#------------------------------------------------------------------------------ #$Date: 2024-10-19 03:01:23 +0300 (Sat, 19 Oct 2024) $ #$Revision: 295545 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/28/1572886.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_1572886 loop_ _publ_author_name 'Cadeddu, Stefano' 'van den Bersselaar, Bart' 'de Waal, Bas FM' 'Cordier, Marie' 'Vanthuyne, Nicolas' 'Meskers, Stefan C. J.' 'Vantomme, Ghislaine' 'Crassous, Jeanne' _publ_section_title ; Engineering Circularly Polarized Light Emission in Nanostructured Oligodimethylsiloxane-Helicene Chiral Materials ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D4NR03389B _journal_year 2024 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C68 H82 N2 O6 Si6' _chemical_formula_sum 'C68 H82 N2 O6 Si6' _chemical_formula_weight 1191.89 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_update_record ; 2024-07-08 deposited with the CCDC. 2024-10-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.551(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 38.942(7) _cell_length_b 9.5940(16) _cell_length_c 19.295(2) _cell_measurement_reflns_used 9383 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.0040 _cell_measurement_theta_min 2.3898 _cell_measurement_wavelength 0.710730 _cell_volume 7036.5(19) _computing_cell_refinement 'Bruker APEX2 (Bruker, 2014)' _computing_data_collection 'Bruker APEX2 (Bruker, 2014)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2014)' _computing_molecular_graphics ; 'PLATON, A.L.Spek, Acta Cryst. 2009, D65, 148-155' ; _computing_publication_material 'CRYSCALC (T. Roisnel, local program, ver. 2022)' _computing_structure_refinement 'SHELXL-2018_3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018_2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150(2) _diffrn_detector CMOS-PHOTON70 _diffrn_detector_area_resol_mean 8.33 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'D8 VENTURE Bruker AXS' _diffrn_measurement_method 'rotation images' _diffrn_orient_matrix_UB_11 -0.0210991 _diffrn_orient_matrix_UB_12 -0.0579850 _diffrn_orient_matrix_UB_13 -0.0205248 _diffrn_orient_matrix_UB_21 -0.0157082 _diffrn_orient_matrix_UB_22 0.0768354 _diffrn_orient_matrix_UB_23 0.0095057 _diffrn_orient_matrix_UB_31 -0.0004124 _diffrn_orient_matrix_UB_32 0.0399787 _diffrn_orient_matrix_UB_33 -0.0480382 _diffrn_radiation_monochromator 'multilayer monochromator' _diffrn_radiation_probe x-ray _diffrn_radiation_source 'Incoatec microfocus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_unetI/netI 0.0399 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 36759 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.143 _diffrn_source_current 1.00 _diffrn_source_power 1500.0 _diffrn_source_voltage 50.00 _exptl_absorpt_coefficient_mu 0.166 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_correction_T_min 0.892 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.125 _exptl_crystal_description stick _exptl_crystal_F_000 2544 _exptl_crystal_size_max 0.680 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.249 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.036 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 683 _refine_ls_number_reflns 7171 _refine_ls_number_restraints 295 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0509 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+3.9828P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1249 _refine_ls_wR_factor_ref 0.1352 _reflns_number_gt 5564 _reflns_number_total 7171 _reflns_threshold_expression >2sigma(I) _cod_data_source_file d4nr03389b2.cif _cod_data_source_block rac-Hel-Si3 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 1572886 _shelx_res_file ; TITL SC121 [Space group= C2/c] job.res created by SHELXL-2018/3 at 18:00:41 on 20-Sep-2022 CELL 0.71073 38.9420 9.5940 19.2950 90.000 102.551 90.000 ZERR 4 0.0070 0.0016 0.0020 0.000 0.006 0.000 LATT 7 SYMM - X , Y , 0.50000 - Z SFAC C H N O SI UNIT 272 328 8 24 24 TEMP -123 SIZE 0.0900 0.2100 0.6800 L.S. 15 FMAP 2 SHEL 20.0 0.80 EADP SI1 SI1B SI1C EADP SI2 SI2B SI2C EADP SI3 SI3B SI3C ISOR 0.004 C1 > C7 ISOR 0.004 C1B > C7B ISOR 0.004 C1C > C7C PLAN -20 ACTA ISOR 0.004 SI1 > C7C REM EADP O3 O3B O3C ISOR 0.004 O3 O3B O3C CONF BOND $H SUMP 1.0 0.00004 1.0 2 1.0 3 1.0 4 WGHT 0.059600 3.982800 FVAR 0.24503 0.34524 0.25886 0.39582 PART -1 21.0 SI1 5 0.179857 -0.603095 -0.020274 21.00000 0.07988 0.07433 = 0.06735 -0.00812 0.02961 0.00523 SI2 5 0.153790 -0.298869 0.030329 21.00000 0.06164 0.06212 = 0.05445 -0.00866 0.00803 0.00304 SI3 5 0.203911 -0.270476 0.176834 21.00000 0.04510 0.04274 = 0.04972 -0.00206 0.00930 0.00284 O1 4 0.175519 -0.435509 0.005348 21.00000 0.11496 0.10843 = 0.12507 -0.02324 0.03989 -0.00080 O2 4 0.171857 -0.310287 0.113060 21.00000 0.06171 0.06008 = 0.06124 -0.00494 0.00804 0.00222 C1 1 0.220268 -0.594203 -0.054092 21.00000 0.10874 0.13571 = 0.12111 -0.00117 0.04979 -0.00417 AFIX 137 H1A 2 0.218910 -0.514965 -0.086628 21.00000 -1.50000 H1B 2 0.223008 -0.680622 -0.079426 21.00000 -1.50000 H1C 2 0.240506 -0.582267 -0.014314 21.00000 -1.50000 AFIX 0 C2 1 0.143067 -0.651485 -0.098640 21.00000 0.08320 0.09721 = 0.08215 -0.00264 0.00766 0.00229 AFIX 137 H2A 2 0.120286 -0.631958 -0.086919 21.00000 -1.50000 H2B 2 0.144608 -0.750921 -0.109184 21.00000 -1.50000 H2C 2 0.145338 -0.596524 -0.140221 21.00000 -1.50000 AFIX 0 C3 1 0.179024 -0.698137 0.056562 21.00000 0.11105 0.11046 = 0.10295 0.00963 0.02069 -0.00394 AFIX 137 H3A 2 