# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'R. Bohra' _publ_contact_author_email rkbohra@sify.com _publ_author_name R.Bohra data_3b _database_code_depnum_ccdc_archive 'CCDC 780743' #TrackingRef '- 3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H116 O20 Si4 Zr' _chemical_formula_weight 1216.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8351(5) _cell_length_b 18.7542(7) _cell_length_c 27.8551(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.141(3) _cell_angle_gamma 90.00 _cell_volume 7186.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10023 _cell_measurement_theta_min 3.2539 _cell_measurement_theta_max 32.8259 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_T_min 0.9389 _exptl_absorpt_correction_T_max 0.9675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58050 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.1206 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12625 _reflns_number_gt 6864 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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.Total 61 restraints such as DELU, SIMU, SADI and DFIX were applied to some atoms for which displacement parameters were found to be high. ; _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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12625 _refine_ls_number_parameters 703 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.1984 _refine_ls_R_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.3581 _refine_ls_wR_factor_gt 0.3160 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.27967(6) 0.24695(4) 0.35569(3) 0.0365(3) Uani 1 1 d . . . Si1 Si 0.19842(19) 0.40980(15) 0.39677(10) 0.0489(7) Uani 1 1 d . . . Si2 Si 0.35239(18) 0.25526(13) 0.23949(9) 0.0392(6) Uani 1 1 d . . . Si3 Si 0.49790(17) 0.20991(16) 0.42541(10) 0.0479(7) Uani 1 1 d U . . Si4 Si 0.09536(18) 0.13083(14) 0.37453(12) 0.0513(7) Uani 1 1 d U . . O1 O 0.2583(9) 0.1397(5) 0.3102(4) 0.130(4) Uani 1 1 d . . . O2 O 0.1223(7) 0.2787(6) 0.3121(4) 0.106(3) Uani 1 1 d . . . O3 O 0.2551(5) 0.3421(3) 0.3806(3) 0.061(2) Uani 1 1 d . . . O4 O 0.1645(7) 0.4005(5) 0.4483(3) 0.094(3) Uani 1 1 d . . . O5 O 0.2582(6) 0.4803(4) 0.3962(3) 0.090(3) Uani 1 1 d . . . O6 O 0.1032(6) 0.4062(4) 0.3577(3) 0.087(3) Uani 1 1 d . . . O7 O 0.3196(4) 0.2688(3) 0.2909(2) 0.0463(16) Uani 1 1 d . . . O8 O 0.3058(5) 0.3061(4) 0.1971(2) 0.068(2) Uani 1 1 d . . . O9 O 0.4681(5) 0.2592(4) 0.2370(3) 0.079(2) Uani 1 1 d . . . O10 O 0.3254(6) 0.1711(4) 0.2278(3) 0.076(2) Uani 1 1 d . . . O11 O 0.4033(5) 0.2170(5) 0.3913(3) 0.085(3) Uani 1 1 d . . . O12 O 0.5567(6) 0.2806(5) 0.4123(3) 0.085(2) Uani 1 1 d U . . O13 O 0.5471(7) 0.1356(4) 0.4176(3) 0.093(3) Uani 1 1 d . . . O14 O 0.4738(6) 0.2150(5) 0.4799(3) 0.091(3) Uani 1 1 d . . . O15 O 0.1779(6) 0.1869(4) 0.3814(4) 0.115(4) Uani 1 1 d . . . O16 O 0.1343(7) 0.0592(4) 0.3521(3) 0.080(2) Uani 1 1 d . . . O17 O 0.0505(6) 0.1091(4) 0.4244(3) 0.085(2) Uani 1 1 d U . . O18 O 0.0130(5) 0.1637(5) 0.3382(3) 0.083(2) Uani 1 1 d U . . C1 C 0.2024(9) 0.4168(9) 0.4979(5) 0.094(5) Uani 1 1 d . . . C2 C 0.3076(11) 0.3994(13) 0.5026(7) 0.171(10) Uani 1 1 d . . . H2A H 0.3327 0.4054 0.4712 0.257 Uiso 1 1 calc R . . H2B H 0.3170 0.3499 0.5133 0.257 Uiso 1 1 calc R . . H2C H 0.3425 0.4313 0.5263 0.257 Uiso 1 1 calc R . . C3 C 0.1475(13) 0.3650(10) 0.5285(5) 0.129(7) Uani 1 1 d . . . H3A H 0.0773 0.3698 0.5196 0.194 Uiso 1 1 calc R . . H3B H 0.1629 0.3763 0.5628 0.194 Uiso 1 1 calc R . . H3C H 0.1674 0.3159 0.5226 0.194 Uiso 1 1 calc R . . C4 C 0.1750(13) 0.4960(8) 0.5035(7) 0.143(8) Uani 1 1 d . . . H4A H 0.1998 0.5241 0.4778 0.215 Uiso 1 1 calc R . . H4B H 0.2037 0.5136 0.5350 0.215 Uiso 1 1 calc R . . H4C H 0.1041 0.5006 0.5013 0.215 Uiso 1 1 calc R . . C5 C 0.3308(9) 0.5086(7) 0.3677(5) 0.077(4) Uani 1 1 d . . . C6 C 0.4242(10) 0.4757(10) 0.3854(7) 0.137(7) Uani 1 1 d . . . H6A H 0.4646 0.5105 0.4046 0.206 Uiso 1 1 calc R . . H6B H 0.4576 0.4602 0.3579 0.206 Uiso 1 1 calc R . . H6C H 0.4126 0.4344 0.4056 0.206 Uiso 1 1 calc R . . C7 C 0.3336(14) 0.5864(8) 0.3757(7) 0.142(8) Uani 1 1 d . . . H7A H 0.2767 0.6009 0.3915 0.213 Uiso 1 1 calc R . . H7B H 0.3329 0.6110 0.3446 0.213 Uiso 1 1 calc R . . H7C H 0.3930 0.5990 0.3963 0.213 Uiso 1 1 calc R . . C8 C 0.3074(11) 0.4875(9) 0.3158(5) 0.113(5) Uani 1 1 d . . . H8A H 0.3329 0.4396 0.3109 0.169 Uiso 1 1 calc R . . H8B H 0.3373 0.5215 0.2952 0.169 Uiso 1 1 calc R . . H8C H 0.2368 0.4876 0.3075 0.169 Uiso 1 1 calc R . . C9 C 0.0123(7) 0.4430(4) 0.3551(4) 0.060(3) Uani 1 1 d DU . . C10 C -0.0557(9) 0.4023(8) 0.3841(6) 0.106(5) Uani 1 1 d DU . . H10A H -0.0656 0.3541 0.3708 0.160 Uiso 1 1 calc R . . H10B H -0.1182 0.4271 0.3825 0.160 Uiso 1 1 calc R . . H10C H -0.0272 0.3991 0.4178 0.160 Uiso 1 1 calc R . . C11 C 0.0221(13) 0.5208(6) 0.3676(7) 0.130(6) Uani 1 1 d DU . . H11A H 0.0562 0.5260 0.4001 0.194 Uiso 1 1 calc R . . H11B H -0.0426 0.5423 0.3666 0.194 Uiso 1 1 calc R . . H11C H 0.0592 0.5448 0.3442 0.194 Uiso 1 1 calc R . . C12 C -0.0169(11) 0.4379(8) 0.3013(4) 0.110(5) Uani 1 1 d DU . . H12A H -0.0543 0.3941 0.2942 0.165 Uiso 1 1 calc R . . H12B H 0.0415 0.4370 0.2843 0.165 Uiso 1 1 calc R . . H12C H -0.0568 0.4793 0.2906 0.165 Uiso 1 1 calc R . . C13 C 0.2098(7) 0.3346(6) 0.1849(4) 0.060(3) Uani 1 1 d . . . C14 C 0.1338(12) 0.2810(12) 0.1928(7) 0.152(8) Uani 1 1 d . . . H14A H 0.1086 0.2598 0.1617 0.228 Uiso 1 1 calc R . . H14B H 0.0806 0.3043 0.2073 0.228 Uiso 1 1 calc R . . H14C H 0.1621 0.2435 0.2144 0.228 Uiso 1 1 calc R . . C15 C 0.1981(13) 0.3960(9) 0.2178(6) 0.128(6) Uani 1 1 d . . . H15A H 0.2047 0.3794 0.2513 0.193 Uiso 1 1 calc R . . H15B H 0.1336 0.4173 0.2099 0.193 Uiso 1 1 calc R . . H15C H 0.2482 0.4318 0.2137 0.193 Uiso 1 1 calc R . . C16 C 0.2043(10) 0.3552(10) 0.1321(5) 0.116(6) Uani 1 