#------------------------------------------------------------------------------ #$Date: 2021-11-26 00:58:15 +0200 (Fri, 26 Nov 2021) $ #$Revision: 270878 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/93/7129313.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7129313 loop_ _publ_author_name 'Ohmura, Toshimichi' 'Kusaka, Satoshi' 'Suginome, Michinori' _publ_section_title ; Iridium-Catalyzed Enantioselective Intramolecular Hydroarylation of Allylic Aryl Ethers Devoid of a Directing Group on the Aryl Group ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D1CC05684K _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_sum 'C12 H18 O2 Si' _chemical_formula_weight 222.35 _chemical_name_systematic (R)-3-methyl-5-(trimethylsilyl)-2,3-dihydrobenzofuran-3-ol _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-07-28 deposited with the CCDC. 2021-11-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 6.7361(17) _cell_length_b 21.906(6) _cell_length_c 26.843(7) _cell_measurement_reflns_used 7682 _cell_measurement_temperature 143(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.0 _cell_volume 3961.0(18) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 143(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku Saturn724+ (4x4 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0970 _diffrn_reflns_av_unetI/netI 0.1111 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 32323 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.488 _diffrn_reflns_theta_min 3.036 _diffrn_source 'Rotating Anode' _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.791 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.119 _exptl_crystal_description Prism _exptl_crystal_F_000 1440 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: hot hexane' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.220 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Flack x determined using 1515 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.04(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 421 _refine_ls_number_reflns 9056 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.141 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.0903 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.9645P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1317 _refine_ls_wR_factor_ref 0.1464 _reflns_Friedel_coverage 0.771 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 6333 _reflns_number_total 9056 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cc05684k2.cif _cod_data_source_block cKSS10_a_a_a _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 7129313 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL cKSS10_a_a_a.res in P2(1)2(1)2(1) cKSS10_a_a_a.res created by SHELXL-2018/3 at 11:00:18 on 15-Jul-2021 REM Yadorkari-X generated CELL 0.71075 6.7361 21.9060 26.8430 90.0000 90.0000 90.0000 ZERR 12.0 0.0017 0.0060 0.0070 0.0000 0.0000 0.0000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, -Z SYMM -X, 1/2+Y, 1/2-Z REM SPGR P212121 orthorhombic SFAC C H O Si UNIT 144 216 24 12 TEMP -130.0 L.S. 10 FMAP 2 PLAN -20 ACTA CONF LIST 4 WPDB -1 BOND $H WGHT 0.031000 0.964500 FVAR 0.46712 SI3 4 0.523348 0.259812 0.099368 11.00000 0.04763 0.03037 = 0.03299 -0.00154 0.00036 -0.00290 SI2 4 0.195303 0.724042 0.090867 11.00000 0.04378 0.03394 = 0.04484 0.00526 0.00900 0.00314 SI1 4 0.855864 0.509042 0.449800 11.00000 0.08027 0.04268 = 0.03035 -0.00284 -0.00387 0.00461 O4 3 0.176328 0.523892 0.233371 11.00000 0.03257 0.03302 = 0.03845 -0.00339 0.00410 -0.00379 AFIX 147 H1 2 0.285460 0.513604 0.220771 11.00000 -1.50000 AFIX 0 O6 3 0.543734 0.500588 0.194675 11.00000 0.03760 0.03975 = 0.02570 -0.00258 0.00107 0.00604 AFIX 147 H19 2 0.626632 0.480029 0.210954 11.00000 -1.50000 AFIX 0 O2 3 0.865298 0.445931 0.235633 11.00000 0.03304 0.04472 = 0.03225 0.00643 -0.00436 -0.00862 AFIX 147 H37 2 0.965942 