# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 182/1064 #======================================================================= data_global #======================================================================= # 0. AUDIT DETAILS _audit_creation_date 'Tue Jul 21 14:00:50 1998' _audit_creation_method 'PLATON option' #======================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name ; Dr. A.L. Spek ; _publ_contact_author_address ; Bijvoet Center for Biomolecular Research Department of Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'spea@chem.uu.nl' _publ_contact_author_fax '+31 30 2533940' _publ_contact_author_phone '+31 30 2532538' _publ_requested_journal 'Chem. Commun.' _publ_contact_letter # Include date of submission ; Date of submission ? Dear Sirs, This CIF is supplementary material for the publication 8/06402D, entitled: "Synthesis and structural characterisation of platinum silasesquioxane complexes." by Hendrikus C.L. Abbenhuis, Andrew D. Burrows, Huub Kooijman, Martin Lutz, Mark T. Palmer, Rutger A. van Santen and Anthony L. Spek recently submitted to Chem. Commun. The CIF contains the structural data for compound 3a and 1a. Yours Sincerely, Huub Kooijman ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and structural characterisation of platinum silasesquioxane complexes. ; loop_ _publ_author_name 'Hendrikus C.L. Abbenhuis' 'Andrew D. Burrows' 'Huub Kooijman' 'Martin Lutz' 'Mark T. Palmer' 'Rutger A. van Santen' 'Anthony L. Spek' #======================================================================= data_3a #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H96 O12 P2 Pt Si8, C2 H3 N' _chemical_formula_structural ? _chemical_formula_sum 'C66 H99 N O12 P2 Pt Si8' _chemical_formula_weight 1580.21 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_space_group_name_H-M 'P c c n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,z 1/2+x,-y,1/2-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2+y,-z 1/2-x,y,1/2+z x,1/2-y,1/2+z _cell_length_a 47.997(4) _cell_length_b 13.9845(11) _cell_length_c 21.803(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 14634(2) _cell_formula_units_Z 8 _cell_measurement_temperature 153 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 6544 _exptl_absorpt_coefficient_mu 2.15 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 153 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 6 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 12902 _diffrn_reflns_av_R_equivalents 0.1299 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 12147 # number of observed reflections (> n sig(I)) _reflns_number_gt 7515 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'Locally modified CAD4-Version 5 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1998)' _computing_publication_material 'PLATON (Spek, 1998)' #======================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\' _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment 'H-atom refinement: see text ' _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 12147 _refine_ls_number_parameters 812 _refine_ls_number_restraints 778 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1439 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.973 _refine_diff_density_min -1.570 _refine_diff_density_rms 0.174 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Pt1 Pt Uani 0.07828 1.09406(2) 0.20291(1) 1.000 0.0143(1) P1 P Uani 0.07134(5) 1.24305(16) 0.17524(10) 1.000 0.0177(7) P2 P Uani 0.07153(4) 1.14224(15) 0.29799(10) 1.000 0.0150(6) Si1 Si Uani 0.09282(5) 0.85283(16) 0.21256(11) 1.000 0.0164(7) Si2 Si Uani 0.10301(5) 1.03360(17) 0.05859(11) 1.000 0.0170(8) Si3 Si Uani 0.18823(5) 1.03134(18) 0.21845(11) 1.000 0.0208(8) Si4 Si Uani 0.16794(5) 1.02830(17) 0.07981(11) 1.000 0.0201(8) Si5 Si Uani 0.10214(5) 0.81590(17) 0.07277(11) 1.000 0.0188(7) Si6 Si Uani 0.15907(5) 0.83599(19) 0.22950(12) 1.000 0.0223(8) Si7 Si Uani 0.16577(5) 0.80741(18) 0.08998(12) 1.000 0.0218(8) Si8 Si Uani 0.18702(6) 1.2232(2) 0.29374(15) 1.000 0.0363(10) O1 O Uani 0.08105(13) 0.9548(4) 0.2286(3) 1.000 0.0233(19) O2 O Uani 0.08294(13) 1.0558(4) 0.1134(2) 1.000 0.0227(19) O3 O Uani 0.13567(12) 1.0580(4) 0.0737(3) 1.000 0.0233(19) O4 O Uani 0.10198(12) 0.9200(4) 0.0404(2) 1.000 0.0203(17) O5 O Uani 0.08896(13) 0.8200(4) 0.1405(3) 1.000 0.0237(19) O6 O Uani 0.12591(13) 0.8443(5) 0.2273(3) 1.000 0.031(2) O7 O Uani 0.17796(13) 1.0514(4) 0.1488(3) 1.000 0.028(2) O8 O Uani 0.13392(12) 0.7769(4) 0.0753(3) 1.000 0.0250(19) O9 O Uani 0.17153(12) 0.9146(4) 0.0660(3) 1.000 0.0253(17) O10 O Uani 0.17131(12) 0.8033(4) 0.1633(3) 1.000 0.0263(19) O11 O Uani 0.17171(13) 0.9398(4) 0.2467(3) 1.000 0.0273(17) O12 O Uani 0.17997(13) 1.1223(4) 0.2594(3) 1.000 0.029(2) C1 C Uani 0.2096(2) 1.2956(9) 0.2439(7) 1.000 0.071(5) C2 C Uani 0.1541(2) 1.2870(7) 0.3070(5) 1.000 0.042(4) C3 C Uani 0.2045(3) 1.1976(10) 0.3679(6) 1.000 0.078(5) C4 C Uani 0.05513(18) 1.3065(6) 0.2400(4) 1.000 0.021(3) C5 C Uani 0.07036(16) 1.2736(5) 0.2979(4) 1.000 0.0160(19) C11 C Uani 0.07464(17) 0.7608(6) 0.2586(4) 1.000 0.019(2) C12 C Uani 0.08447(19) 0.6558(6) 0.2462(5) 1.000 0.028(3) C13 C Uani 0.05817(19) 0.5951(6) 0.2486(4) 1.000 0.027(3) C14 C Uani 0.0351(2) 0.6570(7) 0.2741(5) 1.000 0.032(3) C15 C Uani 0.04324(18) 0.7568(7) 0.2511(5) 1.000 0.031(3) C21 C Uani 0.09321(18) 1.1024(6) -0.0102(4) 1.000 0.020(2) C22 C Uani 0.06210(19) 1.0918(7) -0.0285(4) 1.000 0.029(3) C23 C Uani 0.0621(2) 1.0027(7) -0.0674(5) 1.000 0.035(3) C24 C Uani 0.0895(2) 1.0028(7) -0.1028(4) 1.000 0.040(3) C25 C Uani 0.1090(2) 1.0726(8) -0.0684(4) 1.000 0.036(3) C31 C Uani 0.22583(18) 1.0081(7) 0.2215(4) 1.000 0.029(3) C32 C Uani 0.2368(2) 0.9849(9) 0.2870(5) 1.000 0.046(4) C33 C Uani 0.2591(3) 0.9090(11) 0.2804(6) 1.000 0.080(5) C34 C Uani 0.2628(3) 0.8911(11) 0.2141(6) 1.000 0.077(5) C35 C Uani 0.2365(2) 0.9221(8) 0.1836(5) 1.000 0.043(3) C41 C Uani 0.19024(19) 1.0958(7) 0.0260(4) 1.000 0.028(3) C42 C Uani 0.1881(2) 1.0623(8) -0.0411(5) 1.000 0.045(3) C43 C Uani 0.2181(3) 1.0498(11) -0.0629(7) 1.000 0.079(5) C44 C Uani 0.2357(2) 1.1070(10) -0.0194(6) 1.000 0.063(4) C45 C Uani 0.2214(2) 1.0897(11) 0.0404(6) 1.000 0.064(4) C51 C Uani 0.08115(19) 0.7336(6) 0.0253(4) 1.000 0.020(3) C52 C Uani 0.0906(2) 0.7231(7) -0.0417(4) 1.000 0.036(3) C53 C Uani 0.0749(2) 0.6363(7) -0.0658(4) 1.000 0.040(3) C54 C Uani 0.0664(2) 0.5776(7) -0.0084(5) 1.000 0.036(3) C55 C Uani 0.0801(2) 0.6284(6) 0.0449(4) 1.000 0.027(3) C61 C Uani 0.1703(2) 0.7456(7) 0.2858(4) 1.000 0.032(3) C62 C Uani 0.1562(3) 0.7510(9) 0.3492(5) 1.000 0.054(4) C63 C Uani 0.1618(3) 0.6534(9) 0.3775(6) 1.000 0.067(5) C64 C Uani 0.1602(3) 0.5834(8) 0.3245(5) 1.000 0.054(4) C65 C Uani 0.1635(2) 0.6427(7) 0.2654(5) 1.000 0.037(3) C71 C Uani 0.1892(2) 0.7239(8) 0.0510(6) 1.000 0.049(3) C72A C Uiso 0.2180(4) 0.7368(15) 0.0453(9) 0.527(12) 0.038(5) C73A C Uiso 0.2292(5) 0.6496(16) 0.0131(11) 0.527(12) 0.053(6) C74 C Uani 0.2071(3) 0.5688(9) 0.0294(7) 1.000 0.063(5) C75 C Uani 0.1848(3) 0.6193(7) 0.0656(7) 1.000 0.059(4) C81 C Uani 0.04674(17) 1.2555(6) 0.1129(4) 1.000 0.018(2) C82 C Uani 0.02256(18) 1.2010(7) 0.1165(4) 1.000 0.027(3) C83 C Uani 0.0020(2) 1.2100(7) 0.0714(4) 1.000 0.030(3) C84 C Uani 0.0063(2) 1.2713(7) 0.0231(5) 1.000 0.030(3) C85 C Uani 0.0299(2) 1.3258(7) 0.0192(4) 1.000 0.028(3) C86 C Uani 0.0500(2) 1.3180(6) 0.0637(4) 1.000 0.024(3) C91 C Uani 0.10255(18) 1.3097(6) 0.1554(4) 1.000 0.019(3) C92 C Uani 0.10319(18) 1.4110(6) 0.1561(4) 1.000 0.025(3) C93 C Uani 0.1272(2) 1.4588(7) 0.1420(5) 1.000 0.033(3) C94 C Uani 0.1509(2) 1.4094(7) 0.1273(5) 1.000 0.039(3) C95 C Uani 0.1501(2) 1.3100(7) 0.1265(5) 1.000 0.041(4) C96 C Uani 0.12621(19) 1.2606(7) 0.1415(4) 1.000 0.030(3) C101 C Uani 0.03879(17) 1.1013(6) 0.3301(4) 1.000 0.016(2) C102 C Uani 0.0339(2) 1.0048(7) 0.3315(4) 1.000 0.029(3) C103 C Uani 0.0097(2) 0.9697(7) 0.3567(5) 1.000 0.033(3) C104 C Uani -0.01026(19) 1.0287(7) 0.3797(4) 1.000 0.028(3) C105 C Uani -0.00613(19) 1.1282(7) 0.3759(4) 1.000 0.028(3) C106 C Uani 0.01839(18) 1.1635(6) 0.3530(4) 1.000 0.022(3) C111 C Uani 0.09704(18) 1.1118(6) 0.3535(4) 1.000 0.019(3) C112 C Uani 0.1196(2) 1.0536(7) 0.3386(4) 1.000 0.031(3) C113 C Uani 0.1403(2) 1.0314(7) 0.3812(5) 1.000 0.034(3) C114 C Uani 0.1383(2) 1.0699(7) 0.4398(4) 1.000 0.034(3) C115 C Uani 0.1167(2) 1.1267(7) 0.4557(4) 1.000 0.033(3) C116 C Uani 0.09582(18) 1.1489(6) 0.4134(4) 1.000 0.018(3) C73B C Uiso 0.2073(6) 0.6276(18) -0.0272(12) 0.473(12) 0.0530 C72B C Uiso 0.1947(5) 0.7238(16) -0.0098(10) 0.473(12) 0.0380 N121 N Uani -0.0102(2) 0.9230(7) 0.1816(5) 1.000 0.059(4) C122 C Uani 0.0058(2) 0.9266(7) 0.1442(5) 1.000 0.037(4) C123 C Uani 0.0268(2) 0.9299(8) 0.0974(6) 1.000 0.051(4) H1B H Uiso 0.20000 1.30820 0.20500 1.000 0.1070 H1A H Uiso 0.21390 1.35630 0.26420 1.000 0.1070 H2B H Uiso 0.14340 1.29000 0.26870 1.000 0.0630 H2C H Uiso 0.15800 1.35210 0.32140 1.000 0.0630 H3A H Uiso 0.22290 1.16990 0.36010 1.000 0.1170 H3B H Uiso 0.19320 1.15220 0.39150 1.000 0.1170 H3C H Uiso 0.20660 1.25710 0.39120 1.000 0.1170 H4A H Uiso 0.05710 1.37650 0.23470 1.000 0.0250 H4B H Uiso 0.03510 1.29070 0.24270 1.000 0.0250 H5A H Uiso 0.06040 1.29680 0.33480 1.000 0.0190 H5B H Uiso 0.08950 1.29980 0.29850 1.000 0.0190 H11 H Uiso 0.07850 0.77500 0.30280 1.000 0.0230 H12A H Uiso 0.09340 0.65080 0.20540 1.000 0.0330 H12B H Uiso 0.09790 0.63490 0.27790 1.000 0.0330 H13A H Uiso 0.05330 0.57230 0.20700 1.000 0.0330 H13B H Uiso 0.06110 0.53870 0.27530 1.000 0.0330 H14A H Uiso 0.03460 0.65460 0.31940 1.000 0.0380 H14B H Uiso 0.01670 0.63740 0.25780 1.000 0.0380 H15A H Uiso 0.03790 0.76520 0.20760 1.000 0.0370 H15B H Uiso 0.03410 0.80720 0.27590 1.000 0.0370 H21 H Uiso 0.09710 1.17150 -0.00220 1.000 0.0240 H22A H Uiso 0.05010 1.08380 0.00820 1.000 0.0340 H22B H Uiso 0.05560 1.14790 -0.05220 1.000 0.0340 H23A H Uiso 0.04610 1.00340 -0.09610 1.000 0.0430 H23B H Uiso 0.06070 0.94500 -0.04130 1.000 0.0430 H24A H Uiso 0.08650 1.02450 -0.14550 1.000 0.0470 H24B H Uiso 0.09760 0.93780 -0.10360 1.000 0.0470 H25A H Uiso 0.12670 1.04080 -0.05770 1.000 0.0430 H25B H Uiso 0.11310 1.12920 -0.09410 1.000 0.0430 H31 H Uiso 0.23570 1.06670 0.20660 1.000 0.0340 H32A H Uiso 0.24470 1.04310 0.30620 1.000 0.0550 H1C H Uiso 0.22700 1.26080 0.23580 1.000 0.1070 H2A H Uiso 0.14320 1.25310 0.33820 1.000 0.0630 H33B H Uiso 0.25340 0.84950 0.30150 1.000 0.0960 H34A H Uiso 0.26630 0.82240 0.20650 1.000 0.0920 H34B H Uiso 0.27890 0.92820 0.19820 1.000 0.0920 H35A H Uiso 0.22270 0.86960 0.18370 1.000 0.0520 H35B H Uiso 0.24010 0.94130 0.14060 1.000 0.0520 H41 H Uiso 0.18460 1.16460 0.02770 1.000 0.0340 H42A H Uiso 0.17790 1.00100 -0.04370 1.000 0.0550 H42B H Uiso 0.17830 1.11060 -0.06630 1.000 0.0550 H43A H Uiso 0.22350 0.98150 -0.06190 1.000 0.0950 H43B H Uiso 0.22020 1.07380 -0.10540 1.000 0.0950 H44A H Uiso 0.25510 1.08350 -0.01860 1.000 0.0750 H44B H Uiso 0.23560 1.17580 -0.03020 1.000 0.0750 H45A H Uiso 0.22680 1.13880 0.07090 1.000 0.0760 H45B H Uiso 0.22630 1.02580 0.05670 1.000 0.0760 H51 H Uiso 0.06160 0.75830 0.02490 1.000 0.0240 H52A H Uiso 0.08570 0.78090 -0.06570 1.000 0.0430 H52B H Uiso 0.11090 0.71290 -0.04410 1.000 0.0430 H53A H Uiso 0.08710 0.59780 -0.09300 1.000 0.0480 H53B H Uiso 0.05830 0.65630 -0.08920 1.000 0.0480 H54A H Uiso 0.04580 0.57700 -0.00350 1.000 0.0430 H54B H Uiso 0.07310 0.51090 -0.01160 1.000 0.0430 H55A H Uiso 0.09900 0.60310 0.05210 1.000 0.0330 H55B H Uiso 0.06890 0.62060 0.08280 1.000 0.0330 H61 H Uiso 0.19090 0.75120 0.29150 1.000 0.0390 H62A H Uiso 0.16440 0.80260 0.37450 1.000 0.0640 H62B H Uiso 0.13590 0.76260 0.34520 1.000 0.0640 H63A H Uiso 0.18050 0.65170 0.39670 1.000 0.0810 H63B H Uiso 0.14770 0.63790 0.40900 1.000 0.0810 H64A H Uiso 0.14210 0.54970 0.32470 1.000 0.0650 H64B H Uiso 0.17530 0.53540 0.32760 1.000 0.0650 H65A H Uiso 0.14600 0.64140 0.24130 1.000 0.0440 H65B H Uiso 0.17870 0.61660 0.23980 1.000 0.0440 H71A H Uiso 0.18270 0.72800 0.00740 0.527(12) 0.0590 H72A H Uiso 0.22660 0.74350 0.08620 0.527(12) 0.0460 H72B H Uiso 0.22200 0.79510 0.02110 0.527(12) 0.0460 H73A H Uiso 0.24790 0.63270 0.02860 0.527(12) 0.0640 H73B H Uiso 0.23020 0.66010 -0.03180 0.527(12) 0.0640 H74A H Uiso 0.19920 0.54030 -0.00840 0.527(12) 0.0760 H74B H Uiso 0.21580 0.51750 0.05410 0.527(12) 0.0760 H75A H Uiso 0.18710 0.60730 0.11010 1.000 0.0710 H75B H Uiso 0.16600 0.59800 0.05280 1.000 0.0710 H82 H Uiso 0.02000 1.15760 0.14960 1.000 0.0320 H83 H Uiso -0.01480 1.17420 0.07420 1.000 0.0350 H84 H Uiso -0.00740 1.27590 -0.00820 1.000 0.0360 H85 H Uiso 0.03230 1.36890 -0.01400 1.000 0.0330 H86 H Uiso 0.06640 1.35570 0.06090 1.000 0.0300 H92 H Uiso 0.08690 1.44590 0.16640 1.000 0.0300 H93 H Uiso 0.12740 1.52670 0.14250 1.000 0.0390 H94 H Uiso 0.16770 1.44260 0.11770 1.000 0.0470 H95 H Uiso 0.16640 1.27540 0.11540 1.000 0.0500 H96 H Uiso 0.12620 1.19270 0.14210 1.000 0.0370 H102 H Uiso 0.04730 0.96190 0.31510 1.000 0.0350 H103 H Uiso 0.00690 0.90250 0.35810 1.000 0.0400 H104 H Uiso -0.02660 1.00330 0.39790 1.000 0.0330 H105 H Uiso -0.02030 1.17080 0.38920 1.000 0.0340 H106 H Uiso 0.02160 1.23050 0.35260 1.000 0.0260 H112 H Uiso 0.12090 1.02840 0.29830 1.000 0.0370 H113 H Uiso 0.15540 0.99090 0.37050 1.000 0.0410 H114 H Uiso 0.15230 1.05600 0.46910 1.000 0.0410 H115 H Uiso 0.11580 1.15190 0.49620 1.000 0.0400 H116 H Uiso 0.08080 1.18900 0.42520 1.000 0.0210 H32B H Uiso 0.22150 0.96120 0.31320 1.000 0.0550 H33A H Uiso 0.27680 0.93140 0.29880 1.000 0.0960 H71B H Uiso 0.20770 0.73810 0.06980 0.473(12) 0.0590 H72C H Uiso 0.20790 0.77590 -0.01980 0.473(12) 0.0460 H72D H Uiso 0.17730 0.73460 -0.03320 0.473(12) 0.0460 H73C H Uiso 0.19610 0.59660 -0.05980 0.473(12) 0.0640 H73D H Uiso 0.22660 0.63600 -0.04240 0.473(12) 0.0640 H74C H Uiso 0.22530 0.57060 0.05060 0.473(12) 0.0760 H74D H Uiso 0.20200 0.50160 0.02070 0.473(12) 0.0760 H12C H Uiso 0.04120 0.97610 0.10910 1.000 0.0760 H12D H Uiso 0.01830 0.94950 0.05850 1.000 0.0760 H12E H Uiso 0.03520 0.86640 0.09270 1.000 0.0760 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 Pt1 0.0199(2) 0.0100(2) 0.0130(2) -0.0010(1) 0.0011(2) 0.0012(2) P1 0.0255(12) 0.0116(11) 0.0160(11) 0.0005(9) 0.0020(9) 0.0008(10) P2 0.0228(12) 0.0127(11) 0.0096(10) -0.0001(9) -0.0003(9) 0.0014(9) Si1 0.0197(12) 0.0094(12) 0.0200(14) -0.0007(10) 0.0028(10) -0.0003(10) Si2 0.0224(13) 0.0128(13) 0.0157(13) -0.0013(10) -0.0002(10) -0.0001(11) Si3 0.0185(12) 0.0197(14) 0.0242(14) -0.0026(10) -0.0005(10) -0.0007(11) Si4 0.0230(13) 0.0146(13) 0.0226(14) 0.0009(10) 0.0019(11) -0.0023(11) Si5 0.0248(13) 0.0121(12) 0.0194(13) -0.0047(10) 0.0045(11) -0.0021(11) Si6 0.0190(13) 0.0214(14) 0.0264(14) 0.0051(11) 0.0007(11) 0.0003(11) Si7 0.0233(13) 0.0155(13) 0.0265(14) -0.0023(11) 0.0094(11) 0.0020(11) Si8 0.0294(14) 0.0275(16) 0.0521(19) -0.0143(15) -0.0082(15) 0.0005(13) O1 0.036(4) 0.011(3) 0.023(3) 0.003(2) 0.010(3) 0.007(3) O2 0.038(4) 0.018(3) 0.012(3) -0.004(2) 0.005(3) 0.007(3) O3 0.027(3) 0.014(3) 0.029(4) -0.004(3) -0.002(3) -0.002(3) O4 0.034(3) 0.010(3) 0.017(3) -0.002(2) 0.000(3) -0.001(3) O5 0.038(4) 0.017(3) 0.016(3) -0.001(2) 0.008(3) -0.007(3) O6 0.025(3) 0.028(4) 0.040(4) -0.001(3) 0.000(3) -0.002(3) O7 0.034(4) 0.025(4) 0.025(3) 0.001(3) -0.007(3) -0.003(3) O8 0.030(3) 0.019(3) 0.026(4) -0.001(3) 0.000(3) 0.000(3) O9 0.033(3) 0.018(3) 0.025(3) 0.003(3) 0.011(3) 0.002(3) O10 0.025(3) 0.025(4) 0.029(3) 0.007(3) -0.003(3) -0.002(3) O11 0.029(3) 0.028(3) 0.025(3) 0.000(3) 0.000(3) -0.008(3) O12 0.028(4) 0.026(3) 0.034(4) -0.009(3) -0.003(3) 0.000(3) C1 0.037(7) 0.041(7) 0.135(11) -0.004(7) 0.017(7) -0.006(6) C2 0.035(5) 0.032(6) 0.060(8) -0.012(5) 0.002(5) 0.001(4) C3 0.085(10) 0.078(10) 0.072(8) -0.043(6) -0.051(7) 0.035(8) C4 0.029(5) 0.009(4) 0.025(5) -0.002(3) 0.004(4) 0.003(4) C5 0.023(4) 0.010(3) 0.015(3) -0.008(3) 0.003(3) 0.001(3) C11 0.025(4) 0.013(4) 0.020(4) -0.001(3) 0.004(4) -0.001(4) C12 0.035(5) 0.010(4) 0.038(6) 0.007(4) 0.007(4) 0.006(4) C13 0.038(5) 0.013(4) 0.031(5) 0.003(4) -0.012(4) -0.001(4) C14 0.032(5) 0.029(5) 0.034(6) 0.005(4) 0.007(4) -0.004(4) C15 0.026(4) 0.017(4) 0.051(6) -0.002(4) 0.013(4) 0.003(4) C21 0.032(4) 0.011(4) 0.017(4) 0.001(3) -0.001(3) 0.002(4) C22 0.031(4) 0.028(5) 0.027(5) 0.006(4) 0.000(4) 0.009(5) C23 0.036(5) 0.027(6) 0.043(6) -0.002(4) -0.016(4) -0.002(5) C24 0.069(7) 0.031(6) 0.019(5) 0.001(4) 0.002(4) 0.007(5) C25 0.038(5) 0.056(7) 0.014(4) 0.011(4) 0.003(4) 0.003(5) C31 0.020(4) 0.038(6) 0.028(5) -0.004(4) 0.001(4) -0.003(4) C32 0.029(5) 0.067(8) 0.041(6) -0.007(5) -0.016(5) 0.007(5) C33 0.081(10) 0.096(11) 0.063(7) -0.015(8) -0.019(7) 0.052(8) C34 0.062(8) 0.084(10) 0.085(8) -0.030(8) -0.021(7) 0.036(7) C35 0.030(5) 0.054(7) 0.044(6) -0.012(5) 0.001(4) 0.013(5) C41 0.033(4) 0.027(5) 0.024(4) 0.009(4) 0.001(4) -0.007(5) C42 0.061(6) 0.041(7) 0.034(5) 0.002(5) 0.012(5) -0.017(6) C43 0.083(8) 0.078(10) 0.075(8) 0.001(7) 0.036(7) 0.026(8) C44 0.034(5) 0.081(9) 0.073(8) 0.062(7) 0.011(5) 0.012(6) C45 0.037(5) 0.095(10) 0.059(6) 0.040(7) -0.001(5) -0.017(7) C51 0.029(5) 0.016(4) 0.015(4) -0.002(3) 0.000(4) 0.000(4) C52 0.056(6) 0.029(6) 0.023(5) -0.011(4) 0.007(5) -0.015(5) C53 0.053(7) 0.039(6) 0.027(5) -0.017(4) 0.001(5) -0.015(5) C54 0.041(6) 0.019(5) 0.049(6) -0.010(4) 0.000(5) -0.013(5) C55 0.037(5) 0.018(4) 0.026(4) -0.001(3) -0.003(4) 0.001(4) C61 0.031(5) 0.027(4) 0.039(5) 0.013(4) 0.004(4) 0.003(4) C62 0.073(8) 0.048(6) 0.040(6) 0.017(5) 0.010(6) 0.014(7) C63 0.100(10) 0.051(7) 0.051(6) 0.030(5) 0.014(7) 0.005(8) C64 0.059(7) 0.042(6) 0.062(7) 0.029(5) 0.014(6) 0.005(6) C65 0.030(5) 0.030(5) 0.050(6) 0.015(4) 0.009(5) 0.002(5) C71 0.049(6) 0.027(5) 0.070(7) 0.001(5) 0.034(6) 0.009(5) C74 0.061(8) 0.036(7) 0.093(10) -0.018(6) 0.009(7) 0.017(6) C75 0.050(7) 0.023(5) 0.103(10) -0.001(6) 0.029(7) 0.009(5) C81 0.021(4) 0.015(4) 0.017(4) 0.000(3) 0.000(3) 0.005(3) C82 0.019(4) 0.028(6) 0.033(5) 0.006(4) 0.004(4) 0.005(4) C83 0.024(5) 0.035(6) 0.030(5) -0.003(4) -0.001(4) -0.005(4) C84 0.028(5) 0.029(6) 0.034(5) 0.000(4) -0.003(4) 0.011(4) C85 0.037(5) 0.028(5) 0.018(5) 0.001(4) -0.006(4) 0.004(4) C86 0.034(5) 0.015(5) 0.024(5) 0.000(4) 0.003(4) -0.002(4) C91 0.026(4) 0.010(4) 0.021(5) 0.001(3) 0.001(3) -0.007(3) C92 0.023(4) 0.016(4) 0.035(5) 0.002(4) 0.000(4) 0.004(4) C93 0.040(5) 0.011(5) 0.047(6) 0.008(4) -0.002(5) -0.010(4) C94 0.027(5) 0.029(5) 0.062(7) 0.001(5) 0.000(5) -0.012(4) C95 0.028(5) 0.020(5) 0.076(8) -0.008(5) 0.015(5) -0.008(4) C96 0.031(5) 0.018(5) 0.042(6) -0.011(4) 0.006(4) -0.007(4) C101 0.024(4) 0.010(4) 0.015(4) -0.002(4) 0.000(3) -0.002(3) C102 0.030(5) 0.020(4) 0.036(6) 0.006(4) 0.007(4) 0.000(4) C103 0.034(5) 0.021(5) 0.045(6) 0.008(4) 0.007(5) -0.002(4) C104 0.021(5) 0.033(5) 0.029(5) 0.010(4) 0.002(4) -0.008(4) C105 0.022(5) 0.033(5) 0.030(5) -0.006(4) 0.000(4) 0.005(4) C106 0.023(4) 0.020(5) 0.023(5) -0.001(4) -0.001(4) -0.001(4) C111 0.032(4) 0.019(5) 0.007(4) 0.003(3) 0.003(3) -0.008(4) C112 0.032(5) 0.035(6) 0.026(5) -0.004(4) -0.003(4) 0.000(4) C113 0.038(6) 0.028(6) 0.037(6) -0.007(4) -0.001(4) 0.012(5) C114 0.035(5) 0.041(7) 0.026(5) 0.002(4) -0.013(4) 0.002(5) C115 0.040(6) 0.039(6) 0.020(5) -0.001(4) -0.004(4) -0.002(5) C116 0.026(5) 0.017(5) 0.010(4) -0.003(3) -0.006(3) -0.003(4) N121 0.056(6) 0.043(6) 0.078(8) 0.011(5) 0.025(5) 0.005(5) C122 0.033(6) 0.028(6) 0.049(7) 0.008(5) -0.001(4) 0.001(5) C123 0.044(7) 0.041(7) 0.067(8) -0.001(6) 0.017(5) 0.001(6) #======================================================================= # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.195(2) . . yes Pt1 P2 2.204(2) . . yes Pt1 O1 2.031(6) . . yes Pt1 O2 2.036(4) . . yes P1 C4 1.840(9) . . yes P1 C81 1.809(9) . . yes P1 C91 1.817(9) . . yes P2 C5 1.838(7) . . yes P2 C101 1.813(9) . . yes P2 C111 1.773(9) . . yes Si1 O1 1.573(6) . . yes Si1 O5 1.647(7) . . yes Si1 O6 1.625(7) . . yes Si1 C11 1.851(9) . . yes Si2 O2 1.566(6) . . yes Si2 O3 1.638(6) . . yes Si2 O4 1.638(6) . . yes Si2 C21 1.843(9) . . yes Si3 O7 1.621(7) . . yes Si3 O11 1.627(6) . . yes Si3 O12 1.604(6) . . yes Si3 C31 1.835(9) . . yes Si4 O3 1.609(6) . . yes Si4 O7 1.612(7) . . yes Si4 O9 1.627(6) . . yes Si4 C41 1.847(9) . . yes Si5 O4 1.618(6) . . yes Si5 O5 1.608(7) . . yes Si5 O8 1.621(6) . . yes Si5 C51 1.847(9) . . yes Si6 O6 1.597(7) . . yes Si6 O10 1.624(7) . . yes Si6 O11 1.617(6) . . yes Si6 C61 1.843(10) . . yes Si7 O8 1.619(6) . . yes Si7 O9 1.611(6) . . yes Si7 O10 1.622(7) . . yes Si7 C71 1.831(11) . . yes Si8 O12 1.633(7) . . yes Si8 C1 1.839(13) . . yes Si8 C2 1.837(10) . . yes Si8 C3 1.856(14) . . yes N121 C122 1.121(15) . . yes C4 C5 1.530(12) . . no C11 C15 1.517(12) . . no C11 C12 1.566(12) . . no C12 C13 1.522(13) . . no C13 C14 1.511(13) . . no C14 C15 1.534(14) . . no C21 C22 1.553(13) . . no C21 C25 1.536(13) . . no C22 C23 1.507(14) . . no C23 C24 1.525(14) . . no C24 C25 1.546(14) . . no C31 C35 1.546(14) . . no C31 C32 1.556(14) . . no C32 C33 1.514(19) . . no C33 C34 1.478(19) . . no C34 C35 1.491(17) . . no C41 C42 1.540(14) . . no C41 C45 1.531(13) . . no C42 C43 1.526(18) . . no C43 C44 1.501(19) . . no C44 C45 1.493(18) . . no C51 C55 1.533(12) . . no C51 C52 1.537(12) . . no C52 C53 1.522(14) . . no C53 C54 1.551(14) . . no C54 C55 1.512(14) . . no C61 C65 1.541(14) . . no C61 C62 1.541(15) . . no C62 C63 1.522(18) . . no C63 C64 1.516(17) . . no C64 C65 1.541(15) . . no C71 C72A 1.40(2) . . no C71 C72B 1.35(3) . . no C71 C75 1.512(15) . . no C72A C73A 1.51(3) . . no C72B C73B 1.52(3) . . no C73A C74 1.59(3) . . no C73B C74 1.48(3) . . no C74 C75 1.51(2) . . no C81 C86 1.393(12) . . no C81 C82 1.391(12) . . no C82 C83 1.399(13) . . no C83 C84 1.373(14) . . no C84 C85 1.368(14) . . no C85 C86 1.373(13) . . no C91 C96 1.361(13) . . no C91 C92 1.417(12) . . no C92 C93 1.367(13) . . no C93 C94 1.369(14) . . no C94 C95 1.391(14) . . no C95 C96 1.378(13) . . no C101 C102 1.370(13) . . no C1 H1A 0.9793 . . no C1 H1C 0.9826 . . no C1 H1B 0.9812 . . no C101 C106 1.402(12) . . no C2 H2C 0.9810 . . no C2 H2B 0.9812 . . no C2 H2A 0.9804 . . no C102 C103 1.375(14) . . no C103 C104 1.360(14) . . no C3 H3B 0.9808 . . no C3 H3C 0.9801 . . no C3 H3A 0.9792 . . no C4 H4B 0.9882 . . no C4 H4A 0.9902 . . no C104 C105 1.408(14) . . no C5 H5B 0.9891 . . no C105 C106 1.370(13) . . no C5 H5A 0.9905 . . no C111 C116 1.407(12) . . no C111 C112 1.393(13) . . no C11 H11 1.0012 . . no C112 C113 1.395(14) . . no C12 H12A 0.9899 . . no C12 H12B 0.9893 . . no C113 C114 1.390(14) . . no C13 H13A 0.9894 . . no C13 H13B 0.9903 . . no C14 H14B 0.9906 . . no C114 C115 1.351(14) . . no C14 H14A 0.9885 . . no C15 H15A 0.9894 . . no C15 H15B 0.9908 . . no C115 C116 1.397(13) . . no C21 H21 0.9995 . . no C22 H22A 0.9922 . . no C22 H22B 0.9899 . . no C23 H23B 0.9897 . . no C23 H23A 0.9907 . . no C24 H24B 0.9888 . . no C24 H24A 0.9897 . . no C25 H25A 0.9869 . . no C25 H25B 0.9896 . . no C31 H31 1.0008 . . no C32 H32A 0.9907 . . no C32 H32B 0.9876 . . no C33 H33B 0.9894 . . no C33 H33A 0.9904 . . no C34 H34A 0.9893 . . no C34 H34B 0.9932 . . no C35 H35A 0.9888 . . no C35 H35B 0.9904 . . no C41 H41 1.0002 . . no C42 H42B 0.9896 . . no C42 H42A 0.9888 . . no C43 H43B 0.9907 . . no C43 H43A 0.9899 . . no C44 H44A 0.9876 . . no C44 H44B 0.9905 . . no C45 H45B 0.9900 . . no C45 H45A 0.9904 . . no C51 H51 0.9999 . . no C52 H52B 0.9861 . . no C52 H52A 0.9912 . . no C53 H53A 0.9922 . . no C53 H53B 0.9866 . . no C54 H54B 0.9891 . . no C54 H54A 0.9945 . . no C55 H55A 0.9863 . . no C55 H55B 0.9918 . . no C61 H61 0.9996 . . no C62 H62B 0.9916 . . no C62 H62A 0.9899 . . no C63 H63A 0.9907 . . no C63 H63B 0.9883 . . no C64 H64A 0.9884 . . no C64 H64B 0.9902 . . no C65 H65B 0.9884 . . no C65 H65A 0.9909 . . no C71 H71A 1.0021 . . no C71 H71B 0.9979 . . no C72A H72B 0.9899 . . no C72A H72A 0.9871 . . no C72B H72D 0.9902 . . no C72B H72C 0.9898 . . no C73A H73B 0.9911 . . no C73A H73A 0.9877 . . no C73B H73C 0.9910 . . no C73B H73D 0.9908 . . no C74 H74C 0.9886 . . no C74 H74D 0.9895 . . no C74 H74B 0.9895 . . no C74 H74A 0.9909 . . no C75 H75B 0.9904 . . no C75 H75A 0.9908 . . no C82 H82 0.9509 . . no C83 H83 0.9511 . . no C84 H84 0.9499 . . no C85 H85 0.9490 . . no C86 H86 0.9494 . . no C92 H92 0.9487 . . no C93 H93 0.9497 . . no C94 H94 0.9537 . . no C95 H95 0.9512 . . no C96 H96 0.9496 . . no C102 H102 0.9494 . . no C103 H103 0.9498 . . no C104 H104 0.9480 . . no C105 H105 0.9495 . . no C106 H106 0.9496 . . no C112 H112 0.9488 . . no C113 H113 0.9489 . . no C114 H114 0.9473 . . no C115 H115 0.9517 . . no C116 H116 0.9489 . . no C122 C123 1.435(15) . . no C123 H12C 0.9799 . . no C123 H12D 0.9803 . . no C123 H12E 0.9806 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 86.91(8) . . . yes P1 Pt1 O1 175.03(19) . . . yes P1 Pt1 O2 90.15(17) . . . yes P2 Pt1 O1 92.49(19) . . . yes P2 Pt1 O2 176.59(18) . . . yes O1 Pt1 O2 90.3(2) . . . yes Pt1 P1 C4 108.1(3) . . . yes Pt1 P1 C81 113.4(3) . . . yes Pt1 P1 C91 115.3(3) . . . yes C4 P1 C81 104.7(4) . . . yes C4 P1 C91 106.5(4) . . . yes C81 P1 C91 108.1(4) . . . yes Pt1 P2 C5 108.0(3) . . . yes Pt1 P2 C101 113.2(3) . . . yes Pt1 P2 C111 117.8(3) . . . yes C5 P2 C101 106.8(4) . . . yes C5 P2 C111 105.2(4) . . . yes C101 P2 C111 105.0(4) . . . yes O1 Si1 O5 115.1(3) . . . yes O1 Si1 O6 111.9(4) . . . yes O1 Si1 C11 109.9(4) . . . yes O5 Si1 O6 106.1(3) . . . yes O5 Si1 C11 105.7(4) . . . yes O6 Si1 C11 107.6(4) . . . yes O2 Si2 O3 113.2(3) . . . yes O2 Si2 O4 111.0(3) . . . yes O2 Si2 C21 111.1(4) . . . yes O3 Si2 O4 106.2(3) . . . yes O3 Si2 C21 107.4(4) . . . yes O4 Si2 C21 107.6(3) . . . yes O7 Si3 O11 110.0(3) . . . yes O7 Si3 O12 108.0(3) . . . yes O7 Si3 C31 111.3(4) . . . yes O11 Si3 O12 107.0(3) . . . yes O11 Si3 C31 109.0(4) . . . yes O12 Si3 C31 111.3(4) . . . yes O3 Si4 O7 108.2(3) . . . yes O3 Si4 O9 109.8(3) . . . yes O3 Si4 C41 111.9(4) . . . yes O7 Si4 O9 109.7(3) . . . yes O7 Si4 C41 108.5(4) . . . yes O9 Si4 C41 108.7(4) . . . yes O4 Si5 O5 111.5(3) . . . yes O4 Si5 O8 108.8(3) . . . yes O4 Si5 C51 108.3(3) . . . yes O5 Si5 O8 110.6(3) . . . yes O5 Si5 C51 108.8(4) . . . yes O8 Si5 C51 108.8(4) . . . yes O6 Si6 O10 110.8(3) . . . yes O6 Si6 O11 108.4(4) . . . yes O6 Si6 C61 111.2(4) . . . yes O10 Si6 O11 108.8(3) . . . yes O10 Si6 C61 107.0(4) . . . yes O11 Si6 C61 110.6(4) . . . yes O8 Si7 O9 110.1(3) . . . yes O8 Si7 O10 109.9(3) . . . yes O8 Si7 C71 108.7(4) . . . yes O9 Si7 O10 108.9(3) . . . yes O9 Si7 C71 109.7(4) . . . yes O10 Si7 C71 109.5(5) . . . yes O12 Si8 C1 109.1(5) . . . yes O12 Si8 C2 108.3(4) . . . yes O12 Si8 C3 109.0(5) . . . yes C1 Si8 C2 109.4(5) . . . yes C1 Si8 C3 110.8(6) . . . yes C2 Si8 C3 110.2(6) . . . yes Pt1 O1 Si1 146.3(4) . . . yes Pt1 O2 Si2 148.3(4) . . . yes Si2 O3 Si4 152.2(4) . . . yes Si2 O4 Si5 140.1(3) . . . yes Si1 O5 Si5 147.3(4) . . . yes Si1 O6 Si6 170.3(5) . . . yes Si3 O7 Si4 158.5(4) . . . yes Si5 O8 Si7 143.8(4) . . . yes Si4 O9 Si7 146.2(4) . . . yes Si6 O10 Si7 143.8(4) . . . yes Si3 O11 Si6 143.2(5) . . . yes Si3 O12 Si8 152.8(5) . . . yes P1 C4 C5 106.6(6) . . . yes P2 C5 C4 108.4(5) . . . yes Si1 C11 C12 114.6(6) . . . yes Si1 C11 C15 115.8(6) . . . yes C12 C11 C15 104.3(7) . . . no C11 C12 C13 105.5(7) . . . no C12 C13 C14 107.5(7) . . . no C13 C14 C15 102.4(8) . . . no C11 C15 C14 104.6(7) . . . no Si2 C21 C22 113.9(6) . . . yes Si2 C21 C25 113.9(6) . . . yes C22 C21 C25 103.7(7) . . . no C21 C22 C23 102.9(7) . . . no C22 C23 C24 106.5(8) . . . no C23 C24 C25 106.1(7) . . . no C21 C25 C24 105.9(7) . . . no Si3 C31 C32 113.8(6) . . . yes Si3 C31 C35 116.4(6) . . . yes C32 C31 C35 102.5(8) . . . no C31 C32 C33 107.3(9) . . . no C32 C33 C34 107.3(11) . . . no C33 C34 C35 106.6(11) . . . no C31 C35 C34 105.6(9) . . . no Si4 C41 C42 114.2(7) . . . yes Si4 C41 C45 114.0(7) . . . yes C42 C41 C45 104.1(8) . . . no C41 C42 C43 105.5(9) . . . no C42 C43 C44 105.8(11) . . . no C43 C44 C45 101.9(10) . . . no C41 C45 C44 105.1(9) . . . no Si5 C51 C52 115.5(6) . . . yes Si5 C51 C55 117.4(6) . . . yes C52 C51 C55 100.5(7) . . . no C51 C52 C53 105.0(7) . . . no C52 C53 C54 105.9(7) . . . no C53 C54 C55 104.9(7) . . . no C51 C55 C54 104.5(7) . . . no Si6 C61 C62 115.8(7) . . . yes Si6 C61 C65 112.7(6) . . . yes C62 C61 C65 102.2(8) . . . no C61 C62 C63 104.0(10) . . . no C62 C63 C64 105.1(10) . . . no C63 C64 C65 106.5(9) . . . no C61 C65 C64 106.4(8) . . . no Si7 C71 C72A 124.5(11) . . . yes Si7 C71 C75 115.7(9) . . . yes Si7 C71 C72B 125.2(12) . . . yes C72A C71 C75 106.3(12) . . . no C72B C71 C75 103.5(13) . . . no C71 C72A C73A 106.8(16) . . . no C71 C72B C73B 108.8(18) . . . no C72A C73A C74 103.5(17) . . . no C72B C73B C74 106.3(19) . . . no C73A C74 C75 105.0(12) . . . no C73B C74 C75 100.4(14) . . . no C71 C75 C74 104.1(11) . . . no P1 C81 C82 116.7(7) . . . yes C82 C81 C86 118.8(8) . . . no P1 C81 C86 124.5(7) . . . yes C81 C82 C83 120.0(8) . . . no C82 C83 C84 119.3(9) . . . no C83 C84 C85 121.3(9) . . . no C84 C85 C86 119.6(9) . . . no C81 C86 C85 121.0(8) . . . no P1 C91 C96 118.8(7) . . . yes P1 C91 C92 121.9(6) . . . yes C92 C91 C96 119.2(8) . . . no C91 C92 C93 120.3(8) . . . no C92 C93 C94 120.4(9) . . . no C93 C94 C95 119.0(9) . . . no C94 C95 C96 121.4(9) . . . no C91 C96 C95 119.6(9) . . . no P2 C101 C102 117.9(7) . . . yes Si8 C1 H1A 109.54 . . . no Si8 C1 H1B 109.45 . . . no Si8 C1 H1C 109.54 . . . no H1A C1 H1B 109.51 . . . no H1A C1 H1C 109.35 . . . no H1B C1 H1C 109.43 . . . no P2 C101 C106 123.2(6) . . . yes C102 C101 C106 118.9(8) . . . no Si8 C2 H2C 109.69 . . . no H2A C2 H2B 109.38 . . . no H2A C2 H2C 109.18 . . . no H2B C2 H2C 109.42 . . . no C101 C102 C103 120.3(9) . . . no Si8 C2 H2A 109.47 . . . no Si8 C2 H2B 109.69 . . . no Si8 C3 H3A 109.43 . . . no C102 C103 C104 121.7(9) . . . no H3B C3 H3C 109.54 . . . no Si8 C3 H3B 109.38 . . . no Si8 C3 H3C 109.52 . . . no H3A C3 H3B 109.50 . . . no H3A C3 H3C 109.46 . . . no C5 C4 H4A 110.37 . . . no C5 C4 H4B 110.40 . . . no P1 C4 H4B 110.44 . . . no C103 C104 C105 118.6(9) . . . no P1 C4 H4A 110.29 . . . no H4A C4 H4B 108.72 . . . no C104 C105 C106 119.9(8) . . . no P2 C5 H5A 109.96 . . . no P2 C5 H5B 109.99 . . . no C4 C5 H5A 109.95 . . . no C4 C5 H5B 110.08 . . . no H5A C5 H5B 108.43 . . . no C101 C106 C105 120.4(8) . . . no Si1 C11 H11 107.27 . . . no P2 C111 C112 121.2(7) . . . yes P2 C111 C116 121.1(7) . . . yes C112 C111 C116 117.7(8) . . . no C15 C11 H11 107.15 . . . no C12 C11 H11 107.24 . . . no C11 C12 H12B 110.66 . . . no C111 C112 C113 121.9(8) . . . no H12A C12 H12B 108.96 . . . no C13 C12 H12A 110.52 . . . no C13 C12 H12B 110.59 . . . no C11 C12 H12A 110.60 . . . no C112 C113 C114 118.5(9) . . . no H13A C13 H13B 108.41 . . . no C12 C13 H13B 110.28 . . . no C14 C13 H13A 110.41 . . . no C12 C13 H13A 110.13 . . . no C14 C13 H13B 110.12 . . . no C13 C14 H14B 111.26 . . . no C15 C14 H14A 111.33 . . . no C113 C114 C115 121.1(9) . . . no C13 C14 H14A 111.46 . . . no H14A C14 H14B 109.11 . . . no C15 C14 H14B 111.20 . . . no H15A C15 H15B 108.90 . . . no C114 C115 C116 120.8(8) . . . no C11 C15 H15A 110.87 . . . no C11 C15 H15B 110.78 . . . no C14 C15 H15A 110.82 . . . no C14 C15 H15B 110.86 . . . no C111 C116 C115 120.1(8) . . . no Si2 C21 H21 108.36 . . . no C22 C21 H21 108.47 . . . no C25 C21 H21 108.32 . . . no C21 C22 H22A 111.21 . . . no C21 C22 H22B 111.20 . . . no C23 C22 H22A 111.14 . . . no C23 C22 H22B 111.19 . . . no H22A C22 H22B 109.11 . . . no C22 C23 H23A 110.32 . . . no C22 C23 H23B 110.52 . . . no C24 C23 H23A 110.42 . . . no C24 C23 H23B 110.51 . . . no H23A C23 H23B 108.58 . . . no C23 C24 H24A 110.54 . . . no C23 C24 H24B 110.32 . . . no C25 C24 H24A 110.53 . . . no C25 C24 H24B 110.54 . . . no H24A C24 H24B 108.81 . . . no C21 C25 H25A 110.60 . . . no C21 C25 H25B 110.43 . . . no C24 C25 H25A 110.56 . . . no C24 C25 H25B 110.53 . . . no H25A C25 H25B 108.85 . . . no Si3 C31 H31 107.98 . . . no C32 C31 H31 107.97 . . . no C35 C31 H31 107.86 . . . no C31 C32 H32A 110.24 . . . no C31 C32 H32B 110.44 . . . no C33 C32 H32A 110.21 . . . no C33 C32 H32B 110.20 . . . no H32A C32 H32B 108.41 . . . no C32 C33 H33A 110.25 . . . no C32 C33 H33B 110.48 . . . no C34 C33 H33A 110.29 . . . no C34 C33 H33B 110.22 . . . no H33A C33 H33B 108.35 . . . no C33 C34 H34A 110.41 . . . no C33 C34 H34B 110.27 . . . no C35 C34 H34A 110.57 . . . no C35 C34 H34B 110.55 . . . no H34A C34 H34B 108.46 . . . no C31 C35 H35A 110.76 . . . no C31 C35 H35B 110.66 . . . no C34 C35 H35A 110.50 . . . no C34 C35 H35B 110.69 . . . no H35A C35 H35B 108.68 . . . no Si4 C41 H41 108.13 . . . no C42 C41 H41 108.05 . . . no C45 C41 H41 108.09 . . . no C41 C42 H42A 110.57 . . . no C41 C42 H42B 110.58 . . . no C43 C42 H42A 110.48 . . . no C43 C42 H42B 110.71 . . . no H42A C42 H42B 108.94 . . . no C42 C43 H43A 110.53 . . . no C42 C43 H43B 110.39 . . . no C44 C43 H43A 110.67 . . . no C44 C43 H43B 110.68 . . . no H43A C43 H43B 108.71 . . . no C43 C44 H44A 111.37 . . . no C43 C44 H44B 111.39 . . . no C45 C44 H44A 111.35 . . . no C45 C44 H44B 111.27 . . . no H44A C44 H44B 109.39 . . . no C41 C45 H45A 110.78 . . . no C41 C45 H45B 110.86 . . . no C44 C45 H45A 110.71 . . . no C44 C45 H45B 110.52 . . . no H45A C45 H45B 108.82 . . . no Si5 C51 H51 107.55 . . . no C52 C51 H51 107.56 . . . no C55 C51 H51 107.65 . . . no C51 C52 H52A 110.73 . . . no C51 C52 H52B 110.85 . . . no C53 C52 H52A 110.52 . . . no C53 C52 H52B 110.82 . . . no H52A C52 H52B 108.93 . . . no C52 C53 H53A 110.30 . . . no C52 C53 H53B 110.62 . . . no C54 C53 H53A 110.50 . . . no C54 C53 H53B 110.78 . . . no H53A C53 H53B 108.74 . . . no C53 C54 H54A 110.65 . . . no C53 C54 H54B 110.89 . . . no C55 C54 H54A 110.71 . . . no C55 C54 H54B 110.84 . . . no H54A C54 H54B 108.84 . . . no C51 C55 H55A 111.00 . . . no C51 C55 H55B 110.83 . . . no C54 C55 H55A 110.71 . . . no C54 C55 H55B 110.66 . . . no H55A C55 H55B 109.05 . . . no Si6 C61 H61 108.57 . . . no C62 C61 H61 108.61 . . . no C65 C61 H61 108.57 . . . no C61 C62 H62A 111.16 . . . no C61 C62 H62B 111.14 . . . no C63 C62 H62A 110.96 . . . no C63 C62 H62B 110.85 . . . no H62A C62 H62B 108.69 . . . no C62 C63 H63A 110.66 . . . no C62 C63 H63B 110.95 . . . no C64 C63 H63A 110.63 . . . no C64 C63 H63B 110.69 . . . no H63A C63 H63B 108.75 . . . no C63 C64 H64A 110.42 . . . no C63 C64 H64B 110.40 . . . no C65 C64 H64A 110.53 . . . no C65 C64 H64B 110.29 . . . no H64A C64 H64B 108.65 . . . no C61 C65 H65A 110.47 . . . no C61 C65 H65B 110.58 . . . no C64 C65 H65A 110.27 . . . no C64 C65 H65B 110.45 . . . no H65A C65 H65B 108.63 . . . no Si7 C71 H71A 102.28 . . . no Si7 C71 H71B 103.24 . . . no C72A C71 H71A 102.47 . . . no C75 C71 H71A 102.22 . . . no C75 C71 H71B 103.32 . . . no C72B C71 H71B 103.25 . . . no C71 C72A H72A 110.18 . . . no C71 C72A H72B 110.18 . . . no C73A C72A H72A 110.41 . . . no C73A C72A H72B 110.43 . . . no H72A C72A H72B 108.80 . . . no C73B C72B H72D 109.96 . . . no H72C C72B H72D 108.30 . . . no C73B C72B H72C 109.95 . . . no C71 C72B H72C 109.89 . . . no C71 C72B H72D 109.90 . . . no C74 C73A H73B 111.00 . . . no C74 C73A H73A 111.08 . . . no H73A C73A H73B 109.23 . . . no C72A C73A H73B 110.96 . . . no C72A C73A H73A 111.01 . . . no H73C C73B H73D 108.61 . . . no C72B C73B H73D 110.48 . . . no C74 C73B H73C 110.53 . . . no C74 C73B H73D 110.50 . . . no C72B C73B H73C 110.47 . . . no C75 C74 H74B 110.78 . . . no C75 C74 H74C 111.78 . . . no C75 C74 H74D 111.72 . . . no H74A C74 H74B 108.82 . . . no C73B C74 H74C 111.67 . . . no C73B C74 H74D 111.64 . . . no C75 C74 H74A 110.65 . . . no C73A C74 H74A 110.81 . . . no C73A C74 H74B 110.82 . . . no H74C C74 H74D 109.41 . . . no C71 C75 H75B 111.04 . . . no C74 C75 H75A 110.77 . . . no H75A C75 H75B 109.06 . . . no C74 C75 H75B 111.03 . . . no C71 C75 H75A 110.76 . . . no C81 C82 H82 120.03 . . . no C83 C82 H82 119.99 . . . no C84 C83 H83 120.34 . . . no C82 C83 H83 120.37 . . . no C85 C84 H84 119.40 . . . no C83 C84 H84 119.28 . . . no C84 C85 H85 120.12 . . . no C86 C85 H85 120.29 . . . no C81 C86 H86 119.42 . . . no C85 C86 H86 119.55 . . . no C93 C92 H92 119.76 . . . no C91 C92 H92 119.93 . . . no C92 C93 H93 119.66 . . . no C94 C93 H93 119.93 . . . no C93 C94 H94 120.55 . . . no C95 C94 H94 120.48 . . . no C96 C95 H95 119.32 . . . no C94 C95 H95 119.27 . . . no C91 C96 H96 120.06 . . . no C95 C96 H96 120.33 . . . no C103 C102 H102 119.80 . . . no C101 C102 H102 119.86 . . . no C102 C103 H103 119.04 . . . no C104 C103 H103 119.25 . . . no C103 C104 H104 120.65 . . . no C105 C104 H104 120.76 . . . no C106 C105 H105 120.03 . . . no C104 C105 H105 120.08 . . . no C101 C106 H106 119.72 . . . no C105 C106 H106 119.88 . . . no C113 C112 H112 119.15 . . . no C111 C112 H112 118.96 . . . no C114 C113 H113 120.66 . . . no C112 C113 H113 120.87 . . . no C113 C114 H114 119.44 . . . no C115 C114 H114 119.46 . . . no C114 C115 H115 119.37 . . . no C116 C115 H115 119.85 . . . no C111 C116 H116 120.09 . . . no C115 C116 H116 119.83 . . . no N121 C122 C123 178.5(11) . . . yes C122 C123 H12C 109.36 . . . no C122 C123 H12D 109.38 . . . no C122 C123 H12E 109.51 . . . no H12C C123 H12D 109.54 . . . no H12C C123 H12E 109.53 . . . no H12D C123 H12E 109.51 . . . no #=END data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H74 O12 Si8' _chemical_formula_sum 'C38 H74 O12 Si8' _chemical_formula_weight 947.69 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' _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 14.5232(12) _cell_length_b 15.7325(8) _cell_length_c 23.4701(15) _cell_angle_alpha 102.358(5) _cell_angle_beta 97.036(6) _cell_angle_gamma 92.941(5) _cell_volume 5182.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.45 _cell_measurement_theta_max 13.75 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_reflns_number 17993 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 25.34 _reflns_number_total 17304 _reflns_number_gt 7874 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'locally modified CAD-4 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1998)' _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 constraint _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17304 _refine_ls_number_parameters 669 _refine_ls_number_restraints 912 _refine_ls_R_factor_all 0.2381 _refine_ls_R_factor_gt 0.1423 _refine_ls_wR_factor_ref 0.4489 _refine_ls_wR_factor_gt 0.3882 _refine_ls_goodness_of_fit_ref 1.364 _refine_ls_restrained_S_all 1.385 _refine_ls_shift/su_max 0.828 _refine_ls_shift/su_mean 0.029 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 Si11 Si 0.1215(2) 0.86548(19) -0.09659(13) 0.0640(8) Uani 1 1 d . . . Si21 Si 0.2194(2) 1.01681(18) 0.08209(13) 0.0610(8) Uani 1 1 d . . . Si31 Si 0.1125(2) 0.6903(2) 0.06614(15) 0.0700(9) Uani 1 1 d . . . Si41 Si 0.2671(2) 0.84088(19) 0.11985(13) 0.0633(8) Uani 1 1 d . . . Si51 Si 0.31399(19) 0.95687(17) -0.02845(13) 0.0582(7) Uani 1 1 d . . . Si61 Si 0.1676(2) 0.69552(19) -0.05657(14) 0.0667(8) Uani 1 1 d . . . Si71 Si 0.36137(18) 0.78689(17) 0.00956(12) 0.0568(7) Uani 1 1 d . . . Si81 Si -0.0821(2) 0.7481(2) 0.08702(18) 0.0884(11) Uani 1 1 d . . . O11 O 0.0508(5) 0.9199(6) -0.0549(4) 0.101(3) Uani 1 1 d . . . H11 H 0.0075 0.9349 -0.0761 0.050 Uiso 1 1 calc RD . . O21 O 0.1095(5) 1.0051(6) 0.0570(4) 0.090(2) Uani 1 1 d . . . H21 H 0.0994 1.0333 0.0310 0.050 Uiso 1 1 calc R . . O31 O 0.2431(5) 0.9355(4) 0.1099(3) 0.078(2) Uani 1 1 d . . . O41 O 0.2786(4) 1.0169(4) 0.0282(3) 0.0651(18) Uani 1 1 d . . . O51 O 0.2242(5) 0.9129(4) -0.0758(3) 0.0671(18) Uani 1 1 d . . . O61 O 0.1210(5) 0.7689(5) -0.0862(3) 0.076(2) Uani 1 1 d . . . O71 O 0.1713(5) 0.7776(5) 0.1010(4) 0.084(2) Uani 1 1 d . . . O81 O 0.3711(4) 0.8795(4) -0.0077(3) 0.0671(18) Uani 1 1 d . . . O91 O 0.3415(5) 0.8018(4) 0.0771(3) 0.0660(18) Uani 1 1 d . . . O101 O 0.2754(4) 0.7273(4) -0.0311(3) 0.0685(19) Uani 1 1 d . . . O111 O 0.1113(5) 0.6828(5) -0.0036(3) 0.084(2) Uani 1 1 d . . . O121 O 0.0094(5) 0.6951(5) 0.0809(4) 0.095(3) Uani 1 1 d . . . C11 C -0.0881(15) 0.7886(14) 0.1625(8) 0.197(9) Uiso 1 1 d . . . H31 H -0.0882 0.7405 0.1824 0.050 Uiso 1 1 calc R . . H41 H -0.1447 0.8180 0.1670 0.050 Uiso 1 1 calc R . . H51 H -0.0346 0.8295 0.1797 0.050 Uiso 1 1 calc R . . C21 C -0.0850(12) 0.8334(10) 0.0447(7) 0.135(6) Uiso 1 1 d . . . H61 H -0.0810 0.8075 0.0037 0.050 Uiso 1 1 calc R . . H71 H -0.0328 0.8764 0.0604 0.050 Uiso 1 1 calc R . . H81 H -0.1428 0.8614 0.0475 0.050 Uiso 1 1 calc R . . C31 C -0.1841(15) 0.6797(14) 0.0631(11) 0.239(12) Uiso 1 1 d . . . H91 H -0.1859 0.6522 0.0218 0.050 Uiso 1 1 calc R . . H101 H -0.2375 0.7138 0.0681 0.050 Uiso 1 1 calc R . . H111 H -0.1856 0.6352 0.0859 0.050 Uiso 1 1 calc R . . C111 C 0.0904(11) 0.8625(9) -0.1752(6) 0.119(5) Uiso 1 1 d D . . H121 H 0.1427 0.8376 -0.1948 0.050 Uiso 1 1 calc R . . C121 C 0.0064(13) 0.8144(11) -0.2087(8) 0.181(8) Uiso 1 1 d D . . H131 H -0.0472 0.8252 -0.1874 0.050 Uiso 1 1 calc R . . H141 H 0.0135 0.7515 -0.2185 0.050 Uiso 1 1 calc R . . C131 C -0.003(2) 0.8511(14) -0.2621(8) 0.35(2) Uiso 1 1 d D . . H151 H 0.0420 0.8281 -0.2885 0.050 Uiso 1 1 calc R . . H161 H -0.0658 0.8386 -0.2836 0.050 Uiso 1 1 calc R . . C141 C 0.0168(19) 0.9380(13) -0.2390(10) 0.280(15) Uiso 1 1 d D . . H171 H -0.0401 0.9650 -0.2290 0.050 Uiso 1 1 calc R . . H181 H 0.0418 0.9661 -0.2679 0.050 Uiso 1 1 calc R . . C151 C 0.0835(17) 0.9498(11) -0.1874(10) 0.238(12) Uiso 1 1 d D . . H191 H 0.0625 0.9899 -0.1543 0.050 Uiso 1 1 calc R . . H201 H 0.1438 0.9735 -0.1943 0.050 Uiso 1 1 calc R . . C211 C 0.2422(9) 1.1199(7) 0.1365(6) 0.094(4) Uiso 1 1 d D . . H211 H 0.2013 1.1141 0.1664 0.050 Uiso 1 1 calc R . . C221 C 0.2156(10) 1.2007(7) 0.1173(6) 0.108(4) Uiso 1 1 d D . . H221 H 0.2456 1.2076 0.0831 0.050 Uiso 1 1 calc R . . H231 H 0.1480 1.1991 0.1069 0.050 Uiso 1 1 calc R . . C231 C 0.2480(12) 1.2706(9) 0.1675(7) 0.163(7) Uiso 1 1 d D . . H241 H 0.2640 1.3245 0.1551 0.050 Uiso 1 1 calc R . . H251 H 0.2004 1.2816 0.1938 0.050 Uiso 1 1 calc R . . C241 C 0.3263(13) 1.2416(10) 0.1954(9) 0.198(9) Uiso 1 1 d D . . H261 H 0.3226 1.2504 0.2376 0.050 Uiso 1 1 calc R . . H271 H 0.3823 1.2753 0.1904 0.050 Uiso 1 1 calc R . . C251 C 0.3325(12) 1.1482(10) 0.1701(10) 0.200(9) Uiso 1 1 d D . . H281 H 0.3816 1.1400 0.1447 0.050 Uiso 1 1 calc R . . H291 H 0.3453 1.1160 0.2012 0.050 Uiso 1 1 calc R . . C311 C 0.1580(9) 0.5945(8) 0.0894(5) 0.099(4) Uiso 1 1 d D . . H301 H 0.1124 0.5454 0.0685 0.050 Uiso 1 1 calc R . . C321 C 0.1604(10) 0.5930(9) 0.1525(5) 0.116(5) Uiso 1 1 d D . . H311 H 0.1941 0.6459 0.1776 0.050 Uiso 1 1 calc R . . H321 H 0.0973 0.5880 0.1628 0.050 Uiso 1 1 calc R . . C331 C 0.2091(14) 0.5158(12) 0.1588(8) 0.175(8) Uiso 1 1 d D . . H331 H 0.2551 0.5287 0.1943 0.050 Uiso 1 1 calc R . . H341 H 0.1651 0.4676 0.1610 0.050 Uiso 1 1 calc R . . C341 C 0.2516(19) 0.4952(14) 0.1094(10) 0.292(16) Uiso 1 1 d D . . H351 H 0.2211 0.4407 0.0841 0.050 Uiso 1 1 calc R . . H361 H 0.3167 0.4855 0.1207 0.050 Uiso 1 1 calc R . . C351 C 0.2477(12) 0.5647(12) 0.0759(8) 0.172(8) Uiso 1 1 d D . . H371 H 0.2985 0.6106 0.0908 0.050 Uiso 1 1 calc R . . H381 H 0.2476 0.5417 0.0337 0.050 Uiso 1 1 calc R . . C411 C 0.3082(9) 0.8439(9) 0.1954(5) 0.102(4) Uiso 1 1 d D . . H391 H 0.3175 0.7828 0.1978 0.050 Uiso 1 1 calc R . . C421 C 0.3934(11) 0.8948(13) 0.2243(7) 0.173(8) Uiso 1 1 d D . . H401 H 0.3929 0.9556 0.2204 0.050 Uiso 1 1 calc R . . H411 H 0.4483 0.8695 0.2093 0.050 Uiso 1 1 calc R . . C431 C 0.3886(16) 0.887(3) 0.2853(9) 1.15(15) Uiso 1 1 d D . . H421 H 0.3993 0.8280 0.2903 0.050 Uiso 1 1 calc R . . H431 H 0.4334 0.9292 0.3134 0.050 Uiso 1 1 calc R . . C441 C 0.2988(15) 0.906(2) 0.2912(8) 0.37(2) Uiso 1 1 d D . . H441 H 0.2964 0.9694 0.3037 0.050 Uiso 1 1 calc R . . H451 H 0.2768 0.8790 0.3214 0.050 Uiso 1 1 calc R . . C451 C 0.2397(10) 0.8746(13) 0.2366(7) 0.160(7) Uiso 1 1 d D . . H461 H 0.2052 0.9213 0.2246 0.050 Uiso 1 1 calc R . . H471 H 0.1956 0.8266 0.2389 0.050 Uiso 1 1 calc R . . C511 C 0.3887(7) 1.0204(6) -0.0640(4) 0.063(3) Uiso 1 1 d D . . H481 H 0.4382 1.0532 -0.0332 0.050 Uiso 1 1 calc R . . C521 C 0.3391(8) 1.0859(7) -0.0923(5) 0.080(3) Uiso 1 1 d D . . H491 H 0.2723 1.0682 -0.1026 0.050 Uiso 1 1 calc R . . H501 H 0.3473 1.1439 -0.0659 0.050 Uiso 1 1 calc R . . C531 C 0.3833(12) 1.0859(9) -0.1458(6) 0.133(6) Uiso 1 1 d D . . H511 H 0.3386 1.0980 -0.1773 0.050 Uiso 1 1 calc R . . H521 H 0.4362 1.1300 -0.1374 0.050 Uiso 1 1 calc R . . C541 C 0.4127(15) 1.0027(11) -0.1616(6) 0.178(8) Uiso 1 1 d D . . H531 H 0.4678 1.0050 -0.1817 0.050 Uiso 1 1 calc R . . H541 H 0.3635 0.9647 -0.1890 0.050 Uiso 1 1 calc R . . C551 C 0.4348(9) 0.9669(8) -0.1102(5) 0.098(4) Uiso 1 1 d D . . H551 H 0.5023 0.9712 -0.0984 0.050 Uiso 1 1 calc R . . H561 H 0.4111 0.9055 -0.1181 0.050 Uiso 1 1 calc R . . C611 C 0.1620(8) 0.5915(7) -0.1114(5) 0.083(3) Uiso 1 1 d D . . H571 H 0.1912 0.5486 -0.0910 0.050 Uiso 1 1 calc R . . C621 C 0.2116(9) 0.5947(9) -0.1627(5) 0.111(4) Uiso 1 1 d D . . H581 H 0.2229 0.6553 -0.1660 0.050 Uiso 1 1 calc R . . H591 H 0.2716 0.5695 -0.1580 0.050 Uiso 1 1 calc R . . C631 C 0.1527(11) 0.5444(11) -0.2154(6) 0.149(6) Uiso 1 1 d D . . H601 H 0.1352 0.5819 -0.2427 0.050 Uiso 1 1 calc R . . H611 H 0.1858 0.4966 -0.2356 0.050 Uiso 1 1 calc R . . C641 C 0.0758(12) 0.5123(13) -0.1968(7) 0.189(9) Uiso 1 1 d D . . H621 H 0.0792 0.4495 -0.1994 0.050 Uiso 1 1 calc R . . H631 H 0.0204 0.5201 -0.2229 0.050 Uiso 1 1 calc R . . C651 C 0.0669(8) 0.5551(9) -0.1366(6) 0.114(5) Uiso 1 1 d D . . H641 H 0.0443 0.5132 -0.1150 0.050 Uiso 1 1 calc R . . H651 H 0.0241 0.6014 -0.1357 0.050 Uiso 1 1 calc R . . C711 C 0.4679(7) 0.7317(5) -0.0005(4) 0.061(3) Uiso 1 1 d D . . H661 H 0.5172 0.7620 0.0314 0.050 Uiso 1 1 calc R . . C721 C 0.4631(8) 0.6374(6) 0.0002(5) 0.079(3) Uiso 1 1 d D . . H671 H 0.4716 0.6293 0.0407 0.050 Uiso 1 1 calc R . . H681 H 0.4028 0.6084 -0.0198 0.050 Uiso 1 1 calc R . . C731 C 0.5392(10) 0.6015(8) -0.0315(6) 0.114(5) Uiso 1 1 d D . . H691 H 0.5958 0.6026 -0.0038 0.050 Uiso 1 1 calc R . . H701 H 0.5216 0.5411 -0.0529 0.050 Uiso 1 1 calc R . . C741 C 0.5536(11) 0.6547(9) -0.0704(6) 0.126(5) Uiso 1 1 d D . . H711 H 0.5331 0.6221 -0.1109 0.050 Uiso 1 1 calc R . . H721 H 0.6202 0.6721 -0.0668 0.050 Uiso 1 1 calc R . . C751 C 0.5027(8) 0.7315(7) -0.0580(5) 0.084(3) Uiso 1 1 d D . . H731 H 0.4505 0.7290 -0.0892 0.050 Uiso 1 1 calc R . . H741 H 0.5434 0.7843 -0.0551 0.050 Uiso 1 1 calc R . . Si12 Si 0.5900(2) 0.4694(2) 0.36856(15) 0.0804(10) Uani 1 1 d . . . Si22 Si 0.7078(2) 0.6163(3) 0.54020(16) 0.0877(11) Uani 1 1 d . . . Si32 Si 0.6229(3) 0.8199(3) 0.40215(19) 0.0933(12) Uani 1 1 d . . . Si42 Si 0.7785(3) 0.7732(2) 0.49002(17) 0.0888(11) Uani 1 1 d . . . Si52 Si 0.7874(2) 0.4895(2) 0.43927(17) 0.0824(10) Uani 1 1 d . . . Si62 Si 0.6436(2) 0.6362(3) 0.32444(15) 0.0855(11) Uani 1 1 d . . . Si72 Si 0.8450(2) 0.6431(2) 0.38735(17) 0.0838(10) Uani 1 1 d . . . Si82 Si 0.4444(3) 0.8176(3) 0.4604(2) 0.1242(16) Uani 1 1 d . . . O12 O 0.5255(6) 0.4851(6) 0.4225(3) 0.099(3) Uani 1 1 d . . . H12 H 0.4960 0.4385 0.4226 0.050 Uiso 1 1 calc RD . . O22 O 0.5938(5) 0.5948(6) 0.5249(4) 0.101(3) Uani 1 1 d . . . H22 H 0.5782 0.5511 0.5370 0.050 Uiso 1 1 calc R . . O32 O 0.7300(6) 0.7061(5) 0.5205(4) 0.104(3) Uani 1 1 d . . . O42 O 0.7594(5) 0.5410(5) 0.5004(4) 0.091(2) Uani 1 1 d . . . O52 O 0.6953(6) 0.4550(5) 0.3957(4) 0.093(2) Uani 1 1 d . . . O62 O 0.5929(5) 0.5571(6) 0.3452(4) 0.096(3) Uani 1 1 d . . . O72 O 0.6978(6) 0.8201(6) 0.4567(4) 0.109(3) Uani 1 1 d . . . O82 O 0.8494(5) 0.5543(6) 0.4106(4) 0.096(3) Uani 1 1 d . . . O92 O 0.8391(5) 0.7210(6) 0.4415(4) 0.101(3) Uani 1 1 d . . . O102 O 0.7538(5) 0.6364(6) 0.3397(4) 0.097(3) Uani 1 1 d . . . O112 O 0.6109(6) 0.7250(6) 0.3590(4) 0.100(3) Uani 1 1 d . . . O122 O 0.5261(6) 0.8442(6) 0.4244(4) 0.109(3) Uani 1 1 d . . . C12 C 0.4061(15) 0.7119(12) 0.4310(9) 0.212(10) Uiso 1 1 d . . . H32 H 0.4570 0.6751 0.4350 0.050 Uiso 1 1 calc R . . H42 H 0.3827 0.7051 0.3896 0.050 Uiso 1 1 calc R . . H52 H 0.3565 0.6949 0.4514 0.050 Uiso 1 1 calc R . . C22 C 0.4940(14) 0.8179(13) 0.5343(8) 0.179(8) Uiso 1 1 d . . . H62 H 0.5164 0.8770 0.5548 0.050 Uiso 1 1 calc R . . H72 H 0.5454 0.7808 0.5334 0.050 Uiso 1 1 calc R . . H82 H 0.4469 0.7959 0.5547 0.050 Uiso 1 1 calc R . . C32 C 0.3511(11) 0.8854(11) 0.4529(8) 0.147(6) Uiso 1 1 d . . . H92 H 0.3722 0.9454 0.4719 0.050 Uiso 1 1 calc R . . H102 H 0.2999 0.8663 0.4714 0.050 Uiso 1 1 calc R . . H112 H 0.3303 0.8814 0.4115 0.050 Uiso 1 1 calc R . . C112 C 0.5431(9) 0.3734(7) 0.3105(5) 0.094(4) Uiso 1 1 d D . . H122 H 0.4801 0.3838 0.2932 0.050 Uiso 1 1 calc R . . C122 C 0.6032(11) 0.3564(8) 0.2632(6) 0.118(5) Uiso 1 1 d D . . H132 H 0.5789 0.3815 0.2302 0.050 Uiso 1 1 calc R . . H142 H 0.6667 0.3821 0.2781 0.050 Uiso 1 1 calc R . . C132 C 0.6021(18) 0.2631(10) 0.2448(9) 0.226(11) Uiso 1 1 d D . . H152 H 0.5618 0.2422 0.2072 0.050 Uiso 1 1 calc R . . H162 H 0.6650 0.2459 0.2399 0.050 Uiso 1 1 calc R . . C142 C 0.5689(19) 0.2288(11) 0.2878(9) 0.245(12) Uiso 1 1 d D . . H172 H 0.6183 0.1990 0.3059 0.050 Uiso 1 1 calc R . . H182 H 0.5174 0.1849 0.2696 0.050 Uiso 1 1 calc R . . C152 C 0.5371(12) 0.2919(9) 0.3327(7) 0.134(6) Uiso 1 1 d D . . H192 H 0.5771 0.2984 0.3704 0.050 Uiso 1 1 calc R . . H202 H 0.4730 0.2759 0.3377 0.050 Uiso 1 1 calc R . . C212 C 0.7484(9) 0.6226(9) 0.6181(6) 0.105(4) Uiso 1 1 d D . . H212 H 0.7153 0.6683 0.6415 0.050 Uiso 1 1 calc R . . C222 C 0.7297(11) 0.5408(10) 0.6372(8) 0.152(7) Uiso 1 1 d D . . H222 H 0.6704 0.5405 0.6531 0.050 Uiso 1 1 calc R . . H232 H 0.7276 0.4902 0.6043 0.050 Uiso 1 1 calc R . . C232 C 0.8069(13) 0.5387(14) 0.6828(9) 0.214(10) Uiso 1 1 d D . . H242 H 0.7888 0.5592 0.7220 0.050 Uiso 1 1 calc R . . H252 H 0.8261 0.4793 0.6795 0.050 Uiso 1 1 calc R . . C242 C 0.8781(12) 0.5933(14) 0.6740(10) 0.211(10) Uiso 1 1 d D . . H262 H 0.9270 0.5580 0.6586 0.050 Uiso 1 1 calc R . . H272 H 0.9049 0.6309 0.7119 0.050 Uiso 1 1 calc R . . C252 C 0.8491(10) 0.6475(11) 0.6337(8) 0.148(6) Uiso 1 1 d D . . H282 H 0.8812 0.6352 0.5988 0.050 Uiso 1 1 calc R . . H292 H 0.8610 0.7095 0.6528 0.050 Uiso 1 1 calc R . . C312 C 0.6623(12) 0.8955(10) 0.3627(9) 0.149(6) Uiso 1 1 d D . . H302 H 0.6214 0.8759 0.3246 0.050 Uiso 1 1 calc R . . C322 C 0.7551(12) 0.8888(10) 0.3430(9) 0.165(7) Uiso 1 1 d D . . H312 H 0.8000 0.8750 0.3737 0.050 Uiso 1 1 calc R . . H322 H 0.7520 0.8423 0.3074 0.050 Uiso 1 1 calc R . . C332 C 0.7835(12) 0.9714(11) 0.3308(10) 0.187(9) Uiso 1 1 d D . . H332 H 0.8396 0.9985 0.3574 0.050 Uiso 1 1 calc R . . H342 H 0.7964 0.9639 0.2901 0.050 Uiso 1 1 calc R . . C342 C 0.7105(15) 1.0209(13) 0.3399(11) 0.231(11) Uiso 1 1 d D . . H352 H 0.6753 1.0229 0.3019 0.050 Uiso 1 1 calc R . . H362 H 0.7338 1.0807 0.3600 0.050 Uiso 1 1 calc R . . C352 C 0.6494(15) 0.9851(11) 0.3754(10) 0.208(10) Uiso 1 1 d D . . H372 H 0.6674 1.0110 0.4174 0.050 Uiso 1 1 calc R . . H382 H 0.5844 0.9954 0.3641 0.050 Uiso 1 1 calc R . . C412 C 0.8592(11) 0.8539(8) 0.5467(6) 0.118(5) Uiso 1 1 d D . . H392 H 0.9044 0.8211 0.5666 0.050 Uiso 1 1 calc R . . C422 C 0.8158(11) 0.9112(10) 0.5924(7) 0.149(6) Uiso 1 1 d D . . H402 H 0.8023 0.8805 0.6230 0.050 Uiso 1 1 calc R . . H412 H 0.7575 0.9300 0.5752 0.050 Uiso 1 1 calc R . . C432 C 0.8838(12) 0.9874(11) 0.6176(7) 0.160(7) Uiso 1 1 d D . . H422 H 0.8522 1.0413 0.6268 0.050 Uiso 1 1 calc R . . H432 H 0.9214 0.9796 0.6534 0.050 Uiso 1 1 calc R . . C442 C 0.9366(15) 0.9892(12) 0.5746(8) 0.212(10) Uiso 1 1 d D . . H442 H 1.0018 0.9871 0.5905 0.050 Uiso 1 1 calc R . . H452 H 0.9309 1.0447 0.5624 0.050 Uiso 1 1 calc R . . C452 C 0.9124(13) 0.9184(10) 0.5233(7) 0.154(7) Uiso 1 1 d D . . H462 H 0.9681 0.8946 0.5085 0.050 Uiso 1 1 calc R . . H472 H 0.8741 0.9374 0.4917 0.050 Uiso 1 1 calc R . . C512 C 0.8516(11) 0.3979(8) 0.4518(7) 0.123(5) Uiso 1 1 d D . . H482 H 0.9057 0.4219 0.4820 0.050 Uiso 1 1 calc R . . C522 C 0.7975(12) 0.3310(9) 0.4751(8) 0.153(7) Uiso 1 1 d D . . H492 H 0.8035 0.3474 0.5182 0.050 Uiso 1 1 calc R . . H502 H 0.7314 0.3268 0.4592 0.050 Uiso 1 1 calc R . . C532 C 0.8370(14) 0.2483(10) 0.4562(9) 0.177(8) Uiso 1 1 d D . . H512 H 0.8754 0.2332 0.4893 0.050 Uiso 1 1 calc R . . H522 H 0.7875 0.2016 0.4403 0.050 Uiso 1 1 calc R . . C542 C 0.8895(19) 0.2590(12) 0.4141(11) 0.278(15) Uiso 1 1 d D . . H532 H 0.8668 0.2156 0.3778 0.050 Uiso 1 1 calc R . . H542 H 0.9539 0.2483 0.4267 0.050 Uiso 1 1 calc R . . C552 C 0.8880(15) 0.3450(11) 0.4019(8) 0.175(8) Uiso 1 1 d D . . H552 H 0.8476 0.3438 0.3651 0.050 Uiso 1 1 calc R . . H562 H 0.9508 0.3680 0.3989 0.050 Uiso 1 1 calc R . . C612 C 0.6127(10) 0.6144(11) 0.2429(7) 0.133(6) Uiso 1 1 d D . . H572 H 0.6272 0.5537 0.2273 0.050 Uiso 1 1 calc R . . C622 C 0.6588(12) 0.6687(13) 0.2099(8) 0.182(8) Uiso 1 1 d D . . H582 H 0.7225 0.6529 0.2060 0.050 Uiso 1 1 calc R . . H592 H 0.6605 0.7307 0.2290 0.050 Uiso 1 1 calc R . . C632 C 0.5998(13) 0.6492(15) 0.1520(7) 0.199(9) Uiso 1 1 d D . . H602 H 0.6033 0.6987 0.1329 0.050 Uiso 1 1 calc R . . H612 H 0.6185 0.5974 0.1259 0.050 Uiso 1 1 calc R . . C642 C 0.5129(12) 0.6346(18) 0.1656(8) 0.237(12) Uiso 1 1 d D . . H622 H 0.4807 0.5843 0.1367 0.050 Uiso 1 1 calc R . . H632 H 0.4779 0.6855 0.1627 0.050 Uiso 1 1 calc R . . C652 C 0.5134(11) 0.6184(14) 0.2242(8) 0.176(8) Uiso 1 1 d D . . H642 H 0.4780 0.5631 0.2231 0.050 Uiso 1 1 calc R . . H652 H 0.4878 0.6659 0.2502 0.050 Uiso 1 1 calc R . . C712 C 0.9505(8) 0.6566(8) 0.3501(6) 0.097(4) Uiso 1 1 d D . . H662 H 0.9524 0.6043 0.3182 0.050 Uiso 1 1 calc R . . C722 C 0.9563(9) 0.7372(9) 0.3253(7) 0.125(5) Uiso 1 1 d D . . H672 H 0.9148 0.7296 0.2880 0.050 Uiso 1 1 calc R . . H682 H 0.9405 0.7885 0.3531 0.050 Uiso 1 1 calc R . . C732 C 1.0537(9) 0.7454(11) 0.3163(7) 0.133(6) Uiso 1 1 d D . . H692 H 1.0627 0.7118 0.2774 0.050 Uiso 1 1 calc R . . H702 H 1.0752 0.8066 0.3199 0.050 Uiso 1 1 calc R . . C742 C 1.0992(11) 0.7127(16) 0.3594(10) 0.225(11) Uiso 1 1 d D . . H712 H 1.1369 0.7603 0.3877 0.050 Uiso 1 1 calc R . . H722 H 1.1416 0.6710 0.3422 0.050 Uiso 1 1 calc R . . C752 C 1.0367(11) 0.6685(13) 0.3909(8) 0.178(8) Uiso 1 1 d D . . H732 H 1.0585 0.6125 0.3963 0.050 Uiso 1 1 calc R . . H742 H 1.0297 0.7052 0.4293 0.050 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 Si11 0.0625(18) 0.0720(19) 0.0530(17) 0.0070(14) 0.0024(14) 0.0056(15) Si21 0.0634(18) 0.0560(16) 0.0603(18) 0.0016(13) 0.0141(14) 0.0069(13) Si31 0.0616(18) 0.0695(19) 0.086(2) 0.0239(16) 0.0272(16) 0.0015(15) Si41 0.0631(18) 0.0678(18) 0.0632(18) 0.0184(14) 0.0181(14) 0.0056(14) Si51 0.0565(17) 0.0552(16) 0.0676(19) 0.0179(14) 0.0183(14) 0.0062(13) Si61 0.0577(18) 0.0654(18) 0.074(2) 0.0098(15) 0.0117(15) -0.0083(14) Si71 0.0506(16) 0.0594(16) 0.0634(18) 0.0156(13) 0.0161(13) 0.0041(12) Si81 0.070(2) 0.101(3) 0.108(3) 0.044(2) 0.032(2) -0.0004(19) O11 0.050(5) 0.125(7) 0.109(7) -0.006(6) -0.007(4) 0.016(5) O21 0.060(5) 0.129(7) 0.080(6) 0.013(5) 0.011(4) 0.026(4) O31 0.086(5) 0.071(5) 0.083(5) 0.017(4) 0.037(4) 0.009(4) O41 0.065(4) 0.063(4) 0.069(4) 0.011(3) 0.025(4) 0.004(3) O51 0.064(4) 0.069(4) 0.067(4) 0.011(3) 0.013(4) 0.004(3) O61 0.061(4) 0.081(5) 0.080(5) 0.024(4) -0.013(4) -0.016(4) O71 0.081(5) 0.076(5) 0.101(6) 0.019(4) 0.039(5) 0.002(4) O81 0.060(4) 0.065(4) 0.084(5) 0.026(4) 0.024(4) 0.005(3) O91 0.066(4) 0.071(4) 0.064(4) 0.016(3) 0.018(3) 0.006(3) O101 0.058(4) 0.067(4) 0.077(5) 0.007(4) 0.013(4) -0.001(3) O111 0.075(5) 0.096(5) 0.085(6) 0.029(4) 0.024(4) -0.010(4) O121 0.067(5) 0.103(6) 0.131(7) 0.046(5) 0.041(5) 0.008(4) Si12 0.072(2) 0.100(2) 0.070(2) 0.0163(18) 0.0254(17) -0.0149(18) Si22 0.078(2) 0.107(3) 0.076(2) 0.019(2) 0.0171(19) -0.026(2) Si32 0.084(3) 0.094(3) 0.120(3) 0.051(2) 0.036(2) 0.016(2) Si42 0.074(2) 0.095(2) 0.098(3) 0.020(2) 0.020(2) -0.0113(19) Si52 0.065(2) 0.094(2) 0.097(3) 0.033(2) 0.0240(19) 0.0055(17) Si62 0.077(2) 0.118(3) 0.071(2) 0.034(2) 0.0254(18) 0.001(2) Si72 0.065(2) 0.100(3) 0.097(3) 0.033(2) 0.0337(19) -0.0068(18) Si82 0.099(3) 0.131(4) 0.163(5) 0.051(3) 0.058(3) 0.024(3) O12 0.083(6) 0.132(7) 0.075(5) 0.006(5) 0.030(4) -0.035(5) O22 0.077(5) 0.143(8) 0.078(6) 0.023(5) 0.018(4) -0.040(5) O32 0.096(6) 0.092(6) 0.133(8) 0.034(5) 0.040(6) -0.006(5) O42 0.080(5) 0.108(6) 0.085(6) 0.029(5) 0.009(5) -0.017(5) O52 0.080(6) 0.102(6) 0.097(6) 0.021(5) 0.025(5) -0.005(5) O62 0.075(5) 0.114(6) 0.102(6) 0.026(5) 0.026(5) -0.004(5) O72 0.095(6) 0.117(7) 0.115(7) 0.025(6) 0.014(6) 0.017(5) O82 0.070(5) 0.112(6) 0.115(7) 0.034(5) 0.033(5) -0.005(4) O92 0.068(5) 0.109(6) 0.132(8) 0.040(6) 0.026(5) -0.017(5) O102 0.071(5) 0.137(7) 0.093(6) 0.045(5) 0.026(5) -0.004(5) O112 0.089(6) 0.113(7) 0.110(7) 0.041(6) 0.027(5) 0.013(5) O122 0.105(7) 0.121(7) 0.119(7) 0.050(6) 0.041(6) 0.025(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 Si11 O61 1.590(7) . ? Si11 O51 1.604(7) . ? Si11 O11 1.650(8) . ? Si11 C111 1.834(14) . ? Si21 O31 1.591(8) . ? Si21 O41 1.613(7) . ? Si21 O21 1.619(8) . ? Si21 C211 1.824(11) . ? Si31 O121 1.579(8) . ? Si31 O71 1.585(8) . ? Si31 O111 