1 d . . . H16A H 0.2564 0.3891 0.1274 0.173 Uiso 1 1 calc R . . H16B H 0.1412 0.3775 0.1222 0.173 Uiso 1 1 calc R . . H16C H 0.2116 0.3125 0.1125 0.173 Uiso 1 1 calc R . . C17 C 0.5364(7) 0.3146(6) 0.2338(4) 0.057(3) Uani 1 1 d . . . C18 C 0.5177(13) 0.3725(10) 0.2642(9) 0.175(10) Uani 1 1 d . . . H18A H 0.4535 0.3925 0.2537 0.262 Uiso 1 1 calc R . . H18B H 0.5674 0.4093 0.2623 0.262 Uiso 1 1 calc R . . H18C H 0.5192 0.3557 0.2976 0.262 Uiso 1 1 calc R . . C19 C 0.5293(11) 0.3405(11) 0.1816(6) 0.142(8) Uani 1 1 d . . . H19A H 0.5411 0.3004 0.1604 0.214 Uiso 1 1 calc R . . H19B H 0.5780 0.3777 0.1786 0.214 Uiso 1 1 calc R . . H19C H 0.4642 0.3599 0.1724 0.214 Uiso 1 1 calc R . . C20 C 0.6347(10) 0.2786(10) 0.2507(6) 0.122(6) Uani 1 1 d . . . H20A H 0.6421 0.2744 0.2860 0.183 Uiso 1 1 calc R . . H20B H 0.6879 0.3076 0.2406 0.183 Uiso 1 1 calc R . . H20C H 0.6366 0.2311 0.2363 0.183 Uiso 1 1 calc R . . C21 C 0.3490(9) 0.1200(6) 0.1960(4) 0.067(3) Uani 1 1 d . . . C22 C 0.3687(11) 0.1515(8) 0.1478(4) 0.099(5) Uani 1 1 d . . . H22A H 0.3101 0.1756 0.1330 0.149 Uiso 1 1 calc R . . H22B H 0.3866 0.1133 0.1264 0.149 Uiso 1 1 calc R . . H22C H 0.4221 0.1860 0.1529 0.149 Uiso 1 1 calc R . . C23 C 0.4445(13) 0.0821(9) 0.2188(5) 0.137(7) Uani 1 1 d . . . H23A H 0.4991 0.1156 0.2196 0.206 Uiso 1 1 calc R . . H23B H 0.4577 0.0405 0.1992 0.206 Uiso 1 1 calc R . . H23C H 0.4363 0.0667 0.2517 0.206 Uiso 1 1 calc R . . C24 C 0.2714(15) 0.0738(11) 0.1884(8) 0.161(8) Uani 1 1 d . . . H24A H 0.2291 0.0796 0.2141 0.242 Uiso 1 1 calc R . . H24B H 0.2954 0.0247 0.1883 0.242 Uiso 1 1 calc R . . H24C H 0.2346 0.0844 0.1571 0.242 Uiso 1 1 calc R . . C25 C 0.6391(8) 0.3162(7) 0.4375(4) 0.071(3) Uani 1 1 d . . . C26 C 0.5960(11) 0.3615(9) 0.4741(5) 0.111(5) Uani 1 1 d . . . H26A H 0.5356 0.3832 0.4593 0.167 Uiso 1 1 calc R . . H26B H 0.6421 0.3991 0.4854 0.167 Uiso 1 1 calc R . . H26C H 0.5821 0.3318 0.5015 0.167 Uiso 1 1 calc R . . C27 C 0.6718(11) 0.3627(9) 0.3966(6) 0.117(6) Uani 1 1 d . . . H27A H 0.6733 0.3337 0.3674 0.176 Uiso 1 1 calc R . . H27B H 0.7369 0.3817 0.4064 0.176 Uiso 1 1 calc R . . H27C H 0.6260 0.4023 0.3899 0.176 Uiso 1 1 calc R . . C28 C 0.7164(12) 0.2653(14) 0.4567(9) 0.207(13) Uani 1 1 d . . . H28A H 0.6893 0.2170 0.4569 0.310 Uiso 1 1 calc R . . H28B H 0.7410 0.2790 0.4897 0.310 Uiso 1 1 calc R . . H28C H 0.7697 0.2664 0.4362 0.310 Uiso 1 1 calc R . . C29 C 0.5767(7) 0.0927(6) 0.3802(5) 0.070(3) Uani 1 1 d . . . C30 C 0.5960(9) 0.1410(8) 0.3378(5) 0.090(4) Uani 1 1 d . . . H30A H 0.5410 0.1734 0.3303 0.135 Uiso 1 1 calc R . . H30B H 0.6041 0.1115 0.3094 0.135 Uiso 1 1 calc R . . H30C H 0.6554 0.1687 0.3465 0.135 Uiso 1 1 calc R . . C31 C 0.6694(11) 0.0569(11) 0.4025(7) 0.154(8) Uani 1 1 d . . . H31A H 0.7247 0.0745 0.3866 0.230 Uiso 1 1 calc R . . H31B H 0.6637 0.0052 0.3981 0.230 Uiso 1 1 calc R . . H31C H 0.6796 0.0680 0.4370 0.230 Uiso 1 1 calc R . . C32 C 0.4991(16) 0.0410(11) 0.3669(8) 0.180(10) Uani 1 1 d . . . H32A H 0.4932 0.0087 0.3940 0.270 Uiso 1 1 calc R . . H32B H 0.5146 0.0135 0.3388 0.270 Uiso 1 1 calc R . . H32C H 0.4375 0.0663 0.3589 0.270 Uiso 1 1 calc R . . C33 C 0.4572(9) 0.1666(9) 0.5173(4) 0.084(4) Uani 1 1 d . . . C34 C 0.5545(11) 0.1401(10) 0.5393(5) 0.128(6) Uani 1 1 d . . . H34A H 0.5715 0.0965 0.5228 0.192 Uiso 1 1 calc R . . H34B H 0.5514 0.1300 0.5736 0.192 Uiso 1 1 calc R . . H34C H 0.6039 0.1766 0.5359 0.192 Uiso 1 1 calc R . . C35 C 0.3887(12) 0.1105(10) 0.4982(6) 0.125(6) Uani 1 1 d . . . H35A H 0.3334 0.1325 0.4787 0.187 Uiso 1 1 calc R . . H35B H 0.3654 0.0843 0.5252 0.187 Uiso 1 1 calc R . . H35C H 0.4218 0.0775 0.4781 0.187 Uiso 1 1 calc R . . C36 C 0.4098(13) 0.2112(12) 0.5532(6) 0.150(8) Uani 1 1 d . . . H36A H 0.4597 0.2383 0.5731 0.225 Uiso 1 1 calc R . . H36B H 0.3754 0.1800 0.5739 0.225 Uiso 1 1 calc R . . H36C H 0.3635 0.2442 0.5359 0.225 Uiso 1 1 calc R . . C37 C 0.1598(7) -0.0111(5) 0.3673(5) 0.064(3) Uani 1 1 d . . . C38 C 0.2114(10) -0.0434(6) 0.3280(6) 0.097(5) Uani 1 1 d . . . H38A H 0.1732 -0.0356 0.2968 0.146 Uiso 1 1 calc R . . H38B H 0.2195 -0.0948 0.3338 0.146 Uiso 1 1 calc R . . H38C H 0.2754 -0.0211 0.3278 0.146 Uiso 1 1 calc R . . C39 C 0.2265(9) -0.0067(9) 0.4143(5) 0.102(5) Uani 1 1 d . . . H39A H 0.2884 0.0150 0.4082 0.153 Uiso 1 1 calc R . . H39B H 0.2384 -0.0548 0.4275 0.153 Uiso 1 1 calc R . . H39C H 0.1957 0.0224 0.4376 0.153 Uiso 1 1 calc R . . C40 C 0.0667(9) -0.0510(8) 0.3732(6) 0.109(5) Uani 1 1 d . . . H40A H 0.0284 -0.0240 0.3946 0.163 Uiso 1 1 calc R . . H40B H 0.0824 -0.0980 0.3873 0.163 Uiso 1 1 calc R . . H40C H 0.0291 -0.0568 0.3416 0.163 Uiso 1 1 calc R . . C41 C 0.0175(9) 0.1466(6) 0.4630(4) 0.070(3) Uani 1 1 d U . . C42 C 0.0968(9) 0.1471(9) 0.5059(5) 0.096(4) Uani 1 1 d . . . H42A H 0.1192 0.0982 0.5128 0.143 Uiso 1 1 calc R . . H42B H 0.0704 0.1669 0.5343 0.143 Uiso 1 1 calc R . . H42C H 0.1516 0.1763 0.4980 0.143 Uiso 1 1 calc R . . C43 C -0.0683(11) 0.1088(9) 0.4801(8) 0.145(8) Uani 1 1 d . . . H43A H -0.1280 0.1244 0.4607 0.217 Uiso 1 1 calc R . . H43B H -0.0725 0.1203 0.5141 0.217 Uiso 1 1 calc R . . H43C H -0.0605 0.0572 0.4765 0.217 Uiso 1 1 calc R . . C44 C -0.0069(10) 0.2234(7) 0.4473(5) 0.090(4) Uani 1 1 d . . . H44A H 0.0480 0.2440 0.4326 0.135 Uiso 1 1 calc R . . H44B H -0.0196 0.2517 0.4755 0.135 Uiso 1 1 calc R . . H44C H -0.0647 0.2235 0.4237 0.135 Uiso 1 1 calc R . . C45 C -0.0591(11) 0.1483(6) 0.3023(5) 0.107(3) Uani 1 1 d DU . . C46 C -0.1196(12) 0.0936(8) 0.3244(7) 0.130(5) Uani 1 1 d DU . . H46A H -0.0872 0.0471 0.3243 0.195 Uiso 1 1 calc R . . H46B H -0.1835 0.0905 0.3056 0.195 Uiso 1 1 calc R . . H46C H -0.1276 0.1073 0.3576 0.195 Uiso 1 1 calc R . . C47 C -0.1133(12) 0.2168(7) 0.2927(6) 0.124(4) Uani 1 1 d DU . . H47A H -0.1484 0.2285 0.3204 0.185 Uiso 1 1 calc R . . H47B