#------------------------------------------------------------------------------ #$Date: 2022-03-08 11:21:08 +0200 (Tue, 08 Mar 2022) $ #$Revision: 273525 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/46/8104682.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_8104682 loop_ _publ_author_name 'Bauer, Jonathan O.' _publ_section_title ; The crystal structure of adamantylmethoxydiphenylsilane, C23H28OSi ; _journal_issue 5 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 1117 _journal_page_last 1120 _journal_paper_doi 10.1515/ncrs-2021-0243 _journal_volume 236 _journal_year 2021 _chemical_formula_moiety 'C23 H28 O Si' _chemical_formula_sum 'C23 H28 O Si' _chemical_formula_weight 348.54 _chemical_name_systematic Adamantylmethoxydiphenylsilane _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _cell_angle_alpha 90 _cell_angle_beta 103.780(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.2882(11) _cell_length_b 17.8169(10) _cell_length_c 7.6201(6) _cell_measurement_reflns_used 3447 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 29.1990 _cell_measurement_theta_min 2.6910 _cell_volume 1884.0(2) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics 'CrystalExplorer 17.5 (Turner et al., 2017)' _computing_publication_material 'WinGX (Version 2018.3) (Farrugia, 2012), Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2008; Sheldrick, 2015; Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 16.0560 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.884 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 4.00 85.00 1.0000 23.0000 omega____ theta____ kappa____ phi______ frames - 19.3164 57.0000 -30.0000 81 #__ type_ start__ end____ width___ exp.time_ 2 omega 21.00 66.00 1.0000 23.0000 omega____ theta____ kappa____ phi______ frames - 19.3164 57.0000 30.0000 45 #__ type_ start__ end____ width___ exp.time_ 3 omega 53.00 87.00 1.0000 23.0000 omega____ theta____ kappa____ phi______ frames - 19.3164 179.0000 -150.0000 34 #__ type_ start__ end____ width___ exp.time_ 4 omega 0.00 89.00 1.0000 23.0000 omega____ theta____ kappa____ phi______ frames - 19.3164 77.0000 -150.0000 89 #__ type_ start__ end____ width___ exp.time_ 5 omega 3.00 48.00 1.0000 23.0000 omega____ theta____ kappa____ phi______ frames - -20.2539 57.0000 90.0000 45 #__ type_ start__ end____ width___ exp.time_ 6 omega -21.00 17.00 1.0000 23.0000 omega____ theta____ kappa____ phi______ frames - -20.2539 -99.0000 60.0000 38 #__ type_ start__ end____ width___ exp.time_ 7 omega -93.00 -34.00 1.0000 23.0000 omega____ theta____ kappa____ phi______ frames - -20.2539 -179.0000 -60.0000 59 ; _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator Graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_unetI/netI 0.0774 