0.202725 -0.701123 0.086893 21.00000 -1.50000 H3B 2 0.170959 -0.793280 0.043582 21.00000 -1.50000 H3C 2 0.162922 -0.653328 0.082318 21.00000 -1.50000 AFIX 0 C4 1 0.168489 -0.146511 -0.009443 21.00000 0.10305 0.09655 = 0.08748 0.01637 0.00581 0.00266 AFIX 137 H4A 2 0.194239 -0.146650 -0.000674 21.00000 -1.50000 H4B 2 0.160529 -0.062611 0.011426 21.00000 -1.50000 H4C 2 0.158697 -0.147374 -0.060720 21.00000 -1.50000 AFIX 0 C5 1 0.106798 -0.319373 0.012352 21.00000 0.05539 0.05407 = 0.06503 -0.00253 -0.00885 -0.00198 AFIX 137 H5A 2 0.098030 -0.339358 -0.038211 21.00000 -1.50000 H5B 2 0.096003 -0.233271 0.024781 21.00000 -1.50000 H5C 2 0.100744 -0.396666 0.040687 21.00000 -1.50000 AFIX 0 C6 1 0.239946 -0.200173 0.139432 21.00000 0.05805 0.07028 = 0.06987 -0.00462 0.01743 -0.00373 AFIX 137 H6A 2 0.244424 -0.262957 0.102315 21.00000 -1.50000 H6B 2 0.261259 -0.192159 0.177078 21.00000 -1.50000 H6C 2 0.233348 -0.107957 0.118980 21.00000 -1.50000 AFIX 0 C7 1 0.213230 -0.437615 0.220775 21.00000 0.10865 0.09651 = 0.10325 0.00232 0.01827 0.00206 AFIX 137 H7A 2 0.191102 -0.486795 0.220083 21.00000 -1.50000 H7B 2 0.225759 -0.422924 0.270055 21.00000 -1.50000 H7C 2 0.227868 -0.493456 0.195934 21.00000 -1.50000 AFIX 0 C8 1 0.193560 -0.139102 0.250898 21.00000 0.02889 0.02805 = 0.03125 -0.00296 0.00579 0.00165 AFIX 23 H8A 2 0.176372 -0.183621 0.274921 21.00000 -1.20000 H8B 2 0.215478 -0.123130 0.287063 21.00000 -1.20000 AFIX 0 C9 1 0.178508 0.005575 0.220220 21.00000 0.05049 0.05157 = 0.05073 0.00301 0.01080 -0.00060 AFIX 23 H9A 2 0.198631 0.067197 0.217987 21.00000 -1.20000 H9B 2 0.165222 -0.009209 0.170880 21.00000 -1.20000 AFIX 0 C10 1 0.156938 0.074917 0.256575 21.00000 0.04340 0.03969 = 0.04317 0.00108 0.00598 0.00057 AFIX 23 H10A 2 0.170367 0.090733 0.305718 21.00000 -1.20000 H10B 2 0.137036 0.012576 0.259443 21.00000 -1.20000 AFIX 0 C11 1 0.141198 0.219854 0.225522 21.00000 0.04007 0.03734 = 0.03841 0.00225 0.00947 -0.00150 AFIX 23 H11A 2 0.160342 0.281639 0.217599 21.00000 -1.20000 H11B 2 0.124501 0.205440 0.179478 21.00000 -1.20000 AFIX 0 C12 1 0.122671 0.285278 0.277414 21.00000 0.04408 0.04350 = 0.04282 0.00079 0.01249 0.00070 AFIX 23 H12A 2 0.139576 0.321902 0.319352 21.00000 -1.20000 H12B 2 0.106606 0.218405 0.293287 21.00000 -1.20000 AFIX 0 O3 4 0.102740 0.400535 0.234294 21.00000 0.04471 0.05040 = 0.04932 -0.00037 0.01580 0.00233 PART -2 31.0 rem SAME 0.004 SI1 > O3 SI1B 5 0.191620 -0.601531 0.003159 31.00000 0.07988 0.07433 = 0.06735 -0.00812 0.02961 0.00523 SI2B 5 0.157221 -0.331636 0.033383 31.00000 0.06164 0.06212 = 0.05445 -0.00866 0.00803 0.00304 SI3B 5 0.201174 -0.270310 0.188170 31.00000 0.04510 0.04274 = 0.04972 -0.00206 0.00930 0.00284 O1B 4 0.170889 -0.486674 0.035203 31.00000 0.06699 0.05229 = 0.04554 0.00213 0.01282 0.01062 O2B 4 0.170190 -0.261208 0.111405 31.00000 0.05029 0.04570 = 0.04785 0.00354 0.00852 -0.00051 C1B 1 0.235173 -0.547031 0.017316 31.00000 0.10697 0.11251 = 0.11763 -0.00767 0.02977 -0.00545 AFIX 137 H1D 2 0.236106 -0.452566 -0.001511 31.00000 -1.50000 H1E 2 0.248390 -0.610630 -0.006916 31.00000 -1.50000 H1F 2 0.245571 -0.547181 0.068352 31.00000 -1.50000 AFIX 0 C2B 1 0.174666 -0.625051 -0.095551 31.00000 0.16903 0.16435 = 0.14508 -0.02536 0.03908 0.00414 AFIX 137 H2D 2 0.151088 -0.584424 -0.109641 31.00000 -1.50000 H2E 2 0.173580 -0.724668 -0.107056 31.00000 -1.50000 H2F 2 0.190534 -0.578264 -0.121169 31.00000 -1.50000 AFIX 0 C3B 1 0.179932 -0.769479 0.034522 31.00000 0.08589 0.08877 = 0.09361 0.00873 0.01664 0.00487 AFIX 137 H3D 2 0.199169 -0.802951 0.072395 31.00000 -1.50000 H3E 2 0.175812 -0.836300 -0.004833 31.00000 -1.50000 H3F 2 0.158500 -0.759936 0.052951 31.00000 -1.50000 AFIX 0 C4B 1 0.174067 -0.222934 -0.022740 31.00000 0.10180 0.09451 = 0.09351 0.00436 0.01075 -0.00332 AFIX 137 H4D 2 0.174039 -0.271755 -0.067366 31.00000 -1.50000 H4E 2 0.198208 -0.196566 -0.000070 31.00000 -1.50000 H4F 2 0.159486 -0.138971 -0.032542 31.00000 -1.50000 AFIX 0 C5B 1 0.109608 -0.361395 0.013053 31.00000 0.08395 0.09349 = 0.09236 -0.00753 0.00653 0.00252 AFIX 137 H5D 2 0.103282 -0.423889 -0.027915 31.00000 -1.50000 H5E 2 0.097342 -0.272272 0.002019 31.00000 -1.50000 H5F 2 0.102734 -0.403943 0.054182 31.00000 -1.50000 AFIX 0 C6B 1 0.242991 -0.247307 0.166507 31.00000 0.09270 0.08642 = 0.08411 -0.00191 0.02460 -0.00091 AFIX 137 H6D 2 0.248607 -0.329605 0.140991 31.00000 -1.50000 H6E 2 0.261012 -0.234975 0.210212 31.00000 -1.50000 H6F 2 0.242369 -0.164683 0.136395 31.00000 -1.50000 AFIX 0 C7B 1 0.200160 -0.450810 0.230743 31.00000 0.06098 0.05347 = 0.07489 0.00413 0.01355 0.00360 AFIX 137 H7D 2 0.176638 -0.468296 0.239313 31.00000 -1.50000 H7E 2 0.217497 -0.453897 0.275908 31.00000 -1.50000 H7F 2 0.205829 -0.522332 0.198729 31.00000 -1.50000 AFIX 0 C8B 1 0.185465 -0.152422 0.246777 31.00000 0.02852 0.02507 = 0.02894 -0.00309 0.00739 0.00220 AFIX 23 H8C 2 0.164905 -0.194663 0.261232 31.00000 -1.20000 H8D 2 0.204125 -0.138883 0.290117 31.00000 -1.20000 AFIX 0 C9B 1 0.174464 -0.005146 0.211440 31.00000 0.03627 0.03651 = 0.03575 0.00214 0.00959 -0.00381 AFIX 23 H9C 2 0.194977 0.040289 0.198321 31.00000 -1.20000 H9D 2 0.155810 -0.016720 0.167918 31.00000 -1.20000 AFIX 0 C10B 1 0.161433 0.080983 0.263706 31.00000 0.03844 0.03677 = 0.03879 0.00215 0.00710 -0.00058 AFIX 23 H10C 2 0.181042 0.092026 0.305626 31.00000 -1.20000 H10D 2 0.142832 0.027018 0.279417 31.00000 -1.20000 AFIX 0 C11B 1 0.146345 0.228943 0.242204 31.00000 0.03959 0.03831 = 0.03964 -0.00201 0.00725 -0.00116 AFIX 23 H11C 2 0.166255 0.294691 0.255977 31.00000 -1.20000 H11D 2 0.139728 0.229986 0.189680 31.00000 -1.20000 AFIX 0 C12B 1 0.117941 0.288119 0.265926 31.00000 0.03749 0.03940 = 0.03908 -0.00047 0.01174 -0.00016 AFIX 23 H12C 2 0.097804 0.223124 0.253304 31.00000 -1.20000 H12D 2 0.124525 0.292451 0.318409 31.00000 -1.20000 AFIX 0 O3B 4 0.106758 0.412962 0.242662 31.00000 0.02693 0.03079 = 0.02627 -0.00650 0.00717 -0.00090 PART 3 41.0 rem SAME 0.004 SI1 > O3 SI1C 5 0.179884 -0.590659 -0.015654 41.00000 0.07988 0.07433 = 0.06735 -0.00812 0.02961 0.00523 SI2C 5 0.155050 -0.313066 0.035128 41.00000 0.06164 0.06212 = 0.05445 -0.00866 0.00803 0.00304 SI3C 5 0.201668 -0.279518 0.186048 41.00000 0.04510 0.04274 = 0.04972 -0.00206 0.00930 0.00284 O1C 4 0.158215 -0.464181 0.006832 41.00000 0.08466 0.08997 = 0.10798 -0.03266 0.03039 0.00377 O2C 4 0.166684 -0.286607 0.121540 41.00000 0.04271 0.05294 = 0.04814 -0.00045 0.01067 -0.00254 C1C 1 0.225434 -0.551754 -0.024710 41.00000 0.10360 0.12772 = 0.12007 0.00255 0.04693 -0.02032 AFIX 137 H1G 2 0.225030 -0.473654 -0.057612 41.00000 -1.50000 H1H 2 0.235393 -0.634085 -0.043121 41.00000 -1.50000 H1I 2 0.239908 -0.527000 0.021827 41.00000 -1.50000 AFIX 0 C2C 1 0.154898 -0.647553 -0.096847 41.00000 0.10663 0.11798 = 0.09462 -0.02163 0.03159 -0.00181 AFIX 137 H2G 2 0.130104 -0.653336 -0.094102 41.00000 -1.50000 H2H 2 0.163128 -0.739753 -0.107904 41.00000 -1.50000 H2I 2 0.157411 -0.581568 -0.134199 41.00000 -1.50000 AFIX 0 C3C 1 0.188137 -0.745677 0.057167 41.00000 0.10710 0.09556 = 0.08783 0.00490 0.03798 -0.00022 AFIX 137 H3G 2 0.205464 -0.715318 0.099213 41.00000 -1.50000 H3H 2 0.196983 -0.828337 0.036825 41.00000 -1.50000 H3I 2 0.165961 -0.768466 0.070736 41.00000 -1.50000 AFIX 0 C4C 1 0.177790 -0.189041 -0.019025 41.00000 0.09546 0.08932 = 0.06986 0.01872 0.02198 -0.01152 AFIX 137 H4G 2 0.201727 -0.222176 -0.017726 41.00000 -1.50000 H4H 2 0.178786 -0.095187 0.001363 41.00000 -1.50000 H4I 2 0.164453 -0.186520 -0.068323 41.00000 -1.50000 AFIX 0 C5C 1 0.106795 -0.267031 0.015656 41.00000 0.07126 0.08362 = 0.07469 -0.00367 0.00413 0.00515 AFIX 137 H5G 2 0.096690 -0.280954 -0.034986 41.00000 -1.50000 H5H 2 0.104018 -0.169276 0.028121 41.00000 -1.50000 H5I 2 0.094614 -0.326953 0.043722 41.00000 -1.50000 AFIX 0 C6C 1 0.243157 -0.228167 0.155502 41.00000 0.04375 0.05751 = 0.06079 -0.00009 0.01837 -0.00126 AFIX 137 H6G 2 0.247779 -0.296337 0.120816 41.00000 -1.50000 H6H 2 0.263094 -0.226048 0.196434 41.00000 -1.50000 H6I 2 0.239987 -0.135648 0.133512 41.00000 -1.50000 AFIX 0 C7C 1 0.212159 -0.443830 0.233872 41.00000 0.06810 0.03628 = 0.07714 0.01483 0.00889 0.01479 AFIX 137 H7G 2 0.193342 -0.467380 0.258308 41.00000 -1.50000 H7H 2 0.234426 -0.434224 0.268789 41.00000 -1.50000 H7I 2 0.214333 -0.517999 0.200167 41.00000 -1.50000 AFIX 0 C8C 1 0.189640 -0.144147 0.234044 41.00000 0.06016 0.10844 = 0.04220 0.01688 0.00642 -0.01246 AFIX 23 H8E 2 0.170852 -0.182138 0.255900 41.00000 -1.20000 H8F 2 0.210153 -0.128122 0.273636 41.00000 -1.20000 AFIX 0 C9C 1 0.177559 -0.005412 0.208634 41.00000 0.04867 0.04287 = 0.08041 -0.00800 0.04065 0.01162 AFIX 23 H9E 2 0.159191 -0.015990 0.164585 41.00000 -1.20000 H9F 2 0.197536 0.045027 0.196070 41.00000 -1.20000 AFIX 0 C10C 1 0.161284 0.092944 0.265469 41.00000 0.05507 0.06137 = 0.10050 -0.02425 0.04498 0.00104 AFIX 23 H10E 2 0.143324 0.039984 0.283809 41.00000 -1.20000 H10F 2 0.180314 0.119885 0.306183 41.00000 -1.20000 AFIX 0 C11C 1 0.145638 0.216100 0.228238 41.00000 0.06083 0.06208 = 0.10171 -0.01121 0.06364 0.01017 AFIX 23 H11E 2 0.131232 0.192206 0.180859 41.00000 -1.20000 H11F 2 0.163844 0.284624 0.222614 41.00000 -1.20000 AFIX 0 C12C 1 0.121571 0.274820 0.279772 41.00000 0.06049 0.04742 = 0.07310 0.01946 0.02976 0.03073 AFIX 23 H12E 2 0.100631 0.214839 0.277028 41.00000 -1.20000 H12F 2 0.135074 0.276360 0.329562 41.00000 -1.20000 AFIX 0 O3C 4 0.110648 0.419120 0.255349 41.00000 0.04219 0.04959 = 0.04417 -0.00071 0.01520 0.00073 PART 0 N1 3 -0.094564 -0.007745 0.619412 11.00000 0.13562 0.16560 = 0.08336 0.00686 0.04223 -0.08510 C13 1 0.080751 0.471025 0.272071 11.00000 0.03862 0.04173 = 0.04887 0.00018 0.01619 0.00164 C14 1 0.064621 0.406735 0.319634 11.00000 0.04412 0.03355 = 0.04739 0.00543 0.01412 0.00521 AFIX 43 H14 2 0.071376 0.315303 0.336020 11.00000 -1.20000 AFIX 0 C15 1 0.037764 0.477884 0.344169 11.00000 0.03830 0.03596 = 0.03672 -0.00043 0.00900 -0.00189 C16 1 0.027483 0.608746 0.319506 11.00000 0.03726 0.03345 = 0.03792 -0.00204 0.00889 0.00024 AFIX 43 H16 2 0.009618 0.655533 0.337054 11.00000 -1.20000 AFIX 0 C17 1 0.042878 0.675124 0.268698 11.00000 0.03746 0.03264 = 0.03888 -0.00116 0.00460 -0.00507 C18 1 0.071186 0.608188 0.247271 11.00000 0.03872 0.04027 = 0.04260 0.00112 0.00974 -0.00593 C19 1 0.090528 0.680600 0.203533 11.00000 0.04548 0.05415 = 0.05611 0.00652 0.01780 -0.00678 AFIX 43 H19 2 0.108434 0.633820 0.186114 11.00000 -1.20000 AFIX 0 C20 1 0.083315 0.815499 0.187022 11.00000 0.05101 0.05479 = 0.06166 0.01397 0.01538 -0.01539 AFIX 43 H20 2 0.097780 0.864745 0.161546 11.00000 -1.20000 AFIX 0 C21 1 0.054745 0.886649 0.206487 11.00000 0.05239 0.03972 = 0.05038 0.00687 0.00157 -0.01295 C22 1 0.031831 0.812606 0.240792 11.00000 0.04613 0.03290 = 0.03980 -0.00023 0.00171 -0.00784 C23 1 0.000000 0.880992 0.250000 10.50000 0.05164 0.03002 = 0.03889 0.00000 0.00036 0.00000 C24 1 0.000000 1.028641 0.250000 10.50000 0.06401 0.03209 = 0.05056 0.00000 -0.00751 0.00000 C25 1 0.025156 1.101800 