1.613(8) . ? Si31 C311 1.835(12) . ? Si41 O31 1.604(8) . ? Si41 O91 1.620(7) . ? Si41 O71 1.625(8) . ? Si41 C411 1.791(13) . ? Si51 O41 1.614(7) . ? Si51 O51 1.624(7) . ? Si51 O81 1.633(7) . ? Si51 C511 1.828(9) . ? Si61 O61 1.607(8) . ? Si61 O111 1.611(7) . ? Si61 O101 1.619(7) . ? Si61 C611 1.844(11) . ? Si71 O81 1.597(7) . ? Si71 O101 1.597(7) . ? Si71 O91 1.616(7) . ? Si71 C711 1.829(9) . ? Si81 O121 1.610(8) . ? Si81 C31 1.74(2) . ? Si81 C11 1.764(19) . ? Si81 C21 1.832(15) . ? O11 H11 0.8300 . ? O21 H21 0.8308 . ? C11 H31 0.9700 . ? C11 H41 0.9700 . ? C11 H51 0.9700 . ? C21 H61 0.9700 . ? C21 H71 0.9700 . ? C21 H81 0.9700 . ? C31 H91 0.9700 . ? C31 H101 0.9700 . ? C31 H111 0.9700 . ? C111 C121 1.447(13) . ? C111 C151 1.469(13) . ? C111 H121 0.9900 . ? C121 C131 1.482(14) . ? C121 H131 0.9800 . ? C121 H141 0.9800 . ? C131 C141 1.361(15) . ? C131 H151 0.9800 . ? C131 H161 0.9800 . ? C141 C151 1.427(14) . ? C141 H171 0.9800 . ? C141 H181 0.9800 . ? C151 H191 0.9800 . ? C151 H201 0.9800 . ? C211 C251 1.441(13) . ? C211 C221 1.491(11) . ? C211 H211 0.9900 . ? C221 C231 1.442(12) . ? C221 H221 0.9800 . ? C221 H231 0.9800 . ? C231 C241 1.388(13) . ? C231 H241 0.9800 . ? C231 H251 0.9800 . ? C241 C251 1.474(13) . ? C241 H261 0.9800 . ? C241 H271 0.9800 . ? C251 H281 0.9800 . ? C251 H291 0.9800 . ? C311 C351 1.456(12) . ? C311 C321 1.483(11) . ? C311 H301 0.9900 . ? C321 C331 1.462(12) . ? C321 H311 0.9800 . ? C321 H321 0.9800 . ? C331 C341 1.365(14) . ? C331 H331 0.9800 . ? C331 H341 0.9800 . ? C341 C351 1.477(14) . ? C341 H351 0.9800 . ? C341 H361 0.9800 . ? C351 H371 0.9800 . ? C351 H381 0.9800 . ? C411 C421 1.447(12) . ? C411 C451 1.497(12) . ? C411 H391 0.9900 . ? C421 C431 1.472(15) . ? C421 H401 0.9800 . ? C421 H411 0.9800 . ? C431 C441 1.369(15) . ? C431 H421 0.9800 . ? C431 H431 0.9800 . ? C441 C451 1.428(14) . ? C441 H441 0.9800 . ? C441 H451 0.9800 . ? C451 H461 0.9800 . ? C451 H471 0.9800 . ? C511 C551 1.475(11) . ? C511 C521 1.509(10) . ? C511 H481 0.9900 . ? C521 C531 1.477(12) . ? C521 H491 0.9800 . ? C521 H501 0.9800 . ? C531 C541 1.386(13) . ? C531 H511 0.9800 . ? C531 H521 0.9800 . ? C541 C551 1.446(12) . ? C541 H531 0.9800 . ? C541 H541 0.9800 . ? C551 H551 0.9800 . ? C551 H561 0.9800 . ? C611 C651 1.470(11) . ? C611 C621 1.487(11) . ? C611 H571 0.9900 . ? C621 C631 1.462(12) . ? C621 H581 0.9800 . ? C621 H591 0.9800 . ? C631 C641 1.360(13) . ? C631 H601 0.9800 . ? C631 H611 0.9800 . ? C641 C651 1.455(13) . ? C641 H621 0.9800 . ? C641 H631 0.9800 . ? C651 H641 0.9800 . ? C651 H651 0.9800 . ? C711 C721 1.486(10) . ? C711 C751 1.498(10) . ? C711 H661 0.9900 . ? C721 C731 1.476(11) . ? C721 H671 0.9800 . ? C721 H681 0.9800 . ? C731 C741 1.391(12) . ? C731 H691 0.9800 . ? C731 H701 0.9800 . ? C741 C751 1.445(12) . ? C741 H711 0.9800 . ? C741 H721 0.9800 . ? C751 H731 0.9800 . ? C751 H741 0.9800 . ? Si12 O62 1.591(9) . ? Si12 O52 1.630(9) . ? Si12 O12 1.650(7) . ? Si12 C112 1.841(12) . ? Si22 O32 1.606(9) . ? Si22 O42 1.621(9) . ? Si22 O22 1.652(8) . ? Si22 C212 1.831(13) . ? Si32 O72 1.575(10) . ? Si32 O122 1.595(9) . ? Si32 O112 1.602(10) . ? Si32 C312 1.770(15) . ? Si42 O32 1.579(8) . ? Si42 O72 1.625(10) . ? Si42 O92 1.632(10) . ? Si42 C412 1.870(14) . ? Si52 O52 1.575(9) . ? Si52 O42 1.601(9) . ? Si52 O82 1.628(8) . ? Si52 C512 1.813(14) . ? Si62 O112 1.585(10) . ? Si62 O102 1.596(9) . ? Si62 O62 1.607(8) . ? Si62 C612 1.865(15) . ? Si72 O92 1.579(10) . ? Si72 O102 1.609(9) . ? Si72 O82 1.608(9) . ? Si72 C712 1.878(12) . ? Si82 O122 1.626(9) . ? Si82 C12 1.695(19) . ? Si82 C32 1.782(15) . ? Si82 C22 1.794(18) . ? O12 H12 0.8300 . ? O22 H22 0.8300 . ? C12 H32 0.9700 . ? C12 H42 0.9700 . ? C12 H52 0.9700 . ? C22 H62 0.9700 . ? C22 H72 0.9700 . ? C22 H82 0.9700 . ? C32 H92 0.9700 . ? C32 H102 0.9700 . ? C32 H112 0.9700 . ? C112 C122 1.482(11) . ? C112 C152 1.486(12) . ? C112 H122 0.9900 . ? C122 C132 1.436(13) . ? C122 H132 0.9800 . ? C122 H142 0.9800 . ? C132 C142 1.366(14) . ? C132 H152 0.9800 . ? C132 H162 0.9800 . ? C142 C152 1.425(13) . ? C142 H172 0.9800 . ? C142 H182 0.9800 . ? C152 H192 0.9800 . ? C152 H202 0.9800 . ? C212 C222 1.475(12) . ? C212 C252 1.475(12) . ? C212 H212 0.9900 . ? C222 C232 1.458(13) . ? C222 H222 0.9800 . ? C222 H232 0.9800 . ? C232 C242 1.374(14) . ? C232 H242 0.9800 . ? C232 H252 0.9800 . ? C242 C252 1.442(13) . ? C242 H262 0.9800 . ? C242 H272 0.9800 . ? C252 H282 0.9800 . ? C252 H292 0.9800 . ? C312 C352 1.405(13) . ? C312 C322 1.479(12) . ? C312 H302 0.9900 . ? C322 C332 1.440(13) . ? C322 H312 0.9800 . ? C322 H322 0.9800 . ? C332 C342 1.359(14) . ? C332 H332 0.9800 . ? C332 H342 0.9800 . ? C342 C352 1.460(14) . ? C342 H352 0.9800 . ? C342 H362 0.9800 . ? C352 H372 0.9800 . ? C352 H382 0.9800 . ? C412 C422 1.474(12) . ? C412 C452 1.480(12) . ? C412 H392 0.9900 . ? C422 C432 1.481(13) . ? C422 H402 0.9800 . ? C422 H412 0.9800 . ? C432 C442 1.343(13) . ? C432 H422 0.9800 . ? C432 H432 0.9800 . ? C442 C452 1.448(13) . ? C442 H442 0.9800 . ? C442 H452 0.9800 . ? C452 H462 0.9800 . ? C452 H472 0.9800 . ? C512 C552 1.456(13) . ? C512 C522 1.514(12) . ? C512 H482 0.9900 . ? C522 C532 1.453(13) . ? C522 H492 0.9800 . ? C522 H502 0.9800 . ? C532 C542 1.352(14) . ? C532 H512 0.9800 . ? C532 H522 0.9800 . ? C542 C552 1.442(14) . ? C542 H532 0.9800 . ? C542 H542 0.9800 . ? C552 H552 0.9800 . ? C552 H562 0.9800 . ? C612 C622 1.458(12) . ? C612 C652 1.464(13) . ? C612 H572 0.9900 . ? C622 C632 1.478(13) . ? C622 H582 0.9800 . ? C622 H592 0.9800 . ? C632 C642 1.360(14) . ? C632 H602 0.9800 . ? C632 H612 0.9800 . ? C642 C652 1.451(14) . ? C642 H622 0.9800 . ? C642 H632 0.9800 . ? C652 H642 0.9800 . ? C652 H652 0.9800 . ? C712 C752 1.457(13) . ? C712 C722 1.509(11) . ? C712 H662 0.9900 . ? C722 C732 1.459(12) . ? C722 H672 0.9800 . ? C722 H682 0.9800 . ? C732 C742 1.349(13) . ? C732 H692 0.9800 . ? C732 H702 0.9800 . ? C742 C752 1.474(13) . ? C742 H712 0.9800 . ? C742 H722 0.9800 . ? C752 H732 0.9800 . ? C752 H742 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O61 Si11 O51 109.1(4) . . ? O61 Si11 O11 108.4(5) . . ? O51 Si11 O11 107.7(4) . . ? O61 Si11 C111 110.0(5) . . ? O51 Si11 C111 108.3(6) . . ? O11 Si11 C111 113.3(6) . . ? O31 Si21 O41 109.0(4) . . ? O31 Si21 O21 107.7(4) . . ? O41 Si21 O21 109.1(4) . . ? O31 Si21 C211 112.1(5) . . ? O41 Si21 C211 110.8(5) . . ? O21 Si21 C211 108.1(5) . . ? O121 Si31 O71 108.4(4) . . ? O121 Si31 O111 108.8(5) . . ? O71 Si31 O111 109.1(4) . . ? O121 Si31 C311 107.2(5) . . ? O71 Si31 C311 111.3(6) . . ? O111 Si31 C311 111.9(5) . . ? O31 Si41 O91 109.7(4) . . ? O31 Si41 O71 107.3(4) . . ? O91 Si41 O71 108.2(4) . . ? O31 Si41 C411 111.8(5) . . ? O91 Si41 C411 111.5(5) . . ? O71 Si41 C411 108.2(5) . . ? O41 Si51 O51 108.9(4) . . ? O41 Si51 O81 108.9(4) . . ? O51 Si51 O81 108.9(4) . . ? O41 Si51 C511 111.8(4) . . ? O51 Si51 C511 108.6(4) . . ? O81 Si51 C511 109.6(4) . . ? O61 Si61 O111 108.1(4) . . ? O61 Si61 O101 109.4(4) . . ? O111 Si61 O101 109.8(4) . . ? O61 Si61 C611 110.4(5) . . ? O111 Si61 C611 109.9(5) . . ? O101 Si61 C611 109.2(4) . . ? O81 Si71 O101 110.3(4) . . ? O81 Si71 O91 108.9(4) . . ? O101 Si71 O91 108.0(4) . . ? O81 Si71 C711 109.6(4) . . ? O101 Si71 C711 109.1(4) . . ? O91 Si71 C711 110.9(4) . . ? O121 Si81 C31 111.9(8) . . ? O121 Si81 C11 108.5(8) . . ? C31 Si81 C11 103.4(11) . . ? O121 Si81 C21 111.9(6) . . ? C31 Si81 C21 107.7(10) . . ? C11 Si81 C21 113.1(9) . . ? Si11 O11 H11 109.5 . . ? Si21 O21 H21 109.6 . . ? Si21 O31 Si41 164.6(5) . . ? Si21 O41 Si51 144.9(4) . . ? Si11 O51 Si51 155.5(5) . . ? Si11 O61 Si61 151.2(5) . . ? Si31 O71 Si41 152.5(5) . . ? Si71 O81 Si51 144.8(4) . . ? Si71 O91 Si41 141.7(5) . . ? Si71 O101 Si61 157.5(5) . . ? Si61 O111 Si31 148.0(5) . . ? Si31 O121 Si81 149.5(5) . . ? Si81 C11 H31 109.5 . . ? Si81 C11 H41 109.5 . . ? H31 C11 H41 109.5 . . ? Si81 C11 H51 109.4 . . ? H31 C11 H51 109.5 . . ? H41 C11 H51 109.5 . . ? Si81 C21 H61 109.5 . . ? Si81 C21 H71 109.4 . . ? H61 C21 H71 109.5 . . ? Si81 C21 H81 109.5 . . ? H61 C21 H81 109.5 . . ? H71 C21 H81 109.5 . . ? Si81 C31 H91 109.6 . . ? Si81 C31 H101 109.5 . . ? H91 C31 H101 109.5 . . ? Si81 C31 H111 109.4 . . ? H91 C31 H111 109.5 . . ? H101 C31 H111 109.5 . . ? C121 C111 C151 102.9(11) . . ? C121 C111 Si11 121.7(12) . . ? C151 C111 Si11 112.7(12) . . ? C121 C111 H121 106.1 . . ? C151 C111 H121 106.2 . . ? Si11 C111 H121 106.2 . . ? C111 C121 C131 101.8(13) . . ? C111 C121 H131 111.4 . . ? C131 C121 H131 111.3 . . ? C111 C121 H141 111.5 . . ? C131 C121 H141 111.4 . . ? H131 C121 H141 109.3 . . ? C141 C131 C121 102.2(15) . . ? C141 C131 H151 111.3 . . ? C121 C131 H151 111.2 . . ? C141 C131 H161 111.3 . . ? C121 C131 H161 111.5 . . ? H151 C131 H161 109.2 . . ? C131 C141 C151 109.0(15) . . ? C131 C141 H171 109.9 . . ? C151 C141 H171 109.9 . . ? C131 C141 H181 109.9 . . ? C151 C141 H181 109.8 . . ? H171 C141 H181 108.3 . . ? C141 C151 C111 105.3(12) . . ? C141 C151 H191 110.7 . . ? C111 C151 H191 110.7 . . ? C141 C151 H201 110.7 . . ? C111 C151 H201 110.7 . . ? H191 C151 H201 108.8 . . ? C251 C211 C221 101.7(10) . . ? C251 C211 Si21 122.6(10) . . ? C221 C211 Si21 117.5(9) . . ? C251 C211 H211 104.4 . . ? C221 C211 H211 104.3 . . ? Si21 C211 H211 104.3 . . ? C231 C221 C211 104.6(10) . . ? C231 C221 H221 110.8 . . ? C211 C221 H221 110.8 . . ? C231 C221 H231 110.9 . . ? C211 C221 H231 110.9 . . ? H221 C221 H231 108.9 . . ? C241 C231 C221 104.8(11) . . ? C241 C231 H241 110.7 . . ? C221 C231 H241 110.8 . . ? C241 C231 H251 110.9 . . ? C221 C231 H251 110.8 . . ? H241 C231 H251 108.9 . . ? C231 C241 C251 109.9(12) . . ? C231 C241 H261 109.6 . . ? C251 C241 H261 109.7 . . ? C231 C241 H271 109.8 . . ? C251 C241 H271 109.7 . . ? H261 C241 H271 108.2 . . ? C211 C251 C241 104.1(11) . . ? C211 C251 H281 111.0 . . ? C241 C251 H281 110.9 . . ? C211 C251 H291 110.9 . . ? C241 C251 H291 110.9 . . ? H281 C251 H291 109.0 . . ? C351 C311 C321 103.2(11) . . ? C351 C311 Si31 121.7(10) . . ? C321 C311 Si31 116.9(9) . . ? C351 C311 H301 104.4 . . ? C321 C311 H301 104.3 . . ? Si31 C311 H301 104.4 . . ? C331 C321 C311 104.3(10) . . ? C331 C321 H311 110.9 . . ? C311 C321 H311 110.9 . . ? C331 C321 H321 110.9 . . ? C311 C321 H321 110.9 . . ? H311 C321 H321 108.9 . . ? C341 C331 C321 104.7(12) . . ? C341 C331 H331 110.6 . . ? C321 C331 H331 110.8 . . ? C341 C331 H341 111.0 . . ? C321 C331 H341 110.9 . . ? H331 C331 H341 108.9 . . ? C331 C341 C351 112.0(14) . . ? C331 C341 H351 109.0 . . ? C351 C341 H351 109.2 . . ? C331 C341 H361 109.4 . . ? C351 C341 H361 109.3 . . ? H351 C341 H361 107.9 . . ? C311 C351 C341 97.9(12) . . ? C311 C351 H371 112.3 . . ? C341 C351 H371 112.1 . . ? C311 C351 H381 112.1 . . ? C341 C351 H381 112.2 . . ? H371 C351 H381 109.8 . . ? C421 C411 C451 102.8(11) . . ? C421 C411 Si41 120.7(11) . . ? C451 C411 Si41 113.8(10) . . ? C421 C411 H391 106.2 . . ? C451 C411 H391 106.2 . . ? Si41 C411 H391 106.2 . . ? C411 C421 C431 99.7(14) . . ? C411 C421 H401 111.8 . . ? C431 C421 H401 111.7 . . ? C411 C421 H411 111.9 . . ? C431 C421 H411 112.0 . . ? H401 C421 H411 109.6 . . ? C441 C431 C421 101.1(15) . . ? C441 C431 H421 111.6 . . ? C421 C431 H421 111.4 . . ? C441 C431 H431 111.6 . . ? C421 C431 H431 111.6 . . ? H421 C431 H431 109.4 . . ? C431 C441 C451 110.4(15) . . ? C431 C441 H441 109.6 . . ? C451 C441 H441 109.7 . . ? C431 C441 H451 109.5 . . ? C451 C441 H451 109.6 . . ? H441 C441 