0.468150 0.239187 11.00000 -1.50000 AFIX 0 O5 3 0.939200 0.502218 0.111103 11.00000 0.03188 0.04192 = 0.05496 -0.00484 0.00267 -0.01010 O3 3 0.519794 0.622584 0.282776 11.00000 0.03348 0.05889 = 0.05275 0.00351 -0.00919 -0.00365 O1 3 1.202370 0.352952 0.287022 11.00000 0.05264 0.07700 = 0.05856 -0.02465 0.00630 0.01932 C27 1 0.665773 0.441656 0.123354 11.00000 0.02509 0.02607 = 0.02778 -0.00037 -0.00044 0.00097 C3 1 0.952372 0.412787 0.318788 11.00000 0.04343 0.02957 = 0.02672 0.00379 -0.00183 0.00372 C32 1 0.855198 0.445358 0.106121 11.00000 0.02935 0.03372 = 0.03312 -0.00183 -0.00331 -0.00514 C28 1 0.564884 0.386894 0.122054 11.00000 0.02661 0.03397 = 0.02859 0.00041 -0.00007 -0.00270 AFIX 43 H20 2 0.432770 0.384571 0.134293 11.00000 -1.20000 AFIX 0 C29 1 0.657237 0.334562 0.102657 11.00000 0.03575 0.03202 = 0.02883 -0.00248 -0.00194 -0.00365 C17 1 0.290220 0.698309 0.152556 11.00000 0.03436 0.02884 = 0.03116 -0.00640 0.00380 -0.00079 C14 1 0.198683 0.581243 0.258663 11.00000 0.03579 0.03542 = 0.02756 -0.00126 0.00203 -0.00009 C2 1 0.880335 0.394100 0.267967 11.00000 0.04492 0.03747 = 0.02778 0.00253 0.00279 -0.00187 C15 1 0.272723 0.630409 0.224173 11.00000 0.03095 0.03048 = 0.03314 -0.00620 -0.00358 0.00509 C4 1 0.870582 0.449411 0.354975 11.00000 0.03933 0.03705 = 0.02814 0.00432 -0.00198 0.00449 AFIX 43 H38 2 0.741645 0.465879 0.349975 11.00000 -1.20000 AFIX 0 C26 1 0.603299 0.502949 0.143178 11.00000 0.03407 0.03521 = 0.02670 -0.00023 -0.00043 0.00283 C16 1 0.189873 0.654597 0.181233 11.00000 0.03395 0.03047 = 0.04069 -0.00733 -0.00177 -0.00399 AFIX 43 H2 2 0.062059 0.641247 0.170983 11.00000 -1.20000 AFIX 0 C20 1 0.454508 0.650467 0.239806 11.00000 0.03255 0.03839 = 0.03766 -0.00216 -0.00027 0.00428 C5 1 0.972713 0.463004 0.398985 11.00000 0.05692 0.03495 = 0.02548 0.00628 0.00037 0.00049 C18 1 0.476353 0.717117 0.171096 11.00000 0.04055 0.03143 = 0.05755 0.00257 0.01522 -0.00510 AFIX 43 H3 2 0.547921 0.747154 0.152955 11.00000 -1.20000 AFIX 0 C8 1 1.137642 0.388634 0.325561 11.00000 0.04162 0.05198 = 0.04033 -0.00277 0.00452 0.01112 C30 1 0.850153 0.341454 0.084682 11.00000 0.03703 0.03517 = 0.04592 -0.01064 0.00332 0.00979 AFIX 43 H21 2 0.914142 0.306695 0.070897 11.00000 -1.20000 AFIX 0 C21 1 0.000193 0.594193 0.282797 11.00000 0.04854 0.04248 = 0.03607 -0.00284 0.01171 0.00614 AFIX 137 H4 2 -0.103428 0.595201 0.257184 11.00000 -1.50000 H5 2 0.005496 0.633730 0.299828 11.00000 -1.50000 H6 2 -0.030092 0.562039 0.307016 11.00000 -1.50000 AFIX 0 C25 1 0.796352 0.539799 0.136853 11.00000 0.04174 0.02991 = 0.04515 -0.00719 0.00107 -0.00426 AFIX 23 H22 2 0.769950 0.577361 0.117445 11.00000 -1.20000 H23 2 0.848873 0.551780 0.169882 11.00000 -1.20000 AFIX 0 C13 1 0.372028 0.578241 0.296386 11.00000 0.04792 0.04994 = 0.03685 -0.00184 -0.00990 -0.00377 AFIX 23 H7 2 0.322296 0.586849 0.330373 11.00000 -1.20000 H8 2 0.431055 0.536853 0.296252 11.00000 -1.20000 AFIX 0 C31 1 0.954665 0.396414 0.085760 11.00000 0.02845 0.04300 = 0.05690 -0.00950 0.01537 -0.00408 AFIX 43 H24 2 1.086105 0.399866 0.073245 11.00000 -1.20000 AFIX 0 C19 1 0.561260 0.693995 0.214681 11.00000 0.03041 0.05212 = 0.06378 -0.00185 -0.00446 -0.01048 AFIX 43 H9 2 0.686701 0.707742 0.226332 11.00000 -1.20000 AFIX 0 C33 1 0.430276 0.530331 0.114850 11.00000 0.04986 0.03527 = 0.03947 -0.00372 -0.00772 0.00906 AFIX 137 H25 2 0.312244 0.504827 0.119578 11.00000 -1.50000 H26 2 0.462930 0.532305 0.079309 11.00000 -1.50000 H27 2 0.403762 0.571569 0.127342 11.00000 -1.50000 AFIX 0 C34 1 0.381503 0.255420 0.040336 11.00000 0.04869 0.04802 = 0.04654 -0.01595 -0.00580 -0.00710 AFIX 137 H28 2 0.288926 0.289849 0.038409 11.00000 -1.50000 H29 2 0.307010 0.217014 0.039282 11.00000 -1.50000 H30 2 0.473551 0.257073 0.012096 11.00000 -1.50000 AFIX 0 C6 1 1.161642 0.437452 0.404160 11.00000 0.05633 0.07116 = 0.04634 0.00055 -0.02770 0.00590 AFIX 43 