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.884 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 15475 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.884 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.861 _diffrn_reflns_theta_min 2.286 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.505 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.057 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 338 _refine_ls_number_reflns 4795 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0538 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.2375P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1088 _refine_ls_wR_factor_ref 0.1241 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3241 _reflns_number_total 4795 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file suppl_j_ncrs-2021-0243_suppl.cif _cod_data_source_block 2421 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 8104682 _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_estimated_absorpt_t_min 0.961 _shelx_estimated_absorpt_t_max 0.974 _shelx_res_file ; TITL 2421_a.res in P2(1)/c shelx.res created by SHELXL-2018/3 at 12:03:47 on 07-Jun-2021 REM Old TITL A in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.127, Rweak 0.008, Alpha 0.034 REM 0.537 for 140 systematic absences, Orientation as input REM Formula found by SHELXT: C23 O Si CELL 0.71073 14.2882 17.8169 7.6201 90 103.78 90 ZERR 4 0.0011 0.001 0.0006 0 0.008 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O Si UNIT 92 112 4 4 L.S. 14 PLAN 20 SIZE 0.3 0.2 0.2 TEMP -100 BOND list 4 fmap 2 53 acta REM REM REM WGHT 0.052100 0.237500 FVAR 0.55942 C1 1 0.391831 0.556090 0.161991 11.00000 0.02884 0.04299 = 0.02163 0.00344 0.01158 -0.00157 H1A 2 0.343949 0.566633 0.055805 11.00000 0.05948 H1B 2 0.416547 0.601898 0.217618 11.00000 0.06562 H1C 2 0.438678 0.527266 0.123970 11.00000 0.06769 C2 1 0.242244 0.464672 0.521890 11.00000 0.01604 0.01740 = 0.01471 0.00041 0.00321 0.00028 C3 1 0.329013 0.429363 0.659101 11.00000 0.01923 0.02361 = 0.01677 0.00015 -0.00049 0.00002 H3A 2 0.356805 0.466667 0.747425 11.00000 0.01626 H3B 2 0.378783 0.414258 0.595941 11.00000 0.02225 C4 1 0.296613 0.361545 0.753838 11.00000 0.02713 0.02358 = 0.01778 0.00514 -0.00241 0.00256 H4 2 0.351240 0.343136 0.837782 11.00000 0.02821 C5 1 0.252692 0.302019 0.613375 11.00000 0.03319 0.01683 = 0.02433 0.00096 0.00834 0.00271 H5A 2 0.236003 0.258331 0.677886 11.00000 0.03216 H5B 2 0.300871 0.285733 0.546992 11.00000 0.02372 C6 1 0.165309 0.335415 0.479237 11.00000 0.02398 0.01851 = 0.01929 -0.00484 0.00301 -0.00253 H6 2 0.139134 0.297387 0.387747 11.00000 0.02151 C7 1 0.197334 0.403260 0.383911 11.00000 0.02120 0.02173 = 0.01598 -0.00153 0.00206 0.00118 H7A 2 0.140395 0.424094 0.297178 