0.220118 11.00000 0.07724 0.03107 = 0.06953 0.00639 -0.00558 -0.01044 AFIX 43 H25 2 0.024621 1.200749 0.218349 11.00000 -1.20000 AFIX 0 C26 1 0.049774 1.031792 0.194266 11.00000 0.06702 0.04443 = 0.06398 0.01329 0.00152 -0.01794 AFIX 43 H26 2 0.063870 1.080204 0.167682 11.00000 -1.20000 AFIX 0 C27 1 0.020014 0.410365 0.392900 11.00000 0.04419 0.03381 = 0.04225 0.00148 0.01296 0.00508 C28 1 0.003637 0.354103 0.430413 11.00000 0.04934 0.03852 = 0.04804 0.00056 0.01778 0.00351 C29 1 -0.017040 0.282315 0.472172 11.00000 0.05335 0.03994 = 0.04446 -0.00223 0.02073 -0.00283 C30 1 -0.001994 0.185284 0.522378 11.00000 0.05680 0.05051 = 0.04980 0.00410 0.01892 0.00285 AFIX 43 H30 2 0.022646 0.169244 0.531096 11.00000 -1.20000 AFIX 0 C31 1 -0.022156 0.111225 0.560100 11.00000 0.08009 0.04875 = 0.04766 0.00495 0.02043 -0.00514 AFIX 43 H31 2 -0.011440 0.044121 0.594214 11.00000 -1.20000 AFIX 0 C32 1 -0.057575 0.134404 0.548388 11.00000 0.07335 0.06971 = 0.04571 -0.00381 0.02324 -0.02831 C33 1 -0.072901 0.232785 0.499224 11.00000 0.05024 0.13266 = 0.08737 0.02969 0.02487 -0.00588 AFIX 43 H33 2 -0.097465 0.249955 0.491544 11.00000 -1.20000 AFIX 0 C34 1 -0.052741 0.306682 0.460993 11.00000 0.05591 0.09623 = 0.08282 0.03806 0.02663 0.01128 AFIX 43 H34 2 -0.063471 0.374122 0.427083 11.00000 -1.20000 AFIX 0 C35 1 -0.078576 0.056181 0.587809 11.00000 0.09687 0.10889 = 0.05792 -0.00434 0.02511 -0.05182 HKLF 4 REM SC121 [Space group= C2/c] REM wR2 = 0.1352, GooF = S = 1.056, Restrained GooF = 1.066 for all data REM R1 = 0.0509 for 5564 Fo > 4sig(Fo) and 0.0687 for all 7171 data REM 683 parameters refined using 295 restraints END WGHT 0.0595 3.9624 REM Highest difference peak 0.249, deepest hole -0.244, 1-sigma level 0.036 Q1 1 0.1555 -0.4135 -0.0276 11.00000 0.05 0.25 Q2 1 0.0202 0.3325 0.4113 11.00000 0.05 0.19 Q3 1 0.0798 0.6317 0.2218 11.00000 0.05 0.18 Q4 1 0.0048 0.4385 0.4183 11.00000 0.05 0.17 Q5 1 0.0371 0.7422 0.2585 11.00000 0.05 0.17 Q6 1 0.1882 -0.4507 0.0422 11.00000 0.05 0.17 Q7 1 0.0723 0.5344 0.2509 11.00000 0.05 0.16 Q8 1 -0.0639 0.2179 0.5398 11.00000 0.05 0.16 Q9 1 0.0386 0.8322 0.2067 11.00000 0.05 0.15 Q10 1 0.0786 0.5504 0.2719 11.00000 0.05 0.15 Q11 1 0.0413 0.6578 0.3067 11.00000 0.05 0.15 Q12 1 0.0328 0.4547 0.3777 11.00000 0.05 0.15 Q13 1 0.0469 0.4426 0.3224 11.00000 0.05 0.15 Q14 1 0.0395 0.5525 0.3466 11.00000 0.05 0.15 Q15 1 0.0511 0.6218 0.2414 11.00000 0.05 0.15 Q16 1 0.0907 0.7498 0.2215 11.00000 0.05 0.15 Q17 1 0.0531 0.4588 0.3342 11.00000 0.05 0.14 Q18 1 0.0834 0.4554 0.3181 11.00000 0.05 0.14 Q19 1 0.1815 -0.5090 0.0714 11.00000 0.05 0.14 Q20 1 -0.0071 0.2764 0.5168 11.00000 0.05 0.14 ; _shelx_res_checksum 3745 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 Si1 Si 0.1799(5) -0.6031(18) -0.0203(9) 0.0718(7) Uani 0.345(3) 1 d . U P A -1 Si2 Si 0.1538(6) -0.2989(17) 0.0303(11) 0.0601(9) Uani 0.345(3) 1 d . U P A -1 Si3 Si 0.2039(4) -0.2705(18) 0.1768(7) 0.0460(8) Uani 0.345(3) 1 d . U P A -1 O1 O 0.1755(3) -0.4355(11) 0.0053(7) 0.114(3) Uani 0.345(3) 1 d . U P A -1 O2 O 0.1719(4) -0.3103(18) 0.1131(9) 0.062(3) Uani 0.345(3) 1 d . U P A -1 C1 C 0.2203(4) -0.5942(18) -0.0541(8) 0.118(5) Uani 0.345(3) 1 d . U P A -1 H1A H 0.218910 -0.514965 -0.086628 0.177 Uiso 0.345(3) 1 calc R U P A -1 H1B H 0.223008 -0.680622 -0.079426 0.177 Uiso 0.345(3) 1 calc R U P A -1 H1C H 0.240506 -0.582267 -0.014314 0.177 Uiso 0.345(3) 1 calc R U P A -1 C2 C 0.1431(4) -0.651(2) -0.0986(11) 0.089(4) Uani 0.345(3) 1 d . U P A -1 H2A H 0.120286 -0.631958 -0.086919 0.134 Uiso 0.345(3) 1 calc R U P A -1 H2B H 0.144608 -0.750921 -0.109184 0.134 Uiso 0.345(3) 1 calc R U P A -1 H2C H 0.145338 -0.596524 -0.140221 0.134 Uiso 0.345(3) 1 calc R U P A -1 C3 C 0.1790(5) -0.6981(17) 0.0566(11) 0.109(5) Uani 0.345(3) 1 d . U P A -1 H3A H 0.202725 -0.701123 0.086893 0.163 Uiso 0.345(3) 1 calc R U P A -1 H3B H 0.170959 -0.793280 0.043582 0.163 Uiso 0.345(3) 1 calc R U P A -1 H3C H 0.162922 -0.653328 0.082318 0.163 Uiso 0.345(3) 1 calc R U P A -1 C4 C 0.1685(4) -0.1465(17) -0.0094(9) 0.098(5) Uani 0.345(3) 1 d . U P A -1 H4A H 0.194239 -0.146650 -0.000674 0.147 Uiso 0.345(3) 1 calc R U P A -1 H4B H 0.160529 -0.062611 0.011426 0.147 Uiso 0.345(3) 1 calc R U P A -1 H4C H 0.158697 -0.147374 -0.060720 0.147 Uiso 0.345(3) 1 calc R U P A -1 C5 C 0.1068(5) -0.3194(17) 0.0124(10) 0.061(3) Uani 0.345(3) 1 d . U P A -1 H5A H 0.098030 -0.339358 -0.038211 0.092 Uiso 0.345(3) 1 calc R U P A -1 H5B H 0.096003 -0.233271 0.024781 0.092 Uiso 0.345(3) 1 calc R U P A -1 H5C H 0.100744 -0.396666 0.040687 0.092 Uiso 0.345(3) 1 calc R U P A -1 C6 C 0.2399(6) -0.2002(19) 0.1394(10) 0.066(4) Uani 0.345(3) 1 d . U P A -1 H6A H 0.244424 -0.262957 0.102315 0.098 Uiso 0.345(3) 1 calc R U P A -1 H6B H 0.261259 -0.192159 0.177078 0.098 Uiso 0.345(3) 1 calc R U P A -1 H6C H 0.233348 -0.107957 0.118980 0.098 Uiso 0.345(3) 1 calc R U P A -1 C7 C 0.2132(10) -0.438(3) 0.2208(14) 0.104(10) Uani 0.345(3) 1 d . U P A -1 H7A H 0.191102 -0.486795 0.220083 0.155 Uiso 0.345(3) 1 calc R U P A -1 H7B H 0.225759 -0.422924 0.270055 0.155 Uiso 0.345(3) 1 calc R U P A -1 H7C H 0.227868 -0.493456 0.195934 0.155 Uiso 0.345(3) 1 calc R U P A -1 C8 C 0.1936(5) -0.1391(18) 0.2509(8) 0.030(3) Uani 0.345(3) 1 d . U P A -1 H8A H 0.176372 -0.183621 0.274921 0.035 Uiso 0.345(3) 1 calc R U P A -1 H8B H 0.215478 -0.123130 0.287063 0.035 Uiso 0.345(3) 1 calc R U P A -1 C9 C 0.1785(11) 0.006(3) 0.2202(15) 0.051(7) Uani 0.345(3) 1 d . U P A -1 H9A H 0.198631 0.067197 