H39 2 1.234438 0.445714 0.433712 11.00000 -1.20000 AFIX 0 C35 1 0.343669 0.253764 0.151727 11.00000 0.08535 0.04970 = 0.04682 0.00013 0.01454 -0.01901 AFIX 137 H31 2 0.234701 0.282707 0.146506 11.00000 -1.50000 H32 2 0.411132 0.263238 0.183136 11.00000 -1.50000 H33 2 0.290480 0.212160 0.153133 11.00000 -1.50000 AFIX 0 C36 1 0.710484 0.197319 0.101722 11.00000 0.07375 0.03218 = 0.07595 0.00655 -0.00643 0.00145 AFIX 137 H34 2 0.642952 0.157789 0.099492 11.00000 -1.50000 H35 2 0.784062 0.199648 0.133159 11.00000 -1.50000 H36 2 0.802929 0.201630 0.073752 11.00000 -1.50000 AFIX 0 C22 1 0.309446 0.798285 0.073036 11.00000 0.07114 0.04497 = 0.06521 0.01870 0.00984 -0.00130 AFIX 137 H10 2 0.275216 0.829299 0.097906 11.00000 -1.50000 H11 2 0.259162 0.810878 0.040355 11.00000 -1.50000 H12 2 0.454049 0.793764 0.071459 11.00000 -1.50000 AFIX 0 C11 1 0.716145 0.456236 0.491367 11.00000 0.06266 0.06432 = 0.04521 -0.00572 0.00477 -0.00613 AFIX 137 H40 2 0.609642 0.436484 0.472426 11.00000 -1.50000 H41 2 0.658714 0.479367 0.519095 11.00000 -1.50000 H42 2 0.806561 0.425071 0.504452 11.00000 -1.50000 AFIX 0 C9 1 0.676522 0.364913 0.267063 11.00000 0.07665 0.06070 = 0.04470 0.00632 -0.00651 -0.03488 AFIX 137 H43 2 0.578625 0.393599 0.280528 11.00000 -1.50000 H44 2 0.677858 0.327758 0.287395 11.00000 -1.50000 H45 2 0.641215 0.354497 0.232681 11.00000 -1.50000 AFIX 0 C23 1 -0.078155 0.733117 0.093679 11.00000 0.04588 0.07050 = 0.06958 0.02481 -0.00059 0.00559 AFIX 137 H13 2 -0.139064 0.694217 0.103242 11.00000 -1.50000 H14 2 -0.127961 0.745544 0.060909 11.00000 -1.50000 H15 2 -0.111965 0.764388 0.118370 11.00000 -1.50000 AFIX 0 C7 1 1.248789 0.400173 0.367746 11.00000 0.04560 0.08916 = 0.05943 -0.00882 -0.00914 0.01833 AFIX 43 H46 2 1.378122 0.383648 0.371905 11.00000 -1.20000 AFIX 0 C24 1 0.254241 0.665794 0.043087 11.00000 0.10387 0.06345 = 0.04335 0.00092 -0.00380 0.02773 AFIX 137 H16 2 0.398597 0.662340 0.039529 11.00000 -1.50000 H17 2 0.195932 0.677921 0.011136 11.00000 -1.50000 H18 2 0.199376 0.626301 0.053314 11.00000 -1.50000 AFIX 0 C10 1 1.053193 0.549818 0.485477 11.00000 0.11151 0.06916 = 0.03968 -0.01358 0.01585 -0.03713 AFIX 137 H47 2 1.145229 0.519978 0.499845 11.00000 -1.50000 H48 2 0.992124 0.573728 0.512259 11.00000 -1.50000 H49 2 1.125860 0.577163 0.463064 11.00000 -1.50000 AFIX 0 C12 1 0.676679 0.564917 0.422517 11.00000 0.16192 0.07517 = 0.05157 -0.00808 0.00480 0.05792 AFIX 137 H50 2 0.748785 0.594412 0.401875 11.00000 -1.50000 H51 2 0.607741 0.586498 0.449413 11.00000 -1.50000 H52 2 0.579533 0.543145 0.401952 11.00000 -1.50000 AFIX 0 C1 1 1.044075 0.350473 0.251732 11.00000 0.10507 0.08889 = 0.04632 -0.02426 -0.01489 0.04390 AFIX 23 H53 2 0.991254 0.308370 0.249742 11.00000 -1.20000 H54 2 1.093497 0.362200 0.218343 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM cKSS10_a_a_a.res in P2(1)2(1)2(1) REM wR2 = 0.1464, GooF = S = 1.141, Restrained GooF = 1.141 for all data REM R1 = 0.0903 for 6333 Fo > 4sig(Fo) and 0.1287 for all 9056 data REM 421 parameters refined using 0 restraints END WGHT 0.0310 0.9646 REM Highest difference peak 0.220, deepest hole -0.225, 1-sigma level 0.051 Q1 1 0.5983 0.3042 0.0983 11.00000 0.05 0.22 Q2 1 1.1785 0.5628 0.4712 11.00000 0.05 0.21 Q3 1 0.4688 0.6991 0.0525 11.00000 0.05 0.21 Q4 1 0.6387 0.2466 0.0083 11.00000 0.05 0.19 Q5 1 0.9505 0.4167 0.1666 11.00000 0.05 0.19 Q6 1 0.4634 0.5805 0.4569 11.00000 0.05 0.19 Q7 1 0.3224 0.4973 0.3112 11.00000 0.05 0.19 Q8 1 1.0010 0.4001 0.4854 11.00000 0.05 0.19 Q9 1 0.4424 0.4574 0.3094 11.00000 0.05 0.18 Q10 1 0.9693 0.3763 0.2540 11.00000 0.05 0.18 Q11 1 0.7696 0.3719 0.5413 11.00000 0.05 0.18 Q12 1 0.0829 0.7219 0.2040 11.00000 0.05 0.18 Q13 1 0.9272 0.2997 0.0163 11.00000 0.05 0.18 Q14 1 0.3839 0.6984 0.0467 11.00000 0.05 0.17 Q15 1 -0.0441 0.5404 0.3297 11.00000 0.05 0.17 Q16 1 1.3668 0.3797 0.2414 11.00000 0.05 0.17 