11.00000 0.02526 H7B 2 0.241695 0.388240 0.318812 11.00000 0.01580 C8 1 0.166167 0.488687 0.626074 11.00000 0.02405 0.01882 = 0.02139 -0.00224 0.01039 -0.00010 H8A 2 0.195141 0.529206 0.717702 11.00000 0.02037 H8B 2 0.107238 0.510535 0.536367 11.00000 0.01577 C9 1 0.134493 0.420153 0.722169 11.00000 0.02898 0.02177 = 0.02748 -0.00166 0.01735 -0.00290 H9 2 0.088867 0.434999 0.785879 11.00000 0.01853 C10 1 0.222278 0.387022 0.855495 11.00000 0.04499 0.02153 = 0.01726 0.00089 0.00947 -0.00617 H10A 2 0.203711 0.345860 0.919453 11.00000 0.03265 H10B 2 0.248408 0.423711 0.947997 11.00000 0.02805 C11 1 0.090542 0.360887 0.581144 11.00000 0.02470 0.02210 = 0.03064 0.00053 0.00772 -0.00433 H11A 2 0.066816 0.316684 0.641196 11.00000 0.02087 H11B 2 0.035665 0.379444 0.501758 11.00000 0.02676 C12 1 0.356657 0.612888 0.587143 11.00000 0.02293 0.01666 = 0.01565 0.00430 0.00294 -0.00041 C13 1 0.317008 0.662504 0.692734 11.00000 0.02779 0.02483 = 0.02398 -0.00051 0.00483 0.00305 H13 2 0.246048 0.665396 0.678538 11.00000 0.01620 C14 1 0.375209 0.707761 0.823371 11.00000 0.04328 0.02657 = 0.02773 -0.00712 0.00466 0.00561 H14 2 0.346868 0.739621 0.898737 11.00000 0.04481 C15 1 0.474638 0.703774 0.853787 11.00000 0.03621 0.03348 = 0.03012 -0.00653 -0.00432 -0.00485 H15 2 0.516544 0.737860 0.940042 11.00000 0.03697 C16 1 0.515675 0.653818 0.754610 11.00000 0.02235 0.03851 = 0.03421 -0.00323 -0.00066 -0.00231 H16 2 0.587720 0.649547 0.776958 11.00000 0.03319 C17 1 0.457514 0.609182 0.623651 11.00000 0.02122 0.02461 = 0.02440 -0.00182 0.00434 0.00098 H17 2 0.488530 0.576185 0.561584 11.00000 0.02195 C18 1 0.182639 0.598578 0.252692 11.00000 0.01674 0.02132 = 0.01819 0.00279 0.00442 0.00003 C19 1 0.135720 0.561100 0.093330 11.00000 0.02980 0.02267 = 0.02306 -0.00036 0.00164 0.00406 H19 2 0.156137 0.511389 0.070987 11.00000 0.03512 C20 1 0.060437 0.593225 -0.034038 11.00000 0.03064 0.03521 = 0.02124 -0.00036 -0.00064 0.00340 H20 2 0.027517 0.563432 -0.146473 11.00000 0.04529 C21 1 0.029686 0.665076 -0.005752 11.00000 0.02539 0.03352 = 0.02786 0.00922 0.00359 0.00745 H21 2 -0.026173 0.686476 -0.094384 11.00000 0.03372 C22 1 0.075703 0.704256 0.147033 11.00000 0.02955 0.02291 = 0.03474 0.00460 0.00703 0.00694 H22 2 0.054411 0.754085 0.163344 11.00000 0.03695 C23 1 0.150840 0.671639 0.274557 11.00000 0.02609 0.02161 = 0.02558 0.00065 0.00394 -0.00047 H23 2 0.179659 0.700591 0.380497 11.00000 0.02969 O 3 0.355229 0.513180 0.289973 11.00000 0.02291 0.02413 = 0.02022 0.00021 0.00925 0.00129 SI 4 0.284314 0.548429 0.410557 11.00000 0.01630 0.01737 = 0.01453 0.00024 0.00307 0.00134 HKLF 4 REM 2421_a.res in P2(1)/c REM wR2 = 0.1241, GooF = S = 1.020, Restrained GooF = 1.020 for all data REM R1 = 0.0538 for 3241 Fo > 4sig(Fo) and 0.0947 for all 4795 