.66(9) . . ? C104 Ti C113 115.49(9) . . ? C112 Ti C113 34.10(8) . . ? C102 Ti C113 98.96(9) . . ? C101 Ti C113 132.26(9) . . ? C103 Ti C113 90.99(9) . . ? O12 Ti C114 137.12(9) . . ? C115 Ti C114 33.82(10) . . ? C105 Ti C114 127.16(9) . . ? C111 Ti C114 56.20(9) . . ? C104 Ti C114 93.20(9) . . ? C112 Ti C114 56.23(8) . . ? C102 Ti C114 108.90(10) . . ? C101 Ti C114 140.06(9) . . ? C103 Ti C114 83.91(9) . . ? C113 Ti C114 33.80(9) . . ? O12 Si1 O4 111.37(9) . . ? O12 Si1 O1 110.13(9) . . ? O4 Si1 O1 106.46(9) . . ? O12 Si1 C11 113.51(9) . . ? O4 Si1 C11 108.14(10) . . ? O1 Si1 C11 106.89(10) . . ? O1 Si2 O5 107.95(9) . . ? O1 Si2 O2 111.35(9) . . ? O5 Si2 O2 109.53(8) . . ? O1 Si2 C21 111.48(10) . . ? O5 Si2 C21 109.98(10) . . ? O2 Si2 C21 106.55(10) . . ? O6 Si3 O3 109.33(9) . . ? O6 Si3 O2 108.89(9) . . ? O3 Si3 O2 109.35(8) . . ? O6 Si3 C31 109.35(9) . . ? O3 Si3 C31 108.86(9) . . ? O2 Si3 C31 111.04(10) . . ? O4 Si4 O7 107.69(9) . . ? O4 Si4 O3 110.57(9) . . ? O7 Si4 O3 108.48(9) . . ? O4 Si4 C41 108.23(13) . . ? O7 Si4 C41 112.18(12) . . ? O3 Si4 C41 109.67(11) . . ? O8 Si5 C53 109.96(12) . . ? O8 Si5 C52 106.86(13) . . ? C53 Si5 C52 110.59(15) . . ? O8 Si5 C51 108.74(12) . . ? C53 Si5 C51 109.12(16) . . ? C52 Si5 C51 111.53(18) . . ? O8 Si6 O9 107.44(9) . . ? O8 Si6 O5 108.86(9) . . ? O9 Si6 O5 109.62(9) . . ? O8 Si6 C61 110.58(10) . . ? O9 Si6 C61 110.50(10) . . ? O5 Si6 C61 109.81(10) . . ? O10 Si7 O9 108.35(9) . . ? O10 Si7 O6 110.08(9) . . ? O9 Si7 O6 109.79(9) . . ? O10 Si7 C71 111.30(10) . . ? O9 Si7 C71 110.27(10) . . ? O6 Si7 C71 107.05(10) . . ? O11 Si8 O7 108.03(9) . . ? O11 Si8 O10 109.61(10) . . ? O7 Si8 O10 109.76(9) . . ? O11 Si8 C81 109.02(11) . . ? O7 Si8 C81 110.38(10) . . ? O10 Si8 C81 110.01(10) . . ? O11 Si9 C92 109.17(17) . . ? O11 Si9 C93 110.01(13) . . ? C92 Si9 C93 110.4(2) . . ? O11 Si9 C91 106.22(16) . . ? C92 Si9 C91 111.3(3) . . ? C93 Si9 C91 109.64(18) . . ? Si2 O1 Si1 150.36(12) . . ? Si3 O2 Si2 152.01(11) . . ? Si3 O3 Si4 143.23(11) . . ? Si4 O4 Si1 155.34(12) . . ? Si2 O5 Si6 146.97(11) . . ? Si3 O6 Si7 148.54(11) . . ? Si4 O7 Si8 154.87(11) . . ? Si6 O8 Si5 146.06(11) . . ? Si7 O9 Si6 148.83(12) . . ? Si7 O10 Si8 148.03(11) . . ? Si8 O11 Si9 147.68(13) . . ? Si1 O12 Ti 177.82(11) . . ? C12 C11 C16 109.89(19) . . ? C12 C11 Si1 114.75(16) . . ? C16 C11 Si1 112.36(15) . . ? C13 C12 C11 111.5(2) . . ? C14 C13 C12 111.3(2) . . ? C13 C14 C15 110.9(2) . . ? C16 C15 C14 110.7(2) . . ? C15 C16 C11 112.34(19) . . ? C26 C21 C22 110.2(2) . . ? C26 C21 Si2 113.72(17) . . ? C22 C21 Si2 113.16(17) . . ? C23 C22 C21 111.3(2) . . ? C24 C23 C22 111.2(3) . . ? C23 C24 C25 112.0(2) . . ? C24 C25 C26 111.5(2) . . ? C25 C26 C21 111.7(2) . . ? C32 C31 C36 110.4(2) . . ? C32 C31 Si3 113.41(15) . . ? C36 C31 Si3 111.58(17) . . ? C33 C32 C31 111.9(2) . . ? C34 C33 C32 111.5(2) . . ? C33 C34 C35 110.5(2) . . ? C34 C35 C36 111.2(2) . . ? C35 C36 C31 111.9(2) . . ? C46 C41 C42 115.2(2) . . ? C46 C41 Si4 115.4(2) . . ? C42 C41 Si4 116.8(2) . . ? C41 C42 C43 113.3(2) . . ? C44 C43 C42 115.8(3) . . ? C45 C44 C43 117.1(3) . . ? C44 C45 C46 115.3(3) . . ? C41 C46 C45 114.2(3) . . ? C66 C61 C62 108.6(2) . . ? C66 C61 Si6 114.02(16) . . ? C62 C61 Si6 113.2(2) . . ? C63 C62 C61 111.0(3) . . ? C64 C63 C62 112.0(2) . . ? C63 C64 C65 112.3(2) . . ? C64 C65 C66 111.4(3) . . ? C65 C66 C61 112.0(2) . . ? C72 C71 C76 110.3(2) . . ? C72 C71 Si7 113.59(18) . . ? C76 C71 Si7 114.34(17) . . ? C71 C72 C73 111.5(3) . . ? C74 C73 C72 111.7(3) . . ? C73 C74 C75 112.2(3) . . ? C74 C75 C76 112.2(3) . . ? C75 C76 C71 110.6(2) . . ? C86 C81 C82 109.2(2) . . ? C86 C81 Si8 114.94(17) . . ? C82 C81 Si8 113.23(18) . . ? C83 C82 C81 111.0(2) . . ? C84 C83 C82 111.7(3) . . ? C85 C84 C83 111.5(2) . . ? C84 C85 C86 111.9(3) . . ? C85 C86 C81 111.0(2) . . ? C105 C101 C102 108.4(2) . . ? C105 C101 C106 127.0(2) . . ? C102 C101 C106 124.5(2) . . ? C105 C101 Ti 72.29(13) . . ? C102 C101 Ti 72.44(15) . . ? C106 C101 Ti 123.28(17) . . ? C103 C102 C101 107.5(2) . . ? C103 C102 C107 126.5(3) . . ? C101 C102 C107 125.3(3) . . ? C103 C102 Ti 74.28(16) . . ? C101 C102 Ti 73.21(14) . . ? C107 C102 Ti 125.62(19) . . ? C104 C103 C102 108.3(2) . . ? C104 C103 C108 126.9(3) . . ? C102 C103 C108 123.4(3) . . ? C104 C103 Ti 71.55(15) . . ? C102 C103 Ti 71.70(15) . . ? C108 C103 Ti 133.3(2) . . ? C103 C104 C105 108.1(2) . . ? C103 C104 C109 126.9(3) . . ? C105 C104 C109 124.6(3) . . ? C103 C104 Ti 74.44(15) . . ? C105 C104 Ti 72.67(14) . . ? C109 C104 Ti 124.5(2) . . ? C101 C105 C104 107.6(2) . . ? C101 C105 C110 126.8(2) . . ? C104 C105 C110 125.5(2) . . ? C101 C105 Ti 73.53(14) . . ? C104 C105 Ti 72.84(14) . . ? C110 C105 Ti 121.05(17) . . ? C112 C111 C115 108.1(2) . . ? C112 C111 C116 125.8(2) . . ? C115 C111 C116 125.8(2) . . ? C112 C111 Ti 72.99(13) . . ? C115 C111 Ti 72.62(14) . . ? C116 C111 Ti 125.22(16) . . ? C111 C112 C113 108.4(2) . . ? C111 C112 C117 125.2(2) . . ? C113 C112 C117 126.3(2) . . ? C111 C112 Ti 72.78(14) . . ? C113 C112 Ti 74.71(14) . . ? C117 C112 Ti 121.40(16) . . ? C112 C113 C114 107.1(2) . . ? C112 C113 C118 125.1(2) . . ? C114 C113 C118 127.1(3) . . ? C112 C113 Ti 71.19(14) . . ? C114 C113 Ti 73.65(14) . . ? C118 C113 Ti 127.68(19) . . ? C115 C114 C113 108.5(2) . . ? C115 C114 C119 123.8(3) . . ? C113 C114 C119 126.2(3) . . ? C115 C114 Ti 70.54(13) . . ? C113 C114 Ti 72.55(13) . . ? C119 C114 Ti 133.4(2) . . ? C114 C115 C111 107.7(2) . . ? C114 C115 C120 126.3(3) . . ? C111 C115 C120 125.5(3) . . ? C114 C115 Ti 75.64(15) . . ? C111 C115 Ti 72.86(13) . . ? C120 C115 Ti 124.16(18) . . ? C203 C201 C202 120.6(4) . . ? C203 C201 C200 117.7(6) . . ? C202 C201 C200 121.5(6) . . ? C201 C202 C203 121.4(4) . 3_675 ? C201 C203 C202 118.0(4) . 3_675 ? 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 O5 Si2 O1 Si1 114.7(2) . . . . ? O2 Si2 O1 Si1 -5.6(3) . . . . ? C21 Si2 O1 Si1 -124.5(2) . . . . ? O12 Si1 O1 Si2 -157.3(2) . . . . ? O4 Si1 O1 Si2 -36.4(3) . . . . ? C11 Si1 O1 Si2 79.0(3) . . . . ? O6 Si3 O2 Si2 63.7(3) . . . . ? O3 Si3 O2 Si2 -55.7(3) . . . . ? C31 Si3 O2 Si2 -175.8(2) . . . . ? O1 Si2 O2 Si3 61.3(3) . . . . ? O5 Si2 O2 Si3 -58.0(3) . . . . ? C21 Si2 O2 Si3 -176.9(2) . . . . ? O6 Si3 O3 Si4 -63.27(19) . . . . ? O2 Si3 O3 Si4 55.9(2) . . . . ? C31 Si3 O3 Si4 177.33(17) . . . . ? O4 Si4 O3 Si3 -60.8(2) . . . . ? O7 Si4 O3 Si3 57.11(19) . . . . ? C41 Si4 O3 Si3 179.93(19) . . . . ? O7 Si4 O4 Si1 -131.5(3) . . . . ? O3 Si4 O4 Si1 -13.1(3) . . . . ? C41 Si4 O4 Si1 107.0(3) . . . . ? O12 Si1 O4 Si4 176.9(3) . . . . ? O1 Si1 O4 Si4 56.8(3) . . . . ? C11 Si1 O4 Si4 -57.7(3) . . . . ? O1 Si2 O5 Si6 -137.71(19) . . . . ? O2 Si2 O5 Si6 -16.3(2) . . . . ? C21 Si2 O5 Si6 100.5(2) . . . . ? O8 Si6 O5 Si2 174.78(19) . . . . ? O9 Si6 O5 Si2 57.5(2) . . . . ? C61 Si6 O5 Si2 -64.0(2) . . . . ? O3 Si3 O6 Si7 62.3(2) . . . . ? O2 Si3 O6 Si7 -57.1(2) . . . . ? C31 Si3 O6 Si7 -178.6(2) . . . . ? O10 Si7 O6 Si3 -70.5(2) . . . . ? O9 Si7 O6 Si3 48.7(2) . . . . ? C71 Si7 O6 Si3 168.4(2) . . . . ? O4 Si4 O7 Si8 151.8(3) . . . . ? O3 Si4 O7 Si8 32.1(3) . . . . ? C41 Si4 O7 Si8 -89.2(3) . . . . ? O11 Si8 O7 Si4 177.2(3) . . . . ? O10 Si8 O7 Si4 -63.4(3) . . . . ? C81 Si8 O7 Si4 58.0(3) . . . . ? O9 Si6 O8 Si5 138.6(2) . . . . ? O5 Si6 O8 Si5 20.0(2) . . . . ? C61 Si6 O8 Si5 -100.8(2) . . . . ? C53 Si5 O8 Si6 -79.5(2) . . . . ? C52 Si5 O8 Si6 160.4(2) . . . . ? C51 Si5 O8 Si6 39.9(3) . . . . ? O10 Si7 O9 Si6 150.8(2) . . . . ? O6 Si7 O9 Si6 30.5(2) . . . . ? C71 Si7 O9 Si6 -87.2(2) . . . . ? O8 Si6 O9 Si7 171.3(2) . . . . ? O5 Si6 O9 Si7 -70.5(2) . . . . ? C61 Si6 O9 Si7 50.6(2) . . . . ? O9 Si7 O10 Si8 -82.1(2) . . . . ? O6 Si7 O10 Si8 38.0(2) . . . . ? C71 Si7 O10 Si8 156.5(2) . . . . ? O11 Si8 O10 Si7 122.7(2) . . . . ? O7 Si8 O10 Si7 4.2(2) . . . . ? C81 Si8 O10 Si7 -117.5(2) . . . . ? O7 Si8 O11 Si9 120.9(2) . . . . ? O10 Si8 O11 Si9 1.4(3) . . . . ? C81 Si8 O11 Si9 -119.1(2) . . . . ? C92 Si9 O11 Si8 -52.0(3) . . . . ? C93 Si9 O11 Si8 69.3(3) . . . . ? C91 Si9 O11 Si8 -172.1(3) . . . . ? O4 Si1 O12 Ti 159(3) . . . . ? O1 Si1 O12 Ti -83(3) . . . . ? C11 Si1 O12 Ti 36(3) . . . . ? C115 Ti O12 Si1 0(3) . . . . ? C105 Ti O12 Si1 -127(3) . . . . ? C111 Ti O12 Si1 24(3) . . . . ? C104 Ti O12 Si1 -116(3) . . . . ? C112 Ti O12 Si1 56(3) . . . . ? C102 Ti O12 Si1 -179(100) . . . . ? C101 Ti O12 Si1 -161(3) . . . . ? C103 Ti O12 Si1 -152(3) . . . . ? C113 Ti O12 Si1 61(3) . . . . ? C114 Ti O12 Si1 19(3) . . . . ? O12 Si1 C11 C12 43.38(19) . . . . ? O4 Si1 C11 C12 -80.72(17) . . . . ? O1 Si1 C11 C12 165.01(16) . . . . ? O12 Si1 C11 C16 169.88(15) . . . . ? O4 Si1 C11 C16 45.78(18) . . . . ? O1 Si1 C11 C16 -68.50(18) . . . . ? C16 C11 C12 C13 54.5(3) . . . . ? Si1 C11 C12 C13 -177.71(17) . . . . ? C11 C12 C13 C14 -55.8(3) . . . . ? C12 C13 C14 C15 56.0(3) . . . . ? C13 C14 C15 C16 -56.1(3) . . . . ? C14 C15 C16 C11 56.4(3) . . . . ? C12 C11 C16 C15 -55.4(3) . . . . ? Si1 C11 C16 C15 175.50(17) . . . . ? O1 Si2 C21 C26 -57.2(2) . . . . ? O5 Si2 C21 C26 62.54(19) . . . . ? O2 Si2 C21 C26 -178.83(17) . . . . ? O1 Si2 C21 C22 69.5(2) . . . . ? O5 Si2 C21 C22 -170.76(17) . . . . ? O2 Si2 C21 C22 -52.1(2) . . . . ? C26 C21 C22 C23 -55.4(3) . . . . ? Si2 C21 C22 C23 176.0(2) . . . . ? C21 C22 C23 C24 56.4(3) . . . . ? C22 C23 C24 C25 -56.0(4) . . . . ? C23 C24 C25 C26 54.8(4) . . . . ? C24 C25 C26 C21 -54.3(3) . . . . ? C22 C21 C26 C25 54.3(3) . . . . ? Si2 C21 C26 C25 -177.46(19) . . . . ? O6 Si3 C31 C32 179.69(17) . . . . ? O3 Si3 C31 C32 -60.92(19) . . . . ? O2 Si3 C31 C32 59.51(19) . . . . ? O6 Si3 C31 C36 -54.91(19) . . . . ? O3 Si3 C31 C36 64.49(18) . . . . ? O2 Si3 C31 C36 -175.08(16) . . . . ? C36 C31 C32 C33 53.4(3) . . . . ? Si3 C31 C32 C33 179.49(19) . . . . ? C31 C32 C33 C34 -55.6(3) . . . . ? C32 C33 C34 C35 56.5(3) . . . . ? C33 C34 C35 C36 -56.7(3) . . . . ? C34 C35 C36 C31 56.0(3) . . . . ? C32 C31 C36 C35 -53.8(3) . . . . ? Si3 C31 C36 C35 179.09(18) . . . . ? O4 Si4 C41 C46 94.4(3) . . . . ? O7 Si4 C41 C46 -24.2(3) . . . . ? O3 Si4 C41 C46 -144.9(2) . . . . ? O4 Si4 C41 C42 -125.4(2) . . . . ? O7 Si4 C41 C42 115.9(2) . . . . ? O3 Si4 C41 C42 -4.7(3) . . . . ? C46 C41 C42 C43 -43.4(4) . . . . ? Si4 C41 C42 C43 176.3(2) . . . . ? C41 C42 C43 C44 41.1(5) . . . . ? C42 C43 C44 C45 -40.9(5) . . . . ? C43 C44 C45 C46 41.3(5) . . . . ? C42 C41 C46 C45 44.4(4) . . . . ? Si4 C41 C46 C45 -174.7(2) . . . . ? C44 C45 C46 C41 -42.8(4) . . . . ? O8 Si6 C61 C66 66.7(2) . . . . ? O9 Si6 C61 C66 -174.45(17) . . . . ? O5 Si6 C61 C66 -53.4(2) . . . . ? O8 Si6 C61 C62 -58.1(2) . . . . ? O9 Si6 C61 C62 60.7(2) . . . . ? O5 Si6 C61 C62 -178.24(17) . . . . ? C66 C61 C62 C63 57.7(3) . . . . ? Si6 C61 C62 C63 -174.59(19) . . . . ? C61 C62 C63 C64 -56.1(3) . . . . ? C62 C63 C64 C65 52.8(4) . . . . ? C63 C64 C65 C66 -52.1(4) . . . . ? C64 C65 C66 C61 55.5(3) . . . . ? C62 C61 C66 C65 -57.9(3) . . . . ? Si6 C61 C66 C65 174.88(19) . . . . ? O10 Si7 C71 C72 -70.0(2) . . . . ? O9 Si7 C71 C72 169.7(2) . . . . ? O6 Si7 C71 C72 50.3(2) . . . . ? O10 Si7 C71 C76 57.8(2) . . . . ? O9 Si7 C71 C76 -62.4(2) . . . . ? O6 Si7 C71 C76 178.16(18) . . . . ? C76 C71 C72 C73 56.7(3) . . . . ? Si7 C71 C72 C73 -173.4(2) . . . . ? C71 C72 C73 C74 -55.5(4) . . . . ? C72 C73 C74 C75 53.4(5) . . . . ? C73 C74 C75 C76 -53.3(5) . . . . ? C74 C75 C76 C71 54.4(4) . . . . ? C72 C71 C76 C75 -55.8(3) . . . . ? Si7 C71 C76 C75 174.7(2) . . . . ? O11 Si8 C81 C86 179.61(17) . . . . ? O7 Si8 C81 C86 -61.9(2) . . . . ? O10 Si8 C81 C86 59.4(2) . . . . ? O11 Si8 C81 C82 53.1(2) . . . . ? O7 Si8 C81 C82 171.62(17) . . . . ? O10 Si8 C81 C82 -67.1(2) . . . . ? C86 C81 C82 C83 57.6(3) . . . . ? Si8 C81 C82 C83 -172.9(2) . . . . ? C81 C82 C83 C84 -56.1(3) . . . . ? C82 C83 C84 C85 53.7(4) . . . . ? C83 C84 C85 C86 -53.8(4) . . . . ? C84 C85 C86 C81 56.4(3) . . . . ? C82 C81 C86 C85 -57.6(3) . . . . ? Si8 C81 C86 C85 173.86(19) . . . . ? O12 Ti C101 C105 94.22(15) . . . . ? C115 Ti C101 C105 -25.2(3) . . . . ? C111 Ti C101 C105 110.0(3) . . . . ? C104 Ti C101 C105 -37.86(15) . . . . ? C112 Ti C101 C105 177.22(14) . . . . ? C102 Ti C101 C105 -116.7(2) . . . . ? C103 Ti C101 C105 -78.88(16) . . . . ? C113 Ti C101 C105 -133.61(15) . . . . ? C114 Ti C101 C105 -85.19(19) . . . . ? O12 Ti C101 C102 -149.12(16) . . . . ? C115 Ti C101 C102 91.4(3) . . . . ? C105 Ti C101 C102 116.7(2) . . . . ? C111 Ti C101 C102 -133.3(3) . . . . ? C104 Ti C101 C102 78.81(17) . . . . ? C112 Ti C101 C102 -66.1(2) . . . . ? C103 Ti C101 C102 37.79(15) . . . . ? C113 Ti C101 C102 -16.9(2) . . . . ? C114 Ti C101 C102 31.5(2) . . . . ? O12 Ti C101 C106 -28.9(2) . . . . ? C115 Ti C101 C106 -148.3(3) . . . . ? C105 Ti C101 C106 -123.1(3) . . . . ? C111 Ti C101 C106 -13.1(5) . . . . ? C104 Ti C101 C106 -161.0(3) . . . . ? C112 Ti C101 C106 54.1(3) . . . . ? C102 Ti C101 C106 120.2(3) . . . . ? C103 Ti C101 C106 158.0(3) . . . . ? C113 Ti C101 C106 103.3(2) . . . . ? C114 Ti C101 C106 151.7(2) . . . . ? C105 C101 C102 C103 -3.1(3) . . . . ? C106 C101 C102 C103 174.3(2) . . . . ? Ti C101 C102 C103 -66.93(19) . . . . ? C105 C101 C102 C107 -174.1(3) . . . . ? C106 C101 C102 C107 3.4(4) . . . . ? Ti C101 C102 C107 122.1(3) . . . . ? C105 C101 C102 Ti 63.80(17) . . . . ? C106 C101 C102 Ti -118.7(2) . . . . ? O12 Ti C102 C103 147.65(15) . . . . ? C115 Ti C102 C103 -31.5(2) . . . . ? C105 Ti C102 C103 77.65(17) . . . . ? C111 Ti C102 C103 -94.7(2) . . . . ? C104 Ti C102 C103 36.32(15) . . . . ? C112 Ti C102 C103 -106.30(16) . . . . ? C101 Ti C102 C103 114.3(2) . . . . ? C113 Ti C102 C103 -78.32(17) . . . . ? C114 Ti C102 C103 -44.96(18) . . . . ? O12 Ti C102 C101 33.36(17) . . . . ? C115 Ti C102 C101 -145.84(16) . . . . ? C105 Ti C102 C101 -36.64(14) . . . . ? C111 Ti C102 C101 151.03(18) . . . . ? C104 Ti C102 C101 -77.97(16) . . . . ? C112 Ti C102 C101 139.41(14) . . . . ? C103 Ti C102 C101 -114.3(2) . . . . ? C113 Ti C102 C101 167.39(15) . . . . ? C114 Ti C102 C101 -159.25(15) . . . . ? O12 Ti C102 C107 -88.4(2) . . . . ? C115 Ti C102 C107 92.4(3) . . . . ? C105 Ti C102 C107 -158.4(3) . . . . ? C111 Ti C102 C107 29.3(4) . . . . ? C104 Ti C102 C107 160.3(3) . . . . ? C112 Ti C102 C107 17.7(3) . . . . ? C101 Ti C102 C107 -121.8(3) . . . . ? C103 Ti C102 C107 124.0(3) . . . . ? C113 Ti C102 C107 45.6(3) . . . . ? C114 Ti C102 C107 79.0(3) . . . . ? C101 C102 C103 C104 3.6(3) . . . . ? C107 C102 C103 C104 174.4(3) . . . . ? Ti C102 C103 C104 -62.61(19) . . . . ? C101 C102 C103 C108 -163.5(3) . . . . ? C107 C102 C103 C108 7.3(4) . . . . ? Ti C102 C103 C108 130.3(3) . . . . ? C101 C102 C103 Ti 66.20(18) . . . . ? C107 C102 C103 Ti -123.0(3) . . . . ? O12 Ti C103 C104 68.7(2) . . . . ? C115 Ti C103 C104 -83.26(16) . . . . ? C105 Ti C103 C104 37.84(14) . . . . ? C111 Ti C103 C104 -104.87(18) . . . . ? C112 Ti C103 C104 -146.59(14) . . . . ? C102 Ti C103 C104 117.3(2) . . . . ? C101 Ti C103 C104 79.10(16) . . . . ? C113 Ti C103 C104 -138.08(16) . . . . ? C114 Ti C103 C104 -104.98(16) . . . . ? O12 Ti C103 C102 -48.6(2) . . . . ? C115 Ti C103 C102 159.48(15) . . . . ? C105 Ti C103 C102 -79.42(17) . . . . ? C111 Ti C103 C102 137.86(16) . . . . ? C104 Ti C103 C102 -117.3(2) . . . . ? C112 Ti C103 C102 96.15(17) . . . . ? C101 Ti C103 C102 -38.17(15) . . . . ? C113 Ti C103 C102 104.65(16) . . . . ? C114 Ti C103 C102 137.76(17) . . . . ? O12 Ti C103 C108 -167.6(3) . . . . ? C115 Ti C103 C108 40.5(3) . . . . ? C105 Ti C103 C108 161.6(4) . . . . ? C111 Ti C103 C108 18.8(4) . . . . ? C104 Ti C103 C108 123.7(4) . . . . ? C112 Ti C103 C108 -22.9(4) . . . . ? C102 Ti C103 C108 -119.0(4) . . . . ? C101 Ti C103 C108 -157.2(4) . . . . ? C113 Ti C103 C108 -14.4(3) . . . . ? C114 Ti C103 C108 18.7(3) . . . . ? C102 C103 C104 C105 -2.7(3) . . . . ? C108 C103 C104 C105 163.8(3) . . . . ? Ti C103 C104 C105 -65.40(18) . . . . ? C102 C103 C104 C109 -175.5(3) . . . . ? C108 C103 C104 C109 -9.1(5) . . . . ? Ti C103 C104 C109 121.8(3) . . . . ? C102 C103 C104 Ti 62.70(19) . . . . ? C108 C103 C104 Ti -130.8(3) . . . . ? O12 Ti C104 C103 -135.13(15) . . . . ? C115 Ti C104 C103 106.94(16) . . . . ? C105 Ti C104 C103 -115.1(2) . . . . ? C111 Ti C104 C103 115.28(17) . . . . ? C112 Ti C104 C103 60.4(2) . . . . ? C102 Ti C104 C103 -36.34(15) . . . . ? C101 Ti C104 C103 -77.61(16) . . . . ? C113 Ti C104 C103 47.73(17) . . . . ? C114 Ti C104 C103 74.17(16) . . . . ? O12 Ti C104 C105 -20.03(19) . . . . ? C115 Ti C104 C105 -137.96(16) . . . . ? C111 Ti C104 C105 -129.62(16) . . . . ? C112 Ti C104 C105 175.51(16) . . . . ? C102 Ti C104 C105 78.76(16) . . . . ? C101 Ti C104 C105 37.50(15) . . . . ? C103 Ti C104 C105 115.1(2) . . . . ? C113 Ti C104 C105 162.84(15) . . . . ? C114 Ti C104 C105 -170.72(17) . . . . ? O12 Ti C104 C109 100.5(3) . . . . ? C115 Ti C104 C109 -17.5(3) . . . . ? C105 Ti C104 C109 120.5(3) . . . . ? C111 Ti C104 C109 -9.1(3) . . . . ? C112 Ti C104 C109 -64.0(3) . . . . ? C102 Ti C104 C109 -160.7(3) . . . . ? C101 Ti C104 C109 158.0(3) . . . . ? C103 Ti C104 C109 -124.4(3) . . . . ? C113 Ti C104 C109 -76.7(3) . . . . ? C114 Ti C104 C109 -50.2(3) . . . . ? C102 C101 C105 C104 1.5(3) . . . . ? C106 C101 C105 C104 -175.9(2) . . . . ? Ti C101 C105 C104 65.37(17) . . . . ? C102 C101 C105 C110 179.3(2) . . . . ? C106 C101 C105 C110 2.0(4) . . . . ? Ti C101 C105 C110 -116.8(3) . . . . ? C102 C101 C105 Ti -63.89(18) . . . . ? C106 C101 C105 Ti 118.7(3) . . . . ? C103 C104 C105 C101 0.8(3) . . . . ? C109 C104 C105 C101 173.8(3) . . . . ? Ti C104 C105 C101 -65.83(17) . . . . ? C103 C104 C105 C110 -177.1(2) . . . . ? C109 C104 C105 C110 -4.1(4) . . . . ? Ti C104 C105 C110 116.3(2) . . . . ? C103 C104 C105 Ti 66.58(18) . . . . ? C109 C104 C105 Ti -120.4(3) . . . . ? O12 Ti C105 C101 -82.48(14) . . . . ? C115 Ti C105 C101 169.21(14) . . . . ? C111 Ti C105 C101 -149.41(16) . . . . ? C104 Ti C105 C101 115.0(2) . . . . ? C112 Ti C105 C101 -26.6(14) . . . . ? C102 Ti C105 C101 36.83(14) . . . . ? C103 Ti C105 C101 77.66(16) . . . . ? C113 Ti C105 C101 85.3(2) . . . . ? C114 Ti C105 C101 126.60(15) . . . . ? O12 Ti C105 C104 162.57(17) . . . . ? C115 Ti C105 C104 54.3(2) . . . . ? C111 Ti C105 C104 95.6(2) . . . . ? C112 Ti C105 C104 -141.6(13) . . . . ? C102 Ti C105 C104 -78.12(17) . . . . ? C101 Ti C105 C104 -115.0(2) . . . . ? C103 Ti C105 C104 -37.29(16) . . . . ? C113 Ti C105 C104 -29.7(3) . . . . ? C114 Ti C105 C104 11.7(2) . . . . ? O12 Ti C105 C110 41.0(2) . . . . ? C115 Ti C105 C110 -67.3(2) . . . . ? C111 Ti C105 C110 -25.9(3) . . . . ? C104 Ti C105 C110 -121.6(3) . . . . ? C112 Ti C105 C110 96.9(13) . . . . ? C102 Ti C105 C110 160.3(2) . . . . ? C101 Ti C105 C110 123.5(3) . . . . ? C103 Ti C105 C110 -158.9(2) . . . . ? C113 Ti C105 C110 -151.3(2) . . . . ? C114 Ti C105 C110 -109.9(2) . . . . ? O12 Ti C111 C112 106.00(14) . . . . ? C115 Ti C111 C112 -115.9(2) . . . . ? C105 Ti C111 C112 174.34(15) . . . . ? C104 Ti C111 C112 -130.35(16) . . . . ? C102 Ti C111 C112 -17.9(3) . . . . ? C101 Ti C111 C112 90.1(3) . . . . ? C103 Ti C111 C112 -78.29(19) . . . . ? C113 Ti C111 C112 -37.33(13) . . . . ? C114 Ti C111 C112 -78.17(15) . . . . ? O12 Ti C111 C115 -138.10(16) . . . . ? C105 Ti C111 C115 -69.8(2) . . . . ? C104 Ti C111 C115 -14.4(2) . . . . ? C112 Ti C111 C115 115.9(2) . . . . ? C102 Ti C111 C115 98.0(2) . . . . ? C101 Ti C111 C115 -154.0(3) . . . . ? C103 Ti C111 C115 37.6(2) . . . . ? C113 Ti C111 C115 78.57(16) . . . . ? C114 Ti C111 C115 37.73(15) . . . . ? O12 Ti C111 C116 -16.2(2) . . . . ? C115 Ti C111 C116 121.9(3) . . . . ? C105 Ti C111 C116 52.2(3) . . . . ? C104 Ti C111 C116 107.5(2) . . . . ? C112 Ti C111 C116 -122.2(3) . . . . ? C102 Ti C111 C116 -140.1(2) . . . . ? C101 Ti C111 C116 -32.0(4) . . . . ? C103 Ti C111 C116 159.5(2) . . . . ? C113 Ti C111 C116 -159.5(3) . . . . ? C114 Ti C111 C116 159.6(3) . . . . ? C115 C111 C112 C113 2.2(3) . . . . ? C116 C111 C112 C113 -171.7(2) . . . . ? Ti C111 C112 C113 66.77(17) . . . . ? C115 C111 C112 C117 178.7(2) . . . . ? C116 C111 C112 C117 4.9(4) . . . . ? Ti C111 C112 C117 -116.7(2) . . . . ? C115 C111 C112 Ti -64.60(16) . . . . ? C116 C111 C112 Ti 121.5(2) . . . . ? O12 Ti C112 C111 -71.81(13) . . . . ? C115 Ti C112 C111 37.34(14) . . . . ? C105 Ti C112 C111 -127.5(13) . . . . ? C104 Ti C112 C111 94.7(2) . . . . ? C102 Ti C112 C111 171.11(13) . . . . ? C101 Ti C112 C111 -151.90(14) . . . . ? C103 Ti C112 C111 130.65(15) . . . . ? C113 Ti