0.217987 0.061 Uiso 0.345(3) 1 calc R U P A -1 H9B H 0.165222 -0.009209 0.170880 0.061 Uiso 0.345(3) 1 calc R U P A -1 C10 C 0.1569(6) 0.075(3) 0.2566(13) 0.043(5) Uani 0.345(3) 1 d . U P A -1 H10A H 0.170367 0.090733 0.305718 0.051 Uiso 0.345(3) 1 calc R U P A -1 H10B H 0.137036 0.012576 0.259443 0.051 Uiso 0.345(3) 1 calc R U P A -1 C11 C 0.1412(5) 0.220(2) 0.2255(14) 0.038(4) Uani 0.345(3) 1 d . U P A -1 H11A H 0.160342 0.281639 0.217599 0.046 Uiso 0.345(3) 1 calc R U P A -1 H11B H 0.124501 0.205440 0.179478 0.046 Uiso 0.345(3) 1 calc R U P A -1 C12 C 0.1227(8) 0.285(4) 0.2774(18) 0.043(7) Uani 0.345(3) 1 d . U P A -1 H12A H 0.139576 0.321902 0.319352 0.052 Uiso 0.345(3) 1 calc R U P A -1 H12B H 0.106606 0.218405 0.293287 0.052 Uiso 0.345(3) 1 calc R U P A -1 O3 O 0.1027(4) 0.4005(17) 0.2343(9) 0.047(4) Uani 0.345(3) 1 d . U P A -1 Si1B Si 0.19162(14) -0.6015(7) 0.0032(3) 0.0718(7) Uani 0.259(3) 1 d . U P A -2 Si2B Si 0.1572(5) -0.3316(14) 0.0334(10) 0.0601(9) Uani 0.259(3) 1 d . U P A -2 Si3B Si 0.2012(8) -0.270(3) 0.1882(16) 0.0460(8) Uani 0.259(3) 1 d . U P A -2 O1B O 0.1709(3) -0.4867(8) 0.0352(4) 0.0548(19) Uani 0.259(3) 1 d . U P A -2 O2B O 0.1702(6) -0.2612(17) 0.1114(10) 0.048(4) Uani 0.259(3) 1 d . U P A -2 C1B C 0.2352(5) -0.547(2) 0.0173(10) 0.112(5) Uani 0.259(3) 1 d . U P A -2 H1D H 0.236106 -0.452566 -0.001511 0.167 Uiso 0.259(3) 1 calc R U P A -2 H1E H 0.248390 -0.610630 -0.006916 0.167 Uiso 0.259(3) 1 calc R U P A -2 H1F H 0.245571 -0.547181 0.068352 0.167 Uiso 0.259(3) 1 calc R U P A -2 C2B C 0.1747(6) -0.625(3) -0.0956(13) 0.159(9) Uani 0.259(3) 1 d . U P A -2 H2D H 0.151088 -0.584424 -0.109641 0.238 Uiso 0.259(3) 1 calc R U P A -2 H2E H 0.173580 -0.724668 -0.107056 0.238 Uiso 0.259(3) 1 calc R U P A -2 H2F H 0.190534 -0.578264 -0.121169 0.238 Uiso 0.259(3) 1 calc R U P A -2 C3B C 0.1799(6) -0.769(2) 0.0345(11) 0.090(6) Uani 0.259(3) 1 d . U P A -2 H3D H 0.199169 -0.802951 0.072395 0.135 Uiso 0.259(3) 1 calc R U P A -2 H3E H 0.175812 -0.836300 -0.004833 0.135 Uiso 0.259(3) 1 calc R U P A -2 H3F H 0.158500 -0.759936 0.052951 0.135 Uiso 0.259(3) 1 calc R U P A -2 C4B C 0.1741(9) -0.223(3) -0.0227(19) 0.098(9) Uani 0.259(3) 1 d . U P A -2 H4D H 0.174039 -0.271755 -0.067366 0.147 Uiso 0.259(3) 1 calc R U P A -2 H4E H 0.198208 -0.196566 -0.000070 0.147 Uiso 0.259(3) 1 calc R U P A -2 H4F H 0.159486 -0.138971 -0.032542 0.147 Uiso 0.259(3) 1 calc R U P A -2 C5B C 0.1096(7) -0.361(2) 0.0131(15) 0.092(7) Uani 0.259(3) 1 d . U P A -2 H5D H 0.103282 -0.423889 -0.027915 0.138 Uiso 0.259(3) 1 calc R U P A -2 H5E H 0.097342 -0.272272 0.002019 0.138 Uiso 0.259(3) 1 calc R U P A -2 H5F H 0.102734 -0.403943 0.054182 0.138 Uiso 0.259(3) 1 calc R U P A -2 C6B C 0.2430(9) -0.247(4) 0.1665(19) 0.087(11) Uani 0.259(3) 1 d . U P A -2 H6D H 0.248607 -0.329605 0.140991 0.130 Uiso 0.259(3) 1 calc R U P A -2 H6E H 0.261012 -0.234975 0.210212 0.130 Uiso 0.259(3) 1 calc R U P A -2 H6F H 0.242369 -0.164683 0.136395 0.130 Uiso 0.259(3) 1 calc R U P A -2 C7B C 0.2002(5) -0.451(3) 0.2307(14) 0.063(5) Uani 0.259(3) 1 d . U P A -2 H7D H 0.176638 -0.468296 0.239313 0.095 Uiso 0.259(3) 1 calc R U P A -2 H7E H 0.217497 -0.453897 0.275908 0.095 Uiso 0.259(3) 1 calc R U P A -2 H7F H 0.205829 -0.522332 0.198729 0.095 Uiso 0.259(3) 1 calc R U P A -2 C8B C 0.1855(6) -0.152(2) 0.2468(14) 0.027(4) Uani 0.259(3) 1 d . U P A -2 H8C H 0.164905 -0.194663 0.261232 0.033 Uiso 0.259(3) 1 calc R U P A -2 H8D H 0.204125 -0.138883 0.290117 0.033 Uiso 0.259(3) 1 calc R U P A -2 C9B C 0.1745(8) -0.005(5) 0.211(2) 0.036(6) Uani 0.259(3) 1 d . U P A -2 H9C H 0.194977 0.040289 0.198321 0.043 Uiso 0.259(3) 1 calc R U P A -2 H9D H 0.155810 -0.016720 0.167918 0.043 Uiso 0.259(3) 1 calc R U P A -2 C10B C 0.1614(9) 0.081(5) 0.2637(19) 0.038(7) Uani 0.259(3) 1 d . U P A -2 H10C H 0.181042 0.092026 0.305626 0.046 Uiso 0.259(3) 1 calc R U P A -2 H10D H 0.142832 0.027018 0.279417 0.046 Uiso 0.259(3) 1 calc R U P A -2 C11B C 0.1463(9) 0.229(2) 0.2422(12) 0.039(5) Uani 0.259(3) 1 d . U P A -2 H11C H 0.166255 0.294691 0.255977 0.047 Uiso 0.259(3) 1 calc R U P A -2 H11D H 0.139728 0.229986 0.189680 0.047 Uiso 0.259(3) 1 calc R U P A -2 C12B C 0.1179(6) 0.288(3) 0.2659(13) 0.038(5) Uani 0.259(3) 1 d . U P A -2 H12C H 0.097804 0.223124 0.253304 0.046 Uiso 0.259(3) 1 calc R U P A -2 H12D H 0.124525 0.292451 0.318409 0.046 Uiso 0.259(3) 1 calc R U P A -2 O3B O 0.1068(7) 0.413(3) 0.2427(14) 0.028(3) Uani 0.259(3) 1 d . U P A -2 Si1C Si 0.1799(5) -0.5907(15) -0.0157(7) 0.0718(7) Uani 0.396(3) 1 d . U P A 3 Si2C Si 0.1550(4) -0.3131(13) 0.0351(9) 0.0601(9) Uani 0.396(3) 1 d . U P A 3 Si3C Si 0.2017(5) -0.280(2) 0.1860(10) 0.0460(8) Uani 0.396(3) 1 d . U P A 3 O1C O 0.15822(18) -0.4642(9) 0.0068(5) 0.093(2) Uani 0.396(3) 1 d . U P A 3 O2C O 0.1667(3) -0.287(2) 0.1215(7) 0.048(2) Uani 0.396(3) 1 d . U P A 3 C1C C 0.2254(4) -0.5518(17) -0.0247(9) 0.114(4) Uani 0.396(3) 1 d . U P A 3 H1G H 0.225030 -0.473654 -0.057612 0.171 Uiso 0.396(3) 1 calc R U P A 3 H1H H 0.235393 -0.634085 -0.043121 0.171 Uiso 0.396(3) 1 calc R U P A 3 H1I H 0.239908 -0.527000 0.021827 0.171 Uiso 0.396(3) 1 calc R U P A 3 C2C C 0.1549(4) -0.648(2) -0.0968(11) 0.105(5) Uani 0.396(3) 1 d . U P A 3 H2G H 0.130104 -0.653336 -0.094102 0.157 Uiso 0.396(3) 1 calc R U P A 3 H2H H 0.163128 -0.739753 -0.107904 0.157 Uiso 0.396(3) 1 calc R U P A 3 H2I H 0.157411 -0.581568 -0.134199 0.157 Uiso 0.396(3) 1 calc R U P A 3 C3C C 0.1881(5) -0.746(2) 0.0572(10) 0.094(4) Uani 0.396(3) 