Q17 1 0.7841 0.4362 0.1411 11.00000 0.05 0.17 Q18 1 -0.2108 0.6369 0.2602 11.00000 0.05 0.17 Q19 1 0.5076 0.5598 0.2085 11.00000 0.05 0.17 Q20 1 0.8171 0.3231 0.1794 11.00000 0.05 0.17 ; _shelx_res_checksum 68281 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si3 Si 0.5233(3) 0.25981(7) 0.09937(6) 0.0370(4) Uani 1 1 d . . . . . Si2 Si 0.1953(3) 0.72404(7) 0.09087(7) 0.0409(4) Uani 1 1 d . . . . . Si1 Si 0.8559(3) 0.50904(8) 0.44980(7) 0.0511(5) Uani 1 1 d . . . . . O4 O 0.1763(6) 0.52389(15) 0.23337(14) 0.0347(9) Uani 1 1 d . . . . . H1 H 0.285460 0.513604 0.220771 0.052 Uiso 1 1 calc R U . . . O6 O 0.5437(6) 0.50059(17) 0.19467(13) 0.0343(9) Uani 1 1 d . . . . . H19 H 0.626632 0.480029 0.210954 0.052 Uiso 1 1 calc R U . . . O2 O 0.8653(6) 0.44593(17) 0.23563(14) 0.0367(9) Uani 1 1 d . . . . . H37 H 0.965942 0.468150 0.239187 0.055 Uiso 1 1 calc R U . . . O5 O 0.9392(6) 0.50222(17) 0.11110(15) 0.0429(10) Uani 1 1 d . . . . . O3 O 0.5198(6) 0.62258(19) 0.28278(16) 0.0484(11) Uani 1 1 d . . . . . O1 O 1.2024(7) 0.3530(2) 0.28702(18) 0.0627(14) Uani 1 1 d . . . . . C27 C 0.6658(8) 0.4417(2) 0.12335(19) 0.0263(12) Uani 1 1 d . . . . . C3 C 0.9524(9) 0.4128(2) 0.3188(2) 0.0332(14) Uani 1 1 d . . . . . C32 C 0.8552(8) 0.4454(2) 0.1061(2) 0.0321(13) Uani 1 1 d . . . . . C28 C 0.5649(8) 0.3869(2) 0.12205(19) 0.0297(12) Uani 1 1 d . . . . . H20 H 0.432770 0.384571 0.134293 0.036 Uiso 1 1 calc R U . . . C29 C 0.6572(8) 0.3346(2) 0.1027(2) 0.0322(13) Uani 1 1 d . . . . . C17 C 0.2902(9) 0.6983(2) 0.1526(2) 0.0315(13) Uani 1 1 d . . . . . C14 C 0.1987(9) 0.5812(2) 0.2587(2) 0.0329(13) Uani 1 1 d . . . . . C2 C 0.8803(9) 0.3941(3) 0.2680(2) 0.0367(14) Uani 1 1 d . . . . . C15 C 0.2727(8) 0.6304(2) 0.2242(2) 0.0315(13) Uani 1 1 d . . . . . C4 C 0.8706(9) 0.4494(2) 0.3550(2) 0.0348(14) Uani 1 1 d . . . . . H38 H 0.741645 0.465879 0.349975 0.042 Uiso 1 1 calc R U . . . C26 C 0.6033(8) 0.5029(2) 0.1432(2) 0.0320(13) Uani 1 1 d . . . . . C16 C 0.1899(9) 0.6546(2) 0.1812(2) 0.0350(14) Uani 1 1 d . . . . . H2 H 0.062059 0.641247 0.170983 0.042 Uiso 1 1 calc R U . . . C20 C 0.4545(9) 0.6505(3) 0.2398(2) 0.0362(14) Uani 1 1 d . . . . . C5 C 0.9727(10) 0.4630(2) 0.3990(2) 0.0391(14) Uani 1 1 d . . . . . C18 C 0.4764(9) 0.7171(3) 0.1711(2) 0.0432(16) Uani 1 1 d . . . . . H3 H 0.547921 0.747154 0.152955 0.052 Uiso 1 1 calc R U . . . C8 C 1.1376(10) 0.3886(3) 0.3256(2) 0.0446(16) Uani 1 1 d . . . . . C30 C 0.8502(9) 0.3415(2) 0.0847(2) 0.0394(15) Uani 1 1 d . . . . . H21 H 0.914142 0.306695 0.070897 0.047 Uiso 1 1 calc R U . . . C21 C 0.0002(9) 0.5942(3) 0.2828(2) 0.0424(16) Uani 1 1 d . . . . . H4 H -0.103428 0.595201 0.257184 0.064 Uiso 1 1 calc R U . . . H5 H 0.005496 0.633730 0.299828 0.064 Uiso 1 1 calc R U . . . H6 H -0.030092 0.562039 0.307016 0.064 Uiso 1 1 calc R U . . . C25 C 0.7964(9) 0.5398(2) 0.1369(2) 0.0389(15) Uani 1 1 d . . . . . H22 H 0.769950 0.577361 0.117445 0.047 Uiso 1 1 calc R U . . . H23 H 0.848873 0.551780 0.169882 0.047 Uiso 1 1 calc R U . . . C13 C 0.3720(9) 0.5782(3) 0.2964(2) 0.0449(16) Uani 1 1 d . . . . . H7 H 0.322296 0.586849 0.330373 0.054 Uiso 1 1 calc R U . . . H8 H 0.431055 0.536853 0.296252 0.054 Uiso 1 1 calc R U . . . C31 C 0.9547(9) 0.3964(2) 0.0858(2) 0.0428(15) Uani 1 1 d . . . . . H24 H 1.086105 0.399866 0.073245 0.051 Uiso 1 1 calc R U . . . C19 C 0.5613(9) 0.6940(3) 0.2147(3) 0.0488(17) Uani 1 1 d . . . . . H9 H 0.686701 0.707742 0.226332 0.059 Uiso 1 1 calc R U . . . C33 C 0.4303(9) 0.5303(2) 0.1148(2) 0.0415(16) Uani 1 1 d . . . . . H25 H 0.312244 0.504827 0.119578 0.062 Uiso 1 1 calc R U . . . H26 H 0.462930 0.532305 0.079309 0.062 Uiso 1 1 calc R U . . . H27 H 0.403762 0.571569 0.127342 0.062 Uiso 1 1 calc R U . . . C34 C 0.3815(9) 0.2554(3) 0.0403(2) 0.0478(17) Uani 1 1 d . . . . . H28 H 0.288926 0.289849 0.038409 0.072 Uiso 1 1 calc R U . . . H29 H 0.307010 0.217014 