C112 C111 115.4(2) . . . . ? C114 Ti C112 C111 78.06(15) . . . . ? O12 Ti C112 C113 172.84(15) . . . . ? C115 Ti C112 C113 -78.01(16) . . . . ? C105 Ti C112 C113 117.1(13) . . . . ? C111 Ti C112 C113 -115.4(2) . . . . ? C104 Ti C112 C113 -20.7(2) . . . . ? C102 Ti C112 C113 55.75(17) . . . . ? C101 Ti C112 C113 92.75(18) . . . . ? C103 Ti C112 C113 15.30(18) . . . . ? C114 Ti C112 C113 -37.29(15) . . . . ? O12 Ti C112 C117 49.4(2) . . . . ? C115 Ti C112 C117 158.5(2) . . . . ? C105 Ti C112 C117 -6.4(14) . . . . ? C111 Ti C112 C117 121.2(3) . . . . ? C104 Ti C112 C117 -144.2(2) . . . . ? C102 Ti C112 C117 -67.7(2) . . . . ? C101 Ti C112 C117 -30.7(3) . . . . ? C103 Ti C112 C117 -108.2(2) . . . . ? C113 Ti C112 C117 -123.5(3) . . . . ? C114 Ti C112 C117 -160.8(3) . . . . ? C111 C112 C113 C114 -0.1(3) . . . . ? C117 C112 C113 C114 -176.6(2) . . . . ? Ti C112 C113 C114 65.41(17) . . . . ? C111 C112 C113 C118 171.1(2) . . . . ? C117 C112 C113 C118 -5.4(4) . . . . ? Ti C112 C113 C118 -123.4(3) . . . . ? C111 C112 C113 Ti -65.50(16) . . . . ? C117 C112 C113 Ti 118.0(2) . . . . ? O12 Ti C113 C112 -8.77(18) . . . . ? C115 Ti C113 C112 79.03(16) . . . . ? C105 Ti C113 C112 -173.73(15) . . . . ? C111 Ti C113 C112 37.48(14) . . . . ? C104 Ti C113 C112 168.17(14) . . . . ? C102 Ti C113 C112 -134.16(15) . . . . ? C101 Ti C113 C112 -124.57(15) . . . . ? C103 Ti C113 C112 -167.38(15) . . . . ? C114 Ti C113 C112 115.1(2) . . . . ? O12 Ti C113 C114 -123.88(16) . . . . ? C115 Ti C113 C114 -36.08(16) . . . . ? C105 Ti C113 C114 71.2(2) . . . . ? C111 Ti C113 C114 -77.63(17) . . . . ? C104 Ti C113 C114 53.06(19) . . . . ? C112 Ti C113 C114 -115.1(2) . . . . ? C102 Ti C113 C114 110.74(17) . . . . ? C101 Ti C113 C114 120.32(17) . . . . ? C103 Ti C113 C114 77.51(18) . . . . ? O12 Ti C113 C118 111.5(2) . . . . ? C115 Ti C113 C118 -160.7(3) . . . . ? C105 Ti C113 C118 -53.4(3) . . . . ? C111 Ti C113 C118 157.8(3) . . . . ? C104 Ti C113 C118 -71.5(3) . . . . ? C112 Ti C113 C118 120.3(3) . . . . ? C102 Ti C113 C118 -13.9(3) . . . . ? C101 Ti C113 C118 -4.3(3) . . . . ? C103 Ti C113 C118 -47.1(3) . . . . ? C114 Ti C113 C118 -124.6(3) . . . . ? C112 C113 C114 C115 -2.0(3) . . . . ? C118 C113 C114 C115 -173.0(3) . . . . ? Ti C113 C114 C115 61.73(18) . . . . ? C112 C113 C114 C119 164.7(3) . . . . ? C118 C113 C114 C119 -6.3(5) . . . . ? Ti C113 C114 C119 -131.5(3) . . . . ? C112 C113 C114 Ti -63.77(17) . . . . ? C118 C113 C114 Ti 125.2(3) . . . . ? O12 Ti C114 C115 -32.5(2) . . . . ? C105 Ti C114 C115 102.04(17) . . . . ? C111 Ti C114 C115 -38.54(15) . . . . ? C104 Ti C114 C115 108.62(16) . . . . ? C112 Ti C114 C115 -80.01(16) . . . . ? C102 Ti C114 C115 164.81(15) . . . . ? C101 Ti C114 C115 146.66(16) . . . . ? C103 Ti C114 C115 141.38(17) . . . . ? C113 Ti C114 C115 -117.6(2) . . . . ? O12 Ti C114 C113 85.2(2) . . . . ? C115 Ti C114 C113 117.6(2) . . . . ? C105 Ti C114 C113 -140.31(16) . . . . ? C111 Ti C114 C113 79.10(17) . . . . ? C104 Ti C114 C113 -133.73(17) . . . . ? C112 Ti C114 C113 37.64(15) . . . . ? C102 Ti C114 C113 -77.55(17) . . . . ? C101 Ti C114 C113 -95.69(19) . . . . ? C103 Ti C114 C113 -100.98(17) . . . . ? O12 Ti C114 C119 -151.1(3) . . . . ? C115 Ti C114 C119 -118.6(4) . . . . ? C105 Ti C114 C119 -16.6(4) . . . . ? C111 Ti C114 C119 -157.2(4) . . . . ? C104 Ti C114 C119 -10.0(3) . . . . ? C112 Ti C114 C119 161.4(4) . . . . ? C102 Ti C114 C119 46.2(3) . . . . ? C101 Ti C114 C119 28.0(4) . . . . ? C103 Ti C114 C119 22.8(3) . . . . ? C113 Ti C114 C119 123.7(4) . . . . ? C113 C114 C115 C111 3.4(3) . . . . ? C119 C114 C115 C111 -163.7(2) . . . . ? Ti C114 C115 C111 66.38(16) . . . . ? C113 C114 C115 C120 174.9(3) . . . . ? C119 C114 C115 C120 7.8(4) . . . . ? Ti C114 C115 C120 -122.1(3) . . . . ? C113 C114 C115 Ti -63.02(18) . . . . ? C119 C114 C115 Ti 129.9(3) . . . . ? C112 C111 C115 C114 -3.4(3) . . . . ? C116 C111 C115 C114 170.5(2) . . . . ? Ti C111 C115 C114 -68.26(18) . . . . ? C112 C111 C115 C120 -175.0(2) . . . . ? C116 C111 C115 C120 -1.2(4) . . . . ? Ti C111 C115 C120 120.1(3) . . . . ? C112 C111 C115 Ti 64.85(16) . . . . ? C116 C111 C115 Ti -121.3(2) . . . . ? O12 Ti C115 C114 157.56(15) . . . . ? C105 Ti C115 C114 -104.26(16) . . . . ? C111 Ti C115 C114 114.0(2) . . . . ? C104 Ti C115 C114 -76.12(17) . . . . ? C112 Ti C115 C114 76.97(16) . . . . ? C102 Ti C115 C114 -23.2(2) . . . . ? C101 Ti C115 C114 -86.9(3) . . . . ? C103 Ti C115 C114 -41.38(17) . . . . ? C113 Ti C115 C114 36.05(15) . . . . ? O12 Ti C115 C111 43.58(16) . . . . ? C105 Ti C115 C111 141.76(14) . . . . ? C104 Ti C115 C111 169.90(15) . . . . ? C112 Ti C115 C111 -37.02(14) . . . . ? C102 Ti C115 C111 -137.20(16) . . . . ? C101 Ti C115 C111 159.1(2) . . . . ? C103 Ti C115 C111 -155.36(15) . . . . ? C113 Ti C115 C111 -77.93(16) . . . . ? C114 Ti C115 C111 -114.0(2) . . . . ? O12 Ti C115 C120 -78.1(3) . . . . ? C105 Ti C115 C120 20.1(3) . . . . ? C111 Ti C115 C120 -121.7(3) . . . . ? C104 Ti C115 C120 48.2(3) . . . . ? C112 Ti C115 C120 -158.7(3) . . . . ? C102 Ti C115 C120 101.2(3) . . . . ? C101 Ti C115 C120 37.4(4) . . . . ? C103 Ti C115 C120 83.0(3) . . . . ? C113 Ti C115 C120 160.4(3) . . . . ? C114 Ti C115 C120 124.4(3) . . . . ? C203 C201 C202 C203 -0.1(8) . . . 3_675 ? C200 C201 C202 C203 -174.6(6) . . . 3_675 ? C202 C201 C203 C202 0.1(8) . . . 3_675 ? C200 C201 C203 C202 174.8(6) . . . 3_675 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.987 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.072 data_meti _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C110.50 H200 O24 Si16 Ti' _chemical_formula_weight 2410.04 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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0428(3) _cell_length_b 22.4605(9) _cell_length_c 25.5404(9) _cell_angle_alpha 106.667(3) _cell_angle_beta 99.602(3) _cell_angle_gamma 100.045(3) _cell_volume 6342.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7384 _cell_measurement_theta_min 0.9 _cell_measurement_theta_max ?26.7 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2602 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker AXS SMART CCD System' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31546 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.86 _diffrn_reflns_theta_max 26.71 _reflns_number_total 24118 _reflns_number_gt 15483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART CCD System' _computing_cell_refinement 'Bruker AXS SMART CCD System' _computing_data_reduction 'Bruker AXS SMART CCD System' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP5' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+17.2592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24118 _refine_ls_number_parameters 1382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1335 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.1943 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.35235(7) 0.04488(4) 0.32099(3) 0.02563(19) Uani 1 d . . . Si1 Si 0.62775(13) 0.28418(7) 0.28500(6) 0.0374(3) Uani 1 d . . . Si2 Si 0.62701(12) 0.14372(7) 0.25407(6) 0.0346(3) Uani 1 d . . . Si3 Si 0.35867(11) 0.10979(6) 0.22304(5) 0.0280(3) Uani 1 d . . . Si4 Si 0.36286(13) 0.25409(6) 0.25398(6) 0.0362(3) Uani 1 d . . . Si5 Si 0.60451(12) 0.28515(6) 0.40282(6) 0.0291(3) Uani 1 d . . . Si6 Si 0.61229(12) 0.14268(6) 0.37076(6) 0.0304(3) Uani 1 d . . . Si7 Si 0.39081(13) 0.33107(7) 0.37632(7) 0.0404(4) Uani 1 d . . . Si8 Si 0.17102(16) 0.33525(8) 0.42698(9) 0.0615(5) Uani 1 d . . . O1 O 0.6578(3) 0.21716(17) 0.26011(15) 0.0423(9) Uani 1 d . . . O2 O 0.4928(3) 0.11514(18) 0.22697(15) 0.0441(9) Uani 1 d . . . O3 O 0.3345(3) 0.17909(15) 0.23635(15) 0.0380(8) Uani 1 d . . . O4 O 0.4972(3) 0.28100(16) 0.25761(16) 0.0432(9) Uani 1 d . . . O5 O 0.6434(3) 0.30079(16) 0.35077(15) 0.0419(9) Uani 1 d . . . O6 O 0.6557(3) 0.13645(16) 0.31421(15) 0.0389(8) Uani 1 d . . . O7 O 0.3179(3) 0.07928(15) 0.26705(13) 0.0332(8) Uani 1 d . . . O8 O 0.3373(3) 0.28258(17) 0.31434(16) 0.0485(10) Uani 1 d . . . O9 O 0.5874(3) 0.21186(15) 0.39316(15) 0.0384(8) Uani 1 d . . . O10 O 0.4963(3) 0.09077(14) 0.35932(13) 0.0308(7) Uani 1 d . . . O11 O 0.2919(3) 0.33537(19) 0.40914(18) 0.0590(11) Uani 1 d . . . O12 O 0.4840(3) 0.30309(16) 0.40739(15) 0.0398(9) Uani 1 d . . . C11 C 0.7268(5) 0.3460(3) 0.2722(2) 0.0490(15) Uani 1 d . . . H11 H 0.7146 0.3362 0.2306 0.059 Uiso 1 calc R . . C12 C 0.8500(6) 0.3454(3) 0.2946(3) 0.071(2) Uani 1 d . . . H12A H 0.8650 0.3037 0.2750 0.085 Uiso 1 calc R . . H12B H 0.8623 0.3506 0.3351 0.085 Uiso 1 calc R . . C13 C 0.9339(7) 0.3989(4) 0.2862(4) 0.091(3) Uani 1 d . . . H13A H 1.0144 0.3988 0.3026 0.109 Uiso 1 calc R . . H13B H 0.9261 0.3918 0.2455 0.109 Uiso 1 calc R . . C14 C 0.9099(8) 0.4609(4) 0.3131(4) 0.097(3) Uani 1 d . . . H14A H 0.9658 0.4954 0.3078 0.117 Uiso 1 calc R . . H14B H 0.9201 0.4685 0.3540 0.117 Uiso 1 calc R . . C15 C 0.7901(8) 0.4629(3) 0.2890(4) 0.093(3) Uani 1 d . . . H15A H 0.7811 0.4578 0.2487 0.112 Uiso 1 calc R . . H15B H 0.7754 0.5048 0.3082 0.112 Uiso 1 calc R . . C16 C 0.7042(6) 0.4104(3) 0.2960(3) 0.070(2) Uani 1 d . . . H16A H 0.7067 0.4190 0.3365 0.084 Uiso 1 calc R . . H16B H 0.6253 0.4105 0.2773 0.084 Uiso 1 calc R . . C21 C 0.7130(5) 0.1047(3) 0.2095(3) 0.071(2) Uani 1 d . . . H21 H 0.7108 0.0692 0.2259 0.085 Uiso 1 calc R . . C22 C 0.6706(7) 0.0679(7) 0.1613(4) 0.213(9) Uani 1 d . . . H22A H 0.6329 0.0926 0.1403 0.256 Uiso 1 calc R . . H22B H 0.6078 0.0348 0.1639 0.256 Uiso 1 calc R . . C23 C 0.7404(6) 0.0333(4) 0.1249(3) 0.106(3) Uani 1 d . . . H23A H 0.7244 -0.0122 0.1229 0.127 Uiso 1 calc R . . H23B H 0.7175 0.0350 0.0864 0.127 Uiso 1 calc R . . C24 C 0.8661(7) 0.0627(9) 0.1477(5) 0.287(13) Uani 1 d . . . H24A H 0.9050 0.0267 0.1422 0.345 Uiso 1 calc R . . H24B H 0.8901 0.0863 0.1226 0.345 Uiso 1 calc R . . C25 C 0.9093(6) 0.0980(4) 0.1950(4) 0.090(3) Uani 1 d . . . H25A H 0.9703 0.1321 0.1923 0.108 Uiso 1 calc R . . H25B H 0.9494 0.0732 0.2150 0.108 Uiso 1 calc R . . C26 C 0.8401(5) 0.1303(3) 0.2320(3) 0.0579(17) Uani 1 d . . . H26A H 0.8594 0.1766 0.2372 0.069 Uiso 1 calc R . . H26B H 0.8617 0.1252 0.2694 0.069 Uiso 1 calc R . . C31 C 0.2864(4) 0.0591(2) 0.15160(19) 0.0315(11) Uani 1 d . . . H31 H 0.3165 0.0195 0.1451 0.038 Uiso 1 calc R . . C32 C 0.1586(4) 0.0375(2) 0.1406(2) 0.0380(12) Uani 1 d . . . H32A H 0.1244 0.0753 0.1469 0.046 Uiso 1 calc R . . H32B H 0.1387 0.0155 0.1674 0.046 Uiso 1 calc R . . C33 C 0.1066(5) -0.0070(3) 0.0816(2) 0.0425(13) Uani 1 d . . . H33A H 0.1333 -0.0472 0.0766 0.051 Uiso 1 calc R . . H33B H 0.0212 -0.0179 0.0754 0.051 Uiso 1 calc R . . C34 C 0.1400(5) 0.0223(3) 0.0397(2) 0.0520(15) Uani 1 d . . . H34A H 0.1101 -0.0095 0.0017 0.062 Uiso 1 calc R . . H34B H 0.1035 0.0588 0.0412 0.062 Uiso 1 calc R . . C35 C 0.2664(5) 0.0450(3) 0.0493(2) 0.0439(13) Uani 1 d . . . H35A H 0.2833 0.0681 0.0228 0.053 Uiso 1 calc R . . H35B H 0.3018 0.0077 0.0416 0.053 Uiso 1 calc R . . C36 C 0.3206(5) 0.0891(2) 0.1092(2) 0.0363(12) Uani 1 d . . . H36A H 0.4060 0.0990 0.1150 0.044 Uiso 1 calc R . . H36B H 0.2956 0.1298 0.1149 0.044 Uiso 1 calc R . . C41 C 0.2725(6) 0.2806(3) 0.2062(3) 0.0644(19) Uani 1 d . . . H41 H 0.2862 0.3278 0.2247 0.077 Uiso 1 calc R . . C42 C 0.1446(6) 0.2543(4) 0.2011(4) 0.089(3) Uani 1 d . . . H42A H 0.1259 0.2071 0.1847 0.107 Uiso 1 calc R . . H42B H 0.1281 0.2653 0.2389 0.107 Uiso 1 calc R . . C43 C 0.0681(8) 0.2810(7) 0.1644(5) 0.140(5) Uani 1 d . . . H43A H -0.0137 0.2585 0.1583 0.168 Uiso 1 calc R . . H43B H 0.0757 0.3268 0.1847 0.168 Uiso 1 calc R . . C44 C 0.0945(8) 0.2751(6) 0.1129(4) 0.109(3) Uani 1 d . . . H44A H 0.0468 0.2973 0.0932 0.131 Uiso 1 calc R . . H44B H 0.0740 0.2293 0.0900 0.131 Uiso 1 calc R . . C45 C 0.2181(8) 0.3019(4) 0.1175(3) 0.085(3) Uani 1 d . . . H45A H 0.2363 0.3490 0.1348 0.102 Uiso 1 calc R . . H45B H 0.2341 0.2920 0.0795 0.102 Uiso 1 calc R . . C46 C 0.2953(7) 0.2735(5) 0.1535(4) 0.096(3) Uani 1 d . . . H46A H 0.2843 0.2274 0.1331 0.115 Uiso 1 calc R . . H46B H 0.3774 0.2945 0.1582 0.115 Uiso 1 calc R . . C51 C 0.7143(6) 0.3281(3) 0.4672(2) 0.0600(18) Uani 1 d . . . H51 H 0.7628 0.2964 0.4685 0.072 Uiso 1 calc R . . C52 C 0.6655(5) 0.3320(3) 0.5186(2) 0.0499(15) Uani 1 d . . . H52A H 0.6077 0.3585 0.5195 0.060 Uiso 1 calc R . . H52B H 0.6251 0.2886 0.5161 0.060 Uiso 1 calc R . . C53 C 0.7579(8) 0.3603(5) 0.5724(3) 0.117(4) Uani 1 d . . . H53A H 0.7193 0.3729 0.6038 0.140 Uiso 1 calc R . . H53B H 0.7964 0.3263 0.5778 0.140 Uiso 1 calc R . . C54 C 0.8390(8) 0.4103(5) 0.5762(3) 0.112(4) Uani 1 d . . . H54A H 0.9029 0.4171 0.6088 0.134 Uiso 1 calc R . . H54B H 0.8060 0.4485 0.5843 0.134 Uiso 1 calc R . . C55 C 0.8890(6) 0.4066(4) 0.5265(3) 0.080(2) Uani 1 d . . . H55A H 0.9433 0.3781 0.5248 0.097 Uiso 1 calc R . . H55B H 0.9332 0.4497 0.5302 0.097 Uiso 1 calc R . . C56 C 0.7965(8) 0.3818(5) 0.4736(3) 0.117(4) Uani 1 d . . . H56A H 0.7566 0.4163 0.4713 0.140 Uiso 1 calc R . . H56B H 0.8342 0.3726 0.4415 0.140 Uiso 1 calc R . . C61 C 0.7273(4) 0.1328(2) 0.4215(2) 0.0364(12) Uani 1 d . . . H61 H 0.7216 0.0857 0.4117 0.044 Uiso 1 calc R . . C62 C 0.7136(5) 0.1557(3) 0.4810(2) 0.0469(14) Uani 1 d . . . H62A H 0.7120 0.2015 0.4912 0.056 Uiso 1 calc R . . H62B H 0.6383 0.1317 0.4832 0.056 Uiso 1 calc R . . C63 C 0.8082(6) 0.1478(3) 0.5226(3) 0.0637(19) Uani 1 d . . . H63A H 0.8030 0.1016 0.5163 0.076 Uiso 1 calc R . . H63B H 0.7985 0.1673 0.5611 0.076 Uiso 1 calc R . . C64 C 0.9245(6) 0.1786(3) 0.5173(3) 0.073(2) Uani 1 d . . . H64A H 0.9325 0.2254 0.5274 0.087 Uiso 1 calc R . . H64B H 0.9858 0.1709 0.5439 0.087 Uiso 1 calc R . . C65 C 0.9400(5) 0.1530(3) 0.4595(3) 0.0630(18) Uani 1 d . . . H65A H 0.9375 0.1068 0.4504 0.076 Uiso 1 calc R . . H65B H 1.0169 0.1749 0.4570 0.076 Uiso 1 calc R . . C66 C 0.8473(5) 0.1626(3) 0.4177(3) 0.0473(14) Uani 1 d . . . H66A H 0.8578 0.1433 0.3793 0.057 Uiso 1 calc R . . H66B H 0.8550 0.2089 0.4245 0.057 Uiso 1 calc R . . C71 C 0.4594(5) 0.4085(2) 0.3753(2) 0.0470(14) Uani 1 d . . . H71 H 0.5227 0.4026 0.3549 0.056 Uiso 1 calc R . . C72 C 0.5141(8) 0.4550(3) 0.4327(3) 0.091(3) Uani 1 d . . . H72A H 0.4530 0.4627 0.4536 0.110 Uiso 1 calc R . . H72B H 0.5676 0.4360 0.4531 0.110 Uiso 1 calc R . . C73 C 0.5797(8) 0.5175(3) 0.4319(4) 0.110(4) Uani 1 d . . . H73A H 0.6103 0.5469 0.4709 0.132 Uiso 1 calc R . . H73B H 0.6464 0.5107 0.4149 0.132 Uiso 1 calc R . . C74 C 0.5079(7) 0.5464(3) 0.4006(3) 0.082(2) Uani 1 d . . . H74A H 0.5559 0.5852 0.3976 0.098 Uiso 1 calc R . . H74B H 0.4480 0.5593 0.4207 0.098 Uiso 1 calc R . . C75 C 0.4525(12) 0.5025(4) 0.3451(4) 0.157(6) Uani 1 d . . . H75A H 0.5122 0.4937 0.3235 0.189 Uiso 1 calc R . . H75B H 0.3998 0.5225 0.3254 0.189 Uiso 1 calc R . . C76 C 0.3840(9) 0.4400(3) 0.3470(4) 0.127(5) Uani 1 d . . . H76A H 0.3221 0.4484 0.3673 0.153 Uiso 1 calc R . . H76B H 0.3468 0.4113 0.3083 0.153 Uiso 1 calc R . . C81 C 0.0559(7) 0.2788(4) 0.3692(5) 0.115(4) Uani 1 d . . . H81A H -0.0196 0.2846 0.3763 0.137 Uiso 1 calc R . . H81B H 0.0616 0.2350 0.3662 0.137 Uiso 1 calc R . . H81C H 0.0641 0.2866 0.3340 0.137 Uiso 1 calc R . . C82 C 0.1813(8) 0.3136(4) 0.4908(4) 0.097(3) Uani 1 d . . . H82A H 0.1938 0.2703 0.4830 0.116 Uiso 1 calc R . . H82B H 0.1092 0.3152 0.5036 0.116 Uiso 1 calc R . . H82C H 0.2464 0.3438 0.5200 0.116 Uiso 1 calc R . . C83 C 0.1440(6) 0.4140(3) 0.4397(3) 0.072(2) Uani 1 d . . . H83A H 0.0704 0.4144 0.4513 0.087 Uiso 1 calc R . . H83B H 0.1398 0.4253 0.4053 0.087 Uiso 1 calc R . . H83C H 0.2070 0.4450 0.4695 0.087 Uiso 1 calc R . . Si1' Si 0.34822(11) -0.27678(6) 0.12945(5) 0.0254(3) Uani 1 d . . . Si2' Si 0.30785(11) -0.14687(6) 0.12465(6) 0.0269(3) Uani 1 d . . . Si3' Si 0.41583(12) -0.08824(6) 0.24792(6) 0.0293(3) Uani 1 d . . . Si4' Si 0.35592(12) -0.22513(6) 0.25213(5) 0.0279(3) Uani 1 d . . . Si5' Si 0.08743(12) -0.33010(6) 0.11025(6) 0.0278(3) Uani 1 d . . . Si6' Si 0.06242(11) -0.19272(6) 0.13836(6) 0.0276(3) Uani 1 d . . . Si7' Si 0.13037(12) -0.32470(6) 0.23145(6) 0.0321(3) Uani 1 d . . . Si8' Si -0.08318(15) -0.30358(8) 0.28096(8) 0.0523(4) Uani 1 d . . . O1' O 0.3466(3) -0.21219(14) 0.11707(13) 0.0314(7) Uani 1 d . . . O2' O 0.3803(3) -0.09600(14) 0.18314(13) 0.0330(8) Uani 1 d . . . O3' O 0.3556(3) -0.15356(14) 0.25537(14) 0.0353(8) Uani 1 d . . . O4' O 0.3904(3) -0.26061(14) 0.19598(13) 0.0289(7) Uani 1 d . . . O5' O 0.2204(3) -0.32123(15) 0.10826(14) 0.0331(8) Uani 1 d . . . O6' O 0.1744(3) -0.15724(16) 0.12510(15) 0.0379(8) Uani 1 d . . . O7' O 0.3699(3) -0.03271(14) 0.28422(14) 0.0334(8) Uani 1 d . . . O8' O 0.2257(3) -0.25865(15) 0.24906(13) 0.0342(8) Uani 1 d . . . O9' O 0.0473(3) -0.26721(15) 0.11007(14) 0.0364(8) Uani 1 d . . . O10' O 0.0741(3) -0.17541(18) 0.20451(15) 0.0440(9) Uani 1 d . . . H10' H 0.1300 -0.1880 0.2185 0.053 Uiso 1 calc R . . O11' O 0.0380(3) -0.31250(18) 0.26756(16) 0.0473(10) Uani 1 d . . . O12' O 0.0713(3) -0.34414(15) 0.16631(14) 0.0347(8) Uani 1 d . . . C11' C 0.4492(4) -0.3157(2) 0.09556(19) 0.0296(11) Uani 1 d . . . H11' H 0.5286 -0.2893 0.1164 0.036 Uiso 1 calc R . . C12' C 0.4444(6) -0.3805(3) 0.1001(3) 0.0532(16) Uani 1 d . . . H12C H 0.3659 -0.4080 0.0813 0.064 Uiso 1 calc R . . H12D H 0.4589 -0.3775 0.1402 0.064 Uiso 1 calc R . . C13' C 0.5327(7) -0.4108(3) 0.0736(3) 0.073(2) Uani 1 d . . . H13C H 0.6117 -0.3860 0.0949 0.088 Uiso 1 calc R . . H13D H 0.5239 -0.4549 0.0752 0.088 Uiso 1 calc R . . C14' C 0.5178(6) -0.4126(3) 0.0143(3) 0.0606(18) Uani 1 d . . . H14C H 0.5776 -0.4316 -0.0021 0.073 Uiso 1 calc R . . H14D H 0.4408 -0.4399 -0.0076 0.073 Uiso 1 calc R . . C15' C 0.5276(6) -0.3481(3) 0.0107(3) 0.0566(16) Uani 1 d . . . H15C H 0.5167 -0.3502 -0.0292 0.068 Uiso 1 calc R . . H15D H 0.6060 -0.3215 0.0309 0.068 Uiso 1 calc R . . C16' C 0.4383(6) -0.3181(3) 0.0357(2) 0.0521(15) Uani 1 d . . . H16C H 0.4478 -0.2741 0.0338 0.063 Uiso 1 calc R . . H16D H 0.3600 -0.3429 0.0135 0.063 Uiso 1 calc R . . C21' C 0.3340(4) -0.1205(2) 0.0665(2) 0.0336(11) Uani 1 d . . . H21' H 0.3055 -0.0806 0.0704 0.040 Uiso 1 calc R . . C22' C 0.2675(5) -0.1686(3) 0.0111(2) 0.0499(15) Uani 1 d . . . H22C H 0.2897 -0.2098 0.0072 0.060 Uiso 1 calc R . . H22D H 0.1836 -0.1758 0.0100 0.060 Uiso 1 calc R . . C23' C 0.2906(7) -0.1467(4) -0.0370(3) 0.072(2) Uani 1 d . . . H23C H 0.2589 -0.1087 -0.0361 0.087 Uiso 1 calc R . . H23D H 0.2510 -0.1810 -0.0729 0.087 Uiso 1 calc R . . C24' C 0.4184(7) -0.1303(5) -0.0340(3) 0.088(3) Uani 1 d . . . H24C H 0.4483 -0.1694 -0.0389 0.106 Uiso 1 calc R . . H24D H 0.4318 -0.1138 -0.0650 0.106 Uiso 1 calc R . . C25' C 0.4822(6) -0.0818(4) 0.0201(3) 0.071(2) Uani 1 d . . . H25C H 0.4569 -0.0415 0.0236 0.086 Uiso 1 calc R . . H25D H 0.5661 -0.0731 0.0211 0.086 Uiso 1 calc R . . C26' C 0.4619(5) -0.1038(3) 0.0679(3) 0.0487(15) Uani 1 d . . . H26C H 0.5028 -0.0697 0.1036 0.058 Uiso 1 calc R . . H26D H 0.4939 -0.1418 0.0663 0.058 Uiso 1 calc R . . C31' C 0.5745(5) -0.0698(3) 0.2685(2) 0.0482(15) Uani 1 d . . . H31' H 0.6005 -0.0306 0.2584 0.058 Uiso 1 calc R . . C32' C 0.6274(5) -0.1180(3) 0.2357(3) 0.0649(18) Uani 1 d . . . H32C H 0.6000 -0.1253 0.1952 0.078 Uiso 1 calc R . . H32D H 0.6038 -0.1590 0.2427 0.078 Uiso 1 calc R . . C33' C 0.7585(6) -0.0950(5) 0.2526(3) 0.090(3) Uani 1 d . . . H33C H 0.7939 -0.1282 0.2318 0.108 Uiso 1 calc R . . H33D H 0.7822 -0.0559 0.2428 0.108 Uiso 1 calc R . . C34' C 0.8007(6) -0.0809(4) 0.3144(3) 0.079(2) Uani 1 d . . . H34C H 0.7767 -0.1199 0.3243 0.095 Uiso 1 calc R . . H34D H 0.8864 -0.0677 0.3247 0.095 Uiso 1 calc R . . C35' C 0.7535(6) -0.0302(3) 0.3454(3) 0.074(2) Uani 1 d . . . H35C H 0.7794 0.0091 0.3362 0.089 Uiso 1 calc R . . H35D H 0.7832 -0.0207 0.3862 0.089 Uiso 1 calc R . . C36' C 0.6200(5) -0.0496(3) 0.3311(2) 0.0426(13) Uani 1 d . . . H36C H 0.5938 -0.0853 0.3450 0.051 Uiso 1 calc R . . H36D H 0.5894 -0.0130 0.3499 0.051 Uiso 1 calc R . . C41' C 0.4573(5) -0.2265(2) 0.3129(2) 0.0365(12) Uani 1 d . . . H41' H 0.5242 -0.1894 0.3208 0.044 Uiso 1 calc R . . C42' C 0.4108(5) -0.2134(3) 0.3647(2) 0.0497(15) Uani 1 d . . . H42C H 0.3868 -0.1724 0.3715 0.060 Uiso 1 calc R . . H42D H 0.3413 -0.2476 0.3587 0.060 Uiso 1 calc R . . C43' C 0.4971(6) -0.2100(3) 0.4148(2) 0.0657(19) Uani 1 d . . . H43C H 0.5593 -0.1707 0.4251 0.079 Uiso 1 calc R . . H43D H 0.4589 -0.2069 0.4467 0.079 Uiso 1 calc R . . C44' C 0.5487(6) -0.2651(4) 0.4062(3) 0.0651(19) Uani 1 d . . . H44C H 0.4891 -0.3033 0.4028 0.078 Uiso 1 calc R . . H44D H 0.6114 -0.2576 0.4394 0.078 Uiso 1 calc R . . C45' C 0.5968(5) -0.2779(3) 0.3552(2) 0.0523(15) Uani 1 d . . . H45C H 0.6231 -0.3182 0.3490 0.063 Uiso 1 calc R . . H45D H 0.6648 -0.2429 0.3608 0.063 Uiso 1 calc R . . C46' C 0.5075(5) -0.2831(3) 0.3046(2) 0.0474(14) Uani 1 d . . . H46C H 0.5435 -0.2881 0.2720 0.057 Uiso 1 calc R . . H46D H 0.4448 -0.3217 0.2960 0.057 Uiso 1 calc R . . C51' C -0.0010(4) -0.3950(2) 0.0498(2) 0.0306(11) Uani 1 d . . . H51' H 0.0351 -0.4324 0.0464 0.037 Uiso 1 calc R . . C52' C -0.1227(4) -0.4156(2) 0.0559(2) 0.0418(13) Uani 1 d . . . H52C H -0.1592 -0.3787 0.0619 0.050 Uiso 1 calc R . . H52D H -0.1202 -0.4298 0.0893 0.050 Uiso 1 calc R . . C53' C -0.1949(5) -0.4694(3) 0.0045(2) 0.0486(15) Uani 1 d . . . H53C H -0.1626 -0.5077 0.0006 0.058 Uiso 1 calc R . . H53D H -0.2751 -0.4805 0.0092 0.058 Uiso 1 calc R . . C54' C -0.1969(6) -0.4512(3) -0.0468(3) 0.0582(17) Uani 1 d . . . H54C H -0.2355 -0.4153 -0.0442 0.070 Uiso 1 calc R . . H54D H -0.2423 -0.4879 -0.0798 0.070 Uiso 1 calc R . . C55' C -0.0777(5) -0.4318(3) -0.0545(2) 0.0532(16) Uani 1 d . . . H55C H -0.0817 -0.4172 -0.0877 0.064 Uiso 1 calc R . . H55D H -0.0423 -0.4691 -0.0614 0.064 Uiso 1 calc R . . C56' C -0.0034(5) -0.3790(3) -0.0038(2) 0.0467(14) Uani 1 d . . . H56C H -0.0327 -0.3399 -0.0003 0.056 Uiso 1 calc R . . H56D H 0.0767 -0.3698 -0.0090 0.056 Uiso 1 calc R . . C61' C -0.0626(4) -0.1682(2) 0.1090(2) 0.0320(11) Uani 1 d . . . H61' H -0.0503 -0.1213 0.1287 0.038 Uiso 1 calc R . . C62' C -0.0736(5) -0.1773(3) 0.0473(2) 0.0402(13) Uani 1 d . . . H62C H -0.0014 -0.1537 0.0418 0.048 Uiso 1 calc R . . H62D H -0.0845 -0.2233 0.0264 0.048 Uiso 1 calc R . . C63' C -0.1740(5) -0.1538(3) 0.0249(3) 0.0489(15) Uani 1 d . . . H63C H -0.1591 -0.1070 0.0434 0.059 Uiso 1 calc R . . H63D H -0.1812 -0.1618 -0.0159 0.059 Uiso 1 calc R . . C64' C -0.2836(5) -0.1850(3) 0.0339(3) 0.0609(18) Uani 1 d . . . H64C H -0.3030 -0.2312 0.0124 0.073 Uiso 1 calc R . . H64D H -0.3468 -0.1665 0.0201 0.073 Uiso 1 calc R . . C65' C -0.2745(5) -0.1763(3) 0.0943(3) 0.0608(18) Uani 1 d . . . H65C H -0.3472 -0.1999 0.0994 0.073 Uiso 1 calc R . . H65D H -0.2635 -0.1304 0.1153 0.073 Uiso 1 calc R . . C66' C -0.1744(5) -0.2003(3) 0.1172(3) 0.0500(15) Uani 1 d . . . H66C H -0.1686 -0.1928 0.1578 0.060 Uiso 1 calc R . . H66D H -0.1890 -0.2469 0.0983 0.060 Uiso 1 calc R . . C71' C 0.1943(4) -0.3883(2) 0.2430(2) 0.0355(12) Uani 1 d . . . H71' H 0.2462 -0.3710 0.2815 0.043 Uiso 1 calc R . . C72' C 0.1060(6) -0.4455(3) 0.2414(3) 0.069(2) Uani 1 d . . . H72C H 0.0597 -0.4320 0.2694 0.083 Uiso 1 calc R . . H72D H 0.0526 -0.4637 0.2038 0.083 Uiso 1 calc R . . C73' C 0.1632(7) -0.4954(3) 0.2539(4) 0.083(3) Uani 1 d . . . H73C H 0.2103 -0.4785 0.2930 0.100 Uiso 1 calc R . . H73D H 0.1030 -0.5332 0.2508 0.100 Uiso 1 calc R . . C74' C 0.2388(6) -0.5155(3) 0.2150(3) 0.0579(17) Uani 1 d . . . H74C H 0.1906 -0.5377 0.1765 0.069 Uiso 1 calc R . . H74D H 0.2797 -0.5459 0.2266 0.069 Uiso 1 calc R . . C75' C 0.3253(5) -0.4593(3) 0.2151(3) 0.0491(15) Uani 1 d . . . H75C H 0.3802 -0.4406 0.2522 0.059 Uiso 1 calc R . . H75D H 0.3700 -0.4734 0.1865 0.059 Uiso 1 calc R . . C76' C 0.2676(5) -0.4100(2) 0.2027(2) 0.0422(13) Uani 1 d . . . H76C H 0.2185 -0.4277 0.1640 0.051 Uiso 1 calc R . . H76D H 0.3274 -0.3727 0.2043 0.051 Uiso 1 calc R . . C81' C -0.1926(9) -0.3354(8) 0.2181(5) 0.216(8) Uani 1 d . . . H81D H -0.2640 -0.3227 0.2251 0.259 Uiso 1 calc R . . H81E H -0.2070 -0.3822 0.2051 0.259 Uiso 1 calc R . . H81F H -0.1674 -0.3190 0.1893 0.259 Uiso 1 calc R . . C82' C -0.0725(8) -0.2193(4) 0.3115(4) 0.106(3) Uani 1 d . . . H82D H -0.1419 -0.2130 0.3255 0.127 Uiso 1 calc R . . H82E H -0.0658 -0.1985 0.2829 0.127 Uiso 1 calc R . . H82F H -0.0038 -0.2006 0.3426 0.127 Uiso 1 calc R . . C83' C -0.1081(9) -0.3420(5) 0.3320(5) 0.136(5) Uani 1 d . . . H83D H -0.1336 -0.3884 0.3134 0.164 Uiso 1 calc R . . H83E H -0.1681 -0.3265 0.3500 0.164 Uiso 1 calc R . . H83F H -0.0361 -0.3322 0.3605 0.164 Uiso 1 calc R . . C101 C 0.1987(5) 0.0813(2) 0.3518(2) 0.0416(13) Uani 1 d . . . C102 C 0.1623(4) 0.0157(2) 0.3270(2) 0.0377(12) Uani 1 d . . . C103 C 0.2269(5) -0.0115(2) 0.3596(2) 0.0398(13) Uani 1 d . . . C104 C 0.3046(5) 0.0372(3) 0.4034(2) 0.0396(13) Uani 1 d . . . C105 C 0.2861(5) 0.0948(2) 0.3985(2) 0.0359(12) Uani 1 d . . . C106 C 0.1493(6) 0.1283(3) 0.3316(3) 0.0659(19) Uani 1 d . . . H10A H 0.0745 0.1297 0.3416 0.079 Uiso 1 calc R . . H10B H 0.1384 0.1160 0.2907 0.079 Uiso 1 calc R . . H10C H 0.2023 0.1707 0.3491 0.079 Uiso 1 calc R . . C107 C 0.0721(5) -0.0181(3) 0.2746(3) 0.0654(19) Uani 1 d . . . H10D H -0.0001 -0.0046 0.2785 0.078 Uiso 1 calc R . . H10E H 0.0587 -0.0644 0.2674 0.078 Uiso 1 calc R . . H10F H 0.0979 -0.0078 0.2431 0.078 Uiso 1 calc R . . C108 C 0.2128(6) -0.0804(3) 0.3503(3) 0.0613(18) Uani 1 d . . . H10G H 0.1764 -0.1043 0.3107 0.074 Uiso 1 calc R . . H10H H 0.1637 -0.0933 0.3740 0.074 Uiso 1 calc R . . H10I H 0.2889 -0.0895 0.3600 0.074 Uiso 1 calc R . . C109 C 0.3897(6) 0.0293(3) 0.4475(3) 0.0628(18) Uani 1 d . . . H10J H 0.4439 0.0706 0.4686 0.075 Uiso 1 calc R . . H10K H 0.4325 -0.0015 0.4305 0.075 Uiso 1 calc R . . H10L H 0.3496 0.0136 0.4731 0.075 Uiso 1 calc R . . C110 C 0.3488(6) 0.1596(3) 0.4378(2) 0.0566(17) Uani 1 d . . . H11A H 0.4290 0.1591 0.4527 0.068 Uiso 1 calc R . . H11B H 0.3102 0.1715 0.4688 0.068 Uiso 1 calc R . . H11C H 0.3486 0.1907 0.4176 0.068 Uiso 1 calc R . . C200 C 0.4531(15) -0.4492(9) -0.1539(5) 0.219(9) Uani 1 d . . . H20A H 0.4211 -0.4956 -0.1680 0.263 Uiso 1 calc R . . H20B H 0.5188 -0.4386 -0.1218 0.263 Uiso 1 calc R . . H20C H 0.4794 -0.4352 -0.1836 0.263 Uiso 1 calc R . . C201 C 0.3717(14) -0.4197(9) -0.1377(5) 0.135(5) Uani 1 d . . . C202 C 0.2781(13) -0.4619(9) -0.1301(5) 0.145(6) Uani 1 d . . . H202 H 0.2759 -0.5055 -0.1339 0.173 Uiso 1 calc R . . C203 C 0.1955(16) -0.4341(8) -0.1172(6) 0.153(6) Uani 1 d . . . H203 H 0.1287 -0.4601 -0.1129 0.183 Uiso 1 calc R . . C204 C 0.1950(16) -0.3662(12) -0.1086(5) 0.177(8) Uani 1 d . . . H204 H 0.1343 -0.3477 -0.0970 0.212 Uiso 1 calc R . . C205 C 0.2816(16) -0.3357(8) -0.1180(5) 0.155(6) Uani 1 d . . . H205 H 0.2847 -0.2922 -0.1148 0.187 Uiso 1 calc R . . C206 C 0.3735(11) -0.3603(7) -0.1327(5) 0.111(3) Uani 1 d . . . H206 H 0.4374 -0.3341 -0.1390 0.133 Uiso 1 calc R . . C301 C 1.1762(12) 0.1056(7) 0.5382(7) 0.075(4) Uani 0.50 d P . . C302 C 1.0880(6) 0.0541(4) 0.5190(4) 0.072(2) Uani 1 d . . . C303 C 1.0734(7) 0.0113(5) 0.4667(3) 0.073(2) Uani 1 d . . . C304 C 1.0128(7) 0.0420(4) 0.5525(3) 0.073(2) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0268(5) 0.0207(4) 0.0288(4) 0.0058(3) 0.0074(4) 0.0068(3) Si1 0.0328(9) 0.0374(8) 0.0383(8) 0.0161(6) 0.0049(7) -0.0046(6) Si2 0.0236(8) 0.0403(8) 0.0310(7) 0.0006(6) 0.0053(6) 0.0046(6) Si3 0.0237(7) 0.0252(6) 0.0279(7) 0.0016(5) 0.0024(6) 0.0019(5) Si4 0.0353(9) 0.0271(7) 0.0427(8) 0.0132(6) -0.0009(7) 0.0046(6) Si5 0.0312(8) 0.0228(6) 0.0310(7) 0.0074(5) 0.0057(6) 0.0042(5) Si6 0.0287(8) 0.0239(6) 0.0367(8) 0.0088(6) 0.0017(6) 0.0089(6) Si7 0.0398(9) 0.0319(7) 0.0463(9) 0.0054(6) 0.0050(7) 0.0171(7) Si8 0.0441(11) 0.0425(9) 0.0961(15) 0.0116(9) 0.0203(10) 0.0200(8) O1 0.037(2) 0.047(2) 0.047(2) 0.0184(18) 0.0171(18) 0.0066(17) O2 0.022(2) 0.057(2) 0.040(2) -0.0020(17) 0.0058(16) 0.0062(17) O3 0.038(2) 0.0251(17) 0.050(2) 0.0087(15) 0.0147(17) 0.0054(15) O4 0.039(2) 0.0352(19) 0.052(2) 0.0191(17) 0.0004(18) 0.0007(16) O5 0.042(2) 0.043(2) 0.038(2) 0.0164(17) 0.0090(17) 0.0005(17) O6 0.029(2) 0.045(2) 0.047(2) 0.0174(17) 0.0093(17) 0.0156(16) O7 0.035(2) 0.0339(18) 0.0304(18) 0.0108(14) 0.0039(15) 0.0105(15) O8 0.037(2) 0.043(2) 0.050(2) -0.0064(17) 0.0018(18) 0.0151(17) O9 0.042(2) 0.0264(17) 0.052(2) 0.0155(16) 0.0124(18) 0.0158(15) O10 0.0295(19) 0.0265(16) 0.0324(18) 0.0080(14) 0.0004(15) 0.0056(14) O11 0.047(3) 0.061(3) 0.069(3) 0.009(2) 0.021(2) 0.029(2) O12 0.043(2) 0.0358(19) 0.050(2) 0.0179(17) 0.0147(18) 0.0214(17) C11 0.039(4) 0.055(4) 0.042(3) 0.020(3) 0.003(3) -0.015(3) C12 0.051(5) 0.078(5) 0.072(5) 0.026(4) 0.015(4) -0.018(4) C13 0.068(5) 0.089(6) 0.093(6) 0.031(5) 0.013(5) -0.038(4) C14 0.098(7) 0.074(6) 0.083(6) 0.011(4) 0.020(5) -0.048(5) C15 0.116(8) 0.052(4) 0.100(7) 0.029(4) 0.030(6) -0.020(5) C16 0.082(5) 0.047(4) 0.075(5) 0.026(3) 0.017(4) -0.012(3) C21 0.027(4) 0.080(5) 0.069(5) -0.028(4) 0.017(3) 0.002(3) C22 0.025(5) 0.330(17) 0.129(9) -0.151(10) -0.003(5) 0.042(7) C23 0.048(5) 0.143(8) 0.077(6) -0.046(5) 0.013(4) 0.037(5) C24 0.026(6) 0.49(3) 0.147(11) -0.182(15) -0.003(6) 0.061(9) C25 0.037(4) 0.119(7) 0.088(6) -0.012(5) 0.025(4) 0.018(4) C26 0.030(4) 0.085(5) 0.046(4) 0.004(3) 0.009(3) 0.012(3) C31 0.030(3) 0.034(3) 0.025(2) 0.006(2) 0.003(2) 0.002(2) C32 0.029(3) 0.041(3) 0.034(3) 0.006(2) 0.003(2) -0.003(2) C33 0.031(3) 0.044(3) 0.040(3) 0.008(2) -0.002(2) -0.002(2) C34 0.045(4) 0.068(4) 0.038(3) 0.017(3) -0.002(3) 0.011(3) C35 0.047(4) 0.060(4) 0.031(3) 0.020(3) 0.010(3) 0.019(3) C36 0.035(3) 0.038(3) 0.037(3) 0.015(2) 0.011(2) 0.006(2) C41 0.058(5) 0.070(4) 0.068(5) 0.045(4) -0.004(4) 0.004(3) C42 0.037(4) 0.134(7) 0.115(7) 0.086(6) -0.009(4) 0.013(4) C43 0.076(7) 0.241(14) 0.132(10) 0.107(10) 0.000(6) 0.060(8) C44 0.082(7) 0.194(11) 0.065(6) 0.056(6) -0.003(5) 0.061(7) C45 0.113(7) 0.114(6) 0.061(5) 0.054(5) 0.023(5) 0.065(6) C46 0.083(6) 0.135(8) 0.083(6) 0.051(6) 0.012(5) 0.038(6) C51 0.051(4) 0.061(4) 0.043(4) -0.002(3) 0.009(3) -0.017(3) C52 0.050(4) 0.050(3) 0.033(3) -0.001(2) 0.009(3) -0.007(3) C53 0.105(7) 0.158(9) 0.035(4) 0.000(5) 0.002(4) -0.038(7) C54 0.085(7) 0.139(8) 0.053(5) -0.003(5) -0.009(5) -0.040(6) C55 0.051(5) 0.092(6) 0.058(5) -0.003(4) -0.004(4) -0.024(4) C56 0.088(6) 0.166(9) 0.049(5) 0.017(5) 0.009(4) -0.054(6) C61 0.036(3) 0.023(2) 0.044(3) 0.007(2) -0.001(2) 0.008(2) C62 0.050(4) 0.042(3) 0.047(3) 0.017(3) 0.001(3) 0.012(3) C63 0.074(5) 0.063(4) 0.049(4) 0.020(3) -0.010(3) 0.021(4) C64 0.061(5) 0.070(5) 0.063(5) 0.009(4) -0.027(4) 0.017(4) C65 0.038(4) 0.064(4) 0.071(5) 0.010(3) -0.012(3) 0.015(3) C66 0.033(3) 0.042(3) 0.056(4) 0.007(3) -0.004(3) 0.009(3) C71 0.062(4) 0.031(3) 0.047(3) 0.010(2) 0.004(3) 0.022(3) C72 0.114(7) 0.034(3) 0.088(6) 0.013(3) -0.042(5) -0.004(4) C73 0.110(7) 0.036(4) 0.139(8) 0.013(4) -0.039(6) -0.002(4) C74 0.114(7) 0.033(3) 0.090(6) 0.017(4) -0.002(5) 0.028(4) C75 0.285(15) 0.043(4) 0.098(7) 0.034(5) -0.073(8) 0.014(7) C76 0.172(10) 0.037(4) 0.127(8) 0.025(4) -0.079(7) 0.015(5) C81 0.068(6) 0.054(5) 0.190(11) 0.010(5) -0.008(6) 0.020(4) C82 0.103(7) 0.083(6) 0.137(8) 0.055(6) 0.062(6) 0.036(5) C83 0.058(5) 0.055(4) 0.109(6) 0.020(4) 0.029(4) 0.028(3) Si1' 0.0289(8) 0.0227(6) 0.0269(7) 0.0078(5) 0.0082(6) 0.0103(5) Si2' 0.0268(7) 0.0251(6) 0.0319(7) 0.0116(5) 0.0084(6) 0.0086(5) Si3' 0.0305(8) 0.0241(6) 0.0314(7) 0.0040(5) 0.0075(6) 0.0096(6) Si4' 0.0364(8) 0.0232(6) 0.0249(7) 0.0066(5) 0.0064(6) 0.0116(6) Si5' 0.0276(8) 0.0222(6) 0.0314(7) 0.0071(5) 0.0041(6) 0.0057(5) Si6' 0.0261(8) 0.0255(6) 0.0325(7) 0.0087(5) 0.0079(6) 0.0095(5) Si7' 0.0332(8) 0.0334(7) 0.0320(7) 0.0107(6) 0.0119(6) 0.0095(6) Si8' 0.0422(10) 0.0525(10) 0.0657(12) 0.0144(8) 0.0281(9) 0.0134(8) O1' 0.039(2) 0.0284(16) 0.0354(19) 0.0155(14) 0.0149(16) 0.0161(15) O2' 0.036(2) 0.0296(17) 0.0325(19) 0.0099(14) 0.0054(15) 0.0069(15) O3' 0.050(2) 0.0236(16) 0.0338(19) 0.0078(14) 0.0118(16) 0.0139(15) O4' 0.037(2) 0.0267(16) 0.0270(17) 0.0092(13) 0.0099(15) 0.0146(14) O5' 0.0277(19) 0.0321(17) 0.0365(19) 0.0071(15) 0.0067(15) 0.0069(14) O6' 0.027(2) 0.0400(19) 0.054(2) 0.0240(17) 0.0117(17) 0.0100(15) O7' 0.035(2) 0.0225(16) 0.042(2) 0.0040(14) 0.0141(16) 0.0091(14) O8' 0.036(2) 0.0319(17) 0.0313(19) 0.0049(14) 0.0085(15) 0.0074(15) O9' 0.036(2) 0.0262(17) 0.044(2) 0.0091(15) 0.0028(16) 0.0100(15) O10' 0.047(3) 0.054(2) 0.035(2) 0.0117(17) 0.0103(18) 0.0268(19) O11' 0.045(2) 0.053(2) 0.053(2) 0.0181(19) 0.0265(19) 0.0183(19) O12' 0.032(2) 0.0359(18) 0.0337(19) 0.0110(15) 0.0046(15) 0.0053(15) C11' 0.037(3) 0.028(2) 0.025(2) 0.0068(19) 0.007(2) 0.014(2) C12' 0.082(5) 0.044(3) 0.054(4) 0.024(3) 0.037(3) 0.036(3) C13' 0.112(6) 0.067(4) 0.078(5) 0.037(4) 0.049(5) 0.067(4) C14' 0.064(4) 0.046(3) 0.068(5) 0.001(3) 0.034(4) 0.018(3) C15' 0.072(5) 0.055(4) 0.048(4) 0.009(3) 0.030(3) 0.024(3) C16' 0.064(4) 0.058(4) 0.044(3) 0.016(3) 0.019(3) 0.032(3) C21' 0.040(3) 0.037(3) 0.036(3) 0.021(2) 0.016(2) 0.019(2) C22' 0.057(4) 0.059(4) 0.038(3) 0.018(3) 0.017(3) 0.017(3) C23' 0.089(6) 0.099(6) 0.042(4) 0.034(4) 0.023(4) 0.030(5) C24' 0.097(6) 0.140(8) 0.081(6) 0.072(6) 0.065(5) 0.062(6) C25' 0.063(5) 0.099(6) 0.089(6) 0.065(5) 0.044(4) 0.030(4) C26' 0.039(3) 0.059(4) 0.064(4) 0.036(3) 0.023(3) 0.017(3) C31' 0.039(3) 0.058(4) 0.039(3) 0.002(3) 0.000(3) 0.023(3) C32' 0.052(4) 0.086(5) 0.054(4) 0.012(4) 0.015(3) 0.025(4) C33' 0.040(4) 0.181(9) 0.052(4) 0.035(5) 0.013(3) 0.036(5) C34' 0.057(5) 0.100(6) 0.077(5) 0.021(4) 0.007(4) 0.031(4) C35' 0.059(5) 0.064(4) 0.065(5) -0.020(3) -0.026(4) 0.035(4) C36' 0.042(3) 0.039(3) 0.041(3) 0.003(2) 0.003(3) 0.019(3) C41' 0.043(3) 0.034(3) 0.031(3) 0.008(2) 0.005(2) 0.014(2) C42' 0.062(4) 0.063(4) 0.033(3) 0.017(3) 0.013(3) 0.036(3) C43' 0.091(5) 0.086(5) 0.029(3) 0.017(3) 0.014(3) 0.047(4) C44' 0.072(5) 0.091(5) 0.046(4) 0.035(4) 0.005(3) 0.038(4) C45' 0.044(4) 0.065(4) 0.049(4) 0.019(3) 0.001(3) 0.024(3) C46' 0.054(4) 0.050(3) 0.042(3) 0.013(3) 0.011(3) 0.025(3) C51' 0.031(3) 0.028(2) 0.031(3) 0.007(2) 0.005(2) 0.007(2) C52' 0.032(3) 0.037(3) 0.047(3) 0.002(2) 0.009(3) 0.003(2) C53' 0.033(3) 0.042(3) 0.051(4) -0.002(3) 0.002(3) -0.004(2) C54' 0.055(4) 0.051(4) 0.046(4) -0.002(3) -0.009(3) 0.007(3) C55' 0.064(4) 0.050(3) 0.033(3) 0.006(3) 0.003(3) 0.001(3) C56' 0.051(4) 0.044(3) 0.040(3) 0.012(3) 0.008(3) 0.003(3) C61' 0.025(3) 0.028(2) 0.045(3) 0.011(2) 0.011(2) 0.012(2) C62' 0.034(3) 0.043(3) 0.047(3) 0.017(3) 0.009(3) 0.014(2) C63' 0.045(4) 0.052(3) 0.058(4) 0.029(3) 0.007(3) 0.021(3) C64' 0.043(4) 0.063(4) 0.084(5) 0.039(4) 0.004(3) 0.015(3) C65' 0.034(4) 0.078(5) 0.091(5) 0.045(4) 0.025(3) 0.026(3) C66' 0.035(3) 0.063(4) 0.067(4) 0.033(3) 0.022(3) 0.022(3) C71' 0.038(3) 0.039(3) 0.034(3) 0.016(2) 0.010(2) 0.009(2) C72' 0.061(5) 0.058(4) 0.113(6) 0.052(4) 0.039(4) 0.021(3) C73' 0.075(5) 0.069(5) 0.144(8) 0.075(5) 0.050(5) 0.025(4) C74' 0.072(5) 0.033(3) 0.063(4) 0.017(3) 0.002(4) 0.011(3) C75' 0.064(4) 0.046(3) 0.051(4) 0.023(3) 0.021(3) 0.029(3) C76' 0.057(4) 0.038(3) 0.036(3) 0.013(2) 0.014(3) 0.019(3) C81' 0.058(7) 0.34(2) 0.136(11) -0.059(12) -0.016(7) 0.018(9) C82' 0.125(8) 0.073(5) 0.154(9) 0.040(6) 0.085(7) 0.058(5) C83' 0.153(9) 0.132(8) 0.237(13) 0.135(9) 0.159(10) 0.088(7) C101 0.038(3) 0.042(3) 0.055(4) 0.017(3) 0.024(3) 0.019(2) C102 0.030(3) 0.043(3) 0.037(3) 0.009(2) 0.012(2) 0.005(2) C103 0.048(3) 0.033(3) 0.045(3) 0.016(2) 0.027(3) 0.005(2) C104 0.045(3) 0.045(3) 0.039(3) 0.018(2) 0.020(3) 0.019(3) C105 0.043(3) 0.033(3) 0.032(3) 0.006(2) 0.018(2) 0.009(2) C106 0.064(5) 0.073(4) 0.090(5) 0.042(4) 0.035(4) 0.049(4) C107 0.039(4) 0.089(5) 0.058(4) 0.019(4) 0.012(3) -0.006(3) C108 0.090(5) 0.033(3) 0.072(4) 0.020(3) 0.046(4) 0.010(3) C109 0.069(5) 0.087(5) 0.047(4) 0.038(4) 0.018(3) 0.025(4) C110 0.070(4) 0.040(3) 0.049(4) -0.005(3) 0.028(3) 0.004(3) C200 0.27(2) 0.34(2) 0.102(10) 0.059(12) 0.068(12) 0.213(19) C201 0.153(13) 0.176(13) 0.079(7) 0.039(8) 0.005(7) 0.074(12) C202 0.100(10) 0.225(17) 0.118(10) 0.100(11) 0.020(8) -0.008(11) C203 0.141(14) 0.174(15) 0.149(13) 0.088(11) 0.005(11) 0.016(11) C204 0.175(16) 0.33(3) 0.086(9) 0.095(13) 0.063(9) 0.146(17) C205 0.167(15) 0.239(17) 0.071(8) 0.063(9) 0.035(9) 0.047(14) C206 0.110(9) 0.136(10) 0.090(8) 0.054(7) 0.006(6) 0.022(8) C301 0.033(8) 0.073(10) 0.114(13) 0.033(9) 0.008(8) 0.002(7) C302 0.056(5) 0.103(6) 0.086(6) 0.056(5) 0.021(4) 0.043(4) C303 0.066(5) 0.116(7) 0.064(5) 0.045(5) 0.027(4) 0.049(5) C304 0.067(5) 0.116(7) 0.060(5) 0.040(5) 0.024(4) 0.053(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O7 1.789(3) . ? Ti O7' 1.794(3) . ? Ti O10 1.805(3) . ? Ti C102 2.311(5) . ? Ti C101 2.315(5) . ? Ti C104 2.317(5) . ? Ti C105 2.319(5) . ? Ti C103 2.324(5) . ? Si1 O5 1.583(4) . ? Si1 O1 1.587(4) . ? Si1 O4 1.592(4) . ? Si1 C11 1.809(5) . ? Si2 O6 1.579(4) . ? Si2 O1 1.582(4) . ? Si2 O2 1.585(4) . ? Si2 C21 1.810(6) . ? Si3 O7 1.575(3) . ? Si3 O2 1.583(4) . ? Si3 O3 1.585(3) . ? Si3 C31 1.821(5) . ? Si4 O3 1.571(3) . ? Si4 O8 1.594(4) . ? Si4 O4 1.602(4) . ? Si4 C41 1.797(6) . ? Si5 O9 1.564(3) . ? Si5 O12 1.586(4) . ? Si5 O5 1.590(4) . ? Si5 C51 1.818(6) . ? Si6 O10 1.580(3) . ? Si6 O6 1.594(4) . ? Si6 O9 1.594(3) . ? Si6 C61 1.822(5) . ? Si7 O11 1.568(4) . ? Si7 O12 1.587(4) . ? Si7 O8 1.592(4) . ? Si7 C71 1.800(6) . ? Si8 O11 1.596(4) . ? Si8 C83 1.801(6) . ? Si8 C82 1.820(9) . ? Si8 C81 1.827(8) . ? C11 C16 1.491(9) . ? C11 C12 1.503(9) . ? C12 C13 1.520(8) . ? C13 C14 1.468(12) . ? C14 C15 1.484(12) . ? C15 C16 1.499(8) . ? C21 C22 1.231(9) . ? C21 C26 1.488(8) . ? C22 C23 1.501(9) . ? C23 C24 1.484(12) . ? C24 C25 1.206(11) . ? C25 C26 1.482(8) . ? C31 C32 1.483(7) . ? C31 C36 1.506(6) . ? C32 C33 1.504(7) . ? C33 C34 1.483(8) . ? C34 C35 1.472(8) . ? C35 C36 1.522(7) . ? C41 C46 1.389(10) . ? C41 C42 1.519(9) . ? C42 C43 1.519(10) . ? C43 C44 1.379(12) . ? C44 C45 1.477(11) . ? C45 C46 1.540(10) . ? C51 C56 1.372(9) . ? C51 C52 1.512(8) . ? C52 C53 1.507(9) . ? C53 C54 1.321(11) . ? C54 C55 1.481(10) . ? C55 C56 1.492(10) . ? C61 C62 1.507(8) . ? C61 C66 1.514(7) . ? C62 C63 1.495(8) . ? C63 C64 1.497(10) . ? C64 C65 1.481(9) . ? C65 C66 1.500(8) . ? C71 C76 1.464(8) . ? C71 C72 1.495(8) . ? C72 C73 1.493(10) . ? C73 C74 1.439(10) . ? C74 C75 1.441(10) . ? C75 C76 1.518(12) . ? Si1' O1' 1.573(3) . ? Si1' O5' 1.593(3) . ? Si1' O4' 1.603(3) . ? Si1' C11' 1.811(5) . ? Si2' O6' 1.585(4) . ? Si2' O1' 1.586(3) . ? Si2' O2' 1.593(3) . ? Si2' C21' 1.802(5) . ? Si3' O7' 1.571(3) . ? Si3' O2' 1.588(3) . ? Si3' O3' 1.597(3) . ? Si3' C31' 1.834(6) . ? Si4' O3' 1.587(3) . ? Si4' O4' 1.588(3) . ? Si4' O8' 1.596(4) . ? Si4' C41' 1.819(5) . ? Si5' O9' 1.572(3) . ? Si5' O12' 1.587(3) . ? Si5' O5' 1.589(3) . ? Si5' C51' 1.807(5) . ? Si6' O6' 1.582(3) . ? Si6' O9' 1.585(3) . ? Si6' O10' 1.597(4) . ? Si6' C61' 1.812(5) . ? Si7' O11' 1.571(4) . ? Si7' O12' 1.595(4) . ? Si7' O8' 1.604(3) . ? Si7' C71' 1.808(5) . ? Si8' O11' 1.586(4) . ? Si8' C81' 1.770(10) . ? Si8' C83' 1.795(8) . ? Si8' C82' 1.800(7) . ? C11' C12' 1.486(7) . ? C11' C16' 1.498(7) . ? C12' C13' 1.511(8) . ? C13' C14' 1.483(9) . ? C14' C15' 1.463(8) . ? C15' C16' 1.501(8) . ? C21' C22' 1.502(7) . ? C21' C26' 1.513(7) . ? C22' C23' 1.498(8) . ? C23' C24' 1.502(10) . ? C24' C25' 1.475(11) . ? C25' C26' 1.482(8) . ? C31' C32' 1.476(8) . ? C31' C36' 1.507(7) . ? C32' C33' 1.519(9) . ? C33' C34' 1.496(10) . ? C34' C35' 1.451(9) . ? C35' C36' 1.542(8) . ? C41' C46' 1.477(7) . ? C41' C42' 1.492(7) . ? C42' C43' 1.483(8) . ? C43' C44' 1.456(9) . ? C44' C45' 1.487(8) . ? C45' C46' 1.499(7) . ? C51' C52' 1.505(7) . ? C51' C56' 1.507(7) . ? C52' C53' 1.511(7) . ? C53' C54' 1.479(8) . ? C54' C55' 1.488(9) . ? C55' C56' 1.498(7) . ? C61' C66' 1.489(7) . ? C61' C62' 1.510(7) . ? C62' C63' 1.495(7) . ? C63' C64' 1.470(8) . ? C64' C65' 1.479(9) . ? C65' C66' 1.503(8) . ? C71' C76' 1.499(7) . ? C71' C72' 1.505(7) . ? C72' C73' 1.495(9) . ? C73' C74' 1.485(9) . ? C74' C75' 1.489(8) . ? C75' C76' 1.485(7) . ? C101 C105 1.373(7) . ? C101 C102 1.382(7) . ? C101 C106 1.472(7) . ? C102 C103 1.383(7) . ? C102 C107 1.481(8) . ? C103 C104 1.384(7) . ? C103 C108 1.472(7) . ? C104 C105 1.388(7) . ? C104 C109 1.464(8) . ? C105 C110 1.490(7) . ? C200 C201 1.333(16) . ? C201 C206 1.298(15) . ? C201 C202 1.420(18) . ? C202 C203 1.303(19) . ? C203 C204 1.48(2) . ? C204 C205 1.243(19) . ? C205 C206 1.381(17) . ? C301 C302 1.333(14) . ? C302 C303 1.365(11) . ? C302 C304 1.390(10) . ? C303 C304 1.347(11) 2_756 ? C304 C303 1.347(11) 2_756 ? 