data REM 338 parameters refined using 0 restraints END WGHT 0.0521 0.2375 REM Highest difference peak 0.505, deepest hole -0.285, 1-sigma level 0.057 Q1 1 0.2610 0.5028 0.4766 11.00000 0.05 0.50 Q2 1 0.2269 0.5731 0.3349 11.00000 0.05 0.39 Q3 1 0.3228 0.5978 0.4832 11.00000 0.05 0.35 Q4 1 0.2847 0.4432 0.5637 11.00000 0.05 0.32 Q5 1 0.2142 0.4809 0.5781 11.00000 0.05 0.29 Q6 1 0.1361 0.3425 0.5552 11.00000 0.05 0.25 Q7 1 0.2645 0.3329 0.6939 11.00000 0.05 0.25 Q8 1 0.3015 0.3968 0.6998 11.00000 0.05 0.25 Q9 1 0.1819 0.3991 0.7803 11.00000 0.05 0.24 Q10 1 0.1443 0.4554 0.6797 11.00000 0.05 0.24 Q11 1 0.2626 0.3800 0.7979 11.00000 0.05 0.24 Q12 1 0.1843 0.3636 0.4178 11.00000 0.05 0.23 Q13 1 0.3601 0.6028 0.1569 11.00000 0.05 0.23 Q14 1 0.3226 0.5246 0.3399 11.00000 0.05 0.22 Q15 1 0.4871 0.6435 0.6522 11.00000 0.05 0.21 Q16 1 0.1582 0.5777 0.1907 11.00000 0.05 0.21 Q17 1 0.1806 0.4190 0.8123 11.00000 0.05 0.21 Q18 1 0.1818 0.6411 0.2219 11.00000 0.05 0.20 Q19 1 0.2128 0.3342 0.5532 11.00000 0.05 0.20 Q20 1 0.2477 0.4340 0.4254 11.00000 0.05 0.20 ; _shelx_res_checksum 67749 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -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 C1 C 0.39183(18) 0.55609(15) 0.1620(3) 0.0302(5) Uani 1 1 d . . . . . H1A H 0.344(2) 0.5666(15) 0.056(4) 0.059(8) Uiso 1 1 d . . . . . H1B H 0.4165(19) 0.6019(17) 0.218(4) 0.066(9) Uiso 1 1 d . . . . . H1C H 0.439(2) 0.5273(15) 0.124(4) 0.068(9) Uiso 1 1 d . . . . . C2 C 0.24224(12) 0.46467(10) 0.5219(3) 0.0161(4) Uani 1 1 d . . . . . C3 C 0.32901(14) 0.42936(11) 0.6591(3) 0.0207(4) Uani 1 1 d . . . . . H3A H 0.3568(13) 0.4667(11) 0.747(3) 0.016(5) Uiso 1 1 d . . . . . H3B H 0.3788(14) 0.4143(11) 0.596(3) 0.022(5) Uiso 1 1 d . . . . . C4 C 0.29661(15) 0.36154(11) 0.7538(3) 0.0241(5) Uani 1 1 d . . . . . H4 H 0.3512(15) 0.3431(11) 0.838(3) 0.028(6) Uiso 1 1 d . . . . . C5 C 0.25269(16) 0.30202(11) 0.6134(3) 0.0245(5) Uani 1 1 d . . . . . H5A H 0.2360(15) 0.2583(13) 0.678(3) 0.032(6) Uiso 1 1 d . . . . . H5B H 0.3009(14) 0.2857(11) 0.547(3) 0.024(5) Uiso 1 1 d . . . . . C6 C 0.16531(14) 0.33542(11) 0.4792(3) 0.0210(4) Uani 1 1 d . . . . . H6 H 0.1391(14) 0.2974(11) 0.388(3) 0.022(5) Uiso 1 1 d . . . . . C7 C 0.19733(15) 0.40326(11) 0.3839(3) 0.0200(4) Uani 1 1 d . . . . . H7A H 0.1404(15) 0.4241(11) 0.297(3) 0.025(6) Uiso 1 1 d . . . . . H7B H 0.2417(14) 0.3882(10) 0.319(3) 0.016(5) Uiso 1 1 d . . . . . C8 C 0.16617(14) 0.48869(10) 0.6261(3) 0.0206(4) Uani 1 1 d . . . . . H8A H 0.1951(13) 0.5292(11) 0.718(3) 0.020(5) Uiso 1 1 d . . . . . H8B H 0.1072(13) 0.5105(10) 0.536(3) 0.016(5) Uiso 1 1 d . . . . . C9 C 0.13449(15) 0.42015(11) 0.7222(3) 0.0243(5) Uani 1 1 d . . . . . H9 H 0.0889(14) 0.4350(10) 0.786(3) 0.019(5) Uiso 1 1 d . . . . . C10 