H451 108.1 . . ? C441 C451 C411 102.1(11) . . ? C441 C451 H461 111.3 . . ? C411 C451 H461 111.4 . . ? C441 C451 H471 111.4 . . ? C411 C451 H471 111.4 . . ? H461 C451 H471 109.2 . . ? C551 C511 C521 106.1(8) . . ? C551 C511 Si51 114.0(7) . . ? C521 C511 Si51 114.0(7) . . ? C551 C511 H481 107.4 . . ? C521 C511 H481 107.5 . . ? Si51 C511 H481 107.4 . . ? C531 C521 C511 104.4(8) . . ? C531 C521 H491 110.8 . . ? C511 C521 H491 110.9 . . ? C531 C521 H501 110.9 . . ? C511 C521 H501 110.8 . . ? H491 C521 H501 108.9 . . ? C541 C531 C521 104.9(11) . . ? C541 C531 H511 110.7 . . ? C521 C531 H511 110.8 . . ? C541 C531 H521 110.8 . . ? C521 C531 H521 110.7 . . ? H511 C531 H521 108.8 . . ? C531 C541 C551 110.6(12) . . ? C531 C541 H531 109.5 . . ? C551 C541 H531 109.5 . . ? C531 C541 H541 109.6 . . ? C551 C541 H541 109.6 . . ? H531 C541 H541 108.1 . . ? C541 C551 C511 105.1(9) . . ? C541 C551 H551 110.8 . . ? C511 C551 H551 110.7 . . ? C541 C551 H561 110.6 . . ? C511 C551 H561 110.7 . . ? H551 C551 H561 108.8 . . ? C651 C611 C621 105.3(9) . . ? C651 C611 Si61 114.0(9) . . ? C621 C611 Si61 115.1(8) . . ? C651 C611 H571 107.3 . . ? C621 C611 H571 107.3 . . ? Si61 C611 H571 107.3 . . ? C631 C621 C611 107.7(9) . . ? C631 C621 H581 110.2 . . ? C611 C621 H581 110.1 . . ? C631 C621 H591 110.2 . . ? C611 C621 H591 110.2 . . ? H581 C621 H591 108.5 . . ? C641 C631 C621 106.5(11) . . ? C641 C631 H601 110.3 . . ? C621 C631 H601 110.4 . . ? C641 C631 H611 110.5 . . ? C621 C631 H611 110.4 . . ? H601 C631 H611 108.6 . . ? C631 C641 C651 112.2(12) . . ? C631 C641 H621 109.1 . . ? C651 C641 H621 109.1 . . ? C631 C641 H631 109.2 . . ? C651 C641 H631 109.3 . . ? H621 C641 H631 107.9 . . ? C641 C651 C611 103.8(10) . . ? C641 C651 H641 111.1 . . ? C611 C651 H641 111.0 . . ? C641 C651 H651 110.9 . . ? C611 C651 H651 111.0 . . ? H641 C651 H651 109.0 . . ? C721 C711 C751 101.8(7) . . ? C721 C711 Si71 116.5(7) . . ? C751 C711 Si71 114.7(7) . . ? C721 C711 H661 107.8 . . ? C751 C711 H661 107.8 . . ? Si71 C711 H661 107.8 . . ? C731 C721 C711 105.6(8) . . ? C731 C721 H671 110.6 . . ? C711 C721 H671 110.6 . . ? C731 C721 H681 110.6 . . ? C711 C721 H681 110.6 . . ? H671 C721 H681 108.8 . . ? C741 C731 C721 105.9(10) . . ? C741 C731 H691 110.6 . . ? C721 C731 H691 110.6 . . ? C741 C731 H701 110.5 . . ? C721 C731 H701 110.6 . . ? H691 C731 H701 108.7 . . ? C731 C741 C751 110.5(10) . . ? C731 C741 H711 109.6 . . ? C751 C741 H711 109.6 . . ? C731 C741 H721 109.5 . . ? C751 C741 H721 109.6 . . ? H711 C741 H721 108.1 . . ? C741 C751 C711 105.9(8) . . ? C741 C751 H731 110.6 . . ? C711 C751 H731 110.6 . . ? C741 C751 H741 110.6 . . ? C711 C751 H741 110.5 . . ? H731 C751 H741 108.7 . . ? O62 Si12 O52 108.5(4) . . ? O62 Si12 O12 106.4(5) . . ? O52 Si12 O12 108.4(5) . . ? O62 Si12 C112 112.6(5) . . ? O52 Si12 C112 109.6(5) . . ? O12 Si12 C112 111.1(5) . . ? O32 Si22 O42 107.7(4) . . ? O32 Si22 O22 105.9(5) . . ? O42 Si22 O22 109.8(5) . . ? O32 Si22 C212 112.8(6) . . ? O42 Si22 C212 109.0(6) . . ? O22 Si22 C212 111.6(5) . . ? O72 Si32 O122 109.4(5) . . ? O72 Si32 O112 109.4(5) . . ? O122 Si32 O112 109.9(5) . . ? O72 Si32 C312 109.2(8) . . ? O122 Si32 C312 111.0(7) . . ? O112 Si32 C312 107.9(7) . . ? O32 Si42 O72 108.3(5) . . ? O32 Si42 O92 109.5(5) . . ? O72 Si42 O92 109.1(5) . . ? O32 Si42 C412 109.5(6) . . ? O72 Si42 C412 112.0(6) . . ? O92 Si42 C412 108.6(5) . . ? O52 Si52 O42 108.3(4) . . ? O52 Si52 O82 108.8(5) . . ? O42 Si52 O82 110.5(5) . . ? O52 Si52 C512 109.5(6) . . ? O42 Si52 C512 109.2(6) . . ? O82 Si52 C512 110.5(6) . . ? O112 Si62 O102 109.1(5) . . ? O112 Si62 O62 108.2(5) . . ? O102 Si62 O62 109.9(5) . . ? O112 Si62 C612 114.6(7) . . ? O102 Si62 C612 108.7(6) . . ? O62 Si62 C612 106.2(6) . . ? O92 Si72 O102 109.3(5) . . ? O92 Si72 O82 108.4(5) . . ? O102 Si72 O82 109.6(5) . . ? O92 Si72 C712 112.9(5) . . ? O102 Si72 C712 108.4(5) . . ? O82 Si72 C712 108.3(5) . . ? O122 Si82 C12 108.1(9) . . ? O122 Si82 C32 109.3(7) . . ? C12 Si82 C32 109.7(10) . . ? O122 Si82 C22 109.1(8) . . ? C12 Si82 C22 104.2(10) . . ? C32 Si82 C22 116.1(9) . . ? Si12 O12 H12 109.5 . . ? Si22 O22 H22 109.5 . . ? Si42 O32 Si22 159.0(6) . . ? Si52 O42 Si22 153.1(6) . . ? Si52 O52 Si12 150.2(6) . . ? Si12 O62 Si62 154.2(6) . . ? Si32 O72 Si42 150.5(7) . . ? Si72 O82 Si52 141.5(6) . . ? Si72 O92 Si42 149.2(5) . . ? Si62 O102 Si72 150.0(6) . . ? Si62 O112 Si32 156.4(6) . . ? Si32 O122 Si82 145.7(6) . . ? Si82 C12 H32 109.5 . . ? Si82 C12 H42 109.5 . . ? H32 C12 H42 109.5 . . ? Si82 C12 H52 109.5 . . ? H32 C12 H52 109.5 . . ? H42 C12 H52 109.5 . . ? Si82 C22 H62 109.5 . . ? Si82 C22 H72 109.4 . . ? H62 C22 H72 109.5 . . ? Si82 C22 H82 109.5 . . ? H62 C22 H82 109.5 . . ? H72 C22 H82 109.5 . . ? Si82 C32 H92 109.4 . . ? Si82 C32 H102 109.5 . . ? H92 C32 H102 109.5 . . ? Si82 C32 H112 109.5 . . ? H92 C32 H112 109.5 . . ? H102 C32 H112 109.5 . . ? C122 C112 C152 105.7(9) . . ? C122 C112 Si12 111.4(9) . . ? C152 C112 Si12 112.7(10) . . ? C122 C112 H122 108.9 . . ? C152 C112 H122 109.0 . . ? Si12 C112 H122 109.0 . . ? C132 C122 C112 106.2(10) . . ? C132 C122 H132 110.5 . . ? C112 C122 H132 110.5 . . ? C132 C122 H142 110.5 . . ? C112 C122 H142 110.5 . . ? H132 C122 H142 108.7 . . ? C142 C132 C122 107.0(13) . . ? C142 C132 H152 110.3 . . ? C122 C132 H152 110.4 . . ? C142 C132 H162 110.3 . . ? C122 C132 H162 110.3 . . ? H152 C132 H162 108.6 . . ? C132 C142 C152 113.8(13) . . ? C132 C142 H172 108.8 . . ? C152 C142 H172 108.7 . . ? C132 C142 H182 108.8 . . ? C152 C142 H182 108.9 . . ? H172 C142 H182 107.7 . . ? C142 C152 C112 103.4(11) . . ? C142 C152 H192 111.2 . . ? C112 C152 H192 111.1 . . ? C142 C152 H202 111.0 . . ? C112 C152 H202 111.0 . . ? H192 C152 H202 109.1 . . ? C222 C212 C252 107.0(10) . . ? C222 C212 Si22 114.0(10) . . ? C252 C212 Si22 112.6(11) . . ? C222 C212 H212 107.7 . . ? C252 C212 H212 107.7 . . ? Si22 C212 H212 107.6 . . ? C232 C222 C212 105.2(11) . . ? C232 C222 H222 110.7 . . ? C212 C222 H222 110.7 . . ? C232 C222 H232 110.7 . . ? C212 C222 H232 110.7 . . ? H222 C222 H232 108.8 . . ? C242 C232 C222 106.1(13) . . ? C242 C232 H242 110.4 . . ? C222 C232 H242 110.5 . . ? C242 C232 H252 110.6 . . ? C222 C232 H252 110.5 . . ? H242 C232 H252 108.7 . . ? C232 C242 C252 113.4(13) . . ? C232 C242 H262 108.8 . . ? C252 C242 H262 108.8 . . ? C232 C242 H272 109.0 . . ? C252 C242 H272 109.0 . . ? H262 C242 H272 107.7 . . ? C242 C252 C212 103.2(11) . . ? C242 C252 H282 111.2 . . ? C212 C252 H282 111.2 . . ? C242 C252 H292 111.0 . . ? C212 C252 H292 111.1 . . ? H282 C252 H292 109.1 . . ? C352 C312 C322 105.4(11) . . ? C352 C312 Si32 125.0(13) . . ? C322 C312 Si32 119.2(12) . . ? C352 C312 H302 100.8 . . ? C322 C312 H302 100.8 . . ? Si32 C312 H302 100.8 . . ? C332 C322 C312 108.0(11) . . ? C332 C322 H312 110.1 . . ? C312 C322 H312 110.1 . . ? C332 C322 H322 110.1 . . ? C312 C322 H322 110.1 . . ? H312 C322 H322 108.4 . . ? C342 C332 C322 105.1(12) . . ? C342 C332 H332 110.8 . . ? C322 C332 H332 110.7 . . ? C342 C332 H342 110.7 . . ? C322 C332 H342 110.7 . . ? H332 C332 H342 108.8 . . ? C332 C342 C352 110.7(13) . . ? C332 C342 H352 109.5 . . ? C352 C342 H352 109.5 . . ? C332 C342 H362 109.5 . . ? C352 C342 H362 109.5 . . ? H352 C342 H362 108.1 . . ? C312 C352 C342 103.7(13) . . ? C312 C352 H372 111.0 . . ? C342 C352 H372 111.0 . . ? C312 C352 H382 111.0 . . ? C342 C352 H382 111.0 . . ? H372 C352 H382 109.0 . . ? C422 C412 C452 101.5(10) . . ? C422 C412 Si42 116.3(11) . . ? C452 C412 Si42 114.9(11) . . ? C422 C412 H392 107.9 . . ? C452 C412 H392 107.9 . . ? Si42 C412 H392 107.9 . . ? C412 C422 C432 106.2(11) . . ? C412 C422 H402 110.5 . . ? C432 C422 H402 110.5 . . ? C412 C422 H412 110.5 . . ? C432 C422 H412 110.4 . . ? H402 C422 H412 108.7 . . ? C442 C432 C422 103.7(12) . . ? C442 C432 H422 111.2 . . ? C422 C432 H422 111.1 . . ? C442 C432 H432 110.9 . . ? C422 C432 H432 111.0 . . ? H422 C432 H432 109.0 . . ? C432 C442 C452 114.1(13) . . ? C432 C442 H442 108.9 . . ? C452 C442 H442 108.8 . . ? C432 C442 H452 108.6 . . ? C452 C442 H452 108.7 . . ? H442 C442 H452 107.6 . . ? C442 C452 C412 102.3(11) . . ? C442 C452 H462 111.3 . . ? C412 C452 H462 111.3 . . ? C442 C452 H472 111.4 . . ? C412 C452 H472 111.3 . . ? H462 C452 H472 109.2 . . ? C552 C512 C522 103.1(10) . . ? C552 C512 Si52 117.9(12) . . ? C522 C512 Si52 114.5(11) . . ? C552 C512 H482 106.9 . . ? C522 C512 H482 106.9 . . ? Si52 C512 H482 106.9 . . ? C532 C522 C512 106.5(11) . . ? C532 C522 H492 110.4 . . ? C512 C522 H492 110.4 . . ? C532 C522 H502 110.5 . . ? C512 C522 H502 110.4 . . ? H492 C522 H502 108.6 . . ? C542 C532 C522 106.4(12) . . ? C542 C532 H512 110.5 . . ? C522 C532 H512 110.5 . . ? C542 C532 H522 110.4 . . ? C522 C532 H522 110.4 . . ? H512 C532 H522 108.6 . . ? C532 C542 C552 113.0(13) . . ? C532 C542 H532 109.1 . . ? C552 C542 H532 109.0 . . ? C532 C542 H542 108.9 . . ? C552 C542 H542 109.0 . . ? H532 C542 H542 107.8 . . ? C542 C552 C512 104.8(12) . . ? C542 C552 H552 110.8 . . ? C512 C552 H552 110.8 . . ? C542 C552 H562 110.8 . . ? C512 C552 H562 110.8 . . ? H552 C552 H562 108.9 . . ? C622 C612 C652 104.1(11) . . ? C622 C612 Si62 119.2(12) . . ? C652 C612 Si62 113.1(12) . . ? C622 C612 H572 106.5 . . ? C652 C612 H572 106.5 . . ? Si62 C612 H572 106.5 . . ? C612 C622 C632 103.3(12) . . ? C612 C622 H582 111.1 . . ? C632 C622 H582 111.1 . . ? C612 C622 H592 111.1 . . ? C632 C622 H592 111.1 . . ? H582 C622 H592 109.1 . . ? C642 C632 C622 103.3(13) . . ? C642 C632 H602 111.0 . . ? C622 C632 H602 111.1 . . ? C642 C632 H612 111.2 . . ? C622 C632 H612 111.1 . . ? H602 C632 H612 109.1 . . ? C632 C642 C652 113.0(13) . . ? C632 C642 H622 108.9 . . ? C652 C642 H622 108.9 . . ? C632 C642 H632 109.1 . . ? C652 C642 H632 109.0 . . ? H622 C642 H632 107.8 . . ? C642 C652 C612 102.1(11) . . ? C642 C652 H642 111.4 . . ? C612 C652 H642 111.3 . . ? C642 C652 H652 111.3 . . ? C612 C652 H652 111.3 . . ? H642 C652 H652 109.2 . . ? C752 C712 C722 101.9(10) . . ? C752 C712 Si72 112.3(10) . . ? C722 C712 Si72 114.8(9) . . ? C752 C712 H662 109.2 . . ? C722 C712 H662 109.1 . . ? Si72 C712 H662 109.2 . . ? C732 C722 C712 102.9(10) . . ? C732 C722 H672 111.3 . . ? C712 C722 H672 111.3 . . ? C732 C722 H682 111.1 . . ? C712 C722 H682 111.1 . . ? H672 C722 H682 109.1 . . ? C742 C732 C722 104.1(12) . . ? C742 C732 H692 110.9 . . ? C722 C732 H692 110.8 . . ? C742 C732 H702 111.0 . . ? C722 C732 H702 111.0 . . ? H692 C732 H702 109.0 . . ? C732 C742 C752 113.4(13) . . ? C732 C742 H712 108.9 . . ? C752 C742 H712 108.9 . . ? C732 C742 H722 108.9 . . ? C752 C742 H722 108.9 . . ? H712 C742 H722 107.7 . . ? C712 C752 C742 100.8(11) . . ? C712 C752 H732 111.6 . . ? C742 C752 H732 111.6 . . ? C712 C752 H742 111.6 . . ? C742 C752 H742 111.6 . . ? H732 C752 H742 109.4 . . ? 