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 O7 Ti O7' 104.29(15) . . ? O7 Ti O10 103.86(15) . . ? O7' Ti O10 105.32(15) . . ? O7 Ti C102 94.38(18) . . ? O7' Ti C102 98.63(17) . . ? O10 Ti C102 144.95(17) . . ? O7 Ti C101 84.45(18) . . ? O7' Ti C101 133.38(17) . . ? O10 Ti C101 117.00(18) . . ? C102 Ti C101 34.76(18) . . ? O7 Ti C104 141.70(17) . . ? O7' Ti C104 105.68(17) . . ? O10 Ti C104 90.64(18) . . ? C102 Ti C104 58.00(19) . . ? C101 Ti C104 57.57(19) . . ? O7 Ti C105 109.50(17) . . ? O7' Ti C105 139.60(16) . . ? O10 Ti C105 87.63(17) . . ? C102 Ti C105 57.88(18) . . ? C101 Ti C105 34.47(19) . . ? C104 Ti C105 34.83(17) . . ? O7 Ti C103 128.64(19) . . ? O7' Ti C103 84.11(17) . . ? O10 Ti C103 122.90(18) . . ? C102 Ti C103 34.71(19) . . ? C101 Ti C103 57.36(19) . . ? C104 Ti C103 34.69(19) . . ? C105 Ti C103 57.59(17) . . ? O5 Si1 O1 109.1(2) . . ? O5 Si1 O4 109.0(2) . . ? O1 Si1 O4 110.0(2) . . ? O5 Si1 C11 108.1(2) . . ? O1 Si1 C11 109.7(3) . . ? O4 Si1 C11 110.8(2) . . ? O6 Si2 O1 109.1(2) . . ? O6 Si2 O2 109.1(2) . . ? O1 Si2 O2 109.0(2) . . ? O6 Si2 C21 111.2(3) . . ? O1 Si2 C21 107.4(3) . . ? O2 Si2 C21 110.9(2) . . ? O7 Si3 O2 110.5(2) . . ? O7 Si3 O3 108.58(19) . . ? O2 Si3 O3 109.22(19) . . ? O7 Si3 C31 110.9(2) . . ? O2 Si3 C31 105.8(2) . . ? O3 Si3 C31 111.8(2) . . ? O3 Si4 O8 109.3(2) . . ? O3 Si4 O4 109.8(2) . . ? O8 Si4 O4 108.5(2) . . ? O3 Si4 C41 111.4(3) . . ? O8 Si4 C41 106.9(3) . . ? O4 Si4 C41 110.9(3) . . ? O9 Si5 O12 108.02(19) . . ? O9 Si5 O5 109.5(2) . . ? O12 Si5 O5 109.1(2) . . ? O9 Si5 C51 108.4(3) . . ? O12 Si5 C51 111.1(3) . . ? O5 Si5 C51 110.7(2) . . ? O10 Si6 O6 110.42(19) . . ? O10 Si6 O9 108.56(19) . . ? O6 Si6 O9 108.48(19) . . ? O10 Si6 C61 111.2(2) . . ? O6 Si6 C61 107.6(2) . . ? O9 Si6 C61 110.5(2) . . ? O11 Si7 O12 107.6(2) . . ? O11 Si7 O8 108.7(2) . . ? O12 Si7 O8 108.7(2) . . ? O11 Si7 C71 111.3(3) . . ? O12 Si7 C71 109.2(2) . . ? O8 Si7 C71 111.2(2) . . ? O11 Si8 C83 109.1(3) . . ? O11 Si8 C82 107.9(3) . . ? C83 Si8 C82 110.2(4) . . ? O11 Si8 C81 108.7(4) . . ? C83 Si8 C81 108.6(4) . . ? C82 Si8 C81 112.2(5) . . ? Si2 O1 Si1 145.0(2) . . ? Si3 O2 Si2 155.7(2) . . ? Si4 O3 Si3 157.8(3) . . ? Si1 O4 Si4 146.6(2) . . ? Si1 O5 Si5 149.6(2) . . ? Si2 O6 Si6 144.5(2) . . ? Si3 O7 Ti 148.9(2) . . ? Si7 O8 Si4 144.6(3) . . ? Si5 O9 Si6 156.1(3) . . ? Si6 O10 Ti 154.8(2) . . ? Si7 O11 Si8 165.5(3) . . ? Si5 O12 Si7 140.0(2) . . ? C16 C11 C12 111.2(5) . . ? C16 C11 Si1 111.9(4) . . ? C12 C11 Si1 110.3(4) . . ? C11 C12 C13 110.7(6) . . ? C14 C13 C12 110.2(7) . . ? C13 C14 C15 111.0(7) . . ? C14 C15 C16 110.2(7) . . ? C11 C16 C15 112.7(6) . . ? C22 C21 C26 122.8(6) . . ? C22 C21 Si2 122.7(5) . . ? C26 C21 Si2 113.6(4) . . ? C21 C22 C23 123.1(7) . . ? C24 C23 C22 110.6(7) . . ? C25 C24 C23 125.2(9) . . ? C24 C25 C26 122.2(7) . . ? C25 C26 C21 113.0(5) . . ? C32 C31 C36 110.9(4) . . ? C32 C31 Si3 115.7(3) . . ? C36 C31 Si3 111.4(3) . . ? C31 C32 C33 112.2(4) . . ? C34 C33 C32 111.3(4) . . ? C35 C34 C33 112.6(5) . . ? C34 C35 C36 112.2(5) . . ? C31 C36 C35 111.5(4) . . ? C46 C41 C42 110.6(7) . . ? C46 C41 Si4 118.2(6) . . ? C42 C41 Si4 111.7(4) . . ? C43 C42 C41 111.8(7) . . ? C44 C43 C42 113.7(9) . . ? C43 C44 C45 112.9(8) . . ? C44 C45 C46 110.4(7) . . ? C41 C46 C45 113.8(7) . . ? C56 C51 C52 113.1(5) . . ? C56 C51 Si5 123.4(5) . . ? C52 C51 Si5 111.6(4) . . ? C53 C52 C51 112.4(6) . . ? C54 C53 C52 117.2(8) . . ? C53 C54 C55 116.6(7) . . ? C54 C55 C56 111.2(6) . . ? C51 C56 C55 116.6(7) . . ? C62 C61 C66 110.5(4) . . ? C62 C61 Si6 113.3(4) . . ? C66 C61 Si6 113.0(4) . . ? C63 C62 C61 113.3(5) . . ? C62 C63 C64 110.7(5) . . ? C65 C64 C63 111.2(5) . . ? C64 C65 C66 111.1(5) . . ? C65 C66 C61 111.7(5) . . ? C76 C71 C72 106.3(5) . . ? C76 C71 Si7 115.4(5) . . ? C72 C71 Si7 113.0(5) . . ? C73 C72 C71 113.1(7) . . ? C74 C73 C72 111.7(7) . . ? C73 C74 C75 110.9(6) . . ? C74 C75 C76 111.8(8) . . ? C71 C76 C75 110.9(8) . . ? O1' Si1' O5' 108.86(18) . . ? O1' Si1' O4' 108.23(17) . . ? O5' Si1' O4' 109.52(18) . . ? O1' Si1' C11' 110.24(19) . . ? O5' Si1' C11' 111.4(2) . . ? O4' Si1' C11' 108.6(2) . . ? O6' Si2' O1' 110.11(18) . . ? O6' Si2' O2' 108.50(19) . . ? O1' Si2' O2' 109.03(18) . . ? O6' Si2' C21' 110.1(2) . . ? O1' Si2' C21' 107.7(2) . . ? O2' Si2' C21' 111.4(2) . . ? O7' Si3' O2' 110.83(19) . . ? O7' Si3' O3' 108.20(18) . . ? O2' Si3' O3' 107.29(18) . . ? O7' Si3' C31' 109.7(2) . . ? O2' Si3' C31' 107.6(2) . . ? O3' Si3' C31' 113.2(2) . . ? O3' Si4' O4' 109.60(17) . . ? O3' Si4' O8' 105.93(19) . . ? O4' Si4' O8' 108.40(18) . . ? O3' Si4' C41' 110.3(2) . . ? O4' Si4' C41' 110.2(2) . . ? O8' Si4' C41' 112.4(2) . . ? O9' Si5' O12' 108.76(19) . . ? O9' Si5' O5' 109.94(18) . . ? O12' Si5' O5' 109.01(19) . . ? O9' Si5' C51' 108.5(2) . . ? O12' Si5' C51' 110.2(2) . . ? O5' Si5' C51' 110.4(2) . . ? O6' Si6' O9' 107.66(19) . . ? O6' Si6' O10' 111.0(2) . . ? O9' Si6' O10' 110.4(2) . . ? O6' Si6' C61' 109.4(2) . . ? O9' Si6' C61' 109.9(2) . . ? O10' Si6' C61' 108.5(2) . . ? O11' Si7' O12' 110.2(2) . . ? O11' Si7' O8' 107.17(19) . . ? O12' Si7' O8' 108.34(18) . . ? O11' Si7' C71' 110.6(2) . . ? O12' Si7' C71' 108.8(2) . . ? O8' Si7' C71' 111.7(2) . . ? O11' Si8' C81' 109.6(4) . . ? O11' Si8' C83' 107.3(3) . . ? C81' Si8' C83' 113.0(7) . . ? O11' Si8' C82' 108.1(3) . . ? C81' Si8' C82' 109.9(6) . . ? C83' Si8' C82' 108.8(5) . . ? Si1' O1' Si2' 153.2(2) . . ? Si3' O2' Si2' 141.1(2) . . ? Si4' O3' Si3' 149.3(2) . . ? Si4' O4' Si1' 139.3(2) . . ? Si5' O5' Si1' 148.4(2) . . ? Si6' O6' Si2' 151.2(2) . . ? Si3' O7' Ti 162.9(2) . . ? Si4' O8' Si7' 146.5(2) . . ? Si5' O9' Si6' 149.1(2) . . ? Si7' O11' Si8' 158.1(3) . . ? Si5' O12' Si7' 142.8(2) . . ? C12' C11' C16' 110.4(4) . . ? C12' C11' Si1' 112.7(4) . . ? C16' C11' Si1' 113.9(4) . . ? C11' C12' C13' 111.6(5) . . ? C14' C13' C12' 110.7(6) . . ? C15' C14' C13' 110.6(5) . . ? C14' C15' C16' 110.6(5) . . ? C11' C16' C15' 111.4(5) . . ? C22' C21' C26' 111.0(5) . . ? C22' C21' Si2' 111.9(4) . . ? C26' C21' Si2' 111.7(4) . . ? C23' C22' C21' 111.6(5) . . ? C22' C23' C24' 110.7(6) . . ? C25' C24' C23' 111.6(6) . . ? C24' C25' C26' 111.1(6) . . ? C25' C26' C21' 111.2(5) . . ? C32' C31' C36' 114.3(5) . . ? C32' C31' Si3' 114.4(4) . . ? C36' C31' Si3' 112.8(4) . . ? C31' C32' C33' 109.7(6) . . ? C34' C33' C32' 110.3(6) . . ? C35' C34' C33' 110.2(7) . . ? C34' C35' C36' 111.0(5) . . ? C31' C36' C35' 109.8(5) . . ? C46' C41' C42' 111.3(4) . . ? C46' C41' Si4' 115.9(4) . . ? C42' C41' Si4' 112.8(4) . . ? C43' C42' C41' 112.4(5) . . ? C44' C43' C42' 113.1(5) . . ? C43' C44' C45' 112.7(5) . . ? C44' C45' C46' 110.8(5) . . ? C41' C46' C45' 112.3(5) . . ? C52' C51' C56' 110.1(4) . . ? C52' C51' Si5' 112.6(3) . . ? C56' C51' Si5' 111.9(3) . . ? C51' C52' C53' 111.4(4) . . ? C54' C53' C52' 111.2(5) . . ? C53' C54' C55' 111.4(5) . . ? C54' C55' C56' 111.2(5) . . ? C55' C56' C51' 112.9(4) . . ? C66' C61' C62' 109.0(4) . . ? C66' C61' Si6' 114.3(4) . . ? C62' C61' Si6' 111.9(3) . . ? C63' C62' C61' 110.7(4) . . ? C64' C63' C62' 112.4(5) . . ? C63' C64' C65' 110.6(5) . . ? C64' C65' C66' 110.6(5) . . ? C61' C66' C65' 112.2(5) . . ? C76' C71' C72' 108.8(5) . . ? C76' C71' Si7' 113.2(3) . . ? C72' C71' Si7' 113.0(4) . . ? C73' C72' C71' 111.0(5) . . ? C74' C73' C72' 112.1(6) . . ? C73' C74' C75' 111.0(5) . . ? C76' C75' C74' 111.0(5) . . ? C75' C76' C71' 112.4(4) . . ? C105 C101 C102 108.8(5) . . ? C105 C101 C106 126.1(5) . . ? C102 C101 C106 125.0(6) . . ? C105 C101 Ti 72.9(3) . . ? C102 C101 Ti 72.5(3) . . ? C106 C101 Ti 121.6(4) . . ? C101 C102 C103 107.3(5) . . ? C101 C102 C107 125.6(6) . . ? C103 C102 C107 127.1(5) . . ? C101 C102 Ti 72.8(3) . . ? C103 C102 Ti 73.2(3) . . ? C107 C102 Ti 118.8(4) . . ? C102 C103 C104 108.4(5) . . ? C102 C103 C108 125.8(5) . . ? C104 C103 C108 125.8(6) . . ? C102 C103 Ti 72.1(3) . . ? C104 C103 Ti 72.4(3) . . ? C108 C103 Ti 122.9(4) . . ? C103 C104 C105 107.6(5) . . ? C103 C104 C109 126.2(5) . . ? C105 C104 C109 126.1(5) . . ? C103 C104 Ti 72.9(3) . . ? C105 C104 Ti 72.7(3) . . ? C109 C104 Ti 120.8(4) . . ? C101 C105 C104 107.8(5) . . ? C101 C105 C110 126.4(5) . . ? C104 C105 C110 125.8(5) . . ? C101 C105 Ti 72.6(3) . . ? C104 C105 Ti 72.5(3) . . ? C110 C105 Ti 121.5(4) . . ? C206 C201 C200 124.4(19) . . ? C206 C201 C202 123.4(15) . . ? C200 C201 C202 112.0(18) . . ? C203 C202 C201 112.2(17) . . ? C202 C203 C204 126.7(18) . . ? C205 C204 C203 113.5(16) . . ? C204 C205 C206 124.8(19) . . ? C201 C206 C205 119.2(14) . . ? C301 C302 C303 120.0(10) . . ? C301 C302 C304 120.7(11) . . ? C303 C302 C304 119.2(8) . . ? C304 C303 C302 120.8(7) 2_756 . ? C303 C304 C302 120.0(8) 2_756 . ? 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 Si2 O1 Si1 -63.9(5) . . . . ? O2 Si2 O1 Si1 55.2(5) . . . . ? C21 Si2 O1 Si1 175.5(5) . . . . ? O5 Si1 O1 Si2 57.7(5) . . . . ? O4 Si1 O1 Si2 -61.9(5) . . . . ? C11 Si1 O1 Si2 175.9(4) . . . . ? O7 Si3 O2 Si2 -73.6(7) . . . . ? O3 Si3 O2 Si2 45.8(8) . . . . ? C31 Si3 O2 Si2 166.3(7) . . . . ? O6 Si2 O2 Si3 60.3(7) . . . . ? O1 Si2 O2 Si3 -58.8(7) . . . . ? C21 Si2 O2 Si3 -176.9(7) . . . . ? O8 Si4 O3 Si3 -109.1(7) . . . . ? O4 Si4 O3 Si3 9.8(8) . . . . ? C41 Si4 O3 Si3 132.9(7) . . . . ? O7 Si3 O3 Si4 115.5(7) . . . . ? O2 Si3 O3 Si4 -5.0(7) . . . . ? C31 Si3 O3 Si4 -121.8(7) . . . . ? O5 Si1 O4 Si4 -47.8(5) . . . . ? O1 Si1 O4 Si4 71.9(5) . . . . ? C11 Si1 O4 Si4 -166.6(5) . . . . ? O3 Si4 O4 Si1 -57.0(5) . . . . ? O8 Si4 O4 Si1 62.4(5) . . . . ? C41 Si4 O4 Si1 179.6(5) . . . . ? O1 Si1 O5 Si5 -65.1(6) . . . . ? O4 Si1 O5 Si5 55.1(6) . . . . ? C11 Si1 O5 Si5 175.6(5) . . . . ? O9 Si5 O5 Si1 45.5(6) . . . . ? O12 Si5 O5 Si1 -72.5(6) . . . . ? C51 Si5 O5 Si1 164.9(5) . . . . ? O1 Si2 O6 Si6 77.2(4) . . . . ? O2 Si2 O6 Si6 -41.9(5) . . . . ? C21 Si2 O6 Si6 -164.5(4) . . . . ? O10 Si6 O6 Si2 66.4(4) . . . . ? O9 Si6 O6 Si2 -52.5(5) . . . . ? C61 Si6 O6 Si2 -172.0(4) . . . . ? O2 Si3 O7 Ti -2.0(5) . . . . ? O3 Si3 O7 Ti -121.7(4) . . . . ? C31 Si3 O7 Ti 115.0(4) . . . . ? O7' Ti O7 Si3 -72.5(4) . . . . ? O10 Ti O7 Si3 37.6(4) . . . . ? C102 Ti O7 Si3 -172.6(4) . . . . ? C101 Ti O7 Si3 154.1(4) . . . . ? C104 Ti O7 Si3 146.9(4) . . . . ? C105 Ti O7 Si3 130.0(4) . . . . ? C103 Ti O7 Si3 -166.4(4) . . . . ? O11 Si7 O8 Si4 172.5(4) . . . . ? O12 Si7 O8 Si4 -70.7(5) . . . . ? C71 Si7 O8 Si4 49.6(5) . . . . ? O3 Si4 O8 Si7 125.6(4) . . . . ? O4 Si4 O8 Si7 5.9(5) . . . . ? C41 Si4 O8 Si7 -113.7(5) . . . . ? O12 Si5 O9 Si6 151.4(6) . . . . ? O5 Si5 O9 Si6 32.7(7) . . . . ? C51 Si5 O9 Si6 -88.2(7) . . . . ? O10 Si6 O9 Si5 -151.1(6) . . . . ? O6 Si6 O9 Si5 -31.1(7) . . . . ? C61 Si6 O9 Si5 86.7(7) . . . . ? O6 Si6 O10 Ti -45.0(5) . . . . ? O9 Si6 O10 Ti 73.8(5) . . . . ? C61 Si6 O10 Ti -164.5(5) . . . . ? O7 Ti O10 Si6 -5.3(5) . . . . ? O7' Ti O10 Si6 104.0(5) . . . . ? C102 Ti O10 Si6 -124.6(5) . . . . ? C101 Ti O10 Si6 -96.1(5) . . . . ? C104 Ti O10 Si6 -149.5(5) . . . . ? C105 Ti O10 Si6 -114.8(5) . . . . ? C103 Ti O10 Si6 -163.1(5) . . . . ? O12 Si7 O11 Si8 -145.2(12) . . . . ? O8 Si7 O11 Si8 -27.7(13) . . . . ? C71 Si7 O11 Si8 95.1(12) . . . . ? C83 Si8 O11 Si7 -88.9(12) . . . . ? C82 Si8 O11 Si7 151.4(12) . . . . ? C81 Si8 O11 Si7 29.4(13) . . . . ? O9 Si5 O12 Si7 -118.4(4) . . . . ? O5 Si5 O12 Si7 0.5(4) . . . . ? C51 Si5 O12 Si7 122.8(4) . . . . ? O11 Si7 O12 Si5 -179.1(3) . . . . ? O8 Si7 O12 Si5 63.4(4) . . . . ? C71 Si7 O12 Si5 -58.1(4) . . . . ? O5 Si1 C11 C16 -59.7(5) . . . . ? O1 Si1 C11 C16 -178.6(4) . . . . ? O4 Si1 C11 C16 59.7(5) . . . . ? O5 Si1 C11 C12 64.6(5) . . . . ? O1 Si1 C11 C12 -54.2(5) . . . . ? O4 Si1 C11 C12 -175.9(4) . . . . ? C16 C11 C12 C13 -52.9(8) . . . . ? Si1 C11 C12 C13 -177.7(5) . . . . ? C11 C12 C13 C14 57.0(9) . . . . ? C12 C13 C14 C15 -59.9(9) . . . . ? C13 C14 C15 C16 58.4(9) . . . . ? C12 C11 C16 C15 52.5(8) . . . . ? Si1 C11 C16 C15 176.3(5) . . . . ? C14 C15 C16 C11 -54.6(9) . . . . ? O6 Si2 C21 C22 131.4(12) . . . . ? O1 Si2 C21 C22 -109.4(12) . . . . ? O2 Si2 C21 C22 9.7(13) . . . . ? O6 Si2 C21 C26 -59.5(7) . . . . ? O1 Si2 C21 C26 59.7(7) . . . . ? O2 Si2 C21 C26 178.8(5) . . . . ? C26 C21 C22 C23 14(2) . . . . ? Si2 C21 C22 C23 -177.4(10) . . . . ? C21 C22 C23 C24 -16(2) . . . . ? C22 C23 C24 C25 17(3) . . . . ? C23 C24 C25 C26 -16(3) . . . . ? C24 C25 C26 C21 11.5(19) . . . . ? C22 C21 C26 C25 -10.7(16) . . . . ? Si2 C21 C26 C25 -179.8(6) . . . . ? O7 Si3 C31 C32 49.6(4) . . . . ? O2 Si3 C31 C32 169.5(4) . . . . ? O3 Si3 C31 C32 -71.7(4) . . . . ? O7 Si3 C31 C36 177.5(3) . . . . ? O2 Si3 C31 C36 -62.7(4) . . . . ? O3 Si3 C31 C36 56.2(4) . . . . ? C36 C31 C32 C33 55.1(6) . . . . ? Si3 C31 C32 C33 -176.7(4) . . . . ? C31 C32 C33 C34 -55.3(6) . . . . ? C32 C33 C34 C35 54.0(7) . . . . ? C33 C34 C35 C36 -53.0(7) . . . . ? C32 C31 C36 C35 -53.2(6) . . . . ? Si3 C31 C36 C35 176.4(4) . . . . ? C34 C35 C36 C31 52.4(6) . . . . ? O3 Si4 C41 C46 -73.8(7) . . . . ? O8 Si4 C41 C46 166.8(6) . . . . ? O4 Si4 C41 C46 48.7(7) . . . . ? O3 Si4 C41 C42 56.1(7) . . . . ? O8 Si4 C41 C42 -63.2(6) . . . . ? O4 Si4 C41 C42 178.7(6) . . . . ? C46 C41 C42 C43 -50.9(11) . . . . ? Si4 C41 C42 C43 175.3(8) . . . . ? C41 C42 C43 C44 51.3(14) . . . . ? C42 C43 C44 C45 -53.0(14) . . . . ? C43 C44 C45 C46 52.7(12) . . . . ? C42 C41 C46 C45 53.4(10) . . . . ? Si4 C41 C46 C45 -176.1(6) . . . . ? C44 C45 C46 C41 -54.4(11) . . . . ? O9 Si5 C51 C56 141.1(8) . . . . ? O12 Si5 C51 C56 -100.4(8) . . . . ? O5 Si5 C51 C56 21.0(9) . . . . ? O9 Si5 C51 C52 -78.7(5) . . . . ? O12 Si5 C51 C52 39.8(6) . . . . ? O5 Si5 C51 C52 161.2(4) . . . . ? C56 C51 C52 C53 -42.5(10) . . . . ? Si5 C51 C52 C53 173.1(6) . . . . ? C51 C52 C53 C54 41.9(13) . . . . ? C52 C53 C54 C55 -44.4(15) . . . . ? C53 C54 C55 C56 45.0(14) . . . . ? C52 C51 C56 C55 47.6(12) . . . . ? Si5 C51 C56 C55 -172.7(6) . . . . ? C54 C55 C56 C51 -47.5(13) . . . . ? O10 Si6 C61 C62 -75.3(4) . . . . ? O6 Si6 C61 C62 163.6(3) . . . . ? O9 Si6 C61 C62 45.3(4) . . . . ? O10 Si6 C61 C66 158.1(3) . . . . ? O6 Si6 C61 C66 37.0(4) . . . . ? O9 Si6 C61 C66 -81.3(4) . . . . ? C66 C61 C62 C63 -51.9(6) . . . . ? Si6 C61 C62 C63 -179.8(4) . . . . ? C61 C62 C63 C64 53.8(7) . . . . ? C62 C63 C64 C65 -56.2(8) . . . . ? C63 C64 C65 C66 57.9(8) . . . . ? C64 C65 C66 C61 -56.3(7) . . . . ? C62 C61 C66 C65 52.5(6) . . . . ? Si6 C61 C66 C65 -179.4(4) . . . . ? O11 Si7 C71 C76 -62.2(7) . . . . ? O12 Si7 C71 C76 179.1(6) . . . . ? O8 Si7 C71 C76 59.1(7) . . . . ? O11 Si7 C71 C72 60.5(6) . . . . ? O12 Si7 C71 C72 -58.2(6) . . . . ? O8 Si7 C71 C72 -178.2(5) . . . . ? C76 C71 C72 C73 -57.3(10) . . . . ? Si7 C71 C72 C73 175.1(6) . . . . ? C71 C72 C73 C74 56.0(11) . . . . ? C72 C73 C74 C75 -53.3(13) . . . . ? C73 C74 C75 C76 55.3(13) . . . . ? C72 C71 C76 C75 57.8(11) . . . . ? Si7 C71 C76 C75 -176.0(7) . . . . ? C74 C75 C76 C71 -59.6(13) . . . . ? O5' Si1' O1' Si2' 63.4(6) . . . . ? O4' Si1' O1' Si2' -55.6(6) . . . . ? C11' Si1' O1' Si2' -174.2(5) . . . . ? O6' Si2' O1' Si1' -42.2(6) . . . . ? O2' Si2' O1' Si1' 76.7(6) . . . . ? C21' Si2' O1' Si1' -162.2(5) . . . . ? O7' Si3' O2' Si2' -119.3(3) . . . . ? O3' Si3' O2' Si2' -1.4(4) . . . . ? C31' Si3' O2' Si2' 120.7(4) . . . . ? O6' Si2' O2' Si3' 69.2(4) . . . . ? O1' Si2' O2' Si3' -50.7(4) . . . . ? C21' Si2' O2' Si3' -169.4(3) . . . . ? O4' Si4' O3' Si3' -43.8(5) . . . . ? O8' Si4' O3' Si3' -160.6(4) . . . . ? C41' Si4' O3' Si3' 77.6(5) . . . . ? O7' Si3' O3' Si4' -158.3(4) . . . . ? O2' Si3' O3' Si4' 82.1(5) . . . . ? C31' Si3' O3' Si4' -36.4(5) . . . . ? O3' Si4' O4' Si1' -56.5(4) . . . . ? O8' Si4' O4' Si1' 58.7(4) . . . . ? C41' Si4' O4' Si1' -178.0(3) . . . . ? O1' Si1' O4' Si4' 55.9(4) . . . . ? O5' Si1' O4' Si4' -62.6(4) . . . . ? C11' Si1' O4' Si4' 175.6(3) . . . . ? O9' Si5' O5' Si1' 41.6(5) . . . . ? O12' Si5' O5' Si1' -77.5(5) . . . . ? C51' Si5' O5' Si1' 161.2(4) . . . . ? O1' Si1' O5' Si5' -55.9(5) . . . . ? O4' Si1' O5' Si5' 62.2(5) . . . . ? C11' Si1' O5' Si5' -177.7(4) . . . . ? O9' Si6' O6' Si2' -52.2(6) . . . . ? O10' Si6' O6' Si2' 68.7(6) . . . . ? C61' Si6' O6' Si2' -171.6(5) . . . . ? O1' Si2' O6' Si6' 30.5(6) . . . . ? O2' Si2' O6' Si6' -88.7(5) . . . . ? C21' Si2' O6' Si6' 149.1(5) . . . . ? O2' Si3' O7' Ti -74.6(8) . . . . ? O3' Si3' O7' Ti 168.0(8) . . . . ? C31' Si3' O7' Ti 44.1(9) . . . . ? O7 Ti O7' Si3' 63.4(8) . . . . ? O10 Ti O7' Si3' -45.7(8) . . . . ? C102 Ti O7' Si3' 160.2(8) . . . . ? C101 Ti O7' Si3' 159.3(7) . . . . ? C104 Ti O7' Si3' -140.8(8) . . . . ? C105 Ti O7' Si3' -150.5(7) . . . . ? C103 Ti O7' Si3' -168.2(8) . . . . ? O3' Si4' O8' Si7' 158.3(4) . . . . ? O4' Si4' O8' Si7' 40.7(5) . . . . ? C41' Si4' O8' Si7' -81.3(4) . . . . ? O11' Si7' O8' Si4' 156.2(4) . . . . ? O12' Si7' O8' Si4' -84.8(4) . . . . ? C71' Si7' O8' Si4' 35.0(5) . . . . ? O12' Si5' O9' Si6' 61.2(5) . . . . ? O5' Si5' O9' Si6' -58.1(5) . . . . ? C51' Si5' O9' Si6' -178.9(5) . . . . ? O6' Si6' O9' Si5' 74.5(5) . . . . ? O10' Si6' O9' Si5' -46.8(5) . . . . ? C61' Si6' O9' Si5' -166.5(5) . . . . ? O12' Si7' O11' Si8' -7.3(8) . . . . ? O8' Si7' O11' Si8' 110.4(7) . . . . ? C71' Si7' O11' Si8' -127.6(7) . . . . ? C81' Si8' O11' Si7' 18.1(10) . . . . ? C83' Si8' O11' Si7' 141.1(8) . . . . ? C82' Si8' O11' Si7' -101.7(8) . . . . ? O9' Si5' O12' Si7' -80.7(4) . . . . ? O5' Si5' O12' Si7' 39.1(4) . . . . ? C51' Si5' O12' Si7' 160.5(4) . . . . ? O11' Si7' O12' Si5' 133.7(4) . . . . ? O8' Si7' O12' Si5' 16.8(4) . . . . ? C71' Si7' O12' Si5' -104.8(4) . . . . ? O1' Si1' C11' C12' -173.2(4) . . . . ? O5' Si1' C11' C12' -52.3(4) . . . . ? O4' Si1' C11' C12' 68.4(4) . . . . ? O1' Si1' C11' C16' -46.5(4) . . . . ? O5' Si1' C11' C16' 74.4(4) . . . . ? O4' Si1' C11' C16' -164.9(4) . . . . ? C16' C11' C12' C13' 53.8(7) . . . . ? Si1' C11' C12' C13' -177.7(5) . . . . ? C11' C12' C13' C14' -55.6(8) . . . . ? C12' C13' C14' C15' 57.7(8) . . . . ? C13' C14' C15' C16' -58.7(8) . . . . ? C12' C11' C16' C15' -54.7(7) . . . . ? Si1' C11' C16' C15' 177.4(4) . . . . ? C14' C15' C16' C11' 57.5(7) . . . . ? O6' Si2' C21' C22' -60.5(4) . . . . ? O1' Si2' C21' C22' 59.5(4) . . . . ? O2' Si2' C21' C22' 179.1(4) . . . . ? O6' Si2' C21' C26' 174.4(4) . . . . ? O1' Si2' C21' C26' -65.6(4) . . . . ? O2' Si2' C21' C26' 54.0(4) . . . . ? C26' C21' C22' C23' -53.9(7) . . . . ? Si2' C21' C22' C23' -179.4(4) . . . . ? C21' C22' C23' C24' 54.3(8) . . . . ? C22' C23' C24' C25' -56.1(9) . . . . ? C23' C24' C25' C26' 57.4(8) . . . . ? C24' C25' C26' C21' -56.6(8) . . . . ? C22' C21' C26' C25' 54.8(7) . . . . ? Si2' C21' C26' C25' -179.6(5) . . . . ? O7' Si3' C31' C32' -178.2(5) . . . . ? O2' Si3' C31' C32' -57.5(5) . . . . ? O3' Si3' C31' C32' 60.8(5) . . . . ? O7' Si3' C31' C36' 48.9(5) . . . . ? O2' Si3' C31' C36' 169.6(4) . . . . ? O3' Si3' C31' C36' -72.0(4) . . . . ? C36' C31' C32' C33' -53.1(8) . . . . ? Si3' C31' C32' C33' 174.8(5) . . . . ? C31' C32' C33' C34' 56.8(9) . . . . ? C32' C33' C34' C35' -61.7(10) . . . . ? C33' C34' C35' C36' 60.2(9) . . . . ? C32' C31' C36' C35' 51.2(7) . . . . ? Si3' C31' C36' C35' -175.9(4) . . . . ? C34' C35' C36' C31' -54.0(8) . . . . ? O3' Si4' C41' C46' -152.8(4) . . . . ? O4' Si4' C41' C46' -31.7(5) . . . . ? O8' Si4' C41' C46' 89.3(4) . . . . ? O3' Si4' C41' C42' 77.3(4) . . . . ? O4' Si4' C41' C42' -161.6(4) . . . . ? O8' Si4' C41' C42' -40.6(4) . . . . ? C46' C41' C42' C43' 51.9(7) . . . . ? Si4' C41' C42' C43' -175.9(4) . . . . ? C41' C42' C43' C44' -51.5(8) . . . . ? C42' C43' C44' C45' 52.3(9) . . . . ? C43' C44' C45' C46' -53.1(8) . . . . ? C42' C41' C46' C45' -53.9(7) . . . . ? Si4' C41' C46' C45' 175.5(4) . . . . ? C44' C45' C46' C41' 54.3(7) . . . . ? O9' Si5' C51' C52' -72.8(4) . . . . ? O12' Si5' C51' C52' 46.1(4) . . . . ? O5' Si5' C51' C52' 166.6(3) . . . . ? O9' Si5' C51' C56' 51.9(4) . . . . ? O12' Si5' C51' C56' 170.8(4) . . . . ? O5' Si5' C51' C56' -68.7(4) . . . . ? C56' C51' C52' C53' 53.8(6) . . . . ? Si5' C51' C52' C53' 179.4(4) . . . . ? C51' C52' C53' C54' -56.6(7) . . . . ? C52' C53' C54' C55' 57.0(7) . . . . ? C53' C54' C55' C56' -55.4(7) . . . . ? C54' C55' C56' C51' 54.0(7) . . . . ? C52' C51' C56' C55' -53.1(6) . . . . ? Si5' C51' C56' C55' -179.1(4) . . . . ? O6' Si6' C61' C66' 178.0(4) . . . . ? O9' Si6' C61' C66' 60.0(4) . . . . ? O10' Si6' C61' C66' -60.8(4) . . . . ? O6' Si6' C61' C62' 53.6(4) . . . . ? O9' Si6' C61' C62' -64.4(4) . . . . ? O10' Si6' C61' C62' 174.7(3) . . . . ? C66' C61' C62' C63' 55.4(6) . . . . ? Si6' C61' C62' C63' -177.3(4) . . . . ? C61' C62' C63' C64' -56.7(7) . . . . ? C62' C63' C64' C65' 56.5(7) . . . . ? C63' C64' C65' C66' -55.6(7) . . . . ? C62' C61' C66' C65' -56.4(6) . . . . ? Si6' C61' C66' C65' 177.6(4) . . . . ? C64' C65' C66' C61' 57.2(7) . . . . ? O11' Si7' C71' C76' 170.0(4) . . . . ? O12' Si7' C71' C76' 48.8(4) . . . . ? O8' Si7' C71' C76' -70.7(4) . . . . ? O11' Si7' C71' C72' 45.8(5) . . . . ? O12' Si7' C71' C72' -75.4(5) . . . . ? O8' Si7' C71' C72' 