H -0.1597 0.2116 0.2638 0.185 Uiso 1 1 calc R . . H47C H -0.0673 0.2550 0.2877 0.185 Uiso 1 1 calc R . . C48 C -0.0130(12) 0.1231(9) 0.2595(5) 0.124(4) Uani 1 1 d DU . . H48A H 0.0578 0.1222 0.2672 0.186 Uiso 1 1 calc R . . H48B H -0.0301 0.1556 0.2323 0.186 Uiso 1 1 calc R . . H48C H -0.0364 0.0750 0.2507 0.186 Uiso 1 1 calc R . . O111 O 0.1790(11) 0.7494(5) 0.3487(5) 0.133(5) Uani 1 1 d . . . O222 O 0.9413(7) 0.2874(6) 0.5810(4) 0.077(3) Uani 0.75 1 d P . . O101 O 0.2358(15) 0.7624(11) 0.3930(12) 0.052(8) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0375(5) 0.0393(5) 0.0354(5) 0.0112(4) 0.0160(3) 0.0129(4) Si1 0.0484(16) 0.0536(16) 0.0479(17) -0.0118(14) 0.0201(13) 0.0037(13) Si2 0.0449(13) 0.0386(13) 0.0357(13) 0.0027(12) 0.0115(10) 0.0059(12) Si3 0.0291(13) 0.0710(19) 0.0443(16) 0.0081(14) 0.0073(11) 0.0018(13) Si4 0.0333(13) 0.0415(15) 0.079(2) -0.0079(14) 0.0034(13) -0.0018(12) O1 0.177(10) 0.097(7) 0.131(9) -0.024(7) 0.084(8) -0.037(7) O2 0.102(7) 0.130(8) 0.084(7) 0.009(6) -0.001(5) 0.013(6) O3 0.064(4) 0.050(4) 0.077(5) -0.032(4) 0.040(4) -0.019(4) O4 0.163(8) 0.076(5) 0.048(5) -0.020(4) 0.029(5) -0.018(6) O5 0.099(6) 0.069(5) 0.111(7) -0.028(5) 0.057(6) -0.018(5) O6 0.075(5) 0.078(6) 0.111(7) 0.019(5) 0.031(5) 0.027(5) O7 0.052(4) 0.055(4) 0.034(4) 0.001(3) 0.010(3) 0.010(3) O8 0.061(4) 0.097(6) 0.046(4) 0.020(4) 0.002(3) 0.016(4) O9 0.061(5) 0.093(6) 0.084(6) 0.031(5) 0.017(4) -0.017(4) O10 0.133(7) 0.047(4) 0.052(5) -0.011(4) 0.028(5) -0.003(5) O11 0.044(4) 0.160(8) 0.050(5) 0.014(5) -0.002(3) 0.057(5) O12 0.073(5) 0.108(5) 0.076(5) -0.010(5) 0.012(4) -0.027(4) O13 0.119(7) 0.077(6) 0.090(6) 0.029(5) 0.049(6) 0.039(5) O14 0.091(6) 0.124(7) 0.061(5) 0.020(5) 0.019(4) 0.023(6) O15 0.051(5) 0.064(5) 0.235(12) -0.065(7) 0.041(6) -0.015(4) O16 0.135(7) 0.047(4) 0.059(5) -0.003(4) 0.023(5) 0.014(5) O17 0.115(5) 0.077(4) 0.066(4) -0.009(4) 0.013(4) 0.027(4) O18 0.056(4) 0.116(6) 0.074(5) -0.014(5) -0.007(4) 0.026(4) C1 0.079(9) 0.145(13) 0.065(8) -0.037(9) 0.039(7) -0.041(9) C2 0.071(10) 0.31(3) 0.130(16) 0.064(18) 0.007(10) 0.019(14) C3 0.163(15) 0.159(16) 0.077(10) -0.014(11) 0.059(11) -0.040(13) C4 0.143(14) 0.128(14) 0.170(18) -0.111(14) 0.070(13) -0.044(12) C5 0.081(9) 0.074(8) 0.078(9) -0.009(7) 0.025(7) -0.030(7) C6 0.068(9) 0.142(15) 0.21(2) 0.052(14) 0.055(11) 0.001(10) C7 0.197(19) 0.092(12) 0.150(17) -0.006(12) 0.081(15) -0.029(13) C8 0.123(12) 0.129(13) 0.088(11) 0.011(10) 0.018(9) 0.003(11) C9 0.060(6) 0.048(5) 0.078(7) -0.007(5) 0.035(5) 0.023(5) C10 0.084(9) 0.109(11) 0.136(14) 0.013(10) 0.052(9) -0.003(8) C11 0.151(14) 0.067(8) 0.177(18) -0.036(10) 0.049(13) 0.025(10) C12 0.149(14) 0.100(11) 0.081(8) -0.009(9) 0.009(9) -0.004(11) C13 0.053(6) 0.072(7) 0.058(7) 0.017(6) 0.013(5) 0.031(6) C14 0.090(11) 0.25(2) 0.114(14) 0.077(15) -0.006(10) -0.054(14) C15 0.159(15) 0.109(12) 0.120(14) -0.013(11) 0.023(12) 0.061(12) C16 0.089(10) 0.176(17) 0.085(10) 0.062(11) 0.029(8) 0.054(10) C17 0.050(6) 0.063(7) 0.061(7) -0.006(6) 0.018(5) -0.011(6) C18 0.114(14) 0.127(15) 0.29(3) -0.098(18) 0.035(16) -0.049(12) C19 0.111(12) 0.22(2) 0.099(12) 0.094(13) 0.008(9) -0.044(13) C20 0.070(9) 0.183(17) 0.114(13) 0.016(12) 0.008(9) 0.002(10) C21 0.077(8) 0.051(6) 0.074(8) -0.024(6) 0.019(6) -0.014(6) C22 0.153(13) 0.108(11) 0.040(7) -0.020(7) 0.019(8) 0.023(10) C23 0.196(17) 0.139(14) 0.074(10) -0.015(10) 0.002(10) 0.111(14) C24 0.168(18) 0.155(18) 0.17(2) -0.045(16) 0.043(15) -0.062(16) C25 0.054(7) 0.097(9) 0.061(8) -0.022(7) 0.004(6) -0.021(7) C26 0.128(12) 0.127(13) 0.081(10) -0.025(10) 0.023(9) -0.021(11) C27 0.108(11) 0.130(14) 0.118(13) -0.026(11) 0.031(10) -0.047(11) C28 0.057(10) 0.34(4) 0.22(3) 0.06(2) -0.007(12) 0.068(15) C29 0.046(6) 0.070(8) 0.095(9) -0.005(7) 0.015(6) 0.003(6) C30 0.077(8) 0.115(11) 0.082(10) -0.002(9) 0.027(7) -0.003(8) C31 0.095(11) 0.19(2) 0.18(2) 0.068(16) 0.047(12) 0.065(13) C32 0.22(2) 0.146(17) 0.19(2) -0.072(16) 0.086(18) -0.114(17) C33 0.070(8) 0.133(12) 0.054(8) 0.047(8) 0.031(6) 0.031(8) C34 0.115(12) 0.185(18) 0.082(11) 0.014(12) -0.005(9) 0.047(12) C35 0.115(13) 0.140(15) 0.125(15) 0.047(13) 0.040(11) -0.005(12) C36 0.150(15) 0.24(2) 0.066(10) 0.024(13) 0.050(11) 0.003(16) C37 0.043(6) 0.040(6) 0.110(10) -0.002(6) 0.018(6) 0.008(5) C38 0.091(9) 0.056(7) 0.152(14) -0.002(8) 0.049(10) 0.010(7) C39 0.057(7) 0.142(14) 0.106(11) 0.030(10) 0.008(7) 0.027(8) C40 0.061(8) 0.108(11) 0.160(15) 0.007(11) 0.027(9) -0.016(8) C41 0.081(7) 0.071(6) 0.058(6) 0.001(5) 0.013(5) 0.028(6) C42 0.078(9) 0.135(13) 0.072(9) 0.005(9) 0.001(7) 0.012(9) C43 0.083(10) 0.124(14) 0.24(2) 0.035(15) 0.054(13) -0.005(10) C44 0.100(10) 0.099(10) 0.073(9) -0.025(8) 0.016(7) 0.022(9) C45 0.110(8) 0.083(7) 0.124(9) -0.038(7) -0.001(6) 0.012(6) C46 0.126(10) 0.102(9) 0.159(11) -0.026(9) 0.002(8) -0.003(8) C47 0.136(10) 0.102(8) 0.129(10) -0.033(8) -0.002(8) 0.035(8) C48 0.136(10) 0.106(9) 0.125(10) -0.042(8) -0.007(8) 0.023(8) O111 0.207(13) 0.062(6) 0.150(11) 0.021(7) 0.113(11) 0.036(7) O222 0.073(6) 0.097(8) 0.072(7) -0.034(6) 0.057(6) -0.029(6) O101 0.020(12) 0.014(12) 0.11(3) 0.000(14) -0.028(13) 0.009(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O3 1.956(6) . ? Zr1 O11 1.965(6) . ? Zr1 O7 1.987(6) . ? Zr1 O15 1.995(8) . ? Zr1 O1 2.379(10) . ? Zr1 O2 2.450(10) . ? Si1 O5 1.560(8) . ? Si1 O4 1.567(8) . ? Si1 O3 1.584(7) . ? Si1 O6 1.617(10) . ? Si2 O7 1.568(6) . ? Si2 O8 1.599(7) . ? Si2 O9 1.612(8) . ? Si2 O10 1.646(7) . ? Si3 O11 1.539(7) . ? Si3 O13 1.577(8) . ? Si3 O14 1.590(8) . ? Si3 O12 1.618(9) . ? Si4 O15 1.549(8) . ? Si4 O18 1.567(8) . ? Si4 O16 1.599(7) . ? Si4 O17 1.633(8) . ? O4 C1 1.456(15) . ? O5 C5 1.446(12) . ? O6 C9 1.430(11) . ? O8 C13 1.437(11) . ? O9 C17 1.413(12) . ? O10 C21 1.367(12) . ? O12 C25 1.438(13) . ? O13 C29 1.410(13) . ? O14 