C 0.22228(17) 0.38702(12) 0.8555(3) 0.0276(5) Uani 1 1 d . . . . . H10A H 0.2037(15) 0.3459(12) 0.919(3) 0.033(6) Uiso 1 1 d . . . . . H10B H 0.2484(14) 0.4237(12) 0.948(3) 0.028(6) Uiso 1 1 d . . . . . C11 C 0.09054(15) 0.36089(12) 0.5811(3) 0.0256(5) Uani 1 1 d . . . . . H11A H 0.0668(13) 0.3167(11) 0.641(3) 0.021(5) Uiso 1 1 d . . . . . H11B H 0.0357(15) 0.3794(11) 0.502(3) 0.027(6) Uiso 1 1 d . . . . . C12 C 0.35666(14) 0.61289(10) 0.5871(3) 0.0187(4) Uani 1 1 d . . . . . C13 C 0.31701(16) 0.66250(11) 0.6927(3) 0.0258(5) Uani 1 1 d . . . . . H13 H 0.2460(14) 0.6654(10) 0.679(3) 0.016(5) Uiso 1 1 d . . . . . C14 C 0.37521(17) 0.70776(12) 0.8234(3) 0.0332(5) Uani 1 1 d . . . . . H14 H 0.3469(17) 0.7396(14) 0.899(3) 0.045(7) Uiso 1 1 d . . . . . C15 C 0.47464(17) 0.70377(13) 0.8538(3) 0.0353(6) Uani 1 1 d . . . . . H15 H 0.5165(15) 0.7379(13) 0.940(3) 0.037(6) Uiso 1 1 d . . . . . C16 C 0.51568(16) 0.65382(12) 0.7546(3) 0.0329(5) Uani 1 1 d . . . . . H16 H 0.5877(16) 0.6495(12) 0.777(3) 0.033(6) Uiso 1 1 d . . . . . C17 C 0.45751(14) 0.60918(11) 0.6237(3) 0.0236(5) Uani 1 1 d . . . . . H17 H 0.4885(14) 0.5762(11) 0.562(3) 0.022(5) Uiso 1 1 d . . . . . C18 C 0.18264(13) 0.59858(10) 0.2527(3) 0.0187(4) Uani 1 1 d . . . . . C19 C 0.13572(15) 0.56110(12) 0.0933(3) 0.0260(5) Uani 1 1 d . . . . . H19 H 0.1561(15) 0.5114(13) 0.071(3) 0.035(6) Uiso 1 1 d . . . . . C20 C 0.06044(16) 0.59322(12) -0.0340(3) 0.0302(5) Uani 1 1 d . . . . . H20 H 0.0275(17) 0.5634(13) -0.146(3) 0.045(7) Uiso 1 1 d . . . . . C21 C 0.02969(15) 0.66508(12) -0.0058(3) 0.0294(5) Uani 1 1 d . . . . . H21 H -0.0262(15) 0.6865(12) -0.094(3) 0.034(6) Uiso 1 1 d . . . . . C22 C 0.07570(15) 0.70426(12) 0.1470(3) 0.0292(5) Uani 1 1 d . . . . . H22 H 0.0544(15) 0.7541(14) 0.163(3) 0.037(6) Uiso 1 1 d . . . . . C23 C 0.15084(15) 0.67164(11) 0.2746(3) 0.0248(5) Uani 1 1 d . . . . . H23 H 0.1797(15) 0.7006(12) 0.380(3) 0.030(6) Uiso 1 1 d . . . . . O O 0.35523(9) 0.51318(7) 0.28997(18) 0.0217(3) Uani 1 1 d . . . . . Si Si 0.28431(4) 0.54843(3) 0.41056(7) 0.01617(14) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0288(12) 0.0430(14) 0.0216(13) 0.0034(11) 0.0116(10) -0.0016(11) C2 0.0160(9) 0.0174(9) 0.0147(10) 0.0004(7) 0.0032(8) 0.0003(7) C3 0.0192(10) 0.0236(10) 0.0168(11) 0.0001(8) -0.0005(8) 0.0000(8) C4 0.0271(11) 0.0236(10) 0.0178(12) 0.0051(8) -0.0024(9) 0.0026(8) C5 0.0332(12) 0.0168(9) 0.0243(13) 0.0010(8) 0.0083(10) 0.0027(8) C6 0.0240(10) 0.0185(9) 0.0193(11) -0.0048(8) 0.0030(8) -0.0025(8) C7 0.0212(10) 0.0217(10) 0.0160(11) -0.0015(8) 0.0021(9) 0.0012(8) C8 0.0240(11) 0.0188(9) 0.0214(12) -0.0022(8) 0.0104(9) -0.0001(8) C9 0.0290(11) 0.0218(10) 0.0275(13) -0.0017(9) 0.0173(10) -0.0029(8) C10 0.0450(13) 0.0215(10) 0.0173(12) 0.0009(9) 