0.039282 0.072 Uiso 1 1 calc R U . . . H30 H 0.473551 0.257073 0.012096 0.072 Uiso 1 1 calc R U . . . C6 C 1.1616(10) 0.4375(3) 0.4042(3) 0.0579(19) Uani 1 1 d . . . . . H39 H 1.234438 0.445714 0.433712 0.070 Uiso 1 1 calc R U . . . C35 C 0.3437(11) 0.2538(3) 0.1517(2) 0.061(2) Uani 1 1 d . . . . . H31 H 0.234701 0.282707 0.146506 0.091 Uiso 1 1 calc R U . . . H32 H 0.411132 0.263238 0.183136 0.091 Uiso 1 1 calc R U . . . H33 H 0.290480 0.212160 0.153133 0.091 Uiso 1 1 calc R U . . . C36 C 0.7105(10) 0.1973(3) 0.1017(3) 0.061(2) Uani 1 1 d . . . . . H34 H 0.642952 0.157789 0.099492 0.091 Uiso 1 1 calc R U . . . H35 H 0.784062 0.199648 0.133159 0.091 Uiso 1 1 calc R U . . . H36 H 0.802929 0.201630 0.073752 0.091 Uiso 1 1 calc R U . . . C22 C 0.3094(11) 0.7983(3) 0.0730(3) 0.060(2) Uani 1 1 d . . . . . H10 H 0.275216 0.829299 0.097906 0.091 Uiso 1 1 calc R U . . . H11 H 0.259162 0.810878 0.040355 0.091 Uiso 1 1 calc R U . . . H12 H 0.454049 0.793764 0.071459 0.091 Uiso 1 1 calc R U . . . C11 C 0.7161(11) 0.4562(3) 0.4914(2) 0.057(2) Uani 1 1 d . . . . . H40 H 0.609642 0.436484 0.472426 0.086 Uiso 1 1 calc R U . . . H41 H 0.658714 0.479367 0.519095 0.086 Uiso 1 1 calc R U . . . H42 H 0.806561 0.425071 0.504452 0.086 Uiso 1 1 calc R U . . . C9 C 0.6765(11) 0.3649(3) 0.2671(2) 0.061(2) Uani 1 1 d . . . . . H43 H 0.578625 0.393599 0.280528 0.091 Uiso 1 1 calc R U . . . H44 H 0.677858 0.327758 0.287395 0.091 Uiso 1 1 calc R U . . . H45 H 0.641215 0.354497 0.232681 0.091 Uiso 1 1 calc R U . . . C23 C -0.0782(9) 0.7331(3) 0.0937(3) 0.062(2) Uani 1 1 d . . . . . H13 H -0.139064 0.694217 0.103242 0.093 Uiso 1 1 calc R U . . . H14 H -0.127961 0.745544 0.060909 0.093 Uiso 1 1 calc R U . . . H15 H -0.111965 0.764388 0.118370 0.093 Uiso 1 1 calc R U . . . C7 C 1.2488(10) 0.4002(3) 0.3677(3) 0.065(2) Uani 1 1 d . . . . . H46 H 1.378122 0.383648 0.371905 0.078 Uiso 1 1 calc R U . . . C24 C 0.2542(13) 0.6658(3) 0.0431(3) 0.070(2) Uani 1 1 d . . . . . H16 H 0.398597 0.662340 0.039529 0.105 Uiso 1 1 calc R U . . . H17 H 0.195932 0.677921 0.011136 0.105 Uiso 1 1 calc R U . . . H18 H 0.199376 0.626301 0.053314 0.105 Uiso 1 1 calc R U . . . C10 C 1.0532(12) 0.5498(3) 0.4855(2) 0.073(3) Uani 1 1 d . . . . . H47 H 1.145229 0.519978 0.499845 0.110 Uiso 1 1 calc R U . . . H48 H 0.992124 0.573728 0.512259 0.110 Uiso 1 1 calc R U . . . H49 H 1.125860 0.577163 0.463064 0.110 Uiso 1 1 calc R U . . . C12 C 0.6767(15) 0.5649(3) 0.4225(3) 0.096(3) Uani 1 1 d . . . . . H50 H 0.748785 0.594412 0.401875 0.144 Uiso 1 1 calc R U . . . H51 H 0.607741 0.586498 0.449413 0.144 Uiso 1 1 calc R U . . . H52 H 0.579533 0.543145 0.401952 0.144 Uiso 1 1 calc R U . . . C1 C 1.0441(13) 0.3505(4) 0.2517(3) 0.080(3) Uani 1 1 d . . . . . H53 H 0.991254 0.308370 0.249742 0.096 Uiso 1 1 calc R U . . . H54 H 1.093497 0.362200 0.218343 0.096 Uiso 1 1 calc R U . . . 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 Si3 0.0476(11) 0.0304(8) 0.0330(9) -0.0015(7) 0.0004(8) -0.0029(7) Si2 0.0438(11) 0.0339(9) 0.0448(10) 0.0053(8) 0.0090(9) 0.0031(8) Si1 0.0803(15) 0.0427(11) 0.0303(9) -0.0028(8) -0.0039(10) 0.0046(10) O4 0.033(2) 0.033(2) 0.038(2) -0.0034(18) 0.004(2) -0.0038(18) O6 0.038(2) 0.040(2) 0.0257(19) -0.0026(17) 0.0011(18) 0.006(2) O2 0.033(2) 0.045(2) 0.032(2) 0.0064(19) -0.0044(19) -0.0086(19) O5 0.032(2) 0.042(2) 0.055(3) -0.005(2) 0.003(2) -0.010(2) O3 0.033(3) 0.059(3) 0.053(3) 0.004(2) -0.009(2) -0.004(2) O1 0.053(3) 0.077(3) 0.059(3) -0.025(3) 0.006(3) 0.019(3) C27 0.025(3) 0.026(3) 0.028(3) 0.000(2) 0.000(2) 0.001(2) C3 0.043(4) 0.030(3) 0.027(3) 0.004(2) -0.002(3) 0.004(3) C32 0.029(3) 0.034(3) 0.033(3) -0.002(3) -0.003(3) -0.005(3) C28 0.027(3) 0.034(3) 0.029(3) 0.000(2) 0.000(3) -0.003(2) C29 0.036(3) 0.032(3) 0.029(3) -0.002(3) -0.002(3) -0.004(3) C17 0.034(3) 0.029(3) 0.031(3) -0.006(2) 0.004(3) -0.001(3) C14 0.036(3) 0.035(3) 