C33 1.420(14) . ? O16 C37 1.419(12) . ? O17 C41 1.401(12) . ? O18 C45 1.366(16) . ? C1 C2 1.483(19) . ? C1 C3 1.546(18) . ? C1 C4 1.55(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.470(19) . ? C5 C7 1.475(18) . ? C5 C8 1.498(18) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.502(9) . ? C9 C10 1.511(8) . ? C9 C12 1.512(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.488(18) . ? C13 C15 1.492(18) . ? C13 C16 1.514(15) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.416(19) . ? C17 C19 1.525(16) . ? C17 C20 1.547(17) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.377(19) . ? C21 C22 1.519(16) . ? C21 C23 1.573(18) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C28 1.49(2) . ? C25 C26 1.499(16) . ? C25 C27 1.541(18) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.464(19) . ? C29 C31 1.520(18) . ? C29 C30 1.535(16) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.48(2) . ? C33 C34 1.502(18) . ? C33 C36 1.51(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.498(15) . ? C37 C40 1.513(15) . ? C37 C39 1.522(18) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.503(17) . ? C41 C44 1.532(17) . ? C41 C42 1.534(17) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C48 1.490(7) . ? C45 C46 1.496(7) . ? C45 C47 1.497(7) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? O111 O101 1.41(3) . ? 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 O3 Zr1 O11 104.9(4) . . ? O3 Zr1 O7 102.1(3) . . ? O11 Zr1 O7 101.9(3) . . ? O3 Zr1 O15 103.4(3) . . ? O11 Zr1 O15 105.5(4) . . ? O7 Zr1 O15 135.9(4) . . ? O3 Zr1 O1 160.6(4) . . ? O11 Zr1 O1 94.5(4) . . ? O7 Zr1 O1 73.8(3) . . ? O15 Zr1 O1 70.2(3) . . ? O3 Zr1 O2 77.0(3) . . ? O11 Zr1 O2 177.3(4) . . ? O7 Zr1 O2 79.5(3) . . ? O15 Zr1 O2 72.0(4) . . ? O1 Zr1 O2 83.6(4) . . ? O5 Si1 O4 108.4(5) . . ? O5 Si1 O3 113.4(4) . . ? O4 Si1 O3 112.2(5) . . ? O5 Si1 O6 115.0(5) . . ? O4 Si1 O6 108.0(5) . . ? O3 Si1 O6 99.6(4) . . ? O7 Si2 O8 116.4(4) . . ? O7 Si2 O9 114.7(4) . . ? O8 Si2 O9 105.3(4) . . ? O7 Si2 O10 104.7(4) . . ? O8 Si2 O10 111.1(4) . . ? O9 Si2 O10 103.9(4) . . ? O11 Si3 O13 110.0(6) . . ? O11 Si3 O14 109.5(4) . . ? O13 Si3 O14 108.9(5) . . ? O11 Si3 O12 101.8(5) . . ? O13 Si3 O12 117.3(5) . . ? O14 Si3 O12 109.1(5) . . ? O15 Si4 O18 106.7(6) . . ? O15 Si4 O16 110.1(4) . . ? O18 Si4 O16 109.3(5) . . ? O15 Si4 O17 114.0(6) . . ? O18 Si4 O17 109.3(4) . . ? O16 Si4 O17 107.3(4) . . ? Si1 O3 Zr1 160.5(4) . . ? C1 O4 Si1 137.1(8) . . ? C5 O5 Si1 135.8(7) . . ? C9 O6 Si1 131.5(7) . . ? Si2 O7 Zr1 158.8(4) . . ? C13 O8 Si2 133.2(6) . . ? C17 O9 Si2 135.2(7) . . ? C21 O10 Si2 137.3(7) . . ? Si3 O11 Zr1 166.7(6) . . ? C25 O12 Si3 131.5(8) . . ? C29 O13 Si3 140.4(8) . . ? C33 O14 Si3 136.7(10) . . ? Si4 O15 Zr1 151.5(7) . . ? C37 O16 Si4 138.3(7) . . ? C41 O17 Si4 135.3(8) . . ? C45 O18 Si4 144.4(9) . . ? O4 C1 C2 106.8(11) . . ? O4 C1 C3 104.1(11) . . ? C2 C1 C3 110.4(15) . . ? O4 C1 C4 103.3(13) . . ? C2 C1 C4 116.9(15) . . ? C3 C1 C4 114.1(11) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O5 C5 C6 107.3(11) . . ? O5 C5 C7 106.8(11) . . ? C6 C5 C7 110.9(14) . . ? O5 C5 C8 109.9(11) . . ? C6 C5 C8 107.7(13) . . ? C7 C5 C8 114.0(14) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O6 C9 C11 113.6(10) . . ? O6 C9 C10 108.8(8) . . ? C11 C9 C10 114.4(10) . . ? O6 C9 C12 99.3(9) . . ? C11 C9 C12 107.4(12) . . ? C10 C9 C12 112.4(11) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O8 C13 C14 111.3(11) . . ? O8 C13 C15 107.5(11) . . ? C14 C13 C15 107.8(12) . . ? O8 C13 C16 105.9(8) . . ? C14 C13 C16 110.7(12) . . ? C15 C13 C16 113.6(12) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O9 C17 C18 111.1(10) . . ? O9 C17 C19 108.5(10) . . ? C18 C17 C19 109.2(15) . . ? O9 C17 C20 103.4(10) . . ? C18 C17 C20 111.4(14) . . ? C19 C17 C20 113.1(11) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O10 C21 C24 107.8(11) . . ? O10 C21 C22 112.2(10) . . ? C24 C21 C22 108.5(13) . . ? O10 C21 C23 107.7(10) . . ? C24 C21 C23 112.7(14) . . ? C22 C21 C23 108.0(11) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O12 C25 C28 112.3(14) . . ? O12 C25 C26 104.0(9) . . ? C28 C25 C26 116.2(15) . . ? O12 C25 C27 100.5(10) . . ? C28 C25 C27 111.9(13) . . ? C26 C25 C27 110.6(12) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O13 C29 C32 107.6(10) . . ? O13 C29 C31 104.5(12) . . ? C32 C29 C31 112.0(16) . . ? O13 C29 C30 108.7(10) . . ? C32 C29 C30 112.2(14) . . ? C31 C29 C30 111.4(10) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O14 C33 C35 109.9(12) . . ? O14 C33 C34 107.7(11) . . ? C35 C33 C34 115.1(14) . . ? O14 C33 C36 104.3(13) . . ? C35 C33 C36 109.0(12) . . ? C34 C33 C36 110.2(13) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O16 C37 C38 106.3(10) . . ? O16 C37 C40 107.8(9) . . ? C38 C37 C40 110.9(10) . . ? O16 C37 C39 108.4(10) . . ? C38 C37 C39 111.0(10) . . ? C40 C37 C39 112.2(11) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O17 C41 C43 109.8(12) . . ? O17 C41 C44 109.5(10) . . ? C43 C41 C44 112.1(11) . . ? O17 C41 C42 109.6(10) . . ? C43 C41 C42 106.2(12) . . ? C44 C41 C42 109.6(12) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O18 C45 C48 108.2(11) . . ? O18 C45 C46 104.0(12) . . ? C48 C45 C46 114.7(13) . . ? O18 C45 C47 105.2(11) . . ? C48 C45 C47 112.2(12) . . ? C46 C45 C47 111.8(13) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Si1 O3 Zr1 -156.6(13) . . . . ? O4 Si1 O3 Zr1 80.2(15) . . . . ? O6 Si1 O3 Zr1 -33.8(15) . . . . ? O11 Zr1 O3 Si1 -148.1(14) . . . . ? O7 Zr1 O3 Si1 106.0(14) . . . . ? O15 Zr1 O3 Si1 -37.7(15) . . . . ? O1 Zr1 O3 Si1 31(2) . . . . ? O2 Zr1 O3 Si1 29.9(14) . . . . ? O5 Si1 O4 C1 -34.0(15) . . . . ? O3 Si1 O4 C1 92.0(14) . . . . ? O6 Si1 O4 C1 -159.2(13) . . . . ? O4 Si1 O5 C5 157.6(13) . . . . ? O3 Si1 O5 C5 