0.0095(10) -0.0062(9) C11 0.0247(11) 0.0221(10) 0.0306(14) 0.0005(9) 0.0077(10) -0.0043(9) C12 0.0229(10) 0.0167(9) 0.0156(11) 0.0043(8) 0.0029(8) -0.0004(7) C13 0.0278(11) 0.0248(10) 0.0240(12) -0.0005(9) 0.0048(9) 0.0031(9) C14 0.0433(14) 0.0266(11) 0.0277(14) -0.0071(10) 0.0047(11) 0.0056(10) C15 0.0362(13) 0.0335(12) 0.0301(15) -0.0065(10) -0.0043(11) -0.0049(10) C16 0.0223(11) 0.0385(12) 0.0342(15) -0.0032(11) -0.0007(10) -0.0023(9) C17 0.0212(10) 0.0246(10) 0.0244(12) -0.0018(9) 0.0043(9) 0.0010(8) C18 0.0167(9) 0.0213(9) 0.0182(11) 0.0028(8) 0.0044(8) 0.0000(7) C19 0.0298(11) 0.0227(10) 0.0231(12) -0.0004(9) 0.0016(9) 0.0041(8) C20 0.0306(12) 0.0352(12) 0.0212(13) -0.0004(10) -0.0006(9) 0.0034(9) C21 0.0254(11) 0.0335(12) 0.0279(14) 0.0092(10) 0.0036(10) 0.0075(9) C22 0.0296(12) 0.0229(11) 0.0347(14) 0.0046(10) 0.0070(10) 0.0069(9) C23 0.0261(11) 0.0216(10) 0.0256(13) 0.0007(9) 0.0039(9) -0.0005(8) O 0.0229(7) 0.0241(7) 0.0202(8) 0.0002(6) 0.0093(6) 0.0013(5) Si 0.0163(3) 0.0174(3) 0.0145(3) 0.0002(2) 0.0031(2) 0.0013(2) 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 C7 C2 C8 108.37(15) . . C7 C2 C3 107.86(15) . . C8 C2 C3 108.16(16) . . C7 C2 Si 112.29(13) . . C8 C2 Si 110.46(12) . . C3 C2 Si 109.57(12) . . C4 C3 C2 110.73(16) . . C10 C4 C5 110.01(18) . . C10 C4 C3 109.22(17) . . C5 C4 C3 109.63(18) . . C4 C5 C6 109.29(16) . . C11 C6 C5 109.43(18) . . C11 C6 C7 109.22(16) . . C5 C6 C7 109.51(16) . . C6 C7 C2 110.95(16) . . C9 C8 C2 110.15(15) . . C11 C9 C10 109.51(17) . . C11 C9 C8 109.26(18) . . C10 C9 C8 109.43(17) . . C4 C10 C9 109.70(17) . . C9 C11 C6 109.96(17) . . C13 C12 C17 116.88(19) . . C13 C12 Si 124.56(15) . . C17 C12 Si 118.48(15) . . C14 C13 C12 121.4(2) . . C15 C14 C13 120.3(2) . . C16 C15 C14 119.5(2) . . C15 C16 C17 120.1(2) . . C16 C17 C12 121.8(2) . . C23 C18 C19 116.22(18) . . C23 C18 Si 126.10(15) . . C19 C18 Si 117.63(14) . . C20 C19 C18 122.52(19) . . C21 C20 C19 119.5(2) . . C22 C21 C20 119.5(2) . . C21 C22 C23 120.7(2) . . C22 C23 C18 121.5(2) . . C1 O Si 123.34(14) . . O Si C18 108.01(8) . . O Si C12 109.03(8) . . C18 Si C12 112.18(8) . . O Si C2 104.71(7) . . C18 Si C2 112.60(8) . . C12 Si C2 109.97(8) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 O 1.432(2) . C2 C7 1.547(3) . C2 C8 1.551(3) . C2 C3 1.552(2) . C2 Si 1.8844(18) . C3 C4 1.534(3) . C4 C10 1.525(3) . C4 C5 1.531(3) . C5 C6 1.533(3) . C6 C11 1.531(3) . C6 C7 1.535(3) . C8 C9 1.546(3) . C9 C11 1.531(3) . C9 C10 1.532(3) . C12 C13 1.402(3) . C12 C17 1.403(3) . C12 Si 1.880(2) . C13 C14 1.392(3) . C14 C15 1.386(3) . C15 C16 1.385(3) . C16 C17 1.387(3) . C18 C23 1.402(3) . C18 C19 1.408(3) . C18 Si 1.8771(19) . C19 C20 1.389(3) . C20 C21 1.387(3) . C21 C22 1.382(3) . C22 C23 1.392(3) . O Si 1.6459(14) .