0.028(3) -0.001(2) 0.002(3) 0.000(3) C2 0.045(4) 0.037(3) 0.028(3) 0.003(3) 0.003(3) -0.002(3) C15 0.031(3) 0.030(3) 0.033(3) -0.006(3) -0.004(3) 0.005(2) C4 0.039(4) 0.037(3) 0.028(3) 0.004(3) -0.002(3) 0.004(3) C26 0.034(3) 0.035(3) 0.027(3) 0.000(3) 0.000(2) 0.003(3) C16 0.034(3) 0.030(3) 0.041(3) -0.007(3) -0.002(3) -0.004(3) C20 0.033(3) 0.038(3) 0.038(3) -0.002(3) 0.000(3) 0.004(3) C5 0.057(4) 0.035(3) 0.025(3) 0.006(3) 0.000(3) 0.000(3) C18 0.041(4) 0.031(3) 0.058(4) 0.003(3) 0.015(3) -0.005(3) C8 0.042(4) 0.052(4) 0.040(4) -0.003(3) 0.005(3) 0.011(3) C30 0.037(4) 0.035(3) 0.046(4) -0.011(3) 0.003(3) 0.010(3) C21 0.049(4) 0.042(3) 0.036(3) -0.003(3) 0.012(3) 0.006(3) C25 0.042(4) 0.030(3) 0.045(4) -0.007(3) 0.001(3) -0.004(3) C13 0.048(4) 0.050(4) 0.037(3) -0.002(3) -0.010(3) -0.004(3) C31 0.028(3) 0.043(4) 0.057(4) -0.009(3) 0.015(3) -0.004(3) C19 0.030(4) 0.052(4) 0.064(5) -0.002(4) -0.004(3) -0.010(3) C33 0.050(4) 0.035(3) 0.039(3) -0.004(3) -0.008(3) 0.009(3) C34 0.049(4) 0.048(4) 0.047(4) -0.016(3) -0.006(3) -0.007(3) C6 0.056(5) 0.071(5) 0.046(4) 0.001(4) -0.028(4) 0.006(4) C35 0.085(6) 0.050(4) 0.047(4) 0.000(3) 0.015(4) -0.019(4) C36 0.074(5) 0.032(3) 0.076(5) 0.007(4) -0.006(5) 0.001(3) C22 0.071(5) 0.045(4) 0.065(5) 0.019(4) 0.010(4) -0.001(4) C11 0.063(5) 0.064(5) 0.045(4) -0.006(4) 0.005(4) -0.006(4) C9 0.077(5) 0.061(4) 0.045(4) 0.006(3) -0.007(4) -0.035(4) C23 0.046(4) 0.070(5) 0.070(5) 0.025(4) -0.001(4) 0.006(4) C7 0.046(5) 0.089(6) 0.059(5) -0.009(4) -0.009(4) 0.018(4) C24 0.104(7) 0.063(5) 0.043(4) 0.001(4) -0.004(4) 0.028(5) C10 0.112(7) 0.069(5) 0.040(4) -0.014(4) 0.016(5) -0.037(5) C12 0.162(9) 0.075(5) 0.052(5) -0.008(4) 0.005(6) 0.058(6) C1 0.105(7) 0.089(6) 0.046(4) -0.024(4) -0.015(5) 0.044(5) 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' 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 C34 Si3 C35 107.9(3) . . ? C34 Si3 C36 109.9(3) . . ? C35 Si3 C36 111.3(3) . . ? C34 Si3 C29 109.5(3) . . ? C35 Si3 C29 109.9(3) . . ? C36 Si3 C29 108.4(3) . . ? C24 Si2 C23 108.4(4) . . ? C24 Si2 C22 109.6(3) . . ? C23 Si2 C22 109.1(3) . . ? C24 Si2 C17 109.5(3) . . ? C23 Si2 C17 109.7(3) . . ? C22 Si2 C17 110.6(3) . . ? C11 Si1 C10 110.5(3) . . ? C11 Si1 C12 108.4(4) . . ? C10 Si1 C12 110.3(4) . . ? C11 Si1 C5 108.3(3) . . ? C10 Si1 C5 109.4(3) . . ? C12 Si1 C5 109.8(3) . . ? C14 O4 H1 109.5 . . ? C26 O6 H19 109.5 . . ? C2 O2 H37 109.5 . . ? C32 O5 C25 106.8(4) . . ? C20 O3 C13 106.9(4) . . ? C8 O1 C1 106.6(5) . . ? C32 C27 C28 120.4(5) . . ? C32 C27 C26 109.2(5) . . ? C28 C27 C26 130.3(5) . . ? C8 C3 C4 119.8(6) . . ? C8 C3 C2 108.0(5) . . ? C4 C3 C2 132.1(6) . . ? C27 C32 O5 114.0(5) . . ? C27 C32 C31 123.0(5) . . ? O5 C32 C31 122.9(5) . . ? C27 C28 C29 120.1(5) . . ? C27 C28 H20 120.0 . . ? C29 C28 H20 120.0 . . ? C30 C29 C28 116.9(5) . . ? C30 C29 Si3 121.8(4) . . ? C28 C29 Si3 121.2(4) . . ? C16 C17 C18 115.7(5) . . ? C16 C17 Si2 122.0(4) . . ? C18 C17 Si2 122.0(5) . . ? O4 C14 C15 111.7(4) . . ? O4 C14 C21 105.9(5) . . ? C15 C14 C21 115.0(5) . . ? O4 C14 C13 110.6(4) . . ? C15 C14 C13 100.5(5) . . ? C21 C14 C13 113.3(5) . . ? O2 C2 C3 110.9(4) . . ? O2 C2 C9 105.1(5) . . ? C3 C2 C9 114.9(5) . . ? O2 C2 C1 112.0(5) . . ? C3 C2 C1 101.3(5) . . ? C9 C2 C1 112.8(6) . . ? C20 C15 C16 119.5(6) . . ? C20 C15 C14 109.8(5) . . ? C16 C15 C14 130.7(5) . . ? C3 C4 C5 121.6(6) . . ? C3 C4 H38 119.2 . . ? C5 C4 H38 119.2 . . ? O6 C26 C27 112.7(4) . . ? O6 C26 C33 106.4(4) . . ? C27 C26 C33 113.0(5) . . ? O6 C26 C25 111.1(4) . . ? C27 C26 C25 101.1(4) . . ? C33 C26 C25 112.7(5) . . ? C15 C16 C17 121.6(6) . . ? C15 C16 H2 119.2 . . ? C17 C16 H2 119.2 . . ? C15 C20 C19 122.8(6) . . ? C15 C20 O3 113.6(5) . . ? C19 C20 O3 123.6(6) . . ? C6 C5 C4 116.5(6) . . ? C6 C5 Si1 121.8(5) . . ? C4 C5 Si1 121.6(5) . . ? C19 C18 C17 123.6(6) . . ? C19 C18 H3 118.2 . . ? C17 C18 H3 118.2 . . ? C3 C8 O1 