165.1(4) . . . . ? C76' C71' C72' C73' 56.1(8) . . . . ? Si7' C71' C72' C73' -177.3(5) . . . . ? C71' C72' C73' C74' -56.3(9) . . . . ? C72' C73' C74' C75' 54.6(9) . . . . ? C73' C74' C75' C76' -54.3(7) . . . . ? C74' C75' C76' C71' 56.8(7) . . . . ? C72' C71' C76' C75' -57.2(6) . . . . ? Si7' C71' C76' C75' 176.4(4) . . . . ? O7 Ti C101 C105 -137.2(3) . . . . ? O7' Ti C101 C105 118.3(3) . . . . ? O10 Ti C101 C105 -34.5(3) . . . . ? C102 Ti C101 C105 116.8(5) . . . . ? C104 Ti C101 C105 37.5(3) . . . . ? C103 Ti C101 C105 79.0(3) . . . . ? O7 Ti C101 C102 105.9(3) . . . . ? O7' Ti C101 C102 1.5(4) . . . . ? O10 Ti C101 C102 -151.3(3) . . . . ? C104 Ti C101 C102 -79.3(3) . . . . ? C105 Ti C101 C102 -116.8(5) . . . . ? C103 Ti C101 C102 -37.9(3) . . . . ? O7 Ti C101 C106 -14.9(5) . . . . ? O7' Ti C101 C106 -119.3(5) . . . . ? O10 Ti C101 C106 87.9(5) . . . . ? C102 Ti C101 C106 -120.8(7) . . . . ? C104 Ti C101 C106 159.9(6) . . . . ? C105 Ti C101 C106 122.4(6) . . . . ? C103 Ti C101 C106 -158.7(6) . . . . ? C105 C101 C102 C103 1.2(6) . . . . ? C106 C101 C102 C103 -177.8(5) . . . . ? Ti C101 C102 C103 65.5(4) . . . . ? C105 C101 C102 C107 -177.9(5) . . . . ? C106 C101 C102 C107 3.2(9) . . . . ? Ti C101 C102 C107 -113.5(5) . . . . ? C105 C101 C102 Ti -64.3(4) . . . . ? C106 C101 C102 Ti 116.7(5) . . . . ? O7 Ti C102 C101 -73.7(3) . . . . ? O7' Ti C102 C101 -178.9(3) . . . . ? O10 Ti C102 C101 48.1(5) . . . . ? C104 Ti C102 C101 78.0(3) . . . . ? C105 Ti C102 C101 36.6(3) . . . . ? C103 Ti C102 C101 114.8(5) . . . . ? O7 Ti C102 C103 171.5(3) . . . . ? O7' Ti C102 C103 66.3(3) . . . . ? O10 Ti C102 C103 -66.6(4) . . . . ? C101 Ti C102 C103 -114.8(5) . . . . ? C104 Ti C102 C103 -36.8(3) . . . . ? C105 Ti C102 C103 -78.2(3) . . . . ? O7 Ti C102 C107 47.9(5) . . . . ? O7' Ti C102 C107 -57.2(5) . . . . ? O10 Ti C102 C107 169.8(4) . . . . ? C101 Ti C102 C107 121.7(6) . . . . ? C104 Ti C102 C107 -160.4(5) . . . . ? C105 Ti C102 C107 158.3(5) . . . . ? C103 Ti C102 C107 -123.6(6) . . . . ? C101 C102 C103 C104 -1.5(6) . . . . ? C107 C102 C103 C104 177.5(5) . . . . ? Ti C102 C103 C104 63.8(4) . . . . ? C101 C102 C103 C108 176.6(5) . . . . ? C107 C102 C103 C108 -4.3(9) . . . . ? Ti C102 C103 C108 -118.1(5) . . . . ? C101 C102 C103 Ti -65.3(4) . . . . ? C107 C102 C103 Ti 113.8(5) . . . . ? O7 Ti C103 C102 -10.8(4) . . . . ? O7' Ti C103 C102 -114.4(3) . . . . ? O10 Ti C103 C102 141.1(3) . . . . ? C101 Ti C103 C102 37.9(3) . . . . ? C104 Ti C103 C102 116.8(5) . . . . ? C105 Ti C103 C102 79.1(3) . . . . ? O7 Ti C103 C104 -127.6(3) . . . . ? O7' Ti C103 C104 128.8(3) . . . . ? O10 Ti C103 C104 24.3(4) . . . . ? C102 Ti C103 C104 -116.8(5) . . . . ? C101 Ti C103 C104 -78.8(3) . . . . ? C105 Ti C103 C104 -37.7(3) . . . . ? O7 Ti C103 C108 110.7(5) . . . . ? O7' Ti C103 C108 7.1(5) . . . . ? O10 Ti C103 C108 -97.4(5) . . . . ? C102 Ti C103 C108 121.5(6) . . . . ? C101 Ti C103 C108 159.5(6) . . . . ? C104 Ti C103 C108 -121.7(7) . . . . ? C105 Ti C103 C108 -159.4(6) . . . . ? C102 C103 C104 C105 1.3(6) . . . . ? C108 C103 C104 C105 -176.9(5) . . . . ? Ti C103 C104 C105 64.9(4) . . . . ? C102 C103 C104 C109 -179.7(5) . . . . ? C108 C103 C104 C109 2.2(9) . . . . ? Ti C103 C104 C109 -116.1(6) . . . . ? C102 C103 C104 Ti -63.6(4) . . . . ? C108 C103 C104 Ti 118.3(5) . . . . ? O7 Ti C104 C103 86.6(4) . . . . ? O7' Ti C104 C103 -53.7(3) . . . . ? O10 Ti C104 C103 -159.8(3) . . . . ? C102 Ti C104 C103 36.8(3) . . . . ? C101 Ti C104 C103 78.2(4) . . . . ? C105 Ti C104 C103 115.3(5) . . . . ? O7 Ti C104 C105 -28.7(5) . . . . ? O7' Ti C104 C105 -169.0(3) . . . . ? O10 Ti C104 C105 84.9(3) . . . . ? C102 Ti C104 C105 -78.5(3) . . . . ? C101 Ti C104 C105 -37.1(3) . . . . ? C103 Ti C104 C105 -115.3(5) . . . . ? O7 Ti C104 C109 -150.9(4) . . . . ? O7' Ti C104 C109 68.8(5) . . . . ? O10 Ti C104 C109 -37.3(5) . . . . ? C102 Ti C104 C109 159.3(5) . . . . ? C101 Ti C104 C109 -159.4(5) . . . . ? C105 Ti C104 C109 -122.2(6) . . . . ? C103 Ti C104 C109 122.5(6) . . . . ? C102 C101 C105 C104 -0.4(6) . . . . ? C106 C101 C105 C104 178.6(5) . . . . ? Ti C101 C105 C104 -64.4(4) . . . . ? C102 C101 C105 C110 -179.3(5) . . . . ? C106 C101 C105 C110 -0.3(9) . . . . ? Ti C101 C105 C110 116.7(5) . . . . ? C102 C101 C105 Ti 64.0(4) . . . . ? C106 C101 C105 Ti -117.0(6) . . . . ? C103 C104 C105 C101 -0.5(6) . . . . ? C109 C104 C105 C101 -179.6(5) . . . . ? Ti C104 C105 C101 64.5(4) . . . . ? C103 C104 C105 C110 178.4(5) . . . . ? C109 C104 C105 C110 -0.7(9) . . . . ? Ti C104 C105 C110 -116.6(5) . . . . ? C103 C104 C105 Ti -65.0(4) . . . . ? C109 C104 C105 Ti 115.9(6) . . . . ? O7 Ti C105 C101 45.8(3) . . . . ? O7' Ti C105 C101 -99.3(4) . . . . ? O10 Ti C105 C101 149.7(3) . . . . ? C102 Ti C105 C101 -36.9(3) . . . . ? C104 Ti C105 C101 -115.8(5) . . . . ? C103 Ti C105 C101 -78.2(3) . . . . ? O7 Ti C105 C104 161.6(3) . . . . ? O7' Ti C105 C104 16.5(5) . . . . ? O10 Ti C105 C104 -94.5(3) . . . . ? C102 Ti C105 C104 78.9(3) . . . . ? C101 Ti C105 C104 115.8(5) . . . . ? C103 Ti C105 C104 37.5(3) . . . . ? O7 Ti C105 C110 -76.7(5) . . . . ? O7' Ti C105 C110 138.2(4) . . . . ? O10 Ti C105 C110 27.2(5) . . . . ? C102 Ti C105 C110 -159.4(5) . . . . ? C101 Ti C105 C110 -122.5(6) . . . . ? C104 Ti C105 C110 121.7(6) . . . . ? C103 Ti C105 C110 159.3(6) . . . . ? C206 C201 C202 C203 -0.4(19) . . . . ? C200 C201 C202 C203 -176.6(13) . . . . ? C201 C202 C203 C204 -2(2) . . . . ? C202 C203 C204 C205 4(2) . . . . ? C203 C204 C205 C206 -3(2) . . . . ? C200 C201 C206 C205 177.2(12) . . . . ? C202 C201 C206 C205 1.4(18) . . . . ? C204 C205 C206 C201 0(2) . . . . ? C301 C302 C303 C304 177.6(9) . . . 2_756 ? C304 C302 C303 C304 0.3(12) . . . 2_756 ? C301 C302 C304 C303 -177.6(9) . . . 2_756 ? C303 C302 C304 C303 -0.3(12) . . . 2_756 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10' H10' O3' 0.84 2.62 3.317(5) 141.4 . _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 1.114 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.082 data_cuti #(20) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H202 O27 Si16 Ti3' _chemical_formula_weight 2549.86 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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 61.6208(6) _cell_length_b 15.6174(6) _cell_length_c 15.3123(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14735.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 0.7 _cell_measurement_theta_max 25.8 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5472 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.39 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Bruker AXS SMART CCD System' _diffrn_measurement_method 'omega-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65890 _diffrn_reflns_av_R_equivalents 0.1149 _diffrn_reflns_av_sigmaI/netI 0.1625 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 75 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 0.66 _diffrn_reflns_theta_max 25.85 _reflns_number_total 24158 _reflns_number_gt 13789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS SMART CCD System' _computing_cell_refinement 'Bruker AXS SMART CCD System' _computing_data_reduction 'Bruker AXS SMART CCD System' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP5' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(5) _refine_ls_number_reflns 24158 _refine_ls_number_parameters 1311 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1851 _refine_ls_R_factor_gt 0.1189 _refine_ls_wR_factor_ref 0.3450 _refine_ls_wR_factor_gt 0.2995 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 1.445 _refine_ls_shift/su_mean 0.013 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 O2' O 0.18306(13) 1.0775(5) 0.1859(5) 0.040(2) Uani 1 1 d . . . O2 O 0.03702(15) 0.6101(6) 0.6860(6) 0.053(2) Uani 1 1 d . . . O3' O 0.15338(15) 0.9635(5) 0.1413(5) 0.046(2) Uani 1 1 d . . . O3 O 0.04739(15) 0.6512(6) 0.5266(6) 0.052(2) Uani 1 1 d . . . O4' O 0.14329(17) 1.0105(6) 0.3000(6) 0.055(2) Uani 1 1 d . . . O4 O 0.08239(18) 0.7409(6) 0.5727(6) 0.056(3) Uani 1 1 d . . . O5 O 0.06995(15) 0.5218(5) 0.7578(5) 0.046(2) Uani 1 1 d . . . O5' O 0.21525(15) 1.0186(6) 0.2794(6) 0.048(2) Uani 1 1 d . . . O6' O 0.19270(15) 0.9518(6) 0.0814(5) 0.047(2) Uani 1 1 d . . . O6 O 0.03118(17) 0.5015(6) 0.5582(6) 0.059(3) Uani 1 1 d . . . Ti1 Ti 0.12832(3) 0.56042(13) 0.20595(12) 0.0301(4) Uani 1 1 d . . . Ti2 Ti 0.11012(3) 0.62716(13) 0.40903(12) 0.0300(5) Uani 1 1 d . . . Ti3 Ti 0.14221(3) 0.75617(13) 0.29633(13) 0.0333(5) Uani 1 1 d . . . Si1 Si 0.09292(7) 0.7193(2) 0.6673(2) 0.0447(9) Uani 1 1 d . . . Si2 Si 0.05685(7) 0.6127(2) 0.7575(2) 0.0453(9) Uani 1 1 d . . . Si3 Si 0.03059(6) 0.5997(2) 0.5849(2) 0.0445(9) Uani 1 1 d . . . Si4 Si 0.06732(6) 0.7106(2) 0.49208(19) 0.0367(8) Uani 1 1 d . . . Si5 Si 0.11737(6) 0.5565(2) 0.61202(19) 0.0409(8) Uani 1 1 d . . . Si6 Si 0.08007(7) 0.4492(2) 0.6975(2) 0.0475(9) Uani 1 1 d . . . Si7 Si 0.03751(8) 0.4046(3) 0.5923(3) 0.0596(11) Uani 1 1 d . . . Si8 Si 0.04545(8) 0.3355(3) 0.4092(3) 0.0632(11) Uani 1 1 d . . . Si1' Si 0.15931(7) 1.0178(2) 0.3847(2) 0.0480(9) Uani 1 1 d . . . Si2' Si 0.19655(6) 1.0888(2) 0.2764(2) 0.0421(8) Uani 1 1 d . . . Si3' Si 0.17427(6) 1.0167(2) 0.1081(2) 0.0380(8) Uani 1 1 d . . . Si4' Si 0.13521(6) 0.9538(2) 0.2183(2) 0.0397(8) Uani 1 1 d . . . Si5' Si 0.18239(6) 0.8417(2) 0.3995(2) 0.0415(8) Uani 1 1 d . . . Si6' Si 0.22156(6) 0.9173(2) 0.2882(2) 0.0446(9) Uani 1 1 d . . . Si7' Si 0.21614(6) 0.9039(2) 0.0926(2) 0.0444(9) Uani 1 1 d . . . Si8' Si 0.20653(9) 0.7714(3) -0.0522(3) 0.0739(14) Uani 1 1 d . . . O1 O 0.07374(16) 0.6883(6) 0.7331(5) 0.049(2) Uani 1 1 d . . . O1' O 0.17950(15) 1.0735(5) 0.3572(5) 0.045(2) Uani 1 1 d . . . O7 O 0.08179(14) 0.6573(5) 0.4238(5) 0.041(2) Uani 1 1 d . . . O7' O 0.13289(16) 0.8538(6) 0.2441(6) 0.052(2) Uani 1 1 d . . . O8' O 0.16733(15) 0.9228(6) 0.4148(5) 0.047(2) Uani 1 1 d . . . O8 O 0.11083(14) 0.6469(5) 0.6588(5) 0.042(2) Uani 1 1 d . . . O9' O 0.20436(14) 0.8721(6) 0.3512(6) 0.047(2) Uani 1 1 d . . . O9 O 0.09862(15) 0.4898(6) 0.6336(5) 0.049(2) Uani 1 1 d . . . O10' O 0.22022(18) 0.8744(6) 0.1927(6) 0.062(3) Uani 1 1 d . . . O10 O 0.06168(17) 0.4081(6) 0.6389(7) 0.060(3) Uani 1 1 d . . . C11' C 0.1437(3) 1.0701(9) 0.4707(10) 0.065(4) Uani 1 1 d . . . H11' H 0.1525 1.0692 0.5254 0.077 Uiso 1 1 calc R . . C11 C 0.1053(3) 0.8154(8) 0.7163(7) 0.055(4) Uani 1 1 d . . . H11 H 0.1164 0.8379 0.6746 0.066 Uiso 1 1 calc R . . O11 O 0.0374(2) 0.3438(7) 0.5094(7) 0.073(3) Uani 1 1 d . . . O11' O 0.21581(19) 0.8187(6) 0.0334(7) 0.065(3) Uani 1 1 d . . . O12 O 0.11889(15) 0.5701(6) 0.5067(5) 0.047(2) Uani 1 1 d . . . O12' O 0.16986(13) 0.7740(5) 0.3368(5) 0.039(2) Uani 1 1 d . . . C12 C 0.1166(3) 0.7962(9) 0.8025(8) 0.059(4) Uani 1 1 d . . . H12A H 0.1065 0.7646 0.8410 0.071 Uiso 1 1 calc R . . H12B H 0.1293 0.7587 0.7911 0.071 Uiso 1 1 calc R . . C12' C 0.1233(3) 1.0178(12) 0.4865(11) 0.071(5) Uani 1 1 d . . . H12C H 0.1275 0.9608 0.5091 0.085 Uiso 1 1 calc R . . H12D H 0.1158 1.0090 0.4300 0.085 Uiso 1 1 calc R . . O13 O 0.12522(12) 0.7239(5) 0.3893(4) 0.0298(17) Uani 1 1 d . . . C13 C 0.1241(3) 0.8741(11) 0.8481(10) 0.066(4) Uani 1 1 d . . . H13C H 0.1363 0.8989 0.8147 0.080 Uiso 1 1 calc R . . H13D H 0.1298 0.8572 0.9061 0.080 Uiso 1 1 calc R . . C13' C 0.1067(3) 1.0613(13) 0.5538(12) 0.083(6) Uani 1 1 d . . . H13E H 0.0932 1.0272 0.5577 0.100 Uiso 1 1 calc R . . H13F H 0.1133 1.0646 0.6126 0.100 Uiso 1 1 calc R . . O14 O 0.11342(12) 0.5622(5) 0.3185(4) 0.0298(17) Uani 1 1 d . . . C14' C 0.1018(4) 1.1500(18) 0.5201(14) 0.109(8) Uani 1 1 d . . . H14C H 0.0945 1.1458 0.4626 0.130 Uiso 1 1 calc R . . H14D H 0.0917 1.1793 0.5610 0.130 Uiso 1 1 calc R . . C14 C 0.1071(3) 0.9427(11) 0.8610(11) 0.068(4) Uiso 1 1 d . . . H14E H 0.0960 0.9221 0.9024 0.081 Uiso 1 1 calc R . . H14F H 0.1140 0.9944 0.8863 0.081 Uiso 1 1 calc R . . O15 O 0.14172(12) 0.6710(5) 0.2200(4) 0.0336(18) Uani 1 1 d . . . C15' C 0.1221(3) 1.2010(11) 0.5112(10) 0.067(5) Uani 1 1 d . . . H15C H 0.1184 1.2590 0.4896 0.081 Uiso 1 1 calc R . . H15D H 0.1289 1.2074 0.5694 0.081 Uiso 1 1 calc R . . C15 C 0.0966(4) 0.9650(10) 0.7755(13) 0.097(8) Uani 1 1 d . . . H15E H 0.1074 0.9935 0.7375 0.117 Uiso 1 1 calc R . . H15F H 0.0847 1.0060 0.7861 0.117 Uiso 1 1 calc R . . C16' C 0.1376(3) 1.1617(9) 0.4518(11) 0.069(5) Uani 1 1 d . . . H16A H 0.1510 1.1965 0.4522 0.082 Uiso 1 1 calc R . . H16B H 0.1315 1.1644 0.3920 0.082 Uiso 1 1 calc R . . C16 C 0.0876(3) 0.8854(10) 0.7283(10) 0.072(5) Uani 1 1 d . . . H16C H 0.0820 0.9025 0.6704 0.086 Uiso 1 1 calc R . . H16D H 0.0754 0.8615 0.7625 0.086 Uiso 1 1 calc R . . C21' C 0.2087(2) 1.1952(8) 0.2844(10) 0.049(3) Uani 1 1 d . . . H21' H 0.2175 1.1965 0.3392 0.058 Uiso 1 1 calc R . . C21 C 0.0437(3) 0.6314(13) 0.8670(10) 0.070(5) Uani 1 1 d . . . H21 H 0.0315 0.5899 0.8749 0.084 Uiso 1 1 calc R . . C22' C 0.1916(2) 1.2663(9) 0.2916(13) 0.063(4) Uani 1 1 d . . . H22A H 0.1825 1.2662 0.2383 0.075 Uiso 1 1 calc R . . H22B H 0.1820 1.2544 0.3421 0.075 Uiso 1 1 calc R . . C22 C 0.0341(4) 0.7286(16) 0.8678(12) 0.109(9) Uani 1 1 d . . . H22C H 0.0460 0.7699 0.8586 0.131 Uiso 1 1 calc R . . H22D H 0.0235 0.7355 0.8196 0.131 Uiso 1 1 calc R . . C23' C 0.2017(3) 1.3535(11) 0.3027(17) 0.095(7) Uani 1 1 d . . . H23A H 0.2113 1.3544 0.3544 0.114 Uiso 1 1 calc R . . H23B H 0.1903 1.3976 0.3104 0.114 Uiso 1 1 calc R . . C23 C 0.0231(4) 0.7467(19) 0.9534(13) 0.123(10) Uani 1 1 d . . . H23C H 0.0119 0.7033 0.9666 0.148 Uiso 1 1 calc R . . H23D H 0.0164 0.8042 0.9534 0.148 Uiso 1 1 calc R . . C24 C 0.0417(5) 0.742(2) 1.018(2) 0.21(2) Uani 1 1 d . . . H24A H 0.0369 0.7655 1.0748 0.247 Uiso 1 1 calc R . . H24B H 0.0540 0.7771 0.9964 0.247 Uiso 1 1 calc R . . C24' C 0.2147(3) 1.3707(12) 0.2193(19) 0.106(8) Uani 1 1 d . . . H24C H 0.2055 1.3629 0.1669 0.127 Uiso 1 1 calc R . . H24D H 0.2206 1.4297 0.2192 0.127 Uiso 1 1 calc R . . C25' C 0.2324(4) 1.3074(13) 0.2206(16) 0.100(7) Uani 1 1 d . . . H25A H 0.2401 1.3111 0.2773 0.120 Uiso 1 1 calc R . . H25B H 0.2429 1.3213 0.1739 0.120 Uiso 1 1 calc R . . C25 C 0.0490(3) 0.6486(15) 1.0292(11) 0.091(6) Uani 1 1 d . . . H25C H 0.0600 0.6438 1.0760 0.109 Uiso 1 1 calc R . . H25D H 0.0366 0.6113 1.0439 0.109 Uiso 1 1 calc R . . C26' C 0.2242(3) 1.2162(10) 0.2077(13) 0.077(5) Uani 1 1 d . . . H26A H 0.2365 1.1756 0.2071 0.093 Uiso 1 1 calc R . . H26B H 0.2164 1.2115 0.1513 0.093 Uiso 1 1 calc R . . C26 C 0.0587(3) 0.6240(12) 0.9406(10) 0.075(5) Uani 1 1 d . . . H26C H 0.0714 0.6610 0.9292 0.091 Uiso 1 1 calc R . . H26D H 0.0639 0.5642 0.9439 0.091 Uiso 1 1 calc R . . C31 C 0.0029(3) 0.6431(9) 0.5677(11) 0.058(4) Uani 1 1 d . . . H31 H 0.0029 0.6669 0.5071 0.070 Uiso 1 1 calc R . . C31' C 0.1656(3) 1.0824(9) 0.0106(9) 0.057(4) Uani 1 1 d . . . H31' H 0.1496 1.0905 0.0187 0.068 Uiso 1 1 calc R . . C32 C -0.0032(3) 0.7170(10) 0.6261(10) 0.063(4) Uani 1 1 d . . . H32A H -0.0041 0.6965 0.6872 0.076 Uiso 1 1 calc R . . H32B H 0.0083 0.7611 0.6232 0.076 Uiso 1 1 calc R . . C32' C 0.1739(5) 1.1659(12) 0.0049(11) 0.116(9) Uani 1 1 d . . . H32C H 0.1899 1.1628 0.0023 0.139 Uiso 1 1 calc R . . H32D H 0.1700 1.1975 0.0587 0.139 Uiso 1 1 calc R . . C33 C -0.0245(3) 0.7570(11) 0.6012(15) 0.076(5) Uani 1 1 d . . . H33A H -0.0284 0.8024 0.6436 0.092 Uiso 1 1 calc R . . H33B H -0.0234 0.7833 0.5426 0.092 Uiso 1 1 calc R . . C33' C 0.1657(4) 1.2165(12) -0.0745(9) 0.085(6) Uani 1 1 d . . . H33C H 0.1505 1.2340 -0.0644 0.102 Uiso 1 1 calc R . . H33D H 0.1745 1.2690 -0.0815 0.102 Uiso 1 1 calc R . . C34 C -0.0401(4) 0.6953(15) 0.6009(16) 0.111(8) Uani 1 1 d . . . H34A H -0.0541 0.7225 0.5856 0.133 Uiso 1 1 calc R . . H34B H -0.0415 0.6725 0.6609 0.133 Uiso 1 1 calc R . . C34' C 0.1670(5) 1.1651(13) -0.1550(9) 0.120(10) Uani 1 1 d . . . H34C H 0.1598 1.1979 -0.2024 0.144 Uiso 1 1 calc R . . H34D H 0.1825 1.1590 -0.1709 0.144 Uiso 1 1 calc R . . C35 C -0.0363(3) 0.6184(14) 0.5375(14) 0.087(6) Uani 1 1 d . . . H35A H -0.0352 0.6391 0.4766 0.105 Uiso 1 1 calc R . . H35B H -0.0486 0.5776 0.5412 0.105 Uiso 1 1 calc R . . C35' C 0.1579(4) 1.085(2) -0.153(2) 0.126(9) Uiso 1 1 d . . . H35C H 0.1611 1.0548 -0.2087 0.152 Uiso 1 1 calc R . . H35D H 0.1420 1.0896 -0.1471 0.152 Uiso 1 1 calc R . . C36' C 0.1676(4) 1.0297(11) -0.0723(10) 0.092(7) Uani 1 1 d . . . H36A H 0.1594 0.9755 -0.0660 0.110 Uiso 1 1 calc R . . H36B H 0.1830 1.0155 -0.0833 0.110 Uiso 1 1 calc R . . C36 C -0.0138(3) 0.5717(16) 0.5669(14) 0.106(8) Uani 1 1 d . . . H36C H -0.0153 0.5457 0.6256 0.127 Uiso 1 1 calc R . . H36D H -0.0097 0.5265 0.5247 0.127 Uiso 1 1 calc R . . C41' C 0.1089(2) 0.9967(9) 0.1831(9) 0.053(4) Uani 1 1 d . . . H41' H 0.0984 0.9803 0.2300 0.064 Uiso 1 1 calc R . . C41 C 0.0561(2) 0.8076(10) 0.4388(9) 0.052(4) Uani 1 1 d . . . H41 H 0.0501 0.7875 0.3818 0.062 Uiso 1 1 calc R . . C42 C 0.0741(3) 0.8692(9) 0.4154(10) 0.058(4) Uani 1 1 d . . . H42A H 0.0848 0.8409 0.3768 0.069 Uiso 1 1 calc R . . H42B H 0.0817 0.8887 0.4688 0.069 Uiso 1 1 calc R . . C42' C 0.0996(3) 0.9595(11) 0.0986(14) 0.086(6) Uani 1 1 d . . . H42C H 0.1095 0.9729 0.0497 0.104 Uiso 1 1 calc R . . H42D H 0.0988 0.8964 0.1041 0.104 Uiso 1 1 calc R . . C43' C 0.0770(3) 0.9944(12) 0.0773(14) 0.082(6) Uani 1 1 d . . . H43A H 0.0723 0.9712 0.0202 0.098 Uiso 1 1 calc R . . H43B H 0.0667 0.9742 0.1221 0.098 Uiso 1 1 calc R . . C43 C 0.0633(4) 0.9484(12) 0.3666(18) 0.123(10) Uani 1 1 d . . . H43C H 0.0746 0.9921 0.3557 0.147 Uiso 1 1 calc R . . H43D H 0.0578 0.9289 0.3092 0.147 Uiso 1 1 calc R . . C44' C 0.0764(3) 1.0890(13) 0.0738(13) 0.094(7) Uani 1 1 d . . . H44A H 0.0613 1.1085 0.0640 0.113 Uiso 1 1 calc R . . H44B H 0.0855 1.1096 0.0247 0.113 Uiso 1 1 calc R . . C44 C 0.0463(4) 0.9865(14) 0.4118(19) 0.115(8) Uani 1 1 d . . . H44C H 0.0401 1.0333 0.3760 0.138 Uiso 1 1 calc R . . H44D H 0.0519 1.0119 0.4666 0.138 Uiso 1 1 calc R . . C45 C 0.0284(4) 0.9210(16) 0.4336(18) 0.115(8) Uiso 1 1 d . . . H45A H 0.0166 0.9495 0.4670 0.138 Uiso 1 1 calc R . . H45B H 0.0220 0.8984 0.3788 0.138 Uiso 1 1 calc R . . C45' C 0.0850(4) 1.1262(14) 0.1608(15) 0.124(10) Uani 1 1 d . . . H45C H 0.0752 1.1088 0.2089 0.149 Uiso 1 1 calc R . . H45D H 0.0848 1.1895 0.1575 0.149 Uiso 1 1 calc R . . C46' C 0.1092(3) 1.0948(11) 0.1825(14) 0.081(5) Uani 1 1 d . . . H46A H 0.1194 1.1160 0.1376 0.097 Uiso 1 1 calc R . . H46B H 0.1138 1.1168 0.2401 0.097 Uiso 1 1 calc R . . C46 C 0.0374(4) 0.8495(14) 0.4856(13) 0.097(7) Uani 1 1 d . . . H46C H 0.0259 0.8064 0.4965 0.116 Uiso 1 1 calc R . . H46D H 0.0425 0.8714 0.5428 0.116 Uiso 1 1 calc R . . C51 C 0.1440(3) 0.5167(10) 0.6512(8) 0.065(4) Uani 1 1 d . . . H51 H 0.1553 0.5508 0.6199 0.077 Uiso 1 1 calc R . . C51' C 0.1874(3) 0.7936(13) 0.5058(10) 0.067(5) Uani 1 1 d . . . H51' H 0.1914 0.8456 0.5404 0.080 Uiso 1 1 calc R . . C52 C 0.1477(4) 0.4244(14) 0.6264(16) 0.110(8) Uani 1 1 d . . . H52A H 0.1475 0.4195 0.5619 0.132 Uiso 1 1 calc R . . H52B H 0.1356 0.3895 0.6495 0.132 Uiso 1 1 calc R . . C52' C 0.1662(4) 0.763(2) 0.5576(19) 0.134(10) Uiso 1 1 d . . . H52C H 0.1542 0.8026 0.5442 0.161 Uiso 1 1 calc R . . H52D H 0.1620 0.7055 0.5352 0.161 Uiso 1 1 calc R . . C53 C 0.1693(5) 0.387(2) 0.661(2) 0.167(12) Uiso 1 1 d . . . H53A H 0.1687 0.3240 0.6598 0.200 Uiso 1 1 calc R . . H53B H 0.1814 0.4057 0.6224 0.200 Uiso 1 1 calc R . . C53' C 0.1685(6) 0.757(2) 0.656(3) 0.178(14) Uiso 1 1 d . . . H53C H 0.1748 0.8096 0.6806 0.213 Uiso 1 1 calc R . . H53D H 0.1544 0.7444 0.6842 0.213 Uiso 1 1 calc R . . C54 C 0.1733(6) 0.419(3) 0.754(3) 0.177(14) Uiso 1 1 d . . . H54A H 0.1654 0.3797 0.7941 0.212 Uiso 1 1 calc R . . H54B H 0.1890 0.4114 0.7665 0.212 Uiso 1 1 calc R . . C54' C 0.1832(6) 0.686(3) 0.663(3) 0.195(16) Uiso 1 1 d . . . H54C H 0.1781 0.6363 0.6278 0.234 Uiso 1 1 calc R . . H54D H 0.1848 0.6674 0.7244 0.234 Uiso 1 1 calc R . . C55 C 0.1677(5) 0.502(2) 0.776(2) 0.144(10) Uiso 1 1 d . . . H55A H 0.1790 0.5400 0.7513 0.173 Uiso 1 1 calc R . . H55B H 0.1688 0.5067 0.8404 0.173 Uiso 1 1 calc R . . C55' C 0.2059(5) 0.722(2) 0.625(2) 0.168(13) Uiso 1 1 d . . . H55C H 0.2172 0.6770 0.6265 0.202 Uiso 1 1 calc R . . H55D H 0.2109 0.7712 0.6606 0.202 Uiso 1 1 calc R . . C56 C 0.1469(3) 0.5364(18) 0.7510(11) 0.109(8) Uani 1 1 d . . . H56A H 0.1465 0.5990 0.7615 0.130 Uiso 1 1 calc R . . H56B H 0.1351 0.5092 0.7852 0.130 Uiso 1 1 calc R . . C56' C 0.2013(5) 0.755(2) 0.516(2) 0.152(12) Uiso 