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 O41 Si21 O31 Si41 -38(2) . . . . ? O21 Si21 O31 Si41 80(2) . . . . ? C211 Si21 O31 Si41 -161(2) . . . . ? O91 Si41 O31 Si21 41(2) . . . . ? O71 Si41 O31 Si21 -76(2) . . . . ? C411 Si41 O31 Si21 165.6(19) . . . . ? O31 Si21 O41 Si51 42.4(9) . . . . ? O21 Si21 O41 Si51 -75.0(9) . . . . ? C211 Si21 O41 Si51 166.2(8) . . . . ? O51 Si51 O41 Si21 62.7(9) . . . . ? O81 Si51 O41 Si21 -56.0(9) . . . . ? C511 Si51 O41 Si21 -177.3(8) . . . . ? O61 Si11 O51 Si51 -68.6(12) . . . . ? O11 Si11 O51 Si51 48.8(12) . . . . ? C111 Si11 O51 Si51 171.7(11) . . . . ? O41 Si51 O51 Si11 -41.9(12) . . . . ? O81 Si51 O51 Si11 76.8(12) . . . . ? C511 Si51 O51 Si11 -164.0(11) . . . . ? O51 Si11 O61 Si61 15.8(13) . . . . ? O11 Si11 O61 Si61 -101.2(11) . . . . ? C111 Si11 O61 Si61 134.4(12) . . . . ? O111 Si61 O61 Si11 104.4(11) . . . . ? O101 Si61 O61 Si11 -15.2(13) . . . . ? C611 Si61 O61 Si11 -135.4(11) . . . . ? O121 Si31 O71 Si41 -179.9(11) . . . . ? O111 Si31 O71 Si41 -61.6(13) . . . . ? C311 Si31 O71 Si41 62.4(13) . . . . ? O31 Si41 O71 Si31 129.5(12) . . . . ? O91 Si41 O71 Si31 11.2(14) . . . . ? C411 Si41 O71 Si31 -109.7(13) . . . . ? O101 Si71 O81 Si51 37.6(9) . . . . ? O91 Si71 O81 Si51 -80.7(9) . . . . ? C711 Si71 O81 Si51 157.8(8) . . . . ? O41 Si51 O81 Si71 79.0(9) . . . . ? O51 Si51 O81 Si71 -39.8(9) . . . . ? C511 Si51 O81 Si71 -158.4(8) . . . . ? O81 Si71 O91 Si41 60.7(8) . . . . ? O101 Si71 O91 Si41 -59.0(8) . . . . ? C711 Si71 O91 Si41 -178.5(7) . . . . ? O31 Si41 O91 Si71 -47.9(8) . . . . ? O71 Si41 O91 Si71 68.8(8) . . . . ? C411 Si41 O91 Si71 -172.3(8) . . . . ? O81 Si71 O101 Si61 -70.0(14) . . . . ? O91 Si71 O101 Si61 48.9(14) . . . . ? C711 Si71 O101 Si61 169.6(12) . . . . ? O61 Si61 O101 Si71 63.8(14) . . . . ? O111 Si61 O101 Si71 -54.7(14) . . . . ? C611 Si61 O101 Si71 -175.3(13) . . . . ? O61 Si61 O111 Si31 -116.3(10) . . . . ? O101 Si61 O111 Si31 3.0(12) . . . . ? C611 Si61 O111 Si31 123.2(10) . . . . ? O121 Si31 O111 Si61 158.6(10) . . . . ? O71 Si31 O111 Si61 40.5(11) . . . . ? C311 Si31 O111 Si61 -83.1(11) . . . . ? O71 Si31 O121 Si81 48.9(14) . . . . ? O111 Si31 O121 Si81 -69.6(14) . . . . ? C311 Si31 O121 Si81 169.2(12) . . . . ? C31 Si81 O121 Si31 142.3(15) . . . . ? C11 Si81 O121 Si31 -104.2(15) . . . . ? C21 Si81 O121 Si31 21.3(16) . . . . ? O61 Si11 C111 C121 53.3(15) . . . . ? O51 Si11 C111 C121 172.4(13) . . . . ? O11 Si11 C111 C121 -68.2(15) . . . . ? O61 Si11 C111 C151 176.2(13) . . . . ? O51 Si11 C111 C151 -64.7(15) . . . . ? O11 Si11 C111 C151 54.7(16) . . . . ? C151 C111 C121 C131 37(2) . . . . ? Si11 C111 C121 C131 164.3(16) . . . . ? C111 C121 C131 C141 -43(3) . . . . ? C121 C131 C141 C151 33(3) . . . . ? C131 C141 C151 C111 -10(3) . . . . ? C121 C111 C151 C141 -18(3) . . . . ? Si11 C111 C151 C141 -150.9(19) . . . . ? O31 Si21 C211 C251 57.7(15) . . . . ? O41 Si21 C211 C251 -64.3(15) . . . . ? O21 Si21 C211 C251 176.3(14) . . . . ? O31 Si21 C211 C221 -175.1(10) . . . . ? O41 Si21 C211 C221 62.9(11) . . . . ? O21 Si21 C211 C221 -56.5(12) . . . . ? C251 C211 C221 C231 -39.2(17) . . . . ? Si21 C211 C221 C231 -175.9(12) . . . . ? C211 C221 C231 C241 31(2) . . . . ? C221 C231 C241 C251 -11(3) . . . . ? C221 C211 C251 C241 31(2) . . . . ? Si21 C211 C251 C241 165.2(14) . . . . ? C231 C241 C251 C211 -14(3) . . . . ? O121 Si31 C311 C351 172.7(13) . . . . ? O71 Si31 C311 C351 -68.9(14) . . . . ? O111 Si31 C311 C351 53.4(15) . . . . ? O121 Si31 C311 C321 -59.4(12) . . . . ? O71 Si31 C311 C321 59.1(12) . . . . ? O111 Si31 C311 C321 -178.6(10) . . . . ? C351 C311 C321 C331 -37.1(17) . . . . ? Si31 C311 C321 C331 -173.6(12) . . . . ? C311 C321 C331 C341 16(2) . . . . ? C321 C331 C341 C351 11(3) . . . . ? C321 C311 C351 C341 40.7(19) . . . . ? Si31 C311 C351 C341 174.4(14) . . . . ? C331 C341 C351 C311 -33(3) . . . . ? O31 Si41 C411 C421 -62.7(14) . . . . ? O91 Si41 C411 C421 60.5(14) . . . . ? O71 Si41 C411 C421 179.4(12) . . . . ? O31 Si41 C411 C451 60.2(12) . . . . ? O91 Si41 C411 C451 -176.6(11) . . . . ? O71 Si41 C411 C451 -57.7(12) . . . . ? C451 C411 C421 C431 44(2) . . . . ? Si41 C411 C421 C431 171.7(16) . . . . ? C411 C421 C431 C441 -48(3) . . . . ? C421 C431 C441 C451 34(4) . . . . ? C431 C441 C451 C411 -7(3) . . . . ? C421 C411 C451 C441 -24(2) . . . . ? Si41 C411 C451 C441 -156.3(17) . . . . ? O41 Si51 C511 C551 170.9(7) . . . . ? O51 Si51 C511 C551 -68.9(8) . . . . ? O81 Si51 C511 C551 50.0(9) . . . . ? O41 Si51 C511 C521 -67.0(8) . . . . ? O51 Si51 C511 C521 53.2(8) . . . . ? O81 Si51 C511 C521 172.1(7) . . . . ? C551 C511 C521 C531 -17.9(13) . . . . ? Si51 C511 C521 C531 -144.2(9) . . . . ? C511 C521 C531 C541 28.7(17) . . . . ? C521 C531 C541 C551 -30(2) . . . . ? C531 C541 C551 C511 18(2) . . . . ? C521 C511 C551 C541 0.9(15) . . . . ? Si51 C511 C551 C541 127.3(12) . . . . ? O61 Si61 C611 C651 -61.1(10) . . . . ? O111 Si61 C611 C651 58.0(10) . . . . ? O101 Si61 C611 C651 178.6(9) . . . . ? O61 Si61 C611 C621 60.8(10) . . . . ? O111 Si61 C611 C621 179.9(9) . . . . ? O101 Si61 C611 C621 -59.5(10) . . . . ? C651 C611 C621 C631 -11.7(16) . . . . ? Si61 C611 C621 C631 -138.2(11) . . . . ? C611 C621 C631 C641 -1(2) . . . . ? C621 C631 C641 C651 15(3) . . . . ? C631 C641 C651 C611 -22(2) . . . . ? C621 C611 C651 C641 19.3(17) . . . . ? Si61 C611 C651 C641 146.5(12) . . . . ? O81 Si71 C711 C721 -166.3(7) . . . . ? O101 Si71 C711 C721 -45.5(9) . . . . ? O91 Si71 C711 C721 73.3(8) . . . . ? O81 Si71 C711 C751 -47.7(8) . . . . ? O101 Si71 C711 C751 73.2(8) . . . . ? O91 Si71 C711 C751 -168.0(7) . . . . ? C751 C711 C721 C731 32.3(12) . . . . ? Si71 C711 C721 C731 157.7(9) . . . . ? C711 C721 C731 C741 -27.1(15) . . . . ? C721 C731 C741 C751 10.3(18) . . . . ? C731 C741 C751 C711 10.3(17) . . . . ? C721 C711 C751 C741 -26.0(13) . . . . ? Si71 C711 C751 C741 -152.7(9) . . . . ? O72 Si42 O32 Si22 133.2(19) . . . . ? O92 Si42 O32 Si22 14(2) . . . . ? C412 Si42 O32 Si22 -104(2) . . . . ? O42 Si22 O32 Si42 -13(2) . . . . ? O22 Si22 O32 Si42 -130.5(19) . . . . ? C212 Si22 O32 Si42 107(2) . . . . ? O52 Si52 O42 Si22 -56.5(13) . . . . ? O82 Si52 O42 Si22 62.6(13) . . . . ? C512 Si52 O42 Si22 -175.7(12) . . . . ? O32 Si22 O42 Si52 -46.4(13) . . . . ? O22 Si22 O42 Si52 68.4(12) . . . . ? C212 Si22 O42 Si52 -169.1(11) . . . . ? O42 Si52 O52 Si12 39.8(12) . . . . ? O82 Si52 O52 Si12 -80.3(12) . . . . ? C512 Si52 O52 Si12 158.7(11) . . . . ? O62 Si12 O52 Si52 54.7(12) . . . . ? O12 Si12 O52 Si52 -60.5(12) . . . . ? C112 Si12 O52 Si52 178.1(10) . . . . ? O52 Si12 O62 Si62 16.7(15) . . . . ? O12 Si12 O62 Si62 133.1(14) . . . . ? C112 Si12 O62 Si62 -104.8(14) . . . . ? O112 Si62 O62 Si12 -130.0(14) . . . . ? O102 Si62 O62 Si12 -11.0(16) . . . . ? C612 Si62 O62 Si12 106.4(15) . . . . ? O122 Si32 O72 Si42 129.8(13) . . . . ? O112 Si32 O72 Si42 9.4(15) . . . . ? C312 Si32 O72 Si42 -108.5(14) . . . . ? O32 Si42 O72 Si32 -81.7(14) . . . . ? O92 Si42 O72 Si32 37.3(15) . . . . ? C412 Si42 O72 Si32 157.5(13) . . . . ? O92 Si72 O82 Si52 65.9(11) . . . . ? O102 Si72 O82 Si52 -53.3(11) . . . . ? C712 Si72 O82 Si52 -171.3(9) . . . . ? O52 Si52 O82 Si72 59.2(11) . . . . ? O42 Si52 O82 Si72 -59.5(11) . . . . ? C512 Si52 O82 Si72 179.5(10) . . . . ? O102 Si72 O92 Si42 45.8(13) . . . . ? O82 Si72 O92 Si42 -73.6(13) . . . . ? C712 Si72 O92 Si42 166.5(11) . . . . ? O32 Si42 O92 Si72 49.5(14) . . . . ? O72 Si42 O92 Si72 -68.7(13) . . . . ? C412 Si42 O92 Si72 169.0(12) . . . . ? O112 Si62 O102 Si72 58.0(14) . . . . ? O62 Si62 O102 Si72 -60.5(14) . . . . ? C612 Si62 O102 Si72 -176.4(12) . . . . ? O92 Si72 O102 Si62 -44.9(14) . . . . ? O82 Si72 O102 Si62 73.7(14) . . . . ? C712 Si72 O102 Si62 -168.3(12) . . . . ? O102 Si62 O112 Si32 0.6(17) . . . . ? O62 Si62 O112 Si32 120.2(15) . . . . ? C612 Si62 O112 Si32 -121.5(15) . . . . ? O72 Si32 O112 Si62 -39.7(17) . . . . ? O122 Si32 O112 Si62 -159.8(14) . . . . ? C312 Si32 O112 Si62 79.0(17) . . . . ? O72 Si32 O122 Si82 -58.9(14) . . . . ? O112 Si32 O122 Si82 61.2(14) . . . . ? C312 Si32 O122 Si82 -179.5(13) . . . . ? C12 Si82 O122 Si32 -53.7(16) . . . . ? C32 Si82 O122 Si32 -173.0(13) . . . . ? C22 Si82 O122 Si32 59.0(15) . . . . ? O62 Si12 C112 C122 63.4(10) . . . . ? O52 Si12 C112 C122 -57.4(10) . . . . ? O12 Si12 C112 C122 -177.2(9) . . . . ? O62 Si12 C112 C152 -177.9(9) . . . . ? O52 Si12 C112 C152 61.2(11) . . . . ? O12 Si12 C112 C152 -58.6(11) . . . . ? C152 C112 C122 C132 20.2(19) . . . . ? Si12 C112 C122 C132 142.9(14) . . . . ? C112 C122 C132 C142 -16(3) . . . . ? C122 C132 C142 C152 6(3) . . . . ? C132 C142 C152 C112 6(3) . . . . ? C122 C112 C152 C142 -16(2) . . . . ? Si12 C112 C152 C142 -138.0(16) . . . . ? O32 Si22 C212 C222 -179.4(10) . . . . ? O42 Si22 C212 C222 -59.8(12) . . . . ? O22 Si22 C212 C222 61.6(13) . . . . ? O32 Si22 C212 C252 -57.2(12) . . . . ? O42 Si22 C212 C252 62.4(11) . . . . ? O22 Si22 C212 C252 -176.2(10) . . . . ? C252 C212 C222 C232 22(2) . . . . ? Si22 C212 C222 C232 147.5(15) . . . . ? C212 C222 C232 C242 -21(3) . . . . ? C222 C232 C242 C252 13(3) . . . . ? C232 C242 C252 C212 1(3) . . . . ? C222 C212 C252 C242 -15(2) . . . . ? Si22 C212 C252 C242 -140.6(15) . . . . ? O72 Si32 C312 C352 -86(2) . . . . ? O122 Si32 C312 C352 35(2) . . . . ? O112 Si32 C312 C352 155.5(19) . . . . ? O72 Si32 C312 C322 53.9(18) . . . . ? O122 Si32 C312 C322 174.6(15) . . . . ? O112 Si32 C312 C322 -64.9(18) . . . . ? C352 C312 C322 C332 -14(3) . . . . ? Si32 C312 C322 C332 -160.6(16) . . . . ? C312 C322 C332 C342 -3(3) . . . . ? C322 C332 C342 C352 19(3) . . . . ? C322 C312 C352 C342 24(3) . . . . ? Si32 C312 C352 C342 168.0(17) . . . . ? C332 C342 C352 C312 -28(3) . . . . ? O32 Si42 C412 C422 -64.2(13) . . . . ? O72 Si42 C412 C422 55.9(13) . . . . ? O92 Si42 C412 C422 176.3(11) . . . . ? O32 Si42 C412 C452 177.4(11) . . . . ? O72 Si42 C412 C452 -62.5(13) . . . . ? O92 Si42 C412 C452 58.0(13) . . . . ? C452 C412 C422 C432 -34.4(19) . . . . ? Si42 C412 C422 C432 -159.8(13) . . . . ? C412 C422 C432 C442 23(2) . . . . ? C422 C432 C442 C452 -2(3) . . . . ? C432 C442 C452 C412 -19(3) . . . . ? C422 C412 C452 C442 31(2) . . . . ? Si42 C412 C452 C442 157.8(14) . . . . ? O52 Si52 C512 C552 64.8(14) . . . . ? O42 Si52 C512 C552 -176.8(12) . . . . ? O82 Si52 C512 C552 -55.1(15) . . . . ? O52 Si52 C512 C522 -56.7(13) . . . . ? O42 Si52 C512 C522 61.7(13) . . . . ? O82 Si52 C512 C522 -176.6(11) . . . . ? C552 C512 C522 C532 24(2) . . . . ? Si52 C512 C522 C532 153.1(14) . . . . ? C512 C522 C532 C542 -15(3) . . . . ? C522 C532 C542 C552 -1(3) . . . . ? C532 C542 C552 C512 16(3) . . . . ? C522 C512 C552 C542 -24(2) . . . . ? Si52 C512 C552 C542 -150.7(17) . . . . ? O112 Si62 C612 C622 68.8(16) . . . . ? O102 Si62 C612 C622 -53.5(16) . . . . ? O62 Si62 C612 C622 -171.7(14) . . . . ? O112 Si62 C612 C652 -54.0(15) . . . . ? O102 Si62 C612 C652 -176.3(13) . . . . ? O62 Si62 C612 C652 65.4(14) . . . . ? C652 C612 C622 C632 -38(2) . . . . ? Si62 C612 C622 C632 -164.9(14) . . . . ? C612 C622 C632 C642 33(3) . . . . ? C622 C632 C642 C652 -17(3) . . . . ? C632 C642 C652 C612 -6(3) . . . . ? C622 C612 C652 C642 27(2) . . . . ? Si62 C612 C652 C642 158.1(16) . . . . ? O92 Si72 C712 C752 55.4(13) . . . . ? O102 Si72 C712 C752 176.6(11) . . . . ? O82 Si72 C712 C752 -64.7(13) . . . . ? O92 Si72 C712 C722 -60.4(11) . . . . ? O102 Si72 C712 C722 60.8(11) . . . . ? O82 Si72 C712 C722 179.5(9) . . . . ? C752 C712 C722 C732 41.6(16) . . . . ? Si72 C712 C722 C732 163.2(11) . . . . ? C712 C722 C732 C742 -31(2) . . . . ? C722 C732 C742 C752 10(3) . . . . ? C722 C712 C752 C742 -33.9(19) . . . . ? Si72 C712 C752 C742 -157.3(14) . . . . ? C732 C742 C752 C712 16(3) . . . . ? 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 O11 H11 O21 0.83 2.04 2.663(9) 131.9 2_575 O12 H12 O22 0.83 2.02 2.659(9) 132.8 2_666 O21 H21 O11 0.83 2.39 2.691(12) 102.1 . O22 H22 O12 0.83 2.00 2.659(9) 136.2 2_666 _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 1.168 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.121 #=END