1 d . U P A 3 H3G H 0.205464 -0.715318 0.099213 0.141 Uiso 0.396(3) 1 calc R U P A 3 H3H H 0.196983 -0.828337 0.036825 0.141 Uiso 0.396(3) 1 calc R U P A 3 H3I H 0.165961 -0.768466 0.070736 0.141 Uiso 0.396(3) 1 calc R U P A 3 C4C C 0.1778(6) -0.189(3) -0.0190(12) 0.084(5) Uani 0.396(3) 1 d . U P A 3 H4G H 0.201727 -0.222176 -0.017726 0.126 Uiso 0.396(3) 1 calc R U P A 3 H4H H 0.178786 -0.095187 0.001363 0.126 Uiso 0.396(3) 1 calc R U P A 3 H4I H 0.164453 -0.186520 -0.068323 0.126 Uiso 0.396(3) 1 calc R U P A 3 C5C C 0.1068(4) -0.2670(12) 0.0157(9) 0.078(3) Uani 0.396(3) 1 d . U P A 3 H5G H 0.096690 -0.280954 -0.034986 0.117 Uiso 0.396(3) 1 calc R U P A 3 H5H H 0.104018 -0.169276 0.028121 0.117 Uiso 0.396(3) 1 calc R U P A 3 H5I H 0.094614 -0.326953 0.043722 0.117 Uiso 0.396(3) 1 calc R U P A 3 C6C C 0.2432(5) -0.228(2) 0.1555(13) 0.053(4) Uani 0.396(3) 1 d . U P A 3 H6G H 0.247779 -0.296337 0.120816 0.079 Uiso 0.396(3) 1 calc R U P A 3 H6H H 0.263094 -0.226048 0.196434 0.079 Uiso 0.396(3) 1 calc R U P A 3 H6I H 0.239987 -0.135648 0.133512 0.079 Uiso 0.396(3) 1 calc R U P A 3 C7C C 0.2122(7) -0.4438(17) 0.2339(12) 0.062(3) Uani 0.396(3) 1 d . U P A 3 H7G H 0.193342 -0.467380 0.258308 0.092 Uiso 0.396(3) 1 calc R U P A 3 H7H H 0.234426 -0.434224 0.268789 0.092 Uiso 0.396(3) 1 calc R U P A 3 H7I H 0.214333 -0.517999 0.200167 0.092 Uiso 0.396(3) 1 calc R U P A 3 C8C C 0.1896(7) -0.144(2) 0.2340(8) 0.071(5) Uani 0.396(3) 1 d . . P A 3 H8E H 0.170852 -0.182138 0.255900 0.085 Uiso 0.396(3) 1 calc R U P A 3 H8F H 0.210153 -0.128122 0.273636 0.085 Uiso 0.396(3) 1 calc R U P A 3 C9C C 0.1776(9) -0.005(3) 0.2086(18) 0.053(7) Uani 0.396(3) 1 d . . P A 3 H9E H 0.159191 -0.015990 0.164585 0.064 Uiso 0.396(3) 1 calc R U P A 3 H9F H 0.197536 0.045027 0.196070 0.064 Uiso 0.396(3) 1 calc R U P A 3 C10C C 0.1613(7) 0.093(3) 0.2655(14) 0.068(7) Uani 0.396(3) 1 d . . P A 3 H10E H 0.143324 0.039984 0.283809 0.082 Uiso 0.396(3) 1 calc R U P A 3 H10F H 0.180314 0.119885 0.306183 0.082 Uiso 0.396(3) 1 calc R U P A 3 C11C C 0.1456(8) 0.216(3) 0.2282(19) 0.068(6) Uani 0.396(3) 1 d . . P A 3 H11E H 0.131232 0.192206 0.180859 0.081 Uiso 0.396(3) 1 calc R U P A 3 H11F H 0.163844 0.284624 0.222614 0.081 Uiso 0.396(3) 1 calc R U P A 3 C12C C 0.1216(7) 0.275(3) 0.2798(19) 0.058(6) Uani 0.396(3) 1 d . . P A 3 H12E H 0.100631 0.214839 0.277028 0.070 Uiso 0.396(3) 1 calc R U P A 3 H12F H 0.135074 0.276360 0.329562 0.070 Uiso 0.396(3) 1 calc R U P A 3 O3C O 0.1106(4) 0.4191(16) 0.2553(6) 0.044(3) Uani 0.396(3) 1 d . U P A 3 N1 N -0.09456(8) -0.0077(4) 0.61941(14) 0.1254(12) Uani 1 1 d . . . . . C13 C 0.08075(5) 0.47103(19) 0.27207(10) 0.0421(4) Uani 1 1 d . . . . . C14 C 0.06462(5) 0.40674(19) 0.31963(10) 0.0411(4) Uani 1 1 d . . . . . H14 H 0.071376 0.315303 0.336020 0.049 Uiso 1 1 calc R U . . . C15 C 0.03776(4) 0.47788(18) 0.34417(9) 0.0369(4) Uani 1 1 d . . . . . C16 C 0.02748(4) 0.60875(17) 0.31951(9) 0.0361(4) Uani 1 1 d . . . . . H16 H 0.009618 0.655533 0.337054 0.043 Uiso 1 1 calc R U . . . C17 C 0.04288(4) 0.67512(18) 0.26870(9) 0.0369(4) Uani 1 1 d . . . . . C18 C 0.07119(4) 0.60819(19) 0.24727(9) 0.0404(4) Uani 1 1 d . . . . . C19 C 0.09053(5) 0.6806(2) 0.20353(11) 0.0509(5) Uani 1 1 d . . . . . H19 H 0.108434 0.633820 0.186114 0.061 Uiso 1 1 calc R U . . . C20 C 0.08331(5) 0.8155(2) 0.18702(11) 0.0553(5) Uani 1 1 d . . . . . H20 H 0.097780 0.864745 0.161546 0.066 Uiso 1 1 calc R U . . . C21 C 0.05474(5) 0.8866(2) 0.20649(11) 0.0490(5) Uani 1 1 d . . . . . C22 C 0.03183(5) 0.81261(18) 0.24079(9) 0.0408(4) Uani 1 1 d . . . . . C23 C 0.000000 0.8810(3) 0.250000 0.0416(6) Uani 1 2 d S T P . . C24 C 0.000000 1.0286(3) 0.250000 0.0519(7) Uani 1 2 d S T P . . C25 C 0.02516(6) 1.1018(2) 0.22012(12) 0.0626(6) Uani 1 1 d . . . . . H25 H 0.024621 1.200749 0.218349 0.075 Uiso 1 1 calc R U . . . C26 C 0.04977(6) 1.0318(2) 0.19427(12) 0.0604(6) Uani 1 1 d . . . . . H26 H 0.063870 1.080204 0.167682 0.072 Uiso 1 1 calc R U . . . C27 C 0.02001(5) 0.41037(18) 0.39290(9) 0.0395(4) Uani 1 1 d . . . . . C28 C 0.00364(5) 0.35410(19) 0.43041(10) 0.0442(4) Uani 1 1 d . . . . . C29 C -0.01704(5) 0.2823(2) 0.47217(10) 0.0444(4) Uani 1 1 d . . . . . C30 C -0.00199(6) 0.1853(2) 0.52238(11) 0.0513(5) Uani 1 1 d . . . . . H30 H 0.022646 0.169244 0.531096 0.062 Uiso 1 1 calc R U . . . C31 C -0.02216(6) 0.1112(2) 0.56010(11) 0.0578(5) Uani 1 1 d . . . . . H31 H -0.011440 0.044121 0.594214 0.069 Uiso 1 1 calc R U . . . C32 C -0.05758(6) 0.1344(3) 0.54839(11) 0.0614(6) Uani 1 1 d . . . . . C33 C -0.07290(7) 0.2328(4) 0.49922(15) 0.0886(9) Uani 1 1 d . . . . . H33 H -0.097465 0.249955 0.491544 0.106 Uiso 1 1 calc R U . . . C34 C -0.05274(6) 0.3067(3) 0.46099(14) 0.0766(8) Uani 1 1 d . . . . . H34 H -0.063471 0.374122 0.427083 0.092 Uiso 1 1 calc R U . . . C35 C -0.07858(8) 0.0562(3) 0.58781(14) 0.0866(9) 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 Si1 0.0799(11) 0.0743(16) 0.0674(17) -0.0081(12) 0.0296(11) 0.0052(14) Si2 0.0616(13) 0.062(2) 0.0544(12) -0.0087(17) 0.0080(10) 0.0030(17) Si3 0.0451(11) 0.0427(15) 0.0497(18) -0.0021(15) 0.0093(11) 0.0028(10) O1 0.115(4) 0.108(4) 0.125(4) -0.023(3) 0.040(3) -0.001(3) O2 0.062(4) 0.060(5) 0.061(4) -0.005(3) 0.008(3) 0.002(3) C1 0.109(7) 0.136(8) 0.121(8) -0.001(6) 0.050(6) -0.004(6) C2 0.083(7) 0.097(6) 0.082(6) -0.003(5) 0.008(5) 0.002(6) C3 0.111(8) 0.110(8) 0.103(7) 0.010(6) 0.021(6) -0.004(6) C4 0.103(8) 0.097(8) 0.087(7) 0.016(5) 0.006(5) 0.003(6) C5 0.055(5) 0.054(7) 