1 1 d . . . H56C H 0.2142 0.7873 0.4962 0.183 Uiso 1 1 calc R . . H56D H 0.2000 0.7034 0.4794 0.183 Uiso 1 1 calc R . . C61 C 0.0918(3) 0.3655(8) 0.7665(9) 0.053(4) Uani 1 1 d . . . H61 H 0.1059 0.3879 0.7901 0.063 Uiso 1 1 calc R . . C61' C 0.2487(3) 0.9047(11) 0.3349(12) 0.071(5) Uani 1 1 d . . . H61' H 0.2591 0.9339 0.2948 0.086 Uiso 1 1 calc R . . C62' C 0.2506(3) 0.9480(12) 0.4245(13) 0.092(7) Uani 1 1 d . . . H62A H 0.2481 1.0103 0.4176 0.111 Uiso 1 1 calc R . . H62B H 0.2391 0.9254 0.4634 0.111 Uiso 1 1 calc R . . C62 C 0.0773(3) 0.3408(11) 0.8454(11) 0.066(4) Uiso 1 1 d . . . H62C H 0.0746 0.3918 0.8821 0.079 Uiso 1 1 calc R . . H62D H 0.0632 0.3188 0.8244 0.079 Uiso 1 1 calc R . . C63 C 0.0890(3) 0.2715(13) 0.8993(14) 0.087(6) Uiso 1 1 d . . . H63A H 0.1023 0.2963 0.9253 0.104 Uiso 1 1 calc R . . H63B H 0.0794 0.2532 0.9478 0.104 Uiso 1 1 calc R . . C63' C 0.2724(4) 0.9339(19) 0.4666(19) 0.128(9) Uiso 1 1 d . . . H63C H 0.2722 0.9571 0.5268 0.154 Uiso 1 1 calc R . . H63D H 0.2837 0.9649 0.4333 0.154 Uiso 1 1 calc R . . C64' C 0.2780(4) 0.8371(14) 0.4694(19) 0.123(10) Uani 1 1 d . . . H64A H 0.2928 0.8299 0.4926 0.148 Uiso 1 1 calc R . . H64B H 0.2678 0.8079 0.5098 0.148 Uiso 1 1 calc R . . C64 C 0.0948(3) 0.1977(13) 0.8483(13) 0.085(5) Uiso 1 1 d . . . H64C H 0.0814 0.1703 0.8266 0.102 Uiso 1 1 calc R . . H64D H 0.1023 0.1560 0.8866 0.102 Uiso 1 1 calc R . . C65 C 0.1092(4) 0.2171(10) 0.7718(11) 0.086(7) Uani 1 1 d . . . H65A H 0.1123 0.1641 0.7385 0.104 Uiso 1 1 calc R . . H65B H 0.1232 0.2416 0.7920 0.104 Uiso 1 1 calc R . . C65' C 0.2765(3) 0.7949(13) 0.3798(19) 0.103(8) Uani 1 1 d . . . H65C H 0.2880 0.8184 0.3414 0.124 Uiso 1 1 calc R . . H65D H 0.2790 0.7326 0.3858 0.124 Uiso 1 1 calc R . . C66' C 0.2554(3) 0.8101(10) 0.3407(13) 0.074(5) Uani 1 1 d . . . H66A H 0.2443 0.7789 0.3751 0.088 Uiso 1 1 calc R . . H66B H 0.2554 0.7856 0.2810 0.088 Uiso 1 1 calc R . . C66 C 0.0970(3) 0.2823(9) 0.7138(9) 0.078(6) Uani 1 1 d . . . H66C H 0.0832 0.2565 0.6927 0.094 Uiso 1 1 calc R . . H66D H 0.1059 0.2968 0.6622 0.094 Uiso 1 1 calc R . . C71' C 0.2383(3) 0.9740(10) 0.0561(9) 0.057(4) Uani 1 1 d . . . H71' H 0.2405 1.0153 0.1052 0.068 Uiso 1 1 calc R . . C71 C 0.0177(3) 0.3599(11) 0.6705(12) 0.071(5) Uani 1 1 d . . . H71 H 0.0035 0.3659 0.6397 0.085 Uiso 1 1 calc R . . C72' C 0.2341(3) 1.0278(15) -0.0206(18) 0.108(8) Uani 1 1 d . . . H72A H 0.2207 1.0610 -0.0092 0.130 Uiso 1 1 calc R . . H72B H 0.2310 0.9894 -0.0706 0.130 Uiso 1 1 calc R . . C72 C 0.0196(5) 0.2734(15) 0.6845(19) 0.139(11) Uani 1 1 d . . . H72C H 0.0336 0.2620 0.7136 0.167 Uiso 1 1 calc R . . H72D H 0.0198 0.2438 0.6273 0.167 Uiso 1 1 calc R . . C73' C 0.2518(3) 1.0910(15) -0.0492(15) 0.095(6) Uiso 1 1 d . . . H73A H 0.2482 1.1140 -0.1077 0.114 Uiso 1 1 calc R . . H73B H 0.2523 1.1396 -0.0078 0.114 Uiso 1 1 calc R . . C74 C 0.0023(7) 0.2785(15) 0.8319(17) 0.162(14) Uani 1 1 d . . . H74A H 0.0170 0.2717 0.8564 0.195 Uiso 1 1 calc R . . H74B H -0.0083 0.2541 0.8737 0.195 Uiso 1 1 calc R . . C75' C 0.2786(3) 0.999(3) 0.0207(17) 0.21(2) Uani 1 1 d . . . H75A H 0.2813 1.0367 0.0713 0.257 Uiso 1 1 calc R . . H75B H 0.2922 0.9679 0.0077 0.257 Uiso 1 1 calc R . . C75 C -0.0029(3) 0.3773(14) 0.8138(14) 0.092(6) Uiso 1 1 d . . . H75C H -0.0022 0.4105 0.8688 0.111 Uiso 1 1 calc R . . H75D H -0.0176 0.3838 0.7884 0.111 Uiso 1 1 calc R . . C76 C 0.0152(3) 0.4102(11) 0.7465(13) 0.083(6) Uani 1 1 d . . . H76A H 0.0115 0.4693 0.7286 0.100 Uiso 1 1 calc R . . H76B H 0.0293 0.4125 0.7773 0.100 Uiso 1 1 calc R . . C76' C 0.2594(3) 0.9264(11) 0.0490(12) 0.077(5) Uani 1 1 d . . . H76C H 0.2583 0.8810 0.0040 0.093 Uiso 1 1 calc R . . H76D H 0.2631 0.8993 0.1055 0.093 Uiso 1 1 calc R . . C81 C 0.0733(3) 0.351(2) 0.404(2) 0.147(13) Uani 1 1 d . . . H81A H 0.0783 0.3427 0.3439 0.177 Uiso 1 1 calc R . . H81B H 0.0806 0.3105 0.4427 0.177 Uiso 1 1 calc R . . H81C H 0.0767 0.4099 0.4225 0.177 Uiso 1 1 calc R . . C81' C 0.2215(5) 0.6749(15) -0.065(2) 0.144(11) Uani 1 1 d . . . H81D H 0.2128 0.6333 -0.0978 0.172 Uiso 1 1 calc R . . H81E H 0.2251 0.6514 -0.0077 0.172 Uiso 1 1 calc R . . H81F H 0.2349 0.6868 -0.0975 0.172 Uiso 1 1 calc R . . C82' C 0.2087(4) 0.8413(16) -0.1509(14) 0.122(9) Uani 1 1 d . . . H82A H 0.1957 0.8343 -0.1871 0.146 Uiso 1 1 calc R . . H82B H 0.2215 0.8251 -0.1848 0.146 Uiso 1 1 calc R . . H82C H 0.2099 0.9013 -0.1327 0.146 Uiso 1 1 calc R . . C82 C 0.0297(3) 0.4174(13) 0.3480(12) 0.079(5) Uani 1 1 d . . . H82D H 0.0327 0.4119 0.2855 0.094 Uiso 1 1 calc R . . H82E H 0.0339 0.4746 0.3679 0.094 Uiso 1 1 calc R . . H82F H 0.0142 0.4088 0.3585 0.094 Uiso 1 1 calc R . . C83' C 0.1786(3) 0.7517(14) -0.0361(14) 0.095(6) Uani 1 1 d . . . H83A H 0.1767 0.7162 0.0161 0.114 Uiso 1 1 calc R . . H83B H 0.1727 0.7216 -0.0870 0.114 Uiso 1 1 calc R . . H83C H 0.1710 0.8062 -0.0284 0.114 Uiso 1 1 calc R . . C83 C 0.0382(4) 0.2245(18) 0.3727(19) 0.127(9) Uiso 1 1 d . . . H83D H 0.0500 0.2012 0.3368 0.153 Uiso 1 1 calc R . . H83E H 0.0248 0.2264 0.3382 0.153 Uiso 1 1 calc R . . H83F H 0.0360 0.1879 0.4239 0.153 Uiso 1 1 calc R . . C101 C 0.1441(4) 0.4177(15) 0.1917(19) 0.102(9) Uani 1 1 d . . . C102 C 0.14551(19) 0.4422(7) 0.2820(10) 0.046(3) Uani 1 1 d . . . C103 C 0.1584(2) 0.5089(8) 0.2881(9) 0.044(3) Uani 1 1 d . . . C104 C 0.1665(2) 0.5299(10) 0.2046(10) 0.058(4) Uani 1 1 d . . . C105 C 0.1574(4) 0.4699(19) 0.1472(10) 0.098(9) Uani 1 1 d . . . C106 C 0.1328(5) 0.322(2) 0.188(3) 0.171(13) Uiso 1 1 d . . . H10A H 0.1170 0.3276 0.1893 0.205 Uiso 1 1 calc R . . H10B H 0.1376 0.2879 0.2385 0.205 Uiso 1 1 calc R . . H10C H 0.1372 0.2925 0.1341 0.205 Uiso 1 1 calc R . . C107 C 0.1350(3) 0.3989(15) 0.3580(19) 0.139(13) Uani 1 1 d . . . H10D H 0.1458 0.3654 0.3898 0.167 Uiso 1 1 calc R . . H10E H 0.1235 0.3608 0.3370 0.167 Uiso 1 1 calc R . . H10F H 0.1287 0.4422 0.3969 0.167 Uiso 1 1 calc R . . C108 C 0.1652(3) 0.5492(11) 0.3751(12) 0.084(6) Uani 1 1 d . . . H10G H 0.1709 0.6068 0.3646 0.101 Uiso 1 1 calc R . . H10H H 0.1765 0.5138 0.4023 0.101 Uiso 1 1 calc R . . H10I H 0.1526 0.5527 0.4139 0.101 Uiso 1 1 calc R . . C109 C 0.1840(3) 0.599(2) 0.183(3) 0.23(3) Uani 1 1 d . . . H10J H 0.1886 0.6273 0.2376 0.278 Uiso 1 1 calc R . . H10K H 0.1778 0.6419 0.1437 0.278 Uiso 1 1 calc R . . H10L H 0.1965 0.5719 0.1557 0.278 Uiso 1 1 calc R . . C110 C 0.1681(4) 0.480(2) 0.0512(19) 0.134(9) Uiso 1 1 d . . . H11A H 0.1840 0.4775 0.0562 0.161 Uiso 1 1 calc R . . H11B H 0.1639 0.5351 0.0259 0.161 Uiso 1 1 calc R . . H11C H 0.1631 0.4334 0.0135 0.161 Uiso 1 1 calc R . . C111 C 0.1013(2) 0.5061(10) 0.1062(11) 0.057(4) Uani 1 1 d . . . C112 C 0.0899(2) 0.5563(9) 0.1695(8) 0.042(3) Uani 1 1 d . . . C113 C 0.09710(18) 0.6416(8) 0.1590(8) 0.038(3) Uani 1 1 d . . . C114 C 0.1121(2) 0.6452(9) 0.0883(7) 0.040(3) Uani 1 1 d . . . C115 C 0.1147(2) 0.5626(10) 0.0556(8) 0.053(4) Uani 1 1 d . . . C116 C 0.0943(4) 0.4150(12) 0.0891(18) 0.114(9) Uani 1 1 d . . . H11D H 0.0934 0.3839 0.1445 0.137 Uiso 1 1 calc R . . H11E H 0.1049 0.3870 0.0510 0.137 Uiso 1 1 calc R . . H11F H 0.0801 0.4151 0.0606 0.137 Uiso 1 1 calc R . . C117 C 0.0725(2) 0.5295(12) 0.2276(11) 0.069(5) Uani 1 1 d . . . H11G H 0.0742 0.4687 0.2415 0.083 Uiso 1 1 calc R . . H11H H 0.0585 0.5387 0.1988 0.083 Uiso 1 1 calc R . . H11I H 0.0731 0.5632 0.2815 0.083 Uiso 1 1 calc R . . C118 C 0.0880(2) 0.7185(9) 0.2057(9) 0.049(3) Uani 1 1 d . . . H11J H 0.0761 0.7428 0.1713 0.059 Uiso 1 1 calc R . . H11K H 0.0994 0.7616 0.2130 0.059 Uiso 1 1 calc R . . H11L H 0.0825 0.7011 0.2632 0.059 Uiso 1 1 calc R . . C119 C 0.1217(2) 0.7224(13) 0.0510(11) 0.072(5) Uani 1 1 d . . . H11M H 0.1333 0.7433 0.0896 0.086 Uiso 1 1 calc R . . H11N H 0.1106 0.7666 0.0449 0.086 Uiso 1 1 calc R . . H11O H 0.1278 0.7092 -0.0065 0.086 Uiso 1 1 calc R . . C120 C 0.1255(4) 0.5392(18) -0.0255(11) 0.120(10) Uani 1 1 d . . . H12E H 0.1152 0.5100 -0.0640 0.145 Uiso 1 1 calc R . . H12F H 0.1377 0.5009 -0.0128 0.145 Uiso 1 1 calc R . . H12G H 0.1309 0.5910 -0.0544 0.145 Uiso 1 1 calc R . . C74' C 0.2731(5) 1.050(2) -0.052(2) 0.149(11) Uiso 1 1 d . . . H74C H 0.2737 1.0142 -0.1055 0.179 Uiso 1 1 calc R . . H74D H 0.2842 1.0956 -0.0586 0.179 Uiso 1 1 calc R . . C73 C 0.0005(6) 0.233(2) 0.743(3) 0.172(13) Uiso 1 1 d . . . H73C H -0.0138 0.2442 0.7158 0.207 Uiso 1 1 calc R . . H73D H 0.0025 0.1707 0.7495 0.207 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 O2' 0.062(5) 0.022(4) 0.035(5) 0.010(3) -0.006(4) -0.006(4) O2 0.065(6) 0.051(6) 0.044(6) -0.001(4) 0.004(4) -0.006(5) O3' 0.073(6) 0.034(5) 0.030(5) -0.004(3) -0.010(4) -0.006(4) O3 0.067(6) 0.044(6) 0.045(5) 0.017(4) 0.010(4) 0.008(5) O4' 0.089(7) 0.030(5) 0.047(6) 0.003(4) -0.006(5) -0.017(5) O4 0.105(8) 0.035(5) 0.029(5) 0.005(4) -0.013(5) -0.013(5) O5 0.070(6) 0.036(5) 0.033(5) 0.009(4) 0.010(4) 0.011(4) O5' 0.068(6) 0.040(5) 0.037(5) 0.015(4) -0.016(4) -0.006(4) O6' 0.070(6) 0.051(6) 0.021(4) -0.003(4) -0.009(4) 0.011(5) O6 0.099(8) 0.046(6) 0.033(5) 0.000(4) -0.004(5) -0.008(5) Ti1 0.0429(11) 0.0351(11) 0.0123(9) 0.0021(8) 0.0022(8) 0.0024(9) Ti2 0.0482(12) 0.0281(10) 0.0136(9) 0.0043(8) 0.0045(8) 0.0027(9) Ti3 0.0515(12) 0.0276(11) 0.0208(10) 0.0079(8) -0.0082(9) -0.0077(10) Si1 0.082(3) 0.0314(18) 0.0201(16) 0.0009(13) -0.0036(16) 0.0003(18) Si2 0.081(3) 0.040(2) 0.0144(15) 0.0031(13) 0.0115(16) 0.0094(19) Si3 0.061(2) 0.041(2) 0.0308(19) 0.0044(15) 0.0090(16) 0.0049(17) Si4 0.059(2) 0.0351(19) 0.0160(15) 0.0022(13) 0.0082(14) 0.0076(16) Si5 0.075(2) 0.0368(18) 0.0106(15) 0.0062(13) -0.0017(14) 0.0076(18) Si6 0.086(3) 0.0267(17) 0.0298(18) 0.0099(14) 0.0080(18) 0.0045(18) Si7 0.099(3) 0.036(2) 0.044(2) 0.0016(17) 0.005(2) -0.005(2) Si8 0.080(3) 0.053(3) 0.057(3) 0.006(2) 0.009(2) 0.002(2) Si1' 0.076(3) 0.039(2) 0.0285(19) -0.0020(14) 0.0044(17) -0.0114(19) Si2' 0.068(2) 0.0323(18) 0.0260(18) 0.0063(13) -0.0015(15) -0.0132(17) Si3' 0.060(2) 0.0338(18) 0.0205(16) 0.0097(13) -0.0020(14) 0.0001(16) Si4' 0.058(2) 0.0329(18) 0.0286(18) 0.0100(14) -0.0069(15) -0.0012(16) Si5' 0.062(2) 0.0389(19) 0.0237(17) 0.0126(14) -0.0121(15) -0.0173(17) Si6' 0.058(2) 0.037(2) 0.039(2) 0.0177(16) -0.0058(17) -0.0052(17) Si7' 0.070(2) 0.0356(19) 0.0273(18) 0.0054(14) -0.0045(17) 0.0036(18) Si8' 0.095(3) 0.061(3) 0.066(3) -0.026(2) 0.021(3) -0.019(3) O1 0.081(6) 0.040(5) 0.028(5) -0.004(4) -0.006(4) -0.013(5) O1' 0.073(6) 0.040(5) 0.022(4) 0.010(4) 0.009(4) -0.007(4) O7 0.067(5) 0.040(5) 0.015(4) -0.002(3) -0.001(4) 0.016(4) O7' 0.088(7) 0.035(5) 0.033(5) 0.006(4) -0.007(4) -0.016(5) O8' 0.065(6) 0.052(6) 0.023(4) -0.003(4) 0.004(4) -0.014(4) O8 0.067(6) 0.042(5) 0.018(4) 0.003(3) 0.002(4) 0.006(4) O9' 0.058(5) 0.039(5) 0.042(5) 0.013(4) -0.013(4) -0.020(4) O9 0.075(6) 0.045(6) 0.026(5) 0.004(4) 0.002(4) -0.007(5) O10' 0.113(8) 0.045(5) 0.028(5) 0.027(4) -0.005(5) 0.006(5) O10 0.082(7) 0.048(6) 0.050(6) -0.001(4) 0.002(5) -0.012(5) C11' 0.114(13) 0.032(8) 0.047(9) -0.003(6) 0.029(8) -0.009(8) C11 0.131(13) 0.027(6) 0.006(5) -0.002(4) -0.009(6) -0.009(7) O11 0.129(10) 0.038(6) 0.051(6) -0.003(5) -0.008(6) -0.001(6) O11' 0.108(8) 0.030(5) 0.058(7) -0.011(5) -0.014(6) 0.001(5) O12 0.087(6) 0.046(5) 0.007(4) 0.012(3) 0.013(4) 0.007(5) O12' 0.047(5) 0.032(5) 0.038(5) 0.012(4) -0.025(4) -0.010(4) C12 0.105(12) 0.052(9) 0.022(7) 0.006(6) -0.023(7) -0.010(8) C12' 0.100(13) 0.065(11) 0.046(9) 0.000(8) 0.003(8) -0.016(10) O13 0.040(4) 0.035(4) 0.015(4) 0.004(3) -0.002(3) -0.005(3) C13 0.094(12) 0.069(11) 0.036(8) -0.007(7) -0.033(8) -0.014(9) C13' 0.110(14) 0.081(14) 0.059(11) -0.031(10) 0.020(10) -0.041(12) O14 0.055(5) 0.025(4) 0.009(3) 0.001(3) 0.009(3) -0.006(4) C14' 0.126(18) 0.14(2) 0.064(13) -0.045(14) 0.025(12) 0.027(17) O15 0.049(5) 0.040(5) 0.012(4) 0.003(3) -0.005(3) -0.002(4) C15' 0.097(13) 0.066(11) 0.038(9) -0.002(7) 0.013(8) -0.008(10) C15 0.17(2) 0.039(9) 0.082(13) -0.018(8) -0.079(14) 0.013(11) C16' 0.111(13) 0.038(8) 0.056(10) 0.006(7) 0.026(9) -0.018(9) C16 0.122(14) 0.051(9) 0.042(9) -0.006(7) -0.037(9) -0.004(9) C21' 0.052(8) 0.038(7) 0.056(9) 0.003(6) -0.015(7) 0.007(6) C21 0.074(10) 0.099(14) 0.038(9) -0.024(8) 0.012(7) 0.003(10) C22' 0.050(8) 0.048(9) 0.090(12) -0.011(8) -0.010(8) -0.001(7) C22 0.135(17) 0.14(2) 0.049(11) 0.025(12) 0.034(11) 0.079(16) C23' 0.101(14) 0.035(9) 0.15(2) -0.026(11) -0.032(14) 0.010(9) C23 0.127(17) 0.18(3) 0.059(13) -0.006(14) -0.014(12) 0.095(18) C24 0.21(3) 0.18(3) 0.22(3) -0.18(3) -0.13(3) 0.14(3) C24' 0.097(14) 0.048(11) 0.17(2) 0.029(13) 0.036(16) 0.014(10) C25' 0.125(17) 0.070(13) 0.105(17) -0.009(12) -0.018(13) -0.048(13) C25 0.103(14) 0.127(19) 0.042(10) -0.010(10) -0.012(9) 0.027(13) C26' 0.080(11) 0.053(10) 0.100(14) 0.038(10) 0.016(10) -0.002(8) C26 0.110(13) 0.067(11) 0.049(9) -0.002(8) -0.008(9) 0.041(10) C31 0.080(10) 0.032(8) 0.064(10) -0.010(7) 0.006(8) 0.009(7) C31' 0.102(12) 0.038(8) 0.031(7) 0.006(6) 0.000(7) -0.001(8) C32 0.084(11) 0.059(10) 0.047(9) -0.020(7) -0.002(7) 0.019(9) C32' 0.25(3) 0.065(13) 0.028(9) 0.017(8) -0.015(13) 0.038(15) C33 0.079(11) 0.041(9) 0.108(16) -0.002(9) 0.008(10) 0.006(9) C33' 0.160(18) 0.068(11) 0.028(8) 0.011(7) -0.004(9) 0.043(12) C34 0.15(2) 0.088(16) 0.099(17) -0.005(13) -0.003(15) 0.068(16) C34' 0.27(3) 0.084(14) 0.006(6) 0.009(7) -0.003(11) 0.066(17) C35 0.073(12) 0.108(17) 0.080(14) -0.006(12) -0.015(10) 0.016(11) C36' 0.18(2) 0.061(11) 0.031(8) 0.021(7) -0.050(10) -0.030(12) C36 0.111(16) 0.14(2) 0.070(14) -0.028(13) 0.031(12) -0.033(15) C41' 0.074(9) 0.049(8) 0.037(8) 0.022(6) -0.001(6) 0.011(7) C41 0.059(8) 0.060(9) 0.036(7) 0.023(6) 0.022(6) -0.005(7) C42 0.093(11) 0.032(7) 0.049(8) 0.011(6) -0.004(8) -0.001(7) C42' 0.121(15) 0.049(10) 0.089(14) -0.006(9) -0.038(12) 0.023(10) C43' 0.082(12) 0.071(12) 0.093(14) -0.032(10) -0.034(10) 0.032(10) C43 0.17(2) 0.044(11) 0.15(2) 0.032(12) 0.089(19) 0.017(13) C44' 0.099(13) 0.091(14) 0.092(15) 0.068(12) 0.013(11) 0.038(11) C44 0.15(2) 0.063(13) 0.13(2) 0.003(14) 0.046(17) -0.002(14) C45' 0.21(3) 0.086(16) 0.079(15) -0.001(12) -0.043(16) 0.092(17) C46' 0.105(14) 0.054(10) 0.083(13) 0.019(9) -0.006(10) 0.014(10) C46 0.141(18) 0.082(14) 0.067(13) 0.041(11) 0.006(12) 0.029(13) C51 0.114(13) 0.060(10) 0.019(7) 0.022(6) -0.002(7) 0.006(9) C51' 0.066(10) 0.087(13) 0.047(9) 0.030(8) -0.012(7) -0.032(9) C52 0.120(16) 0.097(16) 0.113(18) 0.044(13) -0.032(13) 0.068(13) C56 0.105(14) 0.19(3) 0.028(9) 0.010(12) -0.035(9) 0.031(16) C61 0.092(10) 0.029(7) 0.037(7) 0.010(5) 0.024(7) 0.002(7) C61' 0.061(10) 0.074(12) 0.079(12) 0.049(10) -0.018(8) -0.010(8) C62' 0.129(16) 0.056(11) 0.091(15) -0.024(10) -0.060(13) 0.005(11) C64' 0.123(18) 0.073(15) 0.17(3) 0.031(15) -0.102(18) 0.007(13) C65 0.165(18) 0.034(8) 0.060(11) 0.024(7) 0.052(11) 0.049(10) C65' 0.075(12) 0.055(12) 0.18(3) 0.041(14) -0.045(14) -0.010(10) C66' 0.079(11) 0.046(9) 0.096(13) 0.015(9) -0.008(10) 0.024(8) C66 0.182(18) 0.030(7) 0.023(7) 0.012(6) 0.020(9) 0.043(9) C71' 0.081(10) 0.053(9) 0.036(8) 0.007(6) -0.010(7) 0.028(8) C71 0.091(12) 0.058(11) 0.064(11) -0.007(8) 0.007(9) -0.016(9) C72' 0.043(10) 0.115(19) 0.17(2) -0.037(17) 0.004(12) 0.007(11) C72 0.23(3) 0.071(15) 0.12(2) -0.032(15) 0.04(2) -0.043(18) C74 0.33(5) 0.071(16) 0.084(18) 0.030(13) -0.01(2) -0.02(2) C75' 0.047(11) 0.50(7) 0.093(18) 0.13(3) 0.027(11) 0.02(2) C76 0.111(14) 0.048(10) 0.091(14) 0.044(10) -0.009(11) -0.005(10) C76' 0.121(15) 0.055(11) 0.056(11) 0.001(8) 0.001(10) 0.002(10) C81 0.090(15) 0.18(3) 0.17(3) 0.11(2) 0.040(16) 0.031(17) C81' 0.22(3) 0.066(15) 0.14(2) -0.028(15) -0.03(2) 0.011(17) C82' 0.18(2) 0.12(2) 0.070(14) -0.016(13) 0.038(14) -0.082(18) C82 0.080(12) 0.098(15) 0.058(11) 0.023(10) 0.003(9) -0.007(10) C83' 0.119(16) 0.086(15) 0.079(14) 0.012(11) 0.009(12) -0.034(12) C101 0.091(14) 0.089(16) 0.13(2) -0.072(15) -0.048(14) 0.066(13) C102 0.039(7) 0.015(6) 0.083(10) 0.020(6) 0.002(7) 0.011(5) C103 0.051(8) 0.042(7) 0.038(7) -0.003(6) -0.018(6) -0.009(6) C104 0.073(9) 0.053(9) 0.049(9) 0.018(7) 0.023(8) 0.021(7) C105 0.102(15) 0.17(2) 0.024(8) -0.012(11) 0.009(9) 0.102(16) C107 0.102(14) 0.117(18) 0.20(3) 0.137(19) 0.085(16) 0.058(14) C108 0.130(15) 0.049(9) 0.074(12) -0.018(8) -0.072(11) 0.025(10) C109 0.051(12) 0.24(4) 0.41(6) 0.25(4) 0.06(2) 0.029(17) C111 0.051(8) 0.053(9) 0.067(10) -0.026(8) -0.021(7) 0.011(7) C112 0.048(7) 0.048(8) 0.030(6) 0.005(6) -0.005(5) -0.016(6) C113 0.035(6) 0.050(8) 0.029(6) 0.000(5) -0.012(5) 0.010(6) C114 0.056(8) 0.054(8) 0.012(5) 0.009(5) -0.003(5) -0.001(6) C115 0.076(10) 0.064(10) 0.018(6) -0.004(6) 0.004(6) 0.028(8) C116 0.122(16) 0.061(12) 0.16(2) -0.037(13) -0.095(16) 0.010(11) C117 0.049(8) 0.098(14) 0.059(10) 0.022(9) -0.008(7) -0.006(9) C118 0.053(8) 0.055(8) 0.039(7) -0.023(7) -0.006(6) 0.017(7) C119 0.047(9) 0.119(16) 0.049(10) 0.031(9) -0.005(7) -0.002(9) C120 0.133(17) 0.20(3) 0.029(9) -0.021(12) -0.006(10) 0.101(18) _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 O2' Si3' 1.616(9) . ? O2' Si2' 1.626(9) . ? O2 Si3 1.607(10) . ? O2 Si2 1.641(10) . ? O3' Si3' 1.614(10) . ? O3' Si4' 1.633(10) . ? O3 Si3 1.586(9) . ? O3 Si4 1.627(10) . ? O4' Si4' 1.612(10) . ? O4' Si1' 1.634(10) . ? O4 Si4 1.616(10) . ? O4 Si1 1.622(9) . ? O5 Si6 1.590(9) . ? O5 Si2 1.633(9) . ? O5' Si2' 1.591(10) . ? O5' Si6' 1.634(10) . ? O6' Si3' 1.577(9) . ? O6' Si7' 1.635(10) . ? O6 Si3 1.587(10) . ? O6 Si7 1.648(11) . ? Ti1 O15 1.926(8) . ? Ti1 O14 1.953(7) . ? Ti1 C103 2.380(12) . ? Ti1 C104 2.401(15) . ? Ti1 C111 2.413(13) . ? Ti1 C113 2.414(11) . ? Ti1 C102 2.426(11) . ? Ti1 C112 2.431(12) . ? Ti1 C101 2.443(17) . ? Ti1 C114 2.449(11) . ? Ti1 C115 2.450(13) . ? Ti1 C105 2.452(15) . ? Ti2 O14 1.730(7) . ? Ti2 O13 1.801(8) . ? Ti2 O7 1.822(8) . ? Ti2 O12 1.824(8) . ? Ti2 Ti3 3.309(3) . ? Ti3 O15 1.771(8) . ? Ti3 O7' 1.816(9) . ? Ti3 O12' 1.835(8) . ? Ti3 O13 1.837(7) . ? Si1 O8 1.585(9) . ? Si1 O1 1.627(10) . ? Si1 C11 1.844(13) . ? Si2 O1 1.617(10) . ? Si2 C21 1.887(14) . ? Si3 C31 1.856(16) . ? Si4 O7 1.607(8) . ? Si4 C41 1.854(14) . ? Si5 O9 1.591(10) . ? Si5 O12 1.629(8) . ? Si5 O8 1.632(9) . ? Si5 C51 1.855(17) . ? Si6 O10 1.581(11) . ? Si6 O9 1.632(9) . ? Si6 C61 1.829(14) . ? Si7 O11 1.584(11) . ? Si7 O10 1.653(12) . ? Si7 C71 1.846(17) . ? Si8 O11 1.619(12) . ? Si8 C81 1.74(2) . ? Si8 C82 1.857(18) . ? Si8 C83 1.88(3) . ? Si1' O1' 1.576(9) . ? Si1' O8' 1.630(10) . ? Si1' C11' 1.824(15) . ? Si2' O1' 1.640(9) . ? Si2' C21' 1.825(14) . ? Si3' C31' 1.889(14) . ? Si4' O7' 1.617(9) . ? Si4' C41' 1.833(14) . ? Si5' O8' 1.588(10) . ? Si5' O9' 1.614(9) . ? Si5' O12' 1.623(8) . ? Si5' C51' 1.819(15) . ? Si6' O9' 1.597(9) . ? Si6' O10' 1.611(11) . ? Si6' C61' 1.829(15) . ? Si7' O11' 1.611(10) . ? Si7' O10' 1.621(9) . ? Si7' C71' 1.836(17) . ? Si8' O11' 1.610(11) . ? Si8' C83' 1.76(2) . ? Si8' C81' 1.78(2) . ? Si8' C82' 1.87(2) . ? C11' C16' 1.51(2) . ? C11' C12' 1.52(2) . ? C11 C12 1.523(17) . ? C11 C16 1.55(2) . ? C12 C13 1.477(19) . ? C12' C13' 1.60(2) . ? C13 C14 1.51(2) . ? C13' C14' 1.51(3) . ? C14' C15' 1.49(3) . ? C14 C15 1.50(2) . ? C15' C16' 1.46(2) . ? C15 C16 1.54(2) . ? C21' C22' 1.535(19) . ? C21' C26' 1.55(2) . ? C21 C26 1.46(2) . ? C21 C22 1.63(3) . ? C22' C23' 1.51(2) . ? C22 C23 1.50(3) . ? C23' C24' 1.53(3) . ? C23 C24 1.51(3) . ? C24 C25 1.54(4) . ? C24' C25' 1.47(3) . ? C25' C26' 1.52(2) . ? C25 C26 1.53(2) . ? C31 C32 1.507(18) . ? C31 C36 1.52(2) . ? C31' C32' 1.40(3) . ? C31' C36' 1.52(2) . ? C32 C33 1.50(2) . ? C32' C33' 1.54(2) . ? C33 C34 1.36(3) . ? C33' C34' 1.47(2) . ? C34 C35 1.56(3) . ? C34' C35' 1.37(3) . ? C35 C36 1.63(3) . ? C35' C36' 1.62(3) . ? C41' C42' 1.53(2) . ? C41' C46' 1.53(2) . ? C41 C46 1.50(2) . ? C41 C42 1.511(19) . ? C42 C43 1.59(3) . ? C42' C43' 1.53(2) . ? C43' C44' 1.48(3) . ? C43 C44 1.39(3) . ? C44' C45' 1.55(3) . ? C44 C45 1.54(3) . ? C45 C46 1.48(3) . ? C45' C46' 1.60(3) . ? C51 C52 1.51(3) . ? C51 C56 1.57(2) . ? C51' C56' 1.06(3) . ? C51' C52' 1.60(3) . ? C52 C53 1.54(4) . ? C52' C53' 1.51(4) . ? C53 C54 1.53(5) . ? C53' C54' 1.44(4) . ? C54 C55 1.39(4) . ? C54' C55' 1.62(4) . ? C55 C56 1.45(3) . ? C55' C56' 1.76(5) . ? C61 C62 1.55(2) . ? C61 C66 1.562(18) . ? C61' C62' 1.53(3) . ? C61' C66' 1.54(2) . ? C62' C63' 1.51(3) . ? C62 C63 1.54(2) . ? C63 C64 1.44(3) . ? C63' C64' 1.55(3) . ? C64' C65' 1.52(3) . ? C64 C65 1.50(2) . ? C65 C66 1.55(2) . ? C65' C66' 1.45(2) . ? C71' C72' 1.47(3) . ? C71' C76' 1.50(2) . ? C71 C72 1.37(3) . ? C71 C76 1.41(3) . ? C72' C73' 1.54(3) . ? C72 C73 1.60(4) . ? C73' C74' 