32.3(15) . . . . ? O6 Si1 O5 C5 -81.4(14) . . . . ? O5 Si1 O6 C9 -70.6(9) . . . . ? O4 Si1 O6 C9 50.6(10) . . . . ? O3 Si1 O6 C9 167.8(8) . . . . ? O8 Si2 O7 Zr1 140.6(10) . . . . ? O9 Si2 O7 Zr1 -95.8(11) . . . . ? O10 Si2 O7 Zr1 17.5(12) . . . . ? O3 Zr1 O7 Si2 -178.0(11) . . . . ? O11 Zr1 O7 Si2 73.7(12) . . . . ? O15 Zr1 O7 Si2 -53.8(13) . . . . ? O1 Zr1 O7 Si2 -17.6(11) . . . . ? O2 Zr1 O7 Si2 -103.9(11) . . . . ? O7 Si2 O8 C13 -40.0(11) . . . . ? O9 Si2 O8 C13 -168.4(10) . . . . ? O10 Si2 O8 C13 79.7(10) . . . . ? O7 Si2 O9 C17 -81.2(11) . . . . ? O8 Si2 O9 C17 48.2(11) . . . . ? O10 Si2 O9 C17 165.1(10) . . . . ? O7 Si2 O10 C21 -163.9(12) . . . . ? O8 Si2 O10 C21 69.6(13) . . . . ? O9 Si2 O10 C21 -43.2(13) . . . . ? O13 Si3 O11 Zr1 176(2) . . . . ? O14 Si3 O11 Zr1 56(3) . . . . ? O12 Si3 O11 Zr1 -59(2) . . . . ? O3 Zr1 O11 Si3 4(3) . . . . ? O7 Zr1 O11 Si3 110(2) . . . . ? O15 Zr1 O11 Si3 -104(2) . . . . ? O1 Zr1 O11 Si3 -175(2) . . . . ? O2 Zr1 O11 Si3 -130(6) . . . . ? O11 Si3 O12 C25 163.6(10) . . . . ? O13 Si3 O12 C25 -76.3(11) . . . . ? O14 Si3 O12 C25 48.0(11) . . . . ? O11 Si3 O13 C29 51.2(14) . . . . ? O14 Si3 O13 C29 171.1(12) . . . . ? O12 Si3 O13 C29 -64.5(14) . . . . ? O11 Si3 O14 C33 96.4(12) . . . . ? O13 Si3 O14 C33 -23.8(13) . . . . ? O12 Si3 O14 C33 -152.9(11) . . . . ? O18 Si4 O15 Zr1 -62.1(12) . . . . ? O16 Si4 O15 Zr1 56.4(14) . . . . ? O17 Si4 O15 Zr1 177.1(11) . . . . ? O3 Zr1 O15 Si4 131.0(12) . . . . ? O11 Zr1 O15 Si4 -119.1(12) . . . . ? O7 Zr1 O15 Si4 7.3(15) . . . . ? O1 Zr1 O15 Si4 -29.8(12) . . . . ? O2 Zr1 O15 Si4 59.7(12) . . . . ? O15 Si4 O16 C37 106.9(12) . . . . ? O18 Si4 O16 C37 -136.2(11) . . . . ? O17 Si4 O16 C37 -17.7(13) . . . . ? O15 Si4 O17 C41 48.0(12) . . . . ? O18 Si4 O17 C41 -71.4(12) . . . . ? O16 Si4 O17 C41 170.2(11) . . . . ? O15 Si4 O18 C45 147.7(13) . . . . ? O16 Si4 O18 C45 28.7(15) . . . . ? O17 Si4 O18 C45 -88.5(14) . . . . ? Si1 O4 C1 C2 -41(2) . . . . ? Si1 O4 C1 C3 -157.6(11) . . . . ? Si1 O4 C1 C4 83.0(15) . . . . ? Si1 O5 C5 C6 -79.2(17) . . . . ? Si1 O5 C5 C7 161.9(13) . . . . ? Si1 O5 C5 C8 37.7(19) . . . . ? Si1 O6 C9 C11 42.2(14) . . . . ? Si1 O6 C9 C10 -86.5(12) . . . . ? Si1 O6 C9 C12 155.8(9) . . . . ? Si2 O8 C13 C14 -39.3(16) . . . . ? Si2 O8 C13 C15 78.6(14) . . . . ? Si2 O8 C13 C16 -159.6(10) . . . . ? Si2 O9 C17 C18 41.5(18) . . . . ? Si2 O9 C17 C19 -78.5(14) . . . . ? Si2 O9 C17 C20 161.1(10) . . . . ? Si2 O10 C21 C24 -151.1(14) . . . . ? Si2 O10 C21 C22 -31.7(18) . . . . ? Si2 O10 C21 C23 87.1(15) . . . . ? Si3 O12 C25 C28 44.0(17) . . . . ? Si3 O12 C25 C26 -82.5(14) . . . . ? Si3 O12 C25 C27 163.0(9) . . . . ? Si3 O13 C29 C32 -96.8(17) . . . . ? Si3 O13 C29 C31 144.0(13) . . . . ? Si3 O13 C29 C30 25.0(17) . . . . ? Si3 O14 C33 C35 -46.7(16) . . . . ? Si3 O14 C33 C34 79.4(17) . . . . ? Si3 O14 C33 C36 -163.5(11) . . . . ? Si4 O16 C37 C38 -167.7(10) . . . . ? Si4 O16 C37 C40 73.3(16) . . . . ? Si4 O16 C37 C39 -48.4(15) . . . . ? Si4 O17 C41 C43 143.5(12) . . . . ? Si4 O17 C41 C44 20.1(16) . . . . ? Si4 O17 C41 C42 -100.2(13) . . . . ? Si4 O18 C45 C48 -68.3(17) . . . . ? Si4 O18 C45 C46 54.0(17) . . . . ? Si4 O18 C45 C47 171.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.418 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.128 # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 780748' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H90 O13 Si3 Ti' _chemical_formula_weight 911.29 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 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 22.4358(4) _cell_length_b 21.8856(6) _cell_length_c 22.5796(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11087.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14158 _cell_measurement_theta_min 3.2943 _cell_measurement_theta_max 32.8702 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_T_min 0.9407 _exptl_absorpt_correction_T_max 0.9659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78500 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9741 _reflns_number_gt 6194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0686P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9741 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1195 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.62109(2) 0.30256(3) 0.59655(2) 0.02266(16) Uani 1 1 d . . . Si1 Si 0.58177(4) 0.16722(4) 0.64936(4) 0.0261(2) Uani 1 1 d . . . Si2 Si 0.75188(4) 0.31611(4) 0.52859(4) 0.0236(2) Uani 1 1 d . . . Si3 Si 0.57108(4) 0.42892(4) 0.66544(4) 0.0261(2) Uani 1 1 d . . . O1 O 0.57854(10) 0.30059(13) 0.53249(10) 0.0465(7) Uani 1 1 d . . . O2 O 0.60684(9) 0.23569(11) 0.64155(9) 0.0332(6) Uani 1 1 d . . . O3 O 0.51193(10) 0.16381(12) 0.66563(11) 0.0479(7) Uani 1 1 d . . . O4 O 0.58875(11) 0.13686(12) 0.58433(11) 0.0462(7) Uani 1 1 d . . . O5 O 0.61815(10) 0.13104(12) 0.69919(11) 0.0471(7) Uani 1 1 d . . . O6 O 0.69884(9) 0.30499(10) 0.57594(9) 0.0276(5) Uani 1 1 d . . . O7 O 0.74934(9) 0.26978(10) 0.47332(9) 0.0296(5) Uani 1 1 d . . . O8 O 0.81576(9) 0.30767(11) 0.56093(9) 0.0297(6) Uani 1 1 d . . . O9 O 0.74126(9) 0.38383(10) 0.50228(9) 0.0283(5) Uani 1 1 d . . . O10 O 0.60323(10) 0.36847(11) 0.64033(10) 0.0356(6) Uani 1 1 d . . . O11 O 0.57325(9) 0.48357(11) 0.61772(10) 0.0368(6) Uani 1 1 d . . . O12 O 0.60380(10) 0.45222(12) 0.72459(10) 0.0420(7) Uani 1 1 d . . . O13 O 0.50191(9) 0.41135(11) 0.67407(10) 0.0353(6) Uani 1 1 d . . . C1 C 0.54933(14) 0.31209(17) 0.47819(16) 0.0353(9) Uani 1 1 d . . . C2 C 0.5620(2) 0.3772(2) 0.4612(2) 0.0805(16) Uani 1 1 d . . . H2A H 0.5459 0.4046 0.4916 0.121 Uiso 1 1 calc R . . H2B H 0.5433 0.3861 0.4230 0.121 Uiso 1 1 calc R . . H2C H 0.6052 0.3832 0.4581 0.121 Uiso 1 1 calc R . . C3 C 0.48384(16) 0.3018(2) 0.4886(2) 0.0629(13) Uani 1 1 d . . . H3A H 0.4774 0.2599 0.5025 0.094 