114.3(6) . . ? C3 C8 C7 122.2(6) . . ? O1 C8 C7 123.5(6) . . ? C29 C30 C31 123.8(5) . . ? C29 C30 H21 118.1 . . ? C31 C30 H21 118.1 . . ? C14 C21 H4 109.5 . . ? C14 C21 H5 109.5 . . ? H4 C21 H5 109.5 . . ? C14 C21 H6 109.5 . . ? H4 C21 H6 109.5 . . ? H5 C21 H6 109.5 . . ? O5 C25 C26 108.5(4) . . ? O5 C25 H22 110.0 . . ? C26 C25 H22 110.0 . . ? O5 C25 H23 110.0 . . ? C26 C25 H23 110.0 . . ? H22 C25 H23 108.4 . . ? O3 C13 C14 109.1(5) . . ? O3 C13 H7 109.9 . . ? C14 C13 H7 109.9 . . ? O3 C13 H8 109.9 . . ? C14 C13 H8 109.9 . . ? H7 C13 H8 108.3 . . ? C32 C31 C30 115.8(5) . . ? C32 C31 H24 122.1 . . ? C30 C31 H24 122.1 . . ? C20 C19 C18 116.7(6) . . ? C20 C19 H9 121.7 . . ? C18 C19 H9 121.7 . . ? C26 C33 H25 109.5 . . ? C26 C33 H26 109.5 . . ? H25 C33 H26 109.5 . . ? C26 C33 H27 109.5 . . ? H25 C33 H27 109.5 . . ? H26 C33 H27 109.5 . . ? Si3 C34 H28 109.5 . . ? Si3 C34 H29 109.5 . . ? H28 C34 H29 109.5 . . ? Si3 C34 H30 109.5 . . ? H28 C34 H30 109.5 . . ? H29 C34 H30 109.5 . . ? C5 C6 C7 123.0(6) . . ? C5 C6 H39 118.5 . . ? C7 C6 H39 118.5 . . ? Si3 C35 H31 109.5 . . ? Si3 C35 H32 109.5 . . ? H31 C35 H32 109.5 . . ? Si3 C35 H33 109.5 . . ? H31 C35 H33 109.5 . . ? H32 C35 H33 109.5 . . ? Si3 C36 H34 109.5 . . ? Si3 C36 H35 109.5 . . ? H34 C36 H35 109.5 . . ? Si3 C36 H36 109.5 . . ? H34 C36 H36 109.5 . . ? H35 C36 H36 109.5 . . ? Si2 C22 H10 109.5 . . ? Si2 C22 H11 109.5 . . ? H10 C22 H11 109.5 . . ? Si2 C22 H12 109.5 . . ? H10 C22 H12 109.5 . . ? H11 C22 H12 109.5 . . ? Si1 C11 H40 109.5 . . ? Si1 C11 H41 109.5 . . ? H40 C11 H41 109.5 . . ? Si1 C11 H42 109.5 . . ? H40 C11 H42 109.5 . . ? H41 C11 H42 109.5 . . ? C2 C9 H43 109.5 . . ? C2 C9 H44 109.5 . . ? H43 C9 H44 109.5 . . ? C2 C9 H45 109.5 . . ? H43 C9 H45 109.5 . . ? H44 C9 H45 109.5 . . ? Si2 C23 H13 109.5 . . ? Si2 C23 H14 109.5 . . ? H13 C23 H14 109.5 . . ? Si2 C23 H15 109.5 . . ? H13 C23 H15 109.5 . . ? H14 C23 H15 109.5 . . ? C8 C7 C6 116.8(6) . . ? C8 C7 H46 121.6 . . ? C6 C7 H46 121.6 . . ? Si2 C24 H16 109.5 . . ? Si2 C24 H17 109.5 . . ? H16 C24 H17 109.5 . . ? Si2 C24 H18 109.5 . . ? H16 C24 H18 109.5 . . ? H17 C24 H18 109.5 . . ? Si1 C10 H47 109.5 . . ? Si1 C10 H48 109.5 . . ? H47 C10 H48 109.5 . . ? Si1 C10 H49 109.5 . . ? H47 C10 H49 109.5 . . ? H48 C10 H49 109.5 . . ? Si1 C12 H50 109.5 . . ? Si1 C12 H51 109.5 . . ? H50 C12 H51 109.5 . . ? Si1 C12 H52 109.5 . . ? H50 C12 H52 109.5 . . ? H51 C12 H52 109.5 . . ? O1 C1 C2 109.1(5) . . ? O1 C1 H53 109.9 . . ? C2 C1 H53 109.9 . . ? O1 C1 H54 109.9 . . ? C2 C1 H54 109.9 . . ? H53 C1 H54 108.3 . . ? 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 Si3 C34 1.853(6) . ? Si3 C35 1.860(6) . ? Si3 C36 1.862(6) . ? Si3 C29 1.871(5) . ? Si2 C24 1.852(7) . ? Si2 C23 1.854(6) . ? Si2 C22 1.862(6) . ? Si2 C17 1.862(6) . ? Si1 C11 1.862(7) . ? Si1 C10 1.866(7) . ? Si1 C12 1.869(8) . ? Si1 C5 1.870(6) . ? O4 C14 1.436(6) . ? O4 H1 0.8400 . ? O6 C26 1.440(6) . ? O6 H19 0.8400 . ? O2 C2 1.433(6) . ? O2 H37 0.8400 . ? O5 C32 1.375(6) . ? O5 C25 1.443(6) . ? O3 C20 1.377(6) . ? O3 C13 1.438(7) . ? O1 C8 1.368(7) . ? O1 C1 1.427(8) . ? C27 C32 1.360(7) . ? C27 C28 1.379(7) . ? C27 C26 1.504(7) . ? C3 C8 1.368(8) . ? C3 C4 1.375(7) . ? C3 C2 1.505(8) . ? C32 C31 1.377(7) . ? C28 C29 1.404(7) . ? C28 H20 0.9500 . ? C29 C30 1.394(8) . ? C17 C16 1.402(7) . ? C17 C18 1.410(8) . ? C14 C15 1.505(7) . ? C14 C21 1.513(8) . ? C14 C13 1.547(8) . ? C2 C9 1.515(8) . ? C2 C1 1.523(9) . ? C15 C20 1.367(8) . ? C15 C16 1.386(7) . ? C4 C5 1.399(7) . ? C4 H38 0.9500 . ? C26 C33 1.515(7) . ? C26 C25 1.540(7) . ? C16 H2 0.9500 . ? C20 C19 1.372(8) . ? C5 C6 1.397(8) . ? C18 C19 1.397(8) . ? C18 H3 0.9500 . ? C8 C7 1.381(9) . ? C30 C31 1.395(7) . ? C30 H21 0.9500 . ? C21 H4 0.9800 . ? C21 H5 0.9800 . ? C21 H6 0.9800 . ? C25 H22 0.9900 . ? C25 H23 0.9900 . ? C13 H7 0.9900 . ? C13 H8 0.9900 . ? C31 H24 0.9500 . ? C19 H9 0.9500 . ? C33 H25 0.9800 . ? C33 H26 0.9800 . ? C33 H27 0.9800 . ? C34 H28 0.9800 . ? C34 H29 0.9800 . ? C34 H30 0.9800 . ? C6 C7 1.402(9) . ? C6 H39 0.9500 . ? C35 H31 0.9800 . ? C35 H32 0.9800 . ? C35 H33 0.9800 . ? C36 H34 0.9800 . ? C36 H35 0.9800 . ? C36 H36 0.9800 . ? C22 H10 0.9800 . ? C22 H11 0.9800 . ? C22 H12 0.9800 . ? C11 H40 0.9800 . ? C11 H41 0.9800 . ? C11 H42 0.9800 . ? C9 H43 0.9800 . ? C9 H44 0.9800 . ? C9 H45 0.9800 . ? C23 H13 0.9800 . ? C23 H14 0.9800 . ? C23 H15 0.9800 . ? C7 H46 0.9500 . ? C24 H16 0.9800 . ? C24 H17 0.9800 . ? C24 H18 0.9800 . ? C10 H47 0.9800 . ? C10 H48 0.9800 . ? C10 H49 0.9800 . ? C12 H50 0.9800 . ? C12 H51 0.9800 . ? C12 H52 0.9800 . ? C1 H53 0.9900 . ? C1 H54 0.9900 . ? 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 C28 C27 C32 O5 -178.1(5) . . . . ? C26 C27 C32 O5 0.1(6) . . . . ? C28 C27 C32 C31 1.5(9) . . . . ? C26 C27 C32 C31 179.8(5) . . . . ? C25 O5 C32 C27 3.5(6) . . . . ? C25 O5 C32 C31 -176.1(5) . . . . ? C32 C27 C28 C29 -0.3(8) . . . . ? C26 C27 C28 C29 -178.2(5) . . . . ? C27 C28 C29 C30 -0.9(8) . . . . ? C27 C28 C29 Si3 -179.0(4) . . . . ? C34 Si3 C29 C30 -91.0(5) . . . . ? C35 Si3 C29 C30 150.7(5) . . . . ? C36 Si3 C29 C30 28.9(6) . . . . ? C34 Si3 C29 C28 87.0(5) . . . . ? C35 Si3 C29 C28 -31.4(5) . . . . ? C36 Si3 C29 C28 -153.1(5) . . . . ? C24 Si2 C17 C16 -78.2(6) . . . . ? C23 Si2 C17 C16 40.6(5) . . . . ? C22 Si2 C17 C16 161.0(5) . . . . ? C24 Si2 C17 C18 95.6(5) . . . . ? C23 Si2 C17 C18 -145.6(5) . . . . ? C22 Si2 C17 C18 -25.2(6) . . . . ? C8 C3 C2 O2 -112.6(6) . . . . ? C4 C3 C2 O2 64.2(8) . . . . ? C8 C3 C2 C9 128.4(6) . . . . ? C4 C3 C2 C9 -54.8(8) . . . . ? C8 C3 C2 C1 6.5(7) . . . . ? C4 C3 C2 C1 -176.7(7) . . . . ? O4 C14 C15 C20 -116.9(5) . . . . ? C21 C14 C15 C20 122.4(5) . . . . ? C13 C14 C15 C20 0.4(6) . . . . ? O4 C14 C15 C16 61.0(8) . . . . ? C21 C14 C15 C16 -59.7(8) . . . . ? C13 C14 C15 C16 178.3(5) . . . . ? C8 C3 C4 C5 0.2(9) . . . . ? C2 C3 C4 C5 -176.3(6) . . . . ? C32 C27 C26 O6 -122.1(5) . . . . ? C28 C27 C26 O6 56.0(8) . . . . ? C32 C27 C26 C33 117.3(5) . . . . ? C28 C27 C26 C33 -64.6(7) . . . . ? C32 C27 C26 C25 -3.5(6) . . . . ? C28 C27 C26 C25 174.6(5) . . . . ? C20 C15 C16 C17 1.6(8) . . . . ? C14 C15 C16 C17 -176.1(5) . . . . ? C18 C17 C16 C15 -1.9(8) . . . . ? Si2 C17 C16 C15 172.3(4) . . . . ? C16 C15 C20 C19 -0.1(9) . . . . ? C14 C15 C20 C19 178.0(5) . . . . ? C16 C15 C20 O3 -179.8(5) . . . . ? C14 C15 C20 O3 -1.7(7) . . . . ? C13 O3 C20 C15 2.2(6) . . . . ? C13 O3 C20 C19 -177.5(6) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? C3 C4 C5 Si1 -176.4(4) . . . . ? C11 Si1 C5 C6 -89.0(6) . . . . ? C10 Si1 C5 C6 31.5(6) . . . . ? C12 Si1 C5 C6 152.8(6) . . . . ? C11 Si1 C5 C4 87.2(5) . . . . ? C10 Si1 C5 C4 -152.3(5) . . . . ? C12 Si1 C5 C4 -31.0(6) . . . . ? C16 C17 C18 C19 1.0(8) . . . . ? Si2 C17 C18 C19 -173.2(5) . . . . ? C4 C3 C8 O1 179.9(5) . . . . ? C2 C3 C8 O1 -2.8(7) . . . . ? C4 C3 C8 C7 -0.7(10) . . . . ? C2 C3 C8 C7 176.6(6) . . . . ? C1 O1 C8 C3 -2.6(8) . . . . ? C1 O1 C8 C7 178.0(7) . . . . ? C28 C29 C30 C31 1.1(9) . . . . ? Si3 C29 C30 C31 179.1(5) . . . . ? C32 O5 C25 C26 -5.7(6) . . . . ? O6 C26 C25 O5 125.3(5) . . . . ? C27 C26 C25 O5 5.5(6) . . . . ? C33 C26 C25 O5 -115.5(5) . . . . ? C20 O3 C13 C14 -1.8(6) . . . . ? O4 C14 C13 O3 119.0(5) . . . . ? C15 C14 C13 O3 0.8(6) . . . . ? C21 C14 C13 O3 -122.4(5) . . . . ? C27 C32 C31 C30 -1.3(9) . . . . ? O5 C32 C31 C30 178.3(5) . . . . ? C29 C30 C31 C32 0.0(9) . . . . ? C15 C20 C19 C18 -0.8(9) . . . . ? O3 C20 C19 C18 178.8(5) . . . . ? C17 C18 C19 C20 0.3(9) . . . . ? C4 C5 C6 C7 0.3(10) . . . . ? Si1 C5 C6 C7 176.6(5) . . . . ? C3 C8 C7 C6 0.9(11) . . . . ? O1 C8 C7 C6 -179.7(6) . . . . ? C5 C6 C7 C8 -0.7(11) . . . . ? C8 O1 C1 C2 6.8(8) . . . . ? O2 C2 C1 O1 110.2(6) . . . . ? C3 C2 C1 O1 -8.1(7) . . . . ? C9 C2 C1 O1 -131.5(6) . . . . ?