1.46(3) . ? C74 C73 1.54(4) . ? C74 C75 1.60(3) . ? C75' C74' 1.42(4) . ? C75' C76' 1.69(4) . ? C75 C76 1.60(3) . ? C101 C105 1.34(3) . ? C101 C102 1.44(3) . ? C101 C106 1.66(4) . ? C102 C103 1.313(17) . ? C102 C107 1.49(2) . ? C103 C104 1.411(19) . ? C103 C108 1.532(19) . ? C104 C105 1.40(3) . ? C104 C109 1.56(3) . ? C105 C110 1.62(3) . ? C111 C112 1.432(19) . ? C111 C115 1.44(2) . ? C111 C116 1.51(2) . ? C112 C113 1.413(18) . ? C112 C117 1.455(19) . ? C113 C114 1.425(17) . ? C113 C118 1.506(16) . ? C114 C115 1.392(19) . ? C114 C119 1.46(2) . ? C115 C120 1.46(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si3' O2' Si2' 149.6(5) . . ? Si3 O2 Si2 146.0(6) . . ? Si3' O3' Si4' 145.2(6) . . ? Si3 O3 Si4 164.7(7) . . ? Si4' O4' Si1' 147.2(7) . . ? Si4 O4 Si1 148.3(6) . . ? Si6 O5 Si2 144.3(6) . . ? Si2' O5' Si6' 147.3(6) . . ? Si3' O6' Si7' 154.5(6) . . ? Si3 O6 Si7 144.2(6) . . ? O15 Ti1 O14 95.1(3) . . ? O15 Ti1 C103 84.8(4) . . ? O14 Ti1 C103 84.5(4) . . ? O15 Ti1 C104 76.0(5) . . ? O14 Ti1 C104 118.1(4) . . ? C103 Ti1 C104 34.3(5) . . ? O15 Ti1 C111 133.0(5) . . ? O14 Ti1 C111 103.9(5) . . ? C103 Ti1 C111 138.8(5) . . ? C104 Ti1 C111 126.9(5) . . ? O15 Ti1 C113 84.5(4) . . ? O14 Ti1 C113 83.1(4) . . ? C103 Ti1 C113 162.9(4) . . ? C104 Ti1 C113 152.0(5) . . ? C111 Ti1 C113 56.4(4) . . ? O15 Ti1 C102 116.2(4) . . ? O14 Ti1 C102 78.1(4) . . ? C103 Ti1 C102 31.7(4) . . ? C104 Ti1 C102 54.9(4) . . ? C111 Ti1 C102 109.7(5) . . ? C113 Ti1 C102 153.0(4) . . ? O15 Ti1 C112 117.8(4) . . ? O14 Ti1 C112 75.3(4) . . ? C103 Ti1 C112 150.5(4) . . ? C104 Ti1 C112 161.2(5) . . ? C111 Ti1 C112 34.4(5) . . ? C113 Ti1 C112 33.9(4) . . ? C102 Ti1 C112 121.0(4) . . ? O15 Ti1 C101 131.1(6) . . ? O14 Ti1 C101 106.2(8) . . ? C103 Ti1 C101 55.1(5) . . ? C104 Ti1 C101 55.1(7) . . ? C111 Ti1 C101 84.1(6) . . ? C113 Ti1 C101 140.4(5) . . ? C102 Ti1 C101 34.3(7) . . ? C112 Ti1 C101 110.1(6) . . ? O15 Ti1 C114 76.9(4) . . ? O14 Ti1 C114 116.7(4) . . ? C103 Ti1 C114 152.8(4) . . ? C104 Ti1 C114 120.1(4) . . ? C111 Ti1 C114 56.1(5) . . ? C113 Ti1 C114 34.1(4) . . ? C102 Ti1 C114 160.5(5) . . ? C112 Ti1 C114 56.5(4) . . ? C101 Ti1 C114 126.2(7) . . ? O15 Ti1 C115 103.8(5) . . ? O14 Ti1 C115 131.9(4) . . ? C103 Ti1 C115 140.1(5) . . ? C104 Ti1 C115 109.3(5) . . ? C111 Ti1 C115 34.3(5) . . ? C113 Ti1 C115 55.9(4) . . ? C102 Ti1 C115 127.7(5) . . ? C112 Ti1 C115 56.8(4) . . ? C101 Ti1 C115 93.7(7) . . ? C114 Ti1 C115 33.0(4) . . ? O15 Ti1 C105 104.2(8) . . ? O14 Ti1 C105 132.5(5) . . ? C103 Ti1 C105 55.3(5) . . ? C104 Ti1 C105 33.6(7) . . ? C111 Ti1 C105 93.9(7) . . ? C113 Ti1 C105 140.9(5) . . ? C102 Ti1 C105 54.4(6) . . ? C112 Ti1 C105 127.7(7) . . ? C101 Ti1 C105 31.8(8) . . ? C114 Ti1 C105 109.9(5) . . ? C115 Ti1 C105 85.0(5) . . ? O14 Ti2 O13 107.3(3) . . ? O14 Ti2 O7 111.3(4) . . ? O13 Ti2 O7 107.4(4) . . ? O14 Ti2 O12 109.6(4) . . ? O13 Ti2 O12 113.2(4) . . ? O7 Ti2 O12 108.0(4) . . ? O14 Ti2 Ti3 82.4(2) . . ? O13 Ti2 Ti3 24.8(2) . . ? O7 Ti2 Ti3 118.7(3) . . ? O12 Ti2 Ti3 123.3(3) . . ? O15 Ti3 O7' 109.6(4) . . ? O15 Ti3 O12' 110.7(4) . . ? O7' Ti3 O12' 108.3(4) . . ? O15 Ti3 O13 107.2(4) . . ? O7' Ti3 O13 113.0(4) . . ? O12' Ti3 O13 108.0(3) . . ? O15 Ti3 Ti2 82.9(3) . . ? O7' Ti3 Ti2 123.5(3) . . ? O12' Ti3 Ti2 118.1(3) . . ? O13 Ti3 Ti2 24.3(2) . . ? O8 Si1 O4 110.7(5) . . ? O8 Si1 O1 110.1(5) . . ? O4 Si1 O1 108.9(5) . . ? O8 Si1 C11 109.1(6) . . ? O4 Si1 C11 111.0(5) . . ? O1 Si1 C11 106.9(6) . . ? O1 Si2 O5 108.5(5) . . ? O1 Si2 O2 110.1(5) . . ? O5 Si2 O2 110.4(5) . . ? O1 Si2 C21 111.7(7) . . ? O5 Si2 C21 110.2(7) . . ? O2 Si2 C21 106.0(6) . . ? O3 Si3 O6 109.3(5) . . ? O3 Si3 O2 109.3(5) . . ? O6 Si3 O2 109.9(5) . . ? O3 Si3 C31 109.6(6) . . ? O6 Si3 C31 109.7(6) . . ? O2 Si3 C31 109.0(6) . . ? O7 Si4 O4 109.3(5) . . ? O7 Si4 O3 109.6(5) . . ? O4 Si4 O3 110.6(5) . . ? O7 Si4 C41 110.1(5) . . ? O4 Si4 C41 108.1(6) . . ? O3 Si4 C41 109.1(5) . . ? O9 Si5 O12 109.4(5) . . ? O9 Si5 O8 107.2(5) . . ? O12 Si5 O8 109.7(4) . . ? O9 Si5 C51 110.8(6) . . ? O12 Si5 C51 108.2(6) . . ? O8 Si5 C51 111.5(6) . . ? O10 Si6 O5 109.7(6) . . ? O10 Si6 O9 108.7(5) . . ? O5 Si6 O9 110.2(5) . . ? O10 Si6 C61 108.8(7) . . ? O5 Si6 C61 109.2(5) . . ? O9 Si6 C61 110.3(6) . . ? O11 Si7 O6 107.1(5) . . ? O11 Si7 O10 111.7(6) . . ? O6 Si7 O10 108.6(5) . . ? O11 Si7 C71 106.9(7) . . ? O6 Si7 C71 113.3(7) . . ? O10 Si7 C71 109.2(7) . . ? O11 Si8 C81 109.6(12) . . ? O11 Si8 C82 105.2(8) . . ? C81 Si8 C82 113.3(10) . . ? O11 Si8 C83 106.5(10) . . ? C81 Si8 C83 110.7(14) . . ? C82 Si8 C83 111.2(11) . . ? O1' Si1' O8' 109.8(5) . . ? O1' Si1' O4' 107.7(5) . . ? O8' Si1' O4' 110.1(5) . . ? O1' Si1' C11' 111.2(6) . . ? O8' Si1' C11' 111.3(6) . . ? O4' Si1' C11' 106.6(7) . . ? O5' Si2' O2' 108.6(5) . . ? O5' Si2' O1' 110.0(5) . . ? O2' Si2' O1' 107.4(5) . . ? O5' Si2' C21' 109.3(5) . . ? O2' Si2' C21' 111.3(5) . . ? O1' Si2' C21' 110.1(6) . . ? O6' Si3' O3' 108.9(5) . . ? O6' Si3' O2' 109.2(5) . . ? O3' Si3' O2' 109.8(4) . . ? O6' Si3' C31' 110.4(6) . . ? O3' Si3' C31' 107.6(6) . . ? O2' Si3' C31' 111.0(5) . . ? O4' Si4' O7' 111.6(5) . . ? O4' Si4' O3' 107.3(5) . . ? O7' Si4' O3' 109.0(5) . . ? O4' Si4' C41' 107.5(6) . . ? O7' Si4' C41' 110.3(6) . . ? O3' Si4' C41' 111.1(6) . . ? O8' Si5' O9' 108.8(5) . . ? O8' Si5' O12' 109.2(5) . . ? O9' Si5' O12' 108.6(5) . . ? O8' Si5' C51' 107.3(8) . . ? O9' Si5' C51' 112.8(6) . . ? O12' Si5' C51' 110.0(7) . . ? O9' Si6' O10' 109.3(5) . . ? O9' Si6' O5' 108.7(5) . . ? O10' Si6' O5' 108.4(5) . . ? O9' Si6' C61' 108.8(6) . . ? O10' Si6' C61' 110.9(8) . . ? O5' Si6' C61' 110.8(7) . . ? O11' Si7' O10' 107.4(6) . . ? O11' Si7' O6' 107.9(5) . . ? O10' Si7' O6' 111.5(5) . . ? O11' Si7' C71' 109.3(7) . . ? O10' Si7' C71' 110.0(6) . . ? O6' Si7' C71' 110.7(6) . . ? O11' Si8' C83' 108.2(9) . . ? O11' Si8' C81' 107.2(10) . . ? C83' Si8' C81' 112.0(13) . . ? O11' Si8' C82' 111.4(8) . . ? C83' Si8' C82' 106.5(11) . . ? C81' Si8' C82' 111.6(14) . . ? Si2 O1 Si1 145.9(6) . . ? Si1' O1' Si2' 142.0(6) . . ? Si4 O7 Ti2 138.3(5) . . ? Si4' O7' Ti3 153.0(6) . . ? Si5' O8' Si1' 149.5(6) . . ? Si1 O8 Si5 145.5(6) . . ? Si6' O9' Si5' 164.4(6) . . ? Si5 O9 Si6 152.6(6) . . ? Si6' O10' Si7' 138.4(6) . . ? Si6 O10 Si7 154.7(8) . . ? C16' C11' C12' 109.5(15) . . ? C16' C11' Si1' 114.7(10) . . ? C12' C11' Si1' 108.1(11) . . ? C12 C11 C16 110.9(11) . . ? C12 C11 Si1 112.4(9) . . ? C16 C11 Si1 109.4(11) . . ? Si7 O11 Si8 143.7(8) . . ? Si8' O11' Si7' 147.3(8) . . ? Si5 O12 Ti2 149.2(6) . . ? Si5' O12' Ti3 137.8(6) . . ? C13 C12 C11 113.0(12) . . ? C11' C12' C13' 113.7(14) . . ? Ti2 O13 Ti3 130.9(4) . . ? C12 C13 C14 115.5(14) . . ? C14' C13' C12' 107.3(15) . . ? Ti2 O14 Ti1 140.5(4) . . ? C15' C14' C13' 110.7(18) . . ? C15 C14 C13 110.4(15) . . ? Ti3 O15 Ti1 139.0(4) . . ? C16' C15' C14' 112.5(15) . . ? C14 C15 C16 112.1(14) . . ? C15' C16' C11' 116.4(13) . . ? C15 C16 C11 111.7(14) . . ? C22' C21' C26' 109.0(13) . . ? C22' C21' Si2' 112.5(9) . . ? C26' C21' Si2' 113.3(11) . . ? C26 C21 C22 107.3(15) . . ? C26 C21 Si2 113.6(12) . . ? C22 C21 Si2 107.9(12) . . ? C23' C22' C21' 112.3(13) . . ? C23 C22 C21 110.2(17) . . ? C22' C23' C24' 106.3(18) . . ? C22 C23 C24 103(2) . . ? C23 C24 C25 110(2) . . ? C25' C24' C23' 105.0(19) . . ? C24' C25' C26' 112.2(17) . . ? C26 C25 C24 105(2) . . ? C25' C26' C21' 107.7(17) . . ? C21 C26 C25 114.6(15) . . ? C32 C31 C36 113.5(14) . . ? C32 C31 Si3 115.1(11) . . ? C36 C31 Si3 110.9(13) . . ? C32' C31' C36' 115.0(14) . . ? C32' C31' Si3' 116.7(12) . . ? C36' C31' Si3' 110.1(10) . . ? C33 C32 C31 112.6(14) . . ? C31' C32' C33' 114.0(19) . . ? C34 C33 C32 108.9(16) . . ? C34' C33' C32' 111.5(14) . . ? C33 C34 C35 116(2) . . ? C35' C34' C33' 117(2) . . ? C34 C35 C36 107.4(16) . . ? C34' C35' C36' 111(2) . . ? C31' C36' C35' 108.7(17) . . ? C31 C36 C35 104.5(18) . . ? C42' C41' C46' 112.2(13) . . ? C42' C41' Si4' 116.3(11) . . ? C46' C41' Si4' 111.0(11) . . ? C46 C41 C42 113.4(15) . . ? C46 C41 Si4 115.5(9) . . ? C42 C41 Si4 110.5(10) . . ? C41 C42 C43 107.3(14) . . ? C43' C42' C41' 112.8(15) . . ? C44' C43' C42' 112.8(16) . . ? C44 C43 C42 114.5(19) . . ? C43' C44' C45' 109.6(14) . . ? C43 C44 C45 111(2) . . ? C46 C45 C44 110(2) . . ? C44' C45' C46' 112.4(17) . . ? C41' C46' C45' 107.4(16) . . ? C45 C46 C41 111.1(16) . . ? C52 C51 C56 114.6(15) . . ? C52 C51 Si5 112.0(13) . . ? C56 C51 Si5 110.4(12) . . ? C56' C51' C52' 114(3) . . ? C56' C51' Si5' 121(2) . . ? C52' C51' Si5' 115.3(14) . . ? C51 C52 C53 114(2) . . ? C53' C52' C51' 116(3) . . ? C54 C53 C52 110(3) . . ? C54' C53' C52' 100(3) . . ? C55 C54 C53 119(4) . . ? C53' C54' C55' 104(3) . . ? C54 C55 C56 120(3) . . ? C54' C55' C56' 108(3) . . ? C55 C56 C51 107(2) . . ? C51' C56' C55' 116(3) . . ? C62 C61 C66 108.2(12) . . ? C62 C61 Si6 113.6(11) . . ? C66 C61 Si6 112.1(9) . . ? C62' C61' C66' 110.6(14) . . ? C62' C61' Si6' 111.8(14) . . ? C66' C61' Si6' 111.8(12) . . ? C63' C62' C61' 112.7(19) . . ? C63 C62 C61 109.0(13) . . ? C64 C63 C62 112.9(17) . . ? C62' C63' C64' 111(2) . . ? C65' C64' C63' 112.6(19) . . ? C63 C64 C65 114.3(17) . . ? C64 C65 C66 106.9(15) . . ? C66' C65' C64' 111(2) . . ? C65' C66' C61' 114.9(15) . . ? C65 C66 C61 110.5(12) . . ? C72' C71' C76' 112.1(14) . . ? C72' C71' Si7' 117.0(12) . . ? C76' C71' Si7' 111.8(11) . . ? C72 C71 C76 115.3(18) . . ? C72 C71 Si7 114.7(17) . . ? C76 C71 Si7 113.4(13) . . ? C71' C72' C73' 118.1(17) . . ? C71 C72 C73 114(3) . . ? C74' C73' C72' 112(2) . . ? C73 C74 C75 106(2) . . ? C74' C75' C76' 114(2) . . ? C74 C75 C76 106.4(19) . . ? C71 C76 C75 115.4(16) . . ? C71' C76' C75' 107.0(17) . . ? C105 C101 C102 106.9(17) . . ? C105 C101 C106 142(2) . . ? C102 C101 C106 107(3) . . ? C105 C101 Ti1 74.5(12) . . ? C102 C101 Ti1 72.2(8) . . ? C106 C101 Ti1 131.4(17) . . ? C103 C102 C101 108.4(16) . . ? C103 C102 C107 124.5(19) . . ? C101 C102 C107 127(2) . . ? C103 C102 Ti1 72.2(7) . . ? C101 C102 Ti1 73.5(10) . . ? C107 C102 Ti1 121.9(9) . . ? C102 C103 C104 109.6(13) . . ? C102 C103 C108 123.6(15) . . ? C104 C103 C108 126.5(14) . . ? C102 C103 Ti1 76.1(7) . . ? C104 C103 Ti1 73.7(8) . . ? C108 C103 Ti1 122.3(10) . . ? C105 C104 C103 105.6(15) . . ? C105 C104 C109 128(2) . . ? C103 C104 C109 126(2) . . ? C105 C104 Ti1 75.2(9) . . ? C103 C104 Ti1 72.0(8) . . ? C109 C104 Ti1 122.7(12) . . ? C101 C105 C104 109.5(15) . . ? C101 C105 C110 140(3) . . ? C104 C105 C110 110(2) . . ? C101 C105 Ti1 73.8(10) . . ? C104 C105 Ti1 71.2(9) . . ? C110 C105 Ti1 125.2(15) . . ? C112 C111 C115 108.1(12) . . ? C112 C111 C116 119.5(17) . . ? C115 C111 C116 130.6(17) . . ? C112 C111 Ti1 73.5(7) . . ? C115 C111 Ti1 74.2(8) . . ? C116 C111 Ti1 129.7(11) . . ? C113 C112 C111 106.6(12) . . ? C113 C112 C117 124.8(13) . . ? C111 C112 C117 128.2(14) . . ? C113 C112 Ti1 72.4(6) . . ? C111 C112 Ti1 72.1(7) . . ? C117 C112 Ti1 125.8(9) . . ? C112 C113 C114 109.0(11) . . ? C112 C113 C118 125.5(12) . . ? C114 C113 C118 124.9(12) . . ? C112 C113 Ti1 73.7(7) . . ? C114 C113 Ti1 74.3(7) . . ? C118 C113 Ti1 125.1(8) . . ? C115 C114 C113 108.2(12) . . ? C115 C114 C119 125.2(13) . . ? C113 C114 C119 126.4(13) . . ? C115 C114 Ti1 73.5(7) . . ? C113 C114 Ti1 71.6(6) . . ? C119 C114 Ti1 124.6(9) . . ? C114 C115 C111 108.0(11) . . ? C114 C115 C120 126.3(17) . . ? C111 C115 C120 124.6(18) . . ? C114 C115 Ti1 73.5(7) . . ? C111 C115 Ti1 71.4(7) . . ? C120 C115 Ti1 130.0(11) . . ? C75' C74' C73' 116(3) . . ? C74 C73 C72 105(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O14 Ti2 Ti3 O15 -1.3(4) . . . . ? O13 Ti2 Ti3 O15 -179.8(6) . . . . ? O7 Ti2 Ti3 O15 -111.5(4) . . . . ? O12 Ti2 Ti3 O15 107.3(4) . . . . ? O14 Ti2 Ti3 O7' 107.6(4) . . . . ? O13 Ti2 Ti3 O7' -70.9(7) . . . . ? O7 Ti2 Ti3 O7' -2.7(5) . . . . ? O12 Ti2 Ti3 O7' -143.9(5) . . . . ? O14 Ti2 Ti3 O12' -110.9(4) . . . . ? O13 Ti2 Ti3 O12' 70.6(6) . . . . ? O7 Ti2 Ti3 O12' 138.8(4) . . . . ? O12 Ti2 Ti3 O12' -2.4(5) . . . . ? O14 Ti2 Ti3 O13 178.5(6) . . . . ? O7 Ti2 Ti3 O13 68.3(6) . . . . ? O12 Ti2 Ti3 O13 -72.9(7) . . . . ? Si4 O4 Si1 O8 69.4(15) . . . . ? Si4 O4 Si1 O1 -51.8(15) . . . . ? Si4 O4 Si1 C11 -169.3(14) . . . . ? Si6 O5 Si2 O1 -77.1(12) . . . . ? Si6 O5 Si2 O2 43.6(12) . . . . ? Si6 O5 Si2 C21 160.4(11) . . . . ? Si3 O2 Si2 O1 58.5(13) . . . . ? Si3 O2 Si2 O5 -61.2(13) . . . . ? Si3 O2 Si2 C21 179.5(12) . . . . ? Si4 O3 Si3 O6 -122(3) . . . . ? Si4 O3 Si3 O2 -1(3) . . . . ? Si4 O3 Si3 C31 118(3) . . . . ? Si7 O6 Si3 O3 113.7(12) . . . . ? Si7 O6 Si3 O2 -6.3(14) . . . . ? Si7 O6 Si3 C31 -126.1(13) . . . . ? Si2 O2 Si3 O3 -41.3(13) . . . . ? Si2 O2 Si3 O6 78.6(12) . . . . ? Si2 O2 Si3 C31 -161.1(11) . . . . ? Si1 O4 Si4 O7 -86.6(15) . . . . ? Si1 O4 Si4 O3 34.2(16) . . . . ? Si1 O4 Si4 C41 153.6(13) . . . . ? Si3 O3 Si4 O7 125(3) . . . . ? Si3 O3 Si4 O4 4(3) . . . . ? Si3 O3 Si4 C41 -114(3) . . . . ? Si2 O5 Si6 O10 -59.7(12) . . . . ? Si2 O5 Si6 O9 60.0(12) . . . . ? Si2 O5 Si6 C61 -179(100) . . . . ? Si3 O6 Si7 O11 -167.3(12) . . . . ? Si3 O6 Si7 O10 -46.4(14) . . . . ? Si3 O6 Si7 C71 75.1(14) . . . . ? Si4' O4' Si1' O1' 99.5(12) . . . . ? Si4' O4' Si1' O8' -20.2(14) . . . . ? Si4' O4' Si1' C11' -141.1(12) . . . . ? Si6' O5' Si2' O2' -69.3(12) . . . . ? Si6' O5' Si2' O1' 48.1(13) . . . . ? Si6' O5' Si2' C21' 169.1(11) . . . . ? Si3' O2' Si2' O5' 29.3(13) . . . . ? Si3' O2' Si2' O1' -89.7(12) . . . . ? Si3' O2' Si2' C21' 149.7(11) . . . . ? Si7' O6' Si3' O3' -110.6(15) . . . . ? Si7' O6' Si3' O2' 9.3(17) . . . . ? Si7' O6' Si3' C31' 131.5(15) . . . . ? Si4' O3' Si3' O6' 131.2(10) . . . . ? Si4' O3' Si3' O2' 11.7(12) . . . . ? Si4' O3' Si3' C31' -109.1(11) . . . . ? Si2' O2' Si3' O6' -41.0(13) . . . . ? Si2' O2' Si3' O3' 78.4(12) . . . . ? Si2' O2' Si3' C31' -162.9(11) . . . . ? Si1' O4' Si4' O7' 40.4(14) . . . . ? Si1' O4' Si4' O3' -79.1(13) . . . . ? Si1' O4' Si4' C41' 161.4(12) . . . . ? Si3' O3' Si4' O4' -13.2(12) . . . . ? Si3' O3' Si4' O7' -134.3(10) . . . . ? Si3' O3' Si4' C41' 104.0(11) . . . . ? Si2' O5' Si6' O9' -33.2(13) . . . . ? Si2' O5' Si6' O10' 85.4(12) . . . . ? Si2' O5' Si6' C61' -152.7(12) . . . . ? Si3' O6' Si7' O11' 162.9(15) . . . . ? Si3' O6' Si7' O10' 45.3(17) . . . . ? Si3' O6' Si7' C71' -77.5(16) . . . . ? O5 Si2 O1 Si1 47.3(12) . . . . ? O2 Si2 O1 Si1 -73.6(12) . . . . ? C21 Si2 O1 Si1 168.9(11) . . . . ? O8 Si1 O1 Si2 -50.0(12) . . . . ? O4 Si1 O1 Si2 71.6(12) . . . . ? C11 Si1 O1 Si2 -168.4(11) . . . . ? O8' Si1' O1' Si2' 78.5(10) . . . . ? O4' Si1' O1' Si2' -41.4(11) . . . . ? C11' Si1' O1' Si2' -157.8(10) . . . . ? O5' Si2' O1' Si1' -81.5(11) . . . . ? O2' Si2' O1' Si1' 36.6(11) . . . . ? C21' Si2' O1' Si1' 158.0(9) . . . . ? O4 Si4 O7 Ti2 -4.2(9) . . . . ? O3 Si4 O7 Ti2 -125.7(8) . . . . ? C41 Si4 O7 Ti2 114.3(9) . . . . ? O14 Ti2 O7 Si4 177.2(7) . . . . ? O13 Ti2 O7 Si4 -65.7(8) . . . . ? O12 Ti2 O7 Si4 56.8(9) . . . . ? Ti3 Ti2 O7 Si4 -89.8(8) . . . . ? O4' Si4' O7' Ti3 -43.5(16) . . . . ? O3' Si4' O7' Ti3 74.9(14) . . . . ? C41' Si4' O7' Ti3 -162.9(13) . . . . ? O15 Ti3 O7' Si4' -128.7(13) . . . . ? O12' Ti3 O7' Si4' -7.8(15) . . . . ? O13 Ti3 O7' Si4' 111.9(14) . . . . ? Ti2 Ti3 O7' Si4' 136.9(13) . . . . ? O9' Si5' O8' Si1' 28.7(13) . . . . ? O12' Si5' O8' Si1' -89.8(12) . . . . ? C51' Si5' O8' Si1' 151.1(12) . . . . ? O1' Si1' O8' Si5' -42.5(13) . . . . ? O4' Si1' O8' Si5' 75.9(13) . . . . ? C11' Si1' O8' Si5' -166.1(12) . . . . ? O4 Si1 O8 Si5 -40.2(12) . . . . ? O1 Si1 O8 Si5 80.3(10) . . . . ? C11 Si1 O8 Si5 -162.7(9) . . . . ? O9 Si5 O8 Si1 -56.5(11) . . . . ? O12 Si5 O8 Si1 62.2(11) . . . . ? C51 Si5 O8 Si1 -177.9(10) . . . . ? O10' Si6' O9' Si5' -75(3) . . . . ? O5' Si6' O9' Si5' 43(3) . . . . ? C61' Si6' O9' Si5' 164(2) . . . . ? O8' Si5' O9' Si6' -43(3) . . . . ? O12' Si5' O9' Si6' 76(3) . . . . ? C51' Si5' O9' Si6' -162(2) . . . . ? O12 Si5 O9 Si6 -153.5(14) . . . . ? O8 Si5 O9 Si6 -34.7(16) . . . . ? C51 Si5 O9 Si6 87.2(16) . . . . ? O10 Si6 O9 Si5 151.9(14) . . . . ? O5 Si6 O9 Si5 31.6(16) . . . . ? C61 Si6 O9 Si5 -89.0(15) . . . . ? O9' Si6' O10' Si7' 123.7(10) . . . . ? O5' Si6' O10' Si7' 5.4(13) . . . . ? C61' Si6' O10' Si7' -116.4(11) . . . . ? O11' Si7' O10' Si6' -176.4(11) . . . . ? O6' Si7' O10' Si6' -58.4(12) . . . . ? C71' Si7' O10' Si6' 64.8(13) . . . . ? O5 Si6 O10 Si7 16.8(18) . . . . ? O9 Si6 O10 Si7 -103.7(17) . . . . ? C61 Si6 O10 Si7 136.2(16) . . . . ? O11 Si7 O10 Si6 157.4(16) . . . . ? O6 Si7 O10 Si6 39.4(18) . . . . ? C71 Si7 O10 Si6 -84.6(18) . . . . ? O1' Si1' C11' C16' 51.3(15) . . . . ? O8' Si1' C11' C16' 174.0(12) . . . . ? O4' Si1' C11' C16' -65.8(14) . . . . ? O1' Si1' C11' C12' 173.8(11) . . . . ? O8' Si1' C11' C12' -63.4(13) . . . . ? O4' Si1' C11' C12' 56.7(13) . . . . ? O8 Si1 C11 C12 -54.0(12) . . . . ? O4 Si1 C11 C12 -176.3(11) . . . . ? O1 Si1 C11 C12 65.1(13) . . . . ? O8 Si1 C11 C16 -177.7(9) . . . . ? O4 Si1 C11 C16 60.0(11) . . . . ? O1 Si1 C11 C16 -58.6(10) . . . . ? O6 Si7 O11 Si8 46.1(16) . . . . ? O10 Si7 O11 Si8 -72.7(15) . . . . ? C71 Si7 O11 Si8 167.9(14) . . . . ? C81 Si8 O11 Si7 54.4(18) . . . . ? C82 Si8 O11 Si7 -67.6(16) . . . . ? C83 Si8 O11 Si7 174.2(15) . . . . ? C83' Si8' O11' Si7' -68.9(17) . . . . ? C81' Si8' O11' Si7' 170.2(18) . . . . ? C82' Si8' O11' Si7' 47.9(19) . . . . ? O10' Si7' O11' Si8' 149.5(14) . . . . ? O6' Si7' O11' Si8' 29.2(17) . . . . ? C71' Si7' O11' Si8' -91.2(16) . . . . ? O9 Si5 O12 Ti2 88.8(13) . . . . ? O8 Si5 O12 Ti2 -28.5(14) . . . . ? C51 Si5 O12 Ti2 -150.3(12) . . . . ? O14 Ti2 O12 Si5 -154.4(11) . . . . ? O13 Ti2 O12 Si5 85.8(13) . . . . ? O7 Ti2 O12 Si5 -32.9(13) . . . . ? Ti3 Ti2 O12 Si5 111.7(12) . . . . ? O8' Si5' O12' Ti3 -14.2(9) . . . . ? O9' Si5' O12' Ti3 -132.8(7) . . . . ? C51' Si5' O12' Ti3 103.3(9) . . . . ? O15 Ti3 O12' Si5' 174.8(7) . . . . ? O7' Ti3 O12' Si5' 54.6(8) . . . . ? O13 Ti3 O12' Si5' -68.1(8) . . . . ? Ti2 Ti3 O12' Si5' -92.2(7) . . . . ? C16 C11 C12 C13 -49.7(19) . . . . ? Si1 C11 C12 C13 -172.5(12) . . . . ? C16' C11' C12' C13' -48.4(19) . . . . ? Si1' C11' C12' C13' -174.1(13) . . . . ? O14 Ti2 O13 Ti3 -1.6(7) . . . . ? O7 Ti2 O13 Ti3 -121.3(5) . . . . ? O12 Ti2 O13 Ti3 119.5(6) . . . . ? O15 Ti3 O13 Ti2 0.3(6) . . . . ? O7' Ti3 O13 Ti2 121.1(6) . . . . ? O12' Ti3 O13 Ti2 -119.0(5) . . . . ? C11 C12 C13 C14 52(2) . . . . ? C11' C12' C13' C14' 55(2) . . . . ? O13 Ti2 O14 Ti1 1.3(8) . . . . ? O7 Ti2 O14 Ti1 118.5(7) . . . . ? O12 Ti2 O14 Ti1 -122.1(7) . . . . ? Ti3 Ti2 O14 Ti1 0.6(7) . . . . ? O15 Ti1 O14 Ti2 0.2(8) . . . . ? C103 Ti1 O14 Ti2 84.6(8) . . . . ? C104 Ti1 O14 Ti2 77.1(9) . . . . ? C111 Ti1 O14 Ti2 -136.4(7) . . . . ? C113 Ti1 O14 Ti2 -83.6(8) . . . . ? C102 Ti1 O14 Ti2 116.0(8) . . . . ? C112 Ti1 O14 Ti2 -117.2(8) . . . . ? C101 Ti1 O14 Ti2 135.8(8) . . . . ? C114 Ti1 O14 Ti2 -77.6(8) . . . . ? C115 Ti1 O14 Ti2 -113.5(8) . . . . ? C105 Ti1 O14 Ti2 114.8(12) . . . . ? C12' C13' C14' C15' -58.0(19) . . . . ? C12 C13 C14 C15 -53(2) . . . . ? O7' Ti3 O15 Ti1 -120.7(7) . . . . ? O12' Ti3 O15 Ti1 119.9(6) . . . . ? O13 Ti3 O15 Ti1 2.3(7) . . . . ? Ti2 Ti3 O15 Ti1 2.5(6) . . . . ? O14 Ti1 O15 Ti3 -2.5(7) . . . . ? C103 Ti1 O15 Ti3 -86.5(7) . . . . ? C104 Ti1 O15 Ti3 -120.2(7) . . . . ? C111 Ti1 O15 Ti3 111.9(8) . . . . ? C113 Ti1 O15 Ti3 80.1(7) . . . . ? C102 Ti1 O15 Ti3 -81.7(8) . . . . ? C112 Ti1 O15 Ti3 73.6(7) . . . . ? C101 Ti1 O15 Ti3 -119.3(11) . . . . ? C114 Ti1 O15 Ti3 113.8(7) . . . . ? C115 Ti1 O15 Ti3 133.0(7) . . . . ? C105 Ti1 O15 Ti3 -138.7(7) . . . . ? C13' C14' C15' C16' 59(2) . . . . ? C13 C14 C15 C16 54(2) . . . . ? C14' C15' C16' C11' -54(2) . . . . ? C12' C11' C16' C15' 48(2) . . . . ? Si1' C11' C16' C15' 169.8(13) . . . . ? C14 C15 C16 C11 -54(2) . . . . ? C12 C11 C16 C15 51.1(18) . . . . ? Si1 C11 C16 C15 175.7(12) . . . . ? O5' Si2' C21' C22' -174.1(11) . . . . ? O2' Si2' C21' C22' 65.9(13) . . . . ? O1' Si2' C21' C22' -53.1(13) . . . . ? O5' Si2' C21' C26' 61.8(11) . . . . ? O2' Si2' C21' C26' -58.2(11) . . . . ? O1' Si2' C21' C26' -177.3(10) . . . . ? O1 Si2 C21 C26 -67.9(16) . . . . ? O5 Si2 C21 C26 52.7(16) . . . . ? O2 Si2 C21 C26 172.1(14) . . . . ? O1 Si2 C21 C22 50.9(15) . . . . ? O5 Si2 C21 C22 171.5(13) . . . . ? O2 Si2 C21 C22 -69.0(15) . . . . ? C26' C21' C22' C23' -56(2) . . . . ? Si2' C21' C22' C23' 177.1(14) . . . . ? C26 C21 C22 C23 -58(2) . . . . ? Si2 C21 C22 C23 179.4(17) . . . . ? C21' C22' C23' C24' 63(2) . . . . ? C21 C22 C23 C24 65(3) . . . . ? C22 C23 C24 C25 -72(3) . . . . ? C22' C23' C24' C25' -66(2) . . . . ? C23' C24' C25' C26' 