Uiso 1 1 calc R . . H3B H 0.4620 0.3081 0.4515 0.094 Uiso 1 1 calc R . . H3C H 0.4694 0.3307 0.5185 0.094 Uiso 1 1 calc R . . C4 C 0.5749(2) 0.2684(3) 0.4339(2) 0.0842(17) Uani 1 1 d . . . H4A H 0.6177 0.2759 0.4296 0.126 Uiso 1 1 calc R . . H4B H 0.5552 0.2742 0.3955 0.126 Uiso 1 1 calc R . . H4C H 0.5685 0.2264 0.4475 0.126 Uiso 1 1 calc R . . C5 C 0.47418(14) 0.19245(17) 0.70799(15) 0.0326(9) Uani 1 1 d . . . C6 C 0.5029(2) 0.1945(3) 0.76791(19) 0.0804(16) Uani 1 1 d . . . H6A H 0.5140 0.1530 0.7800 0.121 Uiso 1 1 calc R . . H6B H 0.4748 0.2116 0.7967 0.121 Uiso 1 1 calc R . . H6C H 0.5387 0.2202 0.7662 0.121 Uiso 1 1 calc R . . C7 C 0.4589(2) 0.2541(2) 0.6842(3) 0.0897(18) Uani 1 1 d . . . H7A H 0.4929 0.2816 0.6894 0.135 Uiso 1 1 calc R . . H7B H 0.4244 0.2704 0.7057 0.135 Uiso 1 1 calc R . . H7C H 0.4492 0.2507 0.6420 0.135 Uiso 1 1 calc R . . C8 C 0.41934(18) 0.1517(2) 0.7101(2) 0.0685(14) Uani 1 1 d . . . H8A H 0.3993 0.1525 0.6716 0.103 Uiso 1 1 calc R . . H8B H 0.3920 0.1666 0.7407 0.103 Uiso 1 1 calc R . . H8C H 0.4314 0.1098 0.7194 0.103 Uiso 1 1 calc R . . C9 C 0.56236(15) 0.08438(17) 0.55772(15) 0.0339(9) Uani 1 1 d . . . C10 C 0.50143(19) 0.1001(3) 0.5360(2) 0.0872(18) Uani 1 1 d . . . H10A H 0.4754 0.1085 0.5698 0.131 Uiso 1 1 calc R . . H10B H 0.4853 0.0657 0.5132 0.131 Uiso 1 1 calc R . . H10C H 0.5036 0.1363 0.5106 0.131 Uiso 1 1 calc R . . C11 C 0.5620(3) 0.0311(2) 0.5994(2) 0.0884(18) Uani 1 1 d . . . H11A H 0.6027 0.0227 0.6127 0.133 Uiso 1 1 calc R . . H11B H 0.5460 -0.0049 0.5791 0.133 Uiso 1 1 calc R . . H11C H 0.5369 0.0407 0.6337 0.133 Uiso 1 1 calc R . . C12 C 0.6014(2) 0.0700(3) 0.5052(2) 0.0922(18) Uani 1 1 d . . . H12A H 0.6029 0.1055 0.4788 0.138 Uiso 1 1 calc R . . H12B H 0.5849 0.0350 0.4837 0.138 Uiso 1 1 calc R . . H12C H 0.6417 0.0603 0.5189 0.138 Uiso 1 1 calc R . . C13 C 0.68001(15) 0.13206(17) 0.71602(15) 0.0356(9) Uani 1 1 d . . . C14 C 0.69365(18) 0.06987(19) 0.74246(19) 0.0555(12) Uani 1 1 d . . . H14A H 0.6684 0.0632 0.7773 0.083 Uiso 1 1 calc R . . H14B H 0.7357 0.0682 0.7542 0.083 Uiso 1 1 calc R . . H14C H 0.6856 0.0380 0.7130 0.083 Uiso 1 1 calc R . . C15 C 0.71913(18) 0.1425(2) 0.66216(19) 0.0623(13) Uani 1 1 d . . . H15A H 0.7135 0.1089 0.6340 0.093 Uiso 1 1 calc R . . H15B H 0.7610 0.1440 0.6744 0.093 Uiso 1 1 calc R . . H15C H 0.7082 0.1812 0.6433 0.093 Uiso 1 1 calc R . . C16 C 0.68788(19) 0.1834(2) 0.76025(18) 0.0583(12) Uani 1 1 d . . . H16A H 0.6784 0.2225 0.7412 0.087 Uiso 1 1 calc R . . H16B H 0.7292 0.1841 0.7742 0.087 Uiso 1 1 calc R . . H16C H 0.6611 0.1770 0.7940 0.087 Uiso 1 1 calc R . . C17 C 0.76889(15) 0.20787(17) 0.46335(15) 0.0348(9) Uani 1 1 d . . . C18 C 0.7343(2) 0.1851(2) 0.41078(19) 0.0711(15) Uani 1 1 d . . . H18A H 0.6919 0.1822 0.4212 0.107 Uiso 1 1 calc R . . H18B H 0.7491 0.1447 0.3993 0.107 Uiso 1 1 calc R . . H18C H 0.7392 0.2136 0.3776 0.107 Uiso 1 1 calc R . . C19 C 0.7556(2) 0.16873(19) 0.51706(19) 0.0610(12) Uani 1 1 d . . . H19A H 0.7772 0.1847 0.5514 0.091 Uiso 1 1 calc R . . H19B H 0.7682 0.1266 0.5094 0.091 Uiso 1 1 calc R . . H19C H 0.7127 0.1695 0.5252 0.091 Uiso 1 1 calc R . . C20 C 0.83525(18) 0.2089(2) 0.4510(2) 0.0701(15) Uani 1 1 d . . . H20A H 0.8432 0.2349 0.4165 0.105 Uiso 1 1 calc R . . H20B H 0.8492 0.1673 0.4429 0.105 Uiso 1 1 calc R . . H20C H 0.8563 0.2253 0.4856 0.105 Uiso 1 1 calc R . . C21 C 0.83805(14) 0.33006(18) 0.61708(15) 0.0337(9) Uani 1 1 d . . . C22 C 0.82145(19) 0.2844(2) 0.66458(17) 0.0552(12) Uani 1 1 d . . . H22A H 0.7779 0.2812 0.6672 0.083 Uiso 1 1 calc R . . H22B H 0.8374 0.2979 0.7028 0.083 Uiso 1 1 calc R . . H22C H 0.8382 0.2443 0.6546 0.083 Uiso 1 1 calc R . . C23 C 0.90523(15) 0.3347(2) 0.60968(17) 0.0568(13) Uani 1 1 d . . . H23A H 0.9218 0.2940 0.6023 0.085 Uiso 1 1 calc R . . H23B H 0.9228 0.3517 0.6458 0.085 Uiso 1 1 calc R . . H23C H 0.9144 0.3615 0.5761 0.085 Uiso 1 1 calc R . . C24 C 0.81211(16) 0.39207(18) 0.63109(16) 0.0432(10) Uani 1 1 d . . . H24A H 0.8220 0.4207 0.5992 0.065 Uiso 1 1 calc R . . H24B H 0.8288 0.4070 0.6685 0.065 Uiso 1 1 calc R . . H24C H 0.7687 0.3887 0.6346 0.065 Uiso 1 1 calc R . . C25 C 0.76928(14) 0.41480(17) 0.45272(15) 0.0342(9) Uani 1 1 d . . . C26 C 0.83633(15) 0.4047(2) 0.45390(18) 0.0490(11) Uani 1 1 d . . . H26A H 0.8524 0.4185 0.4920 0.073 Uiso 1 1 calc R . . H26B H 0.8550 0.4280 0.4218 0.073 Uiso 1 1 calc R . . H26C H 0.8449 0.3611 0.4487 0.073 Uiso 1 1 calc R . . C27 C 0.75491(18) 0.48139(19) 0.46024(19) 0.0587(12) Uani 1 1 d . . . H27A H 0.7116 0.4868 0.4615 0.088 Uiso 1 1 calc R . . H27B H 0.7714 0.5045 0.4269 0.088 Uiso 1 1 calc R . . H27C H 0.7724 0.4963 0.4973 0.088 Uiso 1 1 calc R . . C28 C 0.7433(2) 0.3904(2) 0.39594(16) 0.0636(13) Uani 1 1 d . . . H28A H 0.7526 0.3468 0.3924 0.095 Uiso 1 1 calc R . . H28B H 0.7604 0.4125 0.3623 0.095 Uiso 1 1 calc R . . H28C H 0.7000 0.3960 0.3963 0.095 Uiso 1 1 calc R . . C29 C 0.61908(14) 0.52626(15) 0.59958(15) 0.0302(8) Uani 1 1 d . . . C30 C 0.68056(14) 0.49864(17) 0.60669(15) 0.0356(9) Uani 1 1 d . . . H30A H 0.6881 0.4903 0.6487 0.053 Uiso 1 1 calc R . . H30B H 0.7106 0.5273 0.5918 0.053 Uiso 1 1 calc R . . H30C H 0.6828 0.4604 0.5842 0.053 Uiso 1 1 calc R . . C31 C 0.60583(16) 0.5387(2) 0.53429(16) 0.0466(10) Uani 1 1 d . . . H31A H 0.6125 0.5014 0.5113 0.070 Uiso 1 1 calc R . . H31B H 0.6323 0.5711 0.5198 0.070 Uiso 1 1 calc R . . H31C H 0.5643 0.5517 0.5300 0.070 Uiso 1 1 calc R . . C32 C 0.61267(17) 0.58363(18) 0.63564(17) 0.0481(10) Uani 1 1 d . . . H32A H 0.5717 0.5989 0.6324 0.072 Uiso 1 1 calc R . . H32B H 0.6404 0.6147 0.6208 0.072 Uiso 1 1 calc R . . H32C H 0.6217 0.5747 0.6772 0.072 Uiso 1 1 calc R . . C33 C 0.62601(18) 0.4198(2) 0.77612(16) 0.0508(11) Uani 1 1 d . . . C34 C 0.6888(2) 0.3983(3) 0.7606(2) 0.0864(18) Uani 1 1 d . . . H34A H 0.6869 0.3698 0.7271 0.130 Uiso 1 1 calc R . . H34B H 0.7064 0.3776 0.7949 0.130 Uiso 1 1 calc R . . H34C H 0.7134 0.4336 0.7498 0.130 Uiso 1 1 calc R . . C35 C 0.6267(2) 0.4663(3) 0.82459(18) 0.0808(16) Uani 1 1 d . . . H35A H 0.6517 0.5009 0.8128 0.121 Uiso 1 1 calc R . . H35B H 0.6428 0.4478 0.8607 0.121 Uiso 1 1 calc R . . H35C H 0.5860 0.4806 0.8320 0.121 Uiso 1 1 calc R . . C36 C 0.5878(2) 0.3663(3) 0.7906(2) 0.0880(18) Uani 1 1 d . . . H36A H 0.5466 0.3799 0.7963 0.132 Uiso 1 1 calc R . . H36B H 0.6023 0.3470 0.8270 0.132 Uiso 1 1 calc R . . H36C H 0.5894 0.3368 0.7580 0.132 Uiso 1 1 calc R . . C37 C 0.45037(15) 0.45051(18) 0.68285(16) 0.0378(9) Uani 1 1 d . . . C38 C 0.4672(2) 0.5057(3) 0.7194(2) 0.0904(19) Uani 1 1 d . . . H38A H 0.4855 0.4923 0.7566 0.136 Uiso 1 1 calc R . . H38B H 0.4315 0.5298 0.7280 0.136 Uiso 1 1 calc R . . H38C H 0.4957 0.5308 0.6972 0.136 Uiso 1 1 calc R . . C39 C 0.40540(18) 0.4114(2) 0.7150(2) 0.0747(16) Uani 1 1 d . . . H39A H 0.3963 0.3751 0.6912 0.112 Uiso 1 1 calc R . . H39B H 0.3688 0.4349 0.7215 0.112 Uiso 1 1 calc R . . H39C H 0.4219 0.3987 0.7533 0.112 Uiso 1 1 calc R . . C40 C 0.42744(19) 0.4681(2) 0.6235(2) 0.0698(14) Uani 1 1 d . . . H40A H 0.4571 0.4933 0.6031 0.105 Uiso 1 1 calc R . . H40B H 0.3904 0.4913 0.6281 0.105 Uiso 1 1 calc R . . H40C H 0.4196 0.4311 0.6002 0.105 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 Ti1 0.0182(3) 0.0263(4) 0.0235(3) -0.0009(3) -0.0016(2) -0.0004(3) Si1 0.0216(5) 0.0250(6) 0.0318(5) -0.0032(4) 0.0028(4) -0.0038(4) Si2 0.0179(4) 0.0301(6) 0.0228(5) -0.0021(4) -0.0006(4) 0.0005(4) Si3 0.0290(5) 0.0255(6) 0.0239(5) 0.0008(4) 0.0021(4) 0.0043(4) O1 0.0357(14) 0.068(2) 0.0355(14) 0.0028(14) -0.0138(11) -0.0014(13) O2 0.0313(13) 0.0299(15) 0.0385(14) 0.0002(12) -0.0022(11) -0.0083(11) O3 0.0400(15) 0.0455(18) 0.0582(17) -0.0057(14) 0.0139(13) -0.0047(13) O4 0.0517(16) 0.0383(17) 0.0486(16) -0.0108(14) 0.0015(13) -0.0089(13) O5 0.0385(15) 0.0449(18) 0.0578(17) 0.0169(14) -0.0147(13) -0.0146(13) O6 0.0221(11) 0.0322(14) 0.0286(12) 0.0024(11) 0.0013(9) -0.0005(10) O7 0.0282(12) 0.0337(15) 0.0269(12) -0.0045(11) -0.0047(10) 0.0048(11) O8 0.0203(11) 0.0429(16) 0.0260(12) -0.0079(11) -0.0044(9) 0.0035(11) O9 0.0233(12) 0.0353(15) 0.0261(12) 0.0026(11) 0.0048(9) 0.0002(10) O10 0.0351(13) 0.0305(15) 0.0412(14) -0.0013(12) 0.0077(11) 0.0043(11) O11 0.0307(13) 0.0405(17) 0.0393(14) 0.0054(12) 0.0026(11) 0.0021(12) O12 0.0475(15) 0.0438(17) 0.0348(14) -0.0003(13) -0.0025(12) 0.0048(13) O13 0.0332(13) 0.0315(15) 0.0412(14) -0.0021(12) 0.0068(11) 0.0012(11) C1 0.0293(19) 0.039(3) 0.038(2) 0.0044(19) -0.0129(16) 0.0010(17) C2 0.056(3) 0.058(3) 0.127(5) 0.042(3) -0.007(3) -0.008(2) C3 0.035(2) 0.060(3) 0.094(3) 0.010(3) -0.024(2) -0.007(2) C4 0.097(4) 0.100(5) 0.056(3) -0.024(3) -0.008(3) 0.022(3) C5 0.0248(18) 0.039(2) 0.034(2) -0.0028(18) 0.0097(15) 0.0020(17) C6 0.077(3) 0.104(5) 0.061(3) -0.014(3) 0.000(3) -0.010(3) C7 0.079(4) 0.051(4) 0.139(5) 0.031(3) 0.030(3) 0.020(3) C8 0.057(3) 0.080(4) 0.069(3) 0.001(3) 0.013(2) -0.019(3) C9 0.036(2) 0.029(2) 0.036(2) -0.0142(17) -0.0003(16) -0.0043(17) C10 0.054(3) 0.087(4) 0.121(4) -0.040(4) -0.037(3) 0.004(3) C11 0.152(5) 0.037(3) 0.076(4) 0.004(3) -0.031(3) -0.022(3) C12 0.090(4) 0.082(4) 0.104(4) -0.046(3) 0.036(3) -0.016(3) C13 0.030(2) 0.037(2) 0.040(2) 0.0040(19) -0.0080(16) -0.0053(17) C14 0.054(3) 0.049(3) 0.064(3) 0.017(2) -0.021(2) -0.002(2) C15 0.047(2) 0.063(3) 0.076(3) 0.018(3) 0.012(2) 0.011(2) C16 0.060(3) 0.053(3) 0.062(3) -0.002(2) -0.015(2) 0.003(2) C17 0.038(2) 0.035(2) 0.032(2) -0.0101(18) -0.0030(16) 0.0066(17) C18 0.098(4) 0.053(3) 0.062(3) -0.028(3) -0.032(3) 0.015(3) C19 0.077(3) 0.039(3) 0.067(3) -0.002(2) 0.002(2) 0.010(2) C20 0.047(3) 0.067(4) 0.097(4) -0.022(3) 0.020(2) 0.015(2) C21 0.0263(19) 0.047(3) 0.0279(19) -0.0068(18) -0.0084(15) 0.0027(17) C22 0.063(3) 0.058(3) 0.044(2) 0.003(2) -0.020(2) -0.002(2) C23 0.026(2) 0.090(4) 0.054(3) -0.024(3) -0.0141(18) 0.003(2) C24 0.041(2) 0.053(3) 0.036(2) -0.015(2) -0.0119(17) 0.0030(19) C25 0.0295(19) 0.040(2) 0.033(2) 0.0075(18) 0.0091(15) -0.0001(17) C26 0.039(2) 0.056(3) 0.051(3) 0.016(2) 0.0177(19) 0.000(2) C27 0.055(3) 0.046(3) 0.075(3) 0.022(2) 0.026(2) 0.004(2) C28 0.075(3) 0.082(4) 0.033(2) 0.020(2) -0.006(2) -0.021(3) C29 0.0272(18) 0.022(2) 0.041(2) 0.0037(17) 0.0101(16) -0.0002(16) C30 0.032(2) 0.035(2) 0.040(2) 0.0033(18) 0.0045(16) 0.0007(17) C31 0.040(2) 0.052(3) 0.048(2) 0.012(2) 0.0034(19) 0.004(2) C32 0.044(2) 0.041(3) 0.059(3) -0.010(2) 0.005(2) 0.001(2) C33 0.063(3) 0.062(3) 0.027(2) 0.005(2) -0.0128(19) 0.005(2) C34 0.074(3) 0.124(5) 0.061(3) 0.029(3) -0.008(3) 0.044(3) C35 0.103(4) 0.097(4) 0.043(3) -0.007(3) -0.017(3) -0.007(3) C36 0.111(4) 0.082(4) 0.070(3) 0.035(3) -0.017(3) -0.023(3) C37 0.0275(19) 0.041(3) 0.045(2) -0.001(2) 0.0081(17) 0.0050(17) C38 0.055(3) 0.091(4) 0.125(5) -0.066(4) 0.010(3) 0.018(3) C39 0.049(3) 0.077(4) 0.098(4) 0.031(3) 0.039(3) 0.014(3) C40 0.049(3) 0.083(4) 0.078(3) 0.028(3) 0.001(2) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.734(2) . ? Ti1 O10 1.794(2) . ? Ti1 O2 1.810(2) . ? Ti1 O6 1.806(2) . ? Si1 O5 1.600(3) . ? Si1 O2 1.610(2) . ? Si1 O3 1.611(2) . ? Si1 O4 1.619(3) . ? Si2 O7 1.609(2) . ? Si2 O9 1.614(2) . ? Si2 O6 1.618(2) . ? Si2 O8 1.619(2) . ? Si3 O12 1.607(2) . ? Si3 O10 1.610(2) . ? Si3 O13 1.611(2) . ? Si3 O11 1.611(3) . ? O1 C1 1.413(4) . ? O3 C5 1.423(4) . ? O4 C9 1.425(4) . ? O5 C13 1.439(4) . ? O7 C17 1.442(4) . ? O8 C21 1.448(4) . ? O9 C25 1.451(4) . ? O11 C29 1.449(4) . ? O12 C33 1.451(4) . ? O13 C37 1.453(4) . ? C1 C3 1.505(5) . ? C1 C2 1.502(6) . ? C1 C4 1.499(6) . ? C5 C7 1.491(6) . ? C5 C6 1.499(5) . ? C5 C8 1.520(5) . ? C9 C10 1.492(5) . ? C9 C11 1.499(6) . ? C9 C12 1.507(5) . ? C13 C15 1.517(5) . ? C13 C16 