69(2) . . . . ? C23 C24 C25 C26 67(3) . . . . ? C24' C25' C26' C21' -62(2) . . . . ? C22' C21' C26' C25' 51.9(18) . . . . ? Si2' C21' C26' C25' 177.9(12) . . . . ? C22 C21 C26 C25 54(2) . . . . ? Si2 C21 C26 C25 173.6(15) . . . . ? C24 C25 C26 C21 -59(2) . . . . ? O3 Si3 C31 C32 -87.7(13) . . . . ? O6 Si3 C31 C32 152.3(11) . . . . ? O2 Si3 C31 C32 31.9(14) . . . . ? O3 Si3 C31 C36 141.8(12) . . . . ? O6 Si3 C31 C36 21.7(14) . . . . ? O2 Si3 C31 C36 -98.7(12) . . . . ? O6' Si3' C31' C32' -101.1(16) . . . . ? O3' Si3' C31' C32' 140.2(16) . . . . ? O2' Si3' C31' C32' 20.1(18) . . . . ? O6' Si3' C31' C36' 32.3(15) . . . . ? O3' Si3' C31' C36' -86.4(14) . . . . ? O2' Si3' C31' C36' 153.5(12) . . . . ? C36 C31 C32 C33 -58(2) . . . . ? Si3 C31 C32 C33 172.3(13) . . . . ? C36' C31' C32' C33' 50(3) . . . . ? Si3' C31' C32' C33' -178.4(14) . . . . ? C31 C32 C33 C34 56(2) . . . . ? C31' C32' C33' C34' -47(3) . . . . ? C32 C33 C34 C35 -59(3) . . . . ? C32' C33' C34' C35' 51(3) . . . . ? C33 C34 C35 C36 61(2) . . . . ? C33' C34' C35' C36' -54(3) . . . . ? C32' C31' C36' C35' -51(3) . . . . ? Si3' C31' C36' C35' 174.8(15) . . . . ? C34' C35' C36' C31' 51(3) . . . . ? C32 C31 C36 C35 56.5(19) . . . . ? Si3 C31 C36 C35 -172.1(11) . . . . ? C34 C35 C36 C31 -54(2) . . . . ? O4' Si4' C41' C42' 172.5(12) . . . . ? O7' Si4' C41' C42' -65.7(14) . . . . ? O3' Si4' C41' C42' 55.3(14) . . . . ? O4' Si4' C41' C46' 42.6(13) . . . . ? O7' Si4' C41' C46' 164.4(11) . . . . ? O3' Si4' C41' C46' -74.6(12) . . . . ? O7 Si4 C41 C46 163.2(14) . . . . ? O4 Si4 C41 C46 -77.5(15) . . . . ? O3 Si4 C41 C46 42.8(16) . . . . ? O7 Si4 C41 C42 -66.3(12) . . . . ? O4 Si4 C41 C42 53.0(11) . . . . ? O3 Si4 C41 C42 173.4(10) . . . . ? C46 C41 C42 C43 -50.8(19) . . . . ? Si4 C41 C42 C43 177.6(13) . . . . ? C46' C41' C42' C43' -54(2) . . . . ? Si4' C41' C42' C43' 176.2(14) . . . . ? C41' C42' C43' C44' 55(2) . . . . ? C41 C42 C43 C44 53(3) . . . . ? C42' C43' C44' C45' -55(2) . . . . ? C42 C43 C44 C45 -57(3) . . . . ? C43 C44 C45 C46 58(3) . . . . ? C43' C44' C45' C46' 58(3) . . . . ? C42' C41' C46' C45' 54(2) . . . . ? Si4' C41' C46' C45' -174.2(13) . . . . ? C44' C45' C46' C41' -56(2) . . . . ? C44 C45 C46 C41 -56(3) . . . . ? C42 C41 C46 C45 56(2) . . . . ? Si4 C41 C46 C45 -174.5(16) . . . . ? O9 Si5 C51 C52 46.5(14) . . . . ? O12 Si5 C51 C52 -73.5(14) . . . . ? O8 Si5 C51 C52 165.8(12) . . . . ? O9 Si5 C51 C56 -82.4(15) . . . . ? O12 Si5 C51 C56 157.6(14) . . . . ? O8 Si5 C51 C56 36.9(15) . . . . ? O8' Si5' C51' C56' -156(3) . . . . ? O9' Si5' C51' C56' -36(3) . . . . ? O12' Si5' C51' C56' 85(3) . . . . ? O8' Si5' C51' C52' 59.7(18) . . . . ? O9' Si5' C51' C52' 179.6(16) . . . . ? O12' Si5' C51' C52' -59.0(19) . . . . ? C56 C51 C52 C53 -51(3) . . . . ? Si5 C51 C52 C53 -177.7(19) . . . . ? C56' C51' C52' C53' 58(4) . . . . ? Si5' C51' C52' C53' -156(2) . . . . ? C51 C52 C53 C54 41(4) . . . . ? C51' C52' C53' C54' -69(4) . . . . ? C52 C53 C54 C55 -38(5) . . . . ? C52' C53' C54' C55' 69(4) . . . . ? C53 C54 C55 C56 46(5) . . . . ? C53' C54' C55' C56' -59(4) . . . . ? C54 C55 C56 C51 -49(4) . . . . ? C52 C51 C56 C55 51(3) . . . . ? Si5 C51 C56 C55 178.9(19) . . . . ? C52' C51' C56' C55' -42(4) . . . . ? Si5' C51' C56' C55' 173.2(19) . . . . ? C54' C55' C56' C51' 48(4) . . . . ? O10 Si6 C61 C62 -76.7(12) . . . . ? O5 Si6 C61 C62 43.0(13) . . . . ? O9 Si6 C61 C62 164.3(10) . . . . ? O10 Si6 C61 C66 46.3(13) . . . . ? O5 Si6 C61 C66 166.0(11) . . . . ? O9 Si6 C61 C66 -72.8(13) . . . . ? O9' Si6' C61' C62' -61.9(14) . . . . ? O10' Si6' C61' C62' 177.9(11) . . . . ? O5' Si6' C61' C62' 57.5(13) . . . . ? O9' Si6' C61' C66' 62.8(15) . . . . ? O10' Si6' C61' C66' -57.4(14) . . . . ? O5' Si6' C61' C66' -177.8(12) . . . . ? C66' C61' C62' C63' 51(2) . . . . ? Si6' C61' C62' C63' 176.5(16) . . . . ? C66 C61 C62 C63 55.9(18) . . . . ? Si6 C61 C62 C63 -179.0(12) . . . . ? C61 C62 C63 C64 -55(2) . . . . ? C61' C62' C63' C64' -53(3) . . . . ? C62' C63' C64' C65' 54(3) . . . . ? C62 C63 C64 C65 58(2) . . . . ? C63 C64 C65 C66 -58(2) . . . . ? C63' C64' C65' C66' -54(3) . . . . ? C64' C65' C66' C61' 54(2) . . . . ? C62' C61' C66' C65' -53(2) . . . . ? Si6' C61' C66' C65' -178.1(17) . . . . ? C64 C65 C66 C61 59(2) . . . . ? C62 C61 C66 C65 -60(2) . . . . ? Si6 C61 C66 C65 173.6(12) . . . . ? O11' Si7' C71' C72' 81.2(14) . . . . ? O10' Si7' C71' C72' -161.2(13) . . . . ? O6' Si7' C71' C72' -37.6(15) . . . . ? O11' Si7' C71' C76' -50.1(12) . . . . ? O10' Si7' C71' C76' 67.6(12) . . . . ? O6' Si7' C71' C76' -168.8(10) . . . . ? O11 Si7 C71 C72 48(2) . . . . ? O6 Si7 C71 C72 165.6(18) . . . . ? O10 Si7 C71 C72 -73(2) . . . . ? O11 Si7 C71 C76 -176.9(14) . . . . ? O6 Si7 C71 C76 -59.1(16) . . . . ? O10 Si7 C71 C76 62.1(16) . . . . ? C76' C71' C72' C73' -53(2) . . . . ? Si7' C71' C72' C73' 176.3(15) . . . . ? C76 C71 C72 C73 53(3) . . . . ? Si7 C71 C72 C73 -173(2) . . . . ? C71' C72' C73' C74' 47(3) . . . . ? C73 C74 C75 C76 -61(3) . . . . ? C72 C71 C76 C75 -49(3) . . . . ? Si7 C71 C76 C75 176.4(13) . . . . ? C74 C75 C76 C71 52(2) . . . . ? C72' C71' C76' C75' 50(2) . . . . ? Si7' C71' C76' C75' -176.8(14) . . . . ? C74' C75' C76' C71' -51(4) . . . . ? O15 Ti1 C101 C105 -37.7(18) . . . . ? O14 Ti1 C101 C105 -149.9(13) . . . . ? C103 Ti1 C101 C105 -78.8(13) . . . . ? C104 Ti1 C101 C105 -36.7(11) . . . . ? C111 Ti1 C101 C105 107.3(15) . . . . ? C113 Ti1 C101 C105 111.0(13) . . . . ? C102 Ti1 C101 C105 -113.9(16) . . . . ? C112 Ti1 C101 C105 130.2(12) . . . . ? C114 Ti1 C101 C105 67.6(14) . . . . ? C115 Ti1 C101 C105 74.3(14) . . . . ? O15 Ti1 C101 C102 76.2(16) . . . . ? O14 Ti1 C101 C102 -36.0(13) . . . . ? C103 Ti1 C101 C102 35.1(8) . . . . ? C104 Ti1 C101 C102 77.3(10) . . . . ? C111 Ti1 C101 C102 -138.8(13) . . . . ? C113 Ti1 C101 C102 -135.1(8) . . . . ? C112 Ti1 C101 C102 -115.9(10) . . . . ? C114 Ti1 C101 C102 -178.5(8) . . . . ? C115 Ti1 C101 C102 -171.8(12) . . . . ? C105 Ti1 C101 C102 113.9(16) . . . . ? O15 Ti1 C101 C106 174(2) . . . . ? O14 Ti1 C101 C106 62(3) . . . . ? C103 Ti1 C101 C106 133(3) . . . . ? C104 Ti1 C101 C106 175(3) . . . . ? C111 Ti1 C101 C106 -41(3) . . . . ? C113 Ti1 C101 C106 -37(3) . . . . ? C102 Ti1 C101 C106 98(3) . . . . ? C112 Ti1 C101 C106 -18(3) . . . . ? C114 Ti1 C101 C106 -81(3) . . . . ? C115 Ti1 C101 C106 -74(3) . . . . ? C105 Ti1 C101 C106 -148(4) . . . . ? C105 C101 C102 C103 2.7(18) . . . . ? C106 C101 C102 C103 166.9(16) . . . . ? Ti1 C101 C102 C103 -64.2(10) . . . . ? C105 C101 C102 C107 -175.2(15) . . . . ? C106 C101 C102 C107 -11(2) . . . . ? Ti1 C101 C102 C107 117.8(14) . . . . ? C105 C101 C102 Ti1 67.0(13) . . . . ? C106 C101 C102 Ti1 -128.9(16) . . . . ? O15 Ti1 C102 C103 -9.2(10) . . . . ? O14 Ti1 C102 C103 -99.1(9) . . . . ? C104 Ti1 C102 C103 38.4(9) . . . . ? C111 Ti1 C102 C103 160.3(9) . . . . ? C113 Ti1 C102 C103 -145.9(10) . . . . ? C112 Ti1 C102 C103 -163.6(8) . . . . ? C101 Ti1 C102 C103 116.2(16) . . . . ? C114 Ti1 C102 C103 119.8(14) . . . . ? C115 Ti1 C102 C103 126.6(9) . . . . ? C105 Ti1 C102 C103 79.9(12) . . . . ? O15 Ti1 C102 C101 -125.3(13) . . . . ? O14 Ti1 C102 C101 144.8(13) . . . . ? C103 Ti1 C102 C101 -116.2(16) . . . . ? C104 Ti1 C102 C101 -77.7(13) . . . . ? C111 Ti1 C102 C101 44.1(14) . . . . ? C113 Ti1 C102 C101 97.9(16) . . . . ? C112 Ti1 C102 C101 80.3(14) . . . . ? C114 Ti1 C102 C101 4(2) . . . . ? C115 Ti1 C102 C101 10.4(15) . . . . ? C105 Ti1 C102 C101 -36.3(12) . . . . ? O15 Ti1 C102 C107 110.9(18) . . . . ? O14 Ti1 C102 C107 21.0(18) . . . . ? C103 Ti1 C102 C107 120(2) . . . . ? C104 Ti1 C102 C107 158(2) . . . . ? C111 Ti1 C102 C107 -79.7(19) . . . . ? C113 Ti1 C102 C107 -26(2) . . . . ? C112 Ti1 C102 C107 -44(2) . . . . ? C101 Ti1 C102 C107 -124(2) . . . . ? C114 Ti1 C102 C107 -120(2) . . . . ? C115 Ti1 C102 C107 -113.4(19) . . . . ? C105 Ti1 C102 C107 -160(2) . . . . ? C101 C102 C103 C104 -1.6(15) . . . . ? C107 C102 C103 C104 176.4(13) . . . . ? Ti1 C102 C103 C104 -66.7(10) . . . . ? C101 C102 C103 C108 -175.2(13) . . . . ? C107 C102 C103 C108 3(2) . . . . ? Ti1 C102 C103 C108 119.8(14) . . . . ? C101 C102 C103 Ti1 65.1(10) . . . . ? C107 C102 C103 Ti1 -116.9(13) . . . . ? O15 Ti1 C103 C102 171.7(9) . . . . ? O14 Ti1 C103 C102 76.1(9) . . . . ? C104 Ti1 C103 C102 -115.6(13) . . . . ? C111 Ti1 C103 C102 -28.8(13) . . . . ? C113 Ti1 C103 C102 120.1(16) . . . . ? C112 Ti1 C103 C102 29.5(14) . . . . ? C101 Ti1 C103 C102 -38.1(12) . . . . ? C114 Ti1 C103 C102 -140.7(10) . . . . ? C115 Ti1 C103 C102 -82.8(12) . . . . ? C105 Ti1 C103 C102 -77.1(12) . . . . ? O15 Ti1 C103 C104 -72.7(9) . . . . ? O14 Ti1 C103 C104 -168.3(9) . . . . ? C111 Ti1 C103 C104 86.8(11) . . . . ? C113 Ti1 C103 C104 -124.3(16) . . . . ? C102 Ti1 C103 C104 115.6(13) . . . . ? C112 Ti1 C103 C104 145.1(10) . . . . ? C101 Ti1 C103 C104 77.5(13) . . . . ? C114 Ti1 C103 C104 -25.1(14) . . . . ? C115 Ti1 C103 C104 32.8(12) . . . . ? C105 Ti1 C103 C104 38.5(12) . . . . ? O15 Ti1 C103 C108 50.5(13) . . . . ? O14 Ti1 C103 C108 -45.2(13) . . . . ? C104 Ti1 C103 C108 123.2(17) . . . . ? C111 Ti1 C103 C108 -150.0(13) . . . . ? C113 Ti1 C103 C108 -1(2) . . . . ? C102 Ti1 C103 C108 -121.2(17) . . . . ? C112 Ti1 C103 C108 -91.8(15) . . . . ? C101 Ti1 C103 C108 -159.3(17) . . . . ? C114 Ti1 C103 C108 98.1(16) . . . . ? C115 Ti1 C103 C108 156.0(13) . . . . ? C105 Ti1 C103 C108 161.7(17) . . . . ? C102 C103 C104 C105 0.0(16) . . . . ? C108 C103 C104 C105 173.3(14) . . . . ? Ti1 C103 C104 C105 -68.3(11) . . . . ? C102 C103 C104 C109 -173.9(16) . . . . ? C108 C103 C104 C109 -1(2) . . . . ? Ti1 C103 C104 C109 117.8(16) . . . . ? C102 C103 C104 Ti1 68.3(9) . . . . ? C108 C103 C104 Ti1 -118.4(14) . . . . ? O15 Ti1 C104 C105 -146.2(12) . . . . ? O14 Ti1 C104 C105 125.4(12) . . . . ? C103 Ti1 C104 C105 112.3(15) . . . . ? C111 Ti1 C104 C105 -12.4(14) . . . . ? C113 Ti1 C104 C105 -98.9(15) . . . . ? C102 Ti1 C104 C105 76.9(12) . . . . ? C112 Ti1 C104 C105 -7(2) . . . . ? C101 Ti1 C104 C105 34.6(11) . . . . ? C114 Ti1 C104 C105 -80.7(12) . . . . ? C115 Ti1 C104 C105 -46.2(13) . . . . ? O15 Ti1 C104 C103 101.6(9) . . . . ? O14 Ti1 C104 C103 13.2(10) . . . . ? C111 Ti1 C104 C103 -124.7(9) . . . . ? C113 Ti1 C104 C103 148.9(9) . . . . ? C102 Ti1 C104 C103 -35.4(8) . . . . ? C112 Ti1 C104 C103 -119.1(14) . . . . ? C101 Ti1 C104 C103 -77.6(11) . . . . ? C114 Ti1 C104 C103 167.1(7) . . . . ? C115 Ti1 C104 C103 -158.4(8) . . . . ? C105 Ti1 C104 C103 -112.3(15) . . . . ? O15 Ti1 C104 C109 -21(2) . . . . ? O14 Ti1 C104 C109 -109(2) . . . . ? C103 Ti1 C104 C109 -122(3) . . . . ? C111 Ti1 C104 C109 113(2) . . . . ? C113 Ti1 C104 C109 27(3) . . . . ? C102 Ti1 C104 C109 -158(2) . . . . ? C112 Ti1 C104 C109 119(3) . . . . ? C101 Ti1 C104 C109 160(3) . . . . ? C114 Ti1 C104 C109 45(2) . . . . ? C115 Ti1 C104 C109 79(2) . . . . ? C105 Ti1 C104 C109 125(3) . . . . ? C102 C101 C105 C104 -2.7(19) . . . . ? C106 C101 C105 C104 -157(3) . . . . ? Ti1 C101 C105 C104 62.7(12) . . . . ? C102 C101 C105 C110 169(2) . . . . ? C106 C101 C105 C110 14(5) . . . . ? Ti1 C101 C105 C110 -126(3) . . . . ? C102 C101 C105 Ti1 -65.4(10) . . . . ? C106 C101 C105 Ti1 140(3) . . . . ? C103 C104 C105 C101 1.7(19) . . . . ? C109 C104 C105 C101 175.6(17) . . . . ? Ti1 C104 C105 C101 -64.3(13) . . . . ? C103 C104 C105 C110 -172.3(15) . . . . ? C109 C104 C105 C110 2(2) . . . . ? Ti1 C104 C105 C110 121.6(16) . . . . ? C103 C104 C105 Ti1 66.1(10) . . . . ? C109 C104 C105 Ti1 -120.1(17) . . . . ? O15 Ti1 C105 C101 151.6(13) . . . . ? O14 Ti1 C105 C101 40.7(19) . . . . ? C103 Ti1 C105 C101 78.3(12) . . . . ? C104 Ti1 C105 C101 117.7(16) . . . . ? C111 Ti1 C105 C101 -72.2(14) . . . . ? C113 Ti1 C105 C101 -109.6(13) . . . . ? C102 Ti1 C105 C101 39.3(11) . . . . ? C112 Ti1 C105 C101 -65.0(14) . . . . ? C114 Ti1 C105 C101 -127.5(12) . . . . ? C115 Ti1 C105 C101 -105.4(14) . . . . ? O15 Ti1 C105 C104 33.8(12) . . . . ? O14 Ti1 C105 C104 -77.0(16) . . . . ? C103 Ti1 C105 C104 -39.4(8) . . . . ? C111 Ti1 C105 C104 170.1(11) . . . . ? C113 Ti1 C105 C104 132.7(9) . . . . ? C102 Ti1 C105 C104 -78.4(10) . . . . ? C112 Ti1 C105 C104 177.2(8) . . . . ? C101 Ti1 C105 C104 -117.7(16) . . . . ? C114 Ti1 C105 C104 114.8(10) . . . . ? C115 Ti1 C105 C104 136.9(12) . . . . ? O15 Ti1 C105 C110 -68(2) . . . . ? O14 Ti1 C105 C110 -178.5(18) . . . . ? C103 Ti1 C105 C110 -141(3) . . . . ? C104 Ti1 C105 C110 -101(3) . . . . ? C111 Ti1 C105 C110 69(2) . . . . ? C113 Ti1 C105 C110 31(3) . . . . ? C102 Ti1 C105 C110 -180(3) . . . . ? C112 Ti1 C105 C110 76(3) . . . . ? C101 Ti1 C105 C110 141(3) . . . . ? C114 Ti1 C105 C110 13(3) . . . . ? C115 Ti1 C105 C110 35(2) . . . . ? O15 Ti1 C111 C112 -76.5(10) . . . . ? O14 Ti1 C111 C112 34.4(9) . . . . ? C103 Ti1 C111 C112 132.0(8) . . . . ? C104 Ti1 C111 C112 176.8(7) . . . . ? C113 Ti1 C111 C112 -37.5(7) . . . . ? C102 Ti1 C111 C112 116.4(8) . . . . ? C101 Ti1 C111 C112 139.7(12) . . . . ? C114 Ti1 C111 C112 -78.7(8) . . . . ? C115 Ti1 C111 C112 -114.8(12) . . . . ? C105 Ti1 C111 C112 169.9(10) . . . . ? O15 Ti1 C111 C115 38.3(10) . . . . ? O14 Ti1 C111 C115 149.1(7) . . . . ? C103 Ti1 C111 C115 -113.2(10) . . . . ? C104 Ti1 C111 C115 -68.4(10) . . . . ? C113 Ti1 C111 C115 77.3(8) . . . . ? C102 Ti1 C111 C115 -128.8(8) . . . . ? C112 Ti1 C111 C115 114.8(12) . . . . ? C101 Ti1 C111 C115 -105.5(11) . . . . ? C114 Ti1 C111 C115 36.1(7) . . . . ? C105 Ti1 C111 C115 -75.3(10) . . . . ? O15 Ti1 C111 C116 168.5(17) . . . . ? O14 Ti1 C111 C116 -80.6(19) . . . . ? C103 Ti1 C111 C116 17(2) . . . . ? C104 Ti1 C111 C116 62(2) . . . . ? C113 Ti1 C111 C116 -152(2) . . . . ? C102 Ti1 C111 C116 1(2) . . . . ? C112 Ti1 C111 C116 -115(2) . . . . ? C101 Ti1 C111 C116 25(2) . . . . ? C114 Ti1 C111 C116 166(2) . . . . ? C115 Ti1 C111 C116 130(2) . . . . ? C105 Ti1 C111 C116 55(2) . . . . ? C115 C111 C112 C113 -2.2(15) . . . . ? C116 C111 C112 C113 -168.6(13) . . . . ? Ti1 C111 C112 C113 64.6(8) . . . . ? C115 C111 C112 C117 171.3(13) . . . . ? C116 C111 C112 C117 5(2) . . . . ? Ti1 C111 C112 C117 -121.9(14) . . . . ? C115 C111 C112 Ti1 -66.8(9) . . . . ? C116 C111 C112 Ti1 126.8(14) . . . . ? O15 Ti1 C112 C113 11.7(8) . . . . ? O14 Ti1 C112 C113 99.8(7) . . . . ? C103 Ti1 C112 C113 148.2(9) . . . . ? C104 Ti1 C112 C113 -122.7(14) . . . . ? C111 Ti1 C112 C113 -114.7(11) . . . . ? C102 Ti1 C112 C113 165.7(7) . . . . ? C101 Ti1 C112 C113 -158.0(10) . . . . ? C114 Ti1 C112 C113 -37.2(7) . . . . ? C115 Ti1 C112 C113 -77.0(8) . . . . ? C105 Ti1 C112 C113 -127.4(10) . . . . ? O15 Ti1 C112 C111 126.5(9) . . . . ? O14 Ti1 C112 C111 -145.5(9) . . . . ? C103 Ti1 C112 C111 -97.1(12) . . . . ? C104 Ti1 C112 C111 -8.0(18) . . . . ? C113 Ti1 C112 C111 114.7(11) . . . . ? C102 Ti1 C112 C111 -79.5(10) . . . . ? C101 Ti1 C112 C111 -43.3(12) . . . . ? C114 Ti1 C112 C111 77.5(9) . . . . ? C115 Ti1 C112 C111 37.7(9) . . . . ? C105 Ti1 C112 C111 -12.7(13) . . . . ? O15 Ti1 C112 C117 -108.9(13) . . . . ? O14 Ti1 C112 C117 -20.9(13) . . . . ? C103 Ti1 C112 C117 27.5(18) . . . . ? C104 Ti1 C112 C117 116.7(17) . . . . ? C111 Ti1 C112 C117 124.6(17) . . . . ? C113 Ti1 C112 C117 -120.6(16) . . . . ? C102 Ti1 C112 C117 45.1(15) . . . . ? C101 Ti1 C112 C117 81.4(16) . . . . ? C114 Ti1 C112 C117 -157.9(15) . . . . ? C115 Ti1 C112 C117 162.4(15) . . . . ? C105 Ti1 C112 C117 111.9(15) . . . . ? C111 C112 C113 C114 2.1(14) . . . . ? C117 C112 C113 C114 -171.7(12) . . . . ? Ti1 C112 C113 C114 66.5(8) . . . . ? C111 C112 C113 C118 173.7(11) . . . . ? C117 C112 C113 C118 0.0(19) . . . . ? Ti1 C112 C113 C118 -121.8(11) . . . . ? C111 C112 C113 Ti1 -64.4(9) . . . . ? C117 C112 C113 Ti1 121.8(13) . . . . ? O15 Ti1 C113 C112 -169.6(7) . . . . ? O14 Ti1 C113 C112 -73.7(7) . . . . ? C103 Ti1 C113 C112 -117.9(15) . . . . ? C104 Ti1 C113 C112 144.6(11) . . . . ? C111 Ti1 C113 C112 38.0(8) . . . . ? C102 Ti1 C113 C112 -27.7(14) . . . . ? C101 Ti1 C113 C112 33.5(16) . . . . ? C114 Ti1 C113 C112 115.8(11) . . . . ? C115 Ti1 C113 C112 79.6(8) . . . . ? C105 Ti1 C113 C112 84.7(15) . . . . ? O15 Ti1 C113 C114 74.7(7) . . . . ? O14 Ti1 C113 C114 170.5(8) . . . . ? C103 Ti1 C113 C114 126.3(15) . . . . ? C104 Ti1 C113 C114 28.9(15) . . . . ? C111 Ti1 C113 C114 -77.8(9) . . . . ? C102 Ti1 C113 C114 -143.5(11) . . . . ? C112 Ti1 C113 C114 -115.8(11) . . . . ? C101 Ti1 C113 C114 -82.2(15) . . . . ? C115 Ti1 C113 C114 -36.2(8) . . . . ? C105 Ti1 C113 C114 -31.1(16) . . . . ? O15 Ti1 C113 C118 -47.3(11) . . . . ? O14 Ti1 C113 C118 48.6(11) . . . . ? C103 Ti1 C113 C118 4(2) . . . . ? C104 Ti1 C113 C118 -93.1(15) . . . . ? C111 Ti1 C113 C118 160.3(13) . . . . ? C102 Ti1 C113 C118 94.6(15) . . . . ? C112 Ti1 C113 C118 122.3(14) . . . . ? C101 Ti1 C113 C118 155.8(15) . . . . ? C114 Ti1 C113 C118 -121.9(14) . . . . ? C115 Ti1 C113 C118 -158.1(13) . . . . ? C105 Ti1 C113 C118 -153.0(15) . . . . ? C112 C113 C114 C115 -1.2(14) . . . . ? C118 C113 C114 C115 -172.9(11) . . . . ? Ti1 C113 C114 C115 64.9(9) . . . . ? C112 C113 C114 C119 173.9(12) . . . . ? C118 C113 C114 C119 2.2(19) . . . . ? Ti1 C113 C114 C119 -119.9(13) . . . . ? C112 C113 C114 Ti1 -66.1(8) . . . . ? C118 C113 C114 Ti1 122.1(11) . . . . ? O15 Ti1 C114 C115 144.1(9) . . . . ? O14 Ti1 C114 C115 -126.8(8) . . . . ? C103 Ti1 C114 C115 95.0(12) . . . . ? C104 Ti1 C114 C115 79.0(10) . . . . ? C111 Ti1 C114 C115 -37.6(8) . . . . ? C113 Ti1 C114 C115 -116.2(12) . . . . ? C102 Ti1 C114 C115 9.8(17) . . . . ? C112 Ti1 C114 C115 -79.2(9) . . . . ? C101 Ti1 C114 C115 12.3(13) . . . . ? C105 Ti1 C114 C115 43.5(12) . . . . ? O15 Ti1 C114 C113 -99.7(8) . . . . ? O14 Ti1 C114 C113 -10.5(9) . . . . ? C103 Ti1 C114 C113 -148.8(9) . . . . ? C104 Ti1 C114 C113 -164.8(8) . . . . ? C111 Ti1 C114 C113 78.6(8) . . . . ? C102 Ti1 C114 C113 126.0(12) . . . . ? C112 Ti1 C114 C113 37.0(7) . . . . ? C101 Ti1 C114 C113 128.6(11) . . . . ? C115 Ti1 C114 C113 116.2(12) . . . . ? C105 Ti1 C114 C113 159.7(11) . . . . ? O15 Ti1 C114 C119 22.3(12) . . . . ? O14 Ti1 C114 C119 111.4(12) . . . . ? C103 Ti1 C114 C119 -26.8(18) . . . . ? C104 Ti1 C114 C119 -42.8(14) . . . . ? C111 Ti1 C114 C119 -159.4(14) . . . . ? C113 Ti1 C114 C119 122.0(16) . . . . ? C102 Ti1 C114 C119 -112.0(16) . . . . ? C112 Ti1 C114 C119 159.0(14) . . . . ? C101 Ti1 C114 C119 -109.5(15) . . . . ? C115 Ti1 C114 C119 -121.8(16) . . . . ? C105 Ti1 C114 C119 -78.3(15) . . . . ? C113 C114 C115 C111 -0.2(15) . . . . ? C119 C114 C115 C111 -175.4(12) . . . . ? Ti1 C114 C115 C111 63.5(10) . . . . ? C113 C114 C115 C120 168.5(15) . . . . ? C119 C114 C115 C120 -7(2) . . . . ? Ti1 C114 C115 C120 -127.8(17) . . . . ? C113 C114 C115 Ti1 -63.7(8) . . . . ? C119 C114 C115 Ti1 121.1(13) . . . . ? C112 C111 C115 C114 1.5(16) . . . . ? C116 C111 C115 C114 165.9(14) . . . . ? Ti1 C111 C115 C114 -64.8(10) . . . . ? C112 C111 C115 C120 -167.5(14) . . . . ? C116 C111 C115 C120 -3(3) . . . . ? Ti1 C111 C115 C120 126.2(15) . . . . ? C112 C111 C115 Ti1 66.3(9) . . . . ? C116 C111 C115 Ti1 -129.3(16) . . . . ? O15 Ti1 C115 C114 -36.1(9) . . . . ? O14 Ti1 C115 C114 74.1(10) . . . . ? C103 Ti1 C115 C114 -134.7(8) . . . . ? C104 Ti1 C115 C114 -115.8(8) . . . . ? C111 Ti1 C115 C114 116.1(11) . . . . ? C113 Ti1 C115 C114 37.3(7) . . . . ? C102 Ti1 C115 C114 -175.9(7) . . . . ? C112 Ti1 C115 C114 78.3(8) . . . . ? C101 Ti1 C115 C114 -170.0(11) . . . . ? C105 Ti1 C115 C114 -139.5(11) . . . . ? O15 Ti1 C115 C111 -152.2(8) . . . . ? O14 Ti1 C115 C111 -42.0(10) . . . . ? C103 Ti1 C115 C111 109.2(9) . . . . ? C104 Ti1 C115 C111 128.0(8) . . . . ? C113 Ti1 C115 C111 -78.8(8) . . . . ? C102 Ti1 C115 C111 68.0(9) . . . . ? C112 Ti1 C115 C111 -37.8(8) . . . . ? C101 Ti1 C115 C111 73.8(11) . . . . ? C114 Ti1 C115 C111 -116.1(11) . . . . ? C105 Ti1 C115 C111 104.4(11) . . . . ? O15 Ti1 C115 C120 88(2) . . . . ? O14 Ti1 C115 C120 -162.0(19) . . . . ? C103 Ti1 C115 C120 -11(2) . . . . ? C104 Ti1 C115 C120 8(2) . . . . ? C111 Ti1 C115 C120 -120(2) . . . . ? C113 Ti1 C115 C120 161(2) . . . . ? C102 Ti1 C115 C120 -52(2) . . . . ? C112 Ti1 C115 C120 -158(2) . . . . ? C101 Ti1 C115 C120 -46(2) . . . . ? C114 Ti1 C115 C120 124(2) . . . . ? C105 Ti1 C115 C120 -16(2) . . . . ? C76' C75' C74' C73' 50(4) . . . . ? C72' C73' C74' C75' -46(4) . . . . ? C75 C74 C73 C72 64(3) . . . . ? C71 C72 C73 C74 -62(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.050 _refine_diff_density_min -0.813 _refine_diff_density_rms 0.149