1.514(5) . ? C13 C14 1.517(5) . ? C17 C18 1.504(5) . ? C17 C20 1.515(5) . ? C17 C19 1.515(5) . ? C21 C22 1.513(5) . ? C21 C24 1.510(5) . ? C21 C23 1.520(5) . ? C25 C27 1.502(5) . ? C25 C28 1.506(5) . ? C25 C26 1.521(5) . ? C29 C32 1.503(5) . ? C29 C30 1.515(4) . ? C29 C31 1.529(5) . ? C33 C35 1.494(6) . ? C33 C36 1.487(6) . ? C33 C34 1.527(6) . ? C37 C40 1.485(5) . ? C37 C39 1.510(5) . ? C37 C38 1.511(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O10 110.90(12) . . ? O1 Ti1 O2 110.54(12) . . ? O10 Ti1 O2 107.54(10) . . ? O1 Ti1 O6 108.51(10) . . ? O10 Ti1 O6 109.52(10) . . ? O2 Ti1 O6 109.82(10) . . ? O5 Si1 O2 111.06(13) . . ? O5 Si1 O3 108.24(14) . . ? O2 Si1 O3 114.06(14) . . ? O5 Si1 O4 112.67(14) . . ? O2 Si1 O4 104.41(13) . . ? O3 Si1 O4 106.37(14) . . ? O7 Si2 O9 106.74(12) . . ? O7 Si2 O6 113.04(12) . . ? O9 Si2 O6 105.82(11) . . ? O7 Si2 O8 108.02(12) . . ? O9 Si2 O8 113.67(12) . . ? O6 Si2 O8 109.62(11) . . ? O12 Si3 O10 110.41(13) . . ? O12 Si3 O13 114.53(13) . . ? O10 Si3 O13 106.14(13) . . ? O12 Si3 O11 107.86(14) . . ? O10 Si3 O11 111.17(12) . . ? O13 Si3 O11 106.70(12) . . ? C1 O1 Ti1 167.2(3) . . ? Si1 O2 Ti1 151.11(14) . . ? C5 O3 Si1 135.4(2) . . ? C9 O4 Si1 132.3(2) . . ? C13 O5 Si1 132.1(2) . . ? Si2 O6 Ti1 152.25(13) . . ? C17 O7 Si2 134.6(2) . . ? C21 O8 Si2 131.4(2) . . ? C25 O9 Si2 130.4(2) . . ? Si3 O10 Ti1 162.72(16) . . ? C29 O11 Si3 133.6(2) . . ? C33 O12 Si3 131.9(3) . . ? C37 O13 Si3 130.0(2) . . ? O1 C1 C3 106.9(3) . . ? O1 C1 C2 107.6(3) . . ? C3 C1 C2 111.5(3) . . ? O1 C1 C4 106.8(3) . . ? C3 C1 C4 112.5(4) . . ? C2 C1 C4 111.3(4) . . ? O3 C5 C7 107.1(3) . . ? O3 C5 C6 111.3(3) . . ? C7 C5 C6 113.4(4) . . ? O3 C5 C8 104.2(3) . . ? C7 C5 C8 110.8(3) . . ? C6 C5 C8 109.7(3) . . ? O4 C9 C10 109.5(3) . . ? O4 C9 C11 111.4(3) . . ? C10 C9 C11 112.4(4) . . ? O4 C9 C12 105.0(3) . . ? C10 C9 C12 108.7(4) . . ? C11 C9 C12 109.6(4) . . ? O5 C13 C15 110.4(3) . . ? O5 C13 C16 107.3(3) . . ? C15 C13 C16 110.5(3) . . ? O5 C13 C14 106.5(3) . . ? C15 C13 C14 109.5(3) . . ? C16 C13 C14 112.5(3) . . ? O7 C17 C18 106.1(3) . . ? O7 C17 C20 108.2(3) . . ? C18 C17 C20 111.6(3) . . ? O7 C17 C19 110.3(3) . . ? C18 C17 C19 110.0(4) . . ? C20 C17 C19 110.5(3) . . ? O8 C21 C22 108.2(3) . . ? O8 C21 C24 110.8(3) . . ? C22 C21 C24 110.5(3) . . ? O8 C21 C23 105.6(3) . . ? C22 C21 C23 111.5(3) . . ? C24 C21 C23 110.2(3) . . ? O9 C25 C27 105.8(3) . . ? O9 C25 C28 108.8(3) . . ? C27 C25 C28 110.9(3) . . ? O9 C25 C26 110.3(3) . . ? C27 C25 C26 110.6(3) . . ? C28 C25 C26 110.2(3) . . ? O11 C29 C32 108.5(3) . . ? O11 C29 C30 111.0(3) . . ? C32 C29 C30 111.3(3) . . ? O11 C29 C31 104.5(3) . . ? C32 C29 C31 110.8(3) . . ? C30 C29 C31 110.5(3) . . ? O12 C33 C35 105.0(4) . . ? O12 C33 C36 111.3(3) . . ? C35 C33 C36 112.4(4) . . ? O12 C33 C34 106.5(3) . . ? C35 C33 C34 111.7(4) . . ? C36 C33 C34 109.8(4) . . ? O13 C37 C40 107.8(3) . . ? O13 C37 C39 105.2(3) . . ? C40 C37 C39 110.5(3) . . ? O13 C37 C38 110.3(3) . . ? C40 C37 C38 111.9(4) . . ? C39 C37 C38 111.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Ti1 O1 C1 55.8(11) . . . . ? O2 Ti1 O1 C1 175.0(10) . . . . ? O6 Ti1 O1 C1 -64.5(11) . . . . ? O5 Si1 O2 Ti1 149.9(3) . . . . ? O3 Si1 O2 Ti1 -87.4(3) . . . . ? O4 Si1 O2 Ti1 28.2(3) . . . . ? O1 Ti1 O2 Si1 17.5(3) . . . . ? O10 Ti1 O2 Si1 138.7(3) . . . . ? O6 Ti1 O2 Si1 -102.2(3) . . . . ? O5 Si1 O3 C5 74.9(4) . . . . ? O2 Si1 O3 C5 -49.3(4) . . . . ? O4 Si1 O3 C5 -163.8(3) . . . . ? O5 Si1 O4 C9 77.3(3) . . . . ? O2 Si1 O4 C9 -162.0(3) . . . . ? O3 Si1 O4 C9 -41.1(3) . . . . ? O2 Si1 O5 C13 -35.6(4) . . . . ? O3 Si1 O5 C13 -161.5(3) . . . . ? O4 Si1 O5 C13 81.1(3) . . . . ? O7 Si2 O6 Ti1 -62.3(3) . . . . ? O9 Si2 O6 Ti1 54.2(3) . . . . ? O8 Si2 O6 Ti1 177.2(3) . . . . ? O1 Ti1 O6 Si2 16.4(4) . . . . ? O10 Ti1 O6 Si2 -104.7(3) . . . . ? O2 Ti1 O6 Si2 137.4(3) . . . . ? O9 Si2 O7 C17 161.9(3) . . . . ? O6 Si2 O7 C17 -82.1(3) . . . . ? O8 Si2 O7 C17 39.3(3) . . . . ? O7 Si2 O8 C21 -169.0(3) . . . . ? O9 Si2 O8 C21 72.8(3) . . . . ? O6 Si2 O8 C21 -45.4(3) . . . . ? O7 Si2 O9 C25 -49.3(3) . . . . ? O6 Si2 O9 C25 -170.0(2) . . . . ? O8 Si2 O9 C25 69.6(3) . . . . ? O12 Si3 O10 Ti1 176.7(5) . . . . ? O13 Si3 O10 Ti1 52.0(5) . . . . ? O11 Si3 O10 Ti1 -63.6(5) . . . . ? O1 Ti1 O10 Si3 10.3(5) . . . . ? O2 Ti1 O10 Si3 -110.7(5) . . . . ? O6 Ti1 O10 Si3 130.1(5) . . . . ? O12 Si3 O11 C29 42.8(3) . . . . ? O10 Si3 O11 C29 -78.3(3) . . . . ? O13 Si3 O11 C29 166.4(3) . . . . ? O10 Si3 O12 C33 -43.4(3) . . . . ? O13 Si3 O12 C33 76.3(3) . . . . ? O11 Si3 O12 C33 -165.1(3) . . . . ? O12 Si3 O13 C37 73.0(3) . . . . ? O10 Si3 O13 C37 -164.9(3) . . . . ? O11 Si3 O13 C37 -46.3(3) . . . . ? Ti1 O1 C1 C3 -127.0(10) . . . . ? Ti1 O1 C1 C2 -7.1(12) . . . . ? Ti1 O1 C1 C4 112.5(11) . . . . ? Si1 O3 C5 C7 80.7(4) . . . . ? Si1 O3 C5 C6 -43.7(5) . . . . ? Si1 O3 C5 C8 -161.9(3) . . . . ? Si1 O4 C9 C10 81.0(4) . . . . ? Si1 O4 C9 C11 -43.9(5) . . . . ? Si1 O4 C9 C12 -162.4(3) . . . . ? Si1 O5 C13 C15 -34.0(5) . . . . ? Si1 O5 C13 C16 86.5(4) . . . . ? Si1 O5 C13 C14 -152.8(3) . . . . ? Si2 O7 C17 C18 160.5(3) . . . . ? Si2 O7 C17 C20 -79.6(4) . . . . ? Si2 O7 C17 C19 41.4(4) . . . . ? Si2 O8 C21 C22 87.7(4) . . . . ? Si2 O8 C21 C24 -33.6(4) . . . . ? Si2 O8 C21 C23 -152.9(3) . . . . ? Si2 O9 C25 C27 -163.9(2) . . . . ? Si2 O9 C25 C28 76.8(4) . . . . ? Si2 O9 C25 C26 -44.3(4) . . . . ? Si3 O11 C29 C32 -93.0(3) . . . . ? Si3 O11 C29 C30 29.6(4) . . . . ? Si3 O11 C29 C31 148.8(3) . . . . ? Si3 O12 C33 C35 -156.0(3) . . . . ? Si3 O12 C33 C36 -34.3(5) . . . . ? Si3 O12 C33 C34 85.4(4) . . . . ? Si3 O13 C37 C40 87.4(4) . . . . ? Si3 O13 C37 C39 -154.7(3) . . . . ? Si3 O13 C37 C38 -35.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.712 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.053