0.065(5) -0.003(6) -0.009(4) -0.002(6) C6 0.058(6) 0.070(7) 0.070(7) -0.005(5) 0.017(5) -0.004(5) C7 0.109(12) 0.097(11) 0.103(12) 0.002(7) 0.018(7) 0.002(7) C8 0.029(4) 0.028(4) 0.031(4) -0.003(3) 0.006(3) 0.002(3) C9 0.050(8) 0.052(7) 0.051(8) 0.003(4) 0.011(4) -0.001(4) C10 0.043(6) 0.040(6) 0.043(6) 0.001(4) 0.006(4) 0.001(3) C11 0.040(5) 0.037(5) 0.038(5) 0.002(4) 0.009(3) -0.002(3) C12 0.044(8) 0.043(8) 0.043(8) 0.001(4) 0.012(4) 0.001(4) O3 0.045(5) 0.050(5) 0.049(5) 0.000(3) 0.016(3) 0.002(3) Si1B 0.0799(11) 0.0743(16) 0.0674(17) -0.0081(12) 0.0296(11) 0.0052(14) Si2B 0.0616(13) 0.062(2) 0.0544(12) -0.0087(17) 0.0080(10) 0.0030(17) Si3B 0.0451(11) 0.0427(15) 0.0497(18) -0.0021(15) 0.0093(11) 0.0028(10) O1B 0.067(3) 0.052(3) 0.046(3) 0.002(2) 0.013(3) 0.011(3) O2B 0.050(5) 0.046(5) 0.048(5) 0.004(3) 0.009(3) -0.001(3) C1B 0.107(8) 0.113(8) 0.118(8) -0.008(7) 0.030(6) -0.005(6) C2B 0.169(11) 0.164(11) 0.145(11) -0.025(7) 0.039(8) 0.004(8) C3B 0.086(8) 0.089(8) 0.094(9) 0.009(6) 0.017(6) 0.005(6) C4B 0.102(11) 0.095(12) 0.094(10) 0.004(7) 0.011(7) -0.003(7) C5B 0.084(9) 0.093(11) 0.092(9) -0.008(7) 0.007(6) 0.003(7) C6B 0.093(12) 0.086(13) 0.084(13) -0.002(7) 0.025(7) -0.001(7) C7B 0.061(7) 0.053(7) 0.075(7) 0.004(5) 0.014(6) 0.004(6) C8B 0.029(4) 0.025(5) 0.029(5) -0.003(3) 0.007(4) 0.002(3) C9B 0.036(6) 0.037(7) 0.036(7) 0.002(4) 0.010(4) -0.004(4) C10B 0.038(8) 0.037(8) 0.039(8) 0.002(4) 0.007(4) -0.001(4) C11B 0.040(6) 0.038(6) 0.040(6) -0.002(4) 0.007(4) -0.001(4) C12B 0.037(6) 0.039(7) 0.039(6) 0.000(4) 0.012(4) 0.000(4) O3B 0.027(5) 0.031(4) 0.026(5) -0.007(3) 0.007(3) -0.001(3) Si1C 0.0799(11) 0.0743(16) 0.0674(17) -0.0081(12) 0.0296(11) 0.0052(14) Si2C 0.0616(13) 0.062(2) 0.0544(12) -0.0087(17) 0.0080(10) 0.0030(17) Si3C 0.0451(11) 0.0427(15) 0.0497(18) -0.0021(15) 0.0093(11) 0.0028(10) O1C 0.085(3) 0.090(3) 0.108(4) -0.033(3) 0.030(3) 0.004(3) O2C 0.043(3) 0.053(4) 0.048(3) 0.000(3) 0.011(3) -0.003(3) C1C 0.104(6) 0.128(7) 0.120(8) 0.003(6) 0.047(6) -0.020(6) C2C 0.107(9) 0.118(8) 0.095(7) -0.022(5) 0.032(7) -0.002(7) C3C 0.107(8) 0.096(7) 0.088(7) 0.005(6) 0.038(6) 0.000(6) C4C 0.095(7) 0.089(8) 0.070(6) 0.019(6) 0.022(5) -0.012(6) C5C 0.071(5) 0.084(7) 0.075(5) -0.004(6) 0.004(4) 0.005(6) C6C 0.044(5) 0.058(7) 0.061(7) 0.000(6) 0.018(5) -0.001(4) C7C 0.068(7) 0.036(4) 0.077(6) 0.015(4) 0.009(5) 0.015(5) C8C 0.060(7) 0.108(9) 0.042(7) 0.017(5) 0.006(5) -0.012(6) C9C 0.049(9) 0.043(7) 0.080(12) -0.008(6) 0.041(7) 0.012(5) C10C 0.055(8) 0.061(9) 0.101(11) -0.024(6) 0.045(7) 0.001(6) C11C 0.061(8) 0.062(9) 0.102(11) -0.011(7) 0.064(7) 0.010(6) C12C 0.060(9) 0.047(8) 0.073(10) 0.019(6) 0.030(6) 0.031(6) O3C 0.042(4) 0.050(4) 0.044(5) -0.001(3) 0.015(3) 0.001(3) N1 0.136(2) 0.166(3) 0.0834(17) 0.0069(18) 0.0422(17) -0.085(2) C13 0.0386(9) 0.0417(10) 0.0489(10) 0.0002(8) 0.0162(8) 0.0016(8) C14 0.0441(10) 0.0335(9) 0.0474(10) 0.0054(8) 0.0141(8) 0.0052(7) C15 0.0383(9) 0.0360(9) 0.0367(9) -0.0004(7) 0.0090(7) -0.0019(7) C16 0.0373(9) 0.0334(9) 0.0379(9) -0.0020(7) 0.0089(7) 0.0002(7) C17 0.0375(9) 0.0326(9) 0.0389(9) -0.0012(7) 0.0046(7) -0.0051(7) C18 0.0387(9) 0.0403(10) 0.0426(10) 0.0011(8) 0.0097(7) -0.0059(7) C19 0.0455(10) 0.0542(12) 0.0561(12) 0.0065(9) 0.0178(9) -0.0068(9) C20 0.0510(11) 0.0548(12) 0.0617(13) 0.0140(10) 0.0154(10) -0.0154(10) C21 0.0524(11) 0.0397(10) 0.0504(11) 0.0069(8) 0.0016(9) -0.0129(8) C22 0.0461(10) 0.0329(9) 0.0398(10) -0.0002(7) 0.0017(7) -0.0078(7) C23 0.0516(15) 0.0300(12) 0.0389(13) 0.000 0.0004(11) 0.000 C24 0.0640(18) 0.0321(14) 0.0506(16) 0.000 -0.0075(13) 0.000 C25 0.0772(15) 0.0311(10) 0.0695(14) 0.0064(10) -0.0056(12) -0.0104(10) C26 0.0670(14) 0.0444(12) 0.0640(14) 0.0133(10) 0.0015(11) -0.0179(10) C27 0.0442(10) 0.0338(9) 0.0423(10) 0.0015(7) 0.0130(8) 0.0051(7) C28 0.0493(10) 0.0385(10) 0.0480(11) 0.0006(8) 0.0178(9) 0.0035(8) C29 0.0534(11) 0.0399(10) 0.0445(10) -0.0022(8) 0.0207(8) -0.0028(8) C30 0.0568(12) 0.0505(11) 0.0498(11) 0.0041(9) 0.0189(9) 0.0028(9) C31 0.0801(16) 0.0488(12) 0.0477(12) 0.0050(9) 0.0204(11) -0.0051(11) C32 0.0734(15) 0.0697(15) 0.0457(12) -0.0038(11) 0.0232(11) -0.0283(12) C33 0.0502(13) 0.133(3) 0.0874(19) 0.0297(18) 0.0249(13) -0.0059(15) C34 0.0559(13) 0.096(2) 0.0828(17) 0.0381(15) 0.0266(12) 0.0113(13) C35 0.097(2) 0.109(2) 0.0579(15) -0.0043(14) 0.0251(14) -0.0518(18) 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' N N 0.0061 0.0033 '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 O1 Si1 C3 103.0(11) . . ? O1 Si1 C1 101.9(12) . . ? C3 Si1 C1 120.2(13) . . ? O1 Si1 C2 110.9(12) . . ? C3 Si1 C2 113.4(14) . . ? C1 Si1 C2 106.6(11) . . ? O2 Si2 O1 95.3(11) . . ? O2 Si2 C5 113.1(16) . . ? O1 Si2 C5 114.4(12) . . ? O2 Si2 C4 111.6(14) . . ? O1 Si2 C4 106.5(13) . . ? C5 Si2 C4 114.3(12) . . ? O2 Si3 C7 101.1(15) . . ? O2 Si3 C6 108.7(12) . . ? C7 Si3 C6 114.5(16) . . ? O2 Si3 C8 117.0(11) . . ? C7 Si3 C8 105.8(12) . . ? C6 Si3 C8 109.7(12) . . ? Si2 O1 Si1 154.9(12) . . ? Si3 O2 Si2 148.4(18) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 C6 H6A 109.5 . . ? Si3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 Si3 113.7(15) . . ? C9 C8 H8A 108.8 . . ? Si3 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? Si3 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 117(2) . . ? C10 C9 H9A 108.1 . . ? C8 C9 H9A 108.1 . . ? C10 C9 H9B 108.1 . . ? C8 C9 H9B 108.1 . . ? H9A C9 H9B 107.3 . . ? C9 C10 C11 117(2) . . ? C9 C10 H10A 108.0 . . ? C11 C10 H10A 108.0 . . ? C9 C10 H10B 108.0 . . ? C11 C10 H10B 108.0 . . ? H10A C10 H10B 107.2 . . ? C12 C11 C10 109(2) . . ? C12 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? C12 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C11 C12 O3 102(3) . . ? C11 C12 H12A 111.4 . . ? O3 C12 H12A 111.4 . . ? C11 C12 H12B 111.4 . . ? O3 C12 H12B 111.4 . . ? H12A C12 H12B 109.3 . . ? C13 O3 C12 111.5(17) . . ? O1B Si1B C1B 107.1(8) . . ? O1B Si1B C3B 107.7(9) . . ? C1B Si1B C3B 121.4(11) . . ? O1B Si1B C2B 112.6(8) . . ? C1B Si1B C2B 108.0(9) . . ? C3B Si1B C2B 99.9(10) . . ? O1B Si2B O2B 109.6(12) . . ? O1B Si2B C4B 114.2(16) . . ? O2B Si2B C4B 104.2(15) . . ? O1B Si2B C5B 100.3(11) . . ? O2B Si2B C5B 111.0(16) . . ? C4B Si2B C5B 117.6(17) . . ? O2B Si3B C6B 108(2) . . ? O2B Si3B C8B 104(2) . . ? C6B Si3B C8B 122(2) . . ? O2B Si3B C7B 110.0(18) . . ? C6B Si3B C7B 108(2) . . ? C8B Si3B C7B 104.9(18) . . ? Si1B O1B Si2B 148.5(10) . . ? Si2B O2B Si3B 143.6(19) . . ? Si1B C1B H1D 109.5 . . ? Si1B C1B H1E 109.5 . . ? H1D C1B H1E 109.5 . . ? Si1B C1B H1F 109.5 . . ? H1D C1B H1F 109.5 . . ? H1E C1B H1F 109.5 . . ? Si1B C2B H2D 109.5 . . ? Si1B C2B H2E 109.5 . . ? H2D C2B H2E 109.5 . . ? Si1B C2B H2F 109.5 . . ? H2D C2B H2F 109.5 . . ? H2E C2B H2F 109.5 . . ? Si1B C3B H3D 109.5 . . ? Si1B C3B H3E 109.5 . . ? H3D C3B H3E 109.5 . . ? Si1B C3B H3F 109.5 . . ? H3D C3B H3F 109.5 . . ? H3E C3B H3F 109.5 . . ? Si2B C4B H4D 109.5 . . ? Si2B C4B H4E 109.5 . . ? H4D C4B H4E 109.5 . . ? Si2B C4B H4F 109.5 . . ? H4D C4B H4F 109.5 . . ? H4E C4B H4F 109.5 . . ? Si2B C5B H5D 109.5 . . ? Si2B C5B H5E 109.5 . . ? H5D C5B H5E 109.5 . . ? Si2B C5B H5F 109.5 . . ? H5D C5B H5F 109.5 . . ? H5E C5B H5F 109.5 . . ? Si3B C6B H6D 109.5 . . ? Si3B C6B H6E 109.5 . . ? H6D C6B H6E 109.5 . . ? Si3B C6B H6F 109.5 . . ? H6D C6B H6F 109.5 . . ? H6E C6B H6F 109.5 . . ? Si3B C7B H7D 109.5 . . ? Si3B C7B H7E 109.5 . . ? H7D C7B H7E 109.5 . . ? Si3B C7B H7F 109.5 . . ? H7D C7B H7F 109.5 . . ? H7E C7B H7F 109.5 . . ? C9B C8B Si3B 113(2) . . ? C9B C8B H8C 109.0 . . ? Si3B C8B H8C 109.0 . . ? C9B C8B H8D 109.0 . . ? Si3B C8B H8D 109.0 . . ? H8C C8B H8D 107.8 . . ? C10B C9B C8B 108(3) . . ? C10B C9B H9C 110.1 . . ? C8B C9B H9C 110.1 . . ? C10B C9B H9D 110.1 . . ? C8B C9B H9D 110.1 . . ? H9C C9B H9D 108.5 . . ? C9B C10B C11B 120(3) . . ? C9B C10B H10C 107.4 . . ? C11B C10B H10C 107.4 . . ? C9B C10B H10D 107.4 . . ? C11B C10B H10D 107.4 . . ? H10C C10B H10D 107.0 . . ? C12B C11B C10B 124(2) . . ? C12B C11B H11C 106.3 . . ? C10B C11B H11C 106.3 . . ? C12B C11B H11D 106.3 . . ? C10B C11B H11D 106.3 . . ? H11C C11B H11D 106.4 . . ? O3B C12B C11B 119(2) . . ? O3B C12B H12C 107.6 . . ? C11B C12B H12C 107.6 . . ? O3B C12B H12D 107.6 . . ? C11B C12B H12D 107.6 . . ? H12C C12B H12D 107.1 . . ? C12B O3B C13 116(2) . . ? O1C Si1C C2C 105.0(12) . . ? O1C Si1C C1C 116.5(10) . . ? C2C Si1C C1C 109.7(11) . . ? O1C Si1C C3C 112.6(11) . . ? C2C Si1C C3C 111.6(12) . . ? C1C Si1C C3C 101.7(10) . . ? O1C Si2C O2C 118.1(11) . . ? O1C Si2C C5C 107.3(10) . . ? O2C Si2C C5C 102.0(11) . . ? O1C Si2C C4C 107.7(13) . . ? O2C Si2C C4C 113.4(13) . . ? C5C Si2C C4C 107.7(10) . . ? O2C Si3C C8C 99.3(15) . . ? O2C Si3C C7C 114.0(15) . . ? C8C Si3C C7C 115.9(14) . . ? O2C Si3C C6C 113.5(13) . . ? C8C Si3C C6C 108.7(15) . . ? C7C Si3C C6C 105.6(15) . . ? Si2C O1C Si1C 152.8(10) . . ? Si3C O2C Si2C 140.9(12) . . ? Si1C C1C H1G 109.5 . . ? Si1C C1C H1H 109.5 . . ? H1G C1C H1H 109.5 . . ? Si1C C1C H1I 109.5 . . ? H1G C1C H1I 109.5 . . ? H1H C1C H1I 109.5 . . ? Si1C C2C H2G 109.5 . . ? Si1C C2C H2H 109.5 . . ? H2G C2C H2H 109.5 . . ? Si1C C2C H2I 109.5 . . ? H2G C2C H2I 109.5 . . ? H2H C2C H2I 109.5 . . ? Si1C C3C H3G 109.5 . . ? Si1C C3C H3H 109.5 . . ? H3G C3C H3H 109.5 . . ? Si1C C3C H3I 109.5 . . ? H3G C3C H3I 109.5 . . ? H3H C3C H3I 109.5 . . ? Si2C C4C H4G 109.5 . . ? Si2C C4C H4H 109.5 . . ? H4G C4C H4H 109.5 . . ? Si2C C4C H4I 109.5 . . ? H4G C4C H4I 109.5 . . ? H4H C4C H4I 109.5 . . ? Si2C C5C H5G 109.5 . . ? Si2C C5C H5H 109.5 . . ? H5G C5C H5H 109.5 . . ? Si2C C5C H5I 109.5 . . ? H5G C5C H5I 109.5 . . ? H5H C5C H5I 109.5 . . ? Si3C C6C H6G 109.5 . . ? Si3C C6C H6H 109.5 . . ? H6G C6C H6H 109.5 . . ? Si3C C6C H6I 109.5 . . ? H6G C6C H6I 109.5 . . ? H6H C6C H6I 109.5 . . ? Si3C C7C H7G 109.5 . . ? Si3C C7C H7H 109.5 . . ? H7G C7C H7H 109.5 . . ? Si3C C7C H7I 109.5 . . ? H7G C7C H7I 109.5 . . ? H7H C7C H7I 109.5 . . ? C9C C8C Si3C 127.8(17) . . ? C9C C8C H8E 105.3 . . ? Si3C C8C H8E 105.3 . . ? C9C C8C H8F 105.3 . . ? Si3C C8C H8F 105.3 . . ? H8E C8C H8F 106.0 . . ? C8C C9C C10C 116(2) . . ? C8C C9C H9E 108.3 . . ? C10C C9C H9E 108.3 . . ? C8C C9C H9F 108.3 . . ? C10C C9C H9F 108.3 . . ? H9E C9C H9F 107.4 . . ? C11C C10C C9C 108(2) . . ? C11C C10C H10E 110.0 . . ? C9C C10C H10E 110.0 . . ? C11C C10C H10F 110.0 . . ? C9C C10C H10F 110.0 . . ? H10E C10C H10F 108.4 . . ? C10C C11C C12C 103(2) . . ? C10C C11C H11E 111.2 . . ? C12C C11C H11E 111.2 . . ? C10C C11C H11F 111.2 . . ? C12C C11C H11F 111.2 . . ? H11E C11C H11F 109.2 . . ? O3C C12C C11C 107(2) . . ? O3C C12C H12E 110.3 . . ? C11C C12C H12E 110.3 . . ? O3C C12C H12F 110.3 . . ? C11C C12C H12F 110.3 . . ? H12E C12C H12F 108.6 . . ? C13 O3C C12C 117.5(15) . . ? C14 C13 O3C 122.2(6) . . ? C14 C13 O3B 125.4(11) . . ? C14 C13 O3 123.3(7) . . ? C14 C13 C18 121.24(16) . . ? O3C C13 C18 115.6(6) . . ? O3B C13 C18 113.4(11) . . ? O3 C13 C18 114.4(7) . . ? C13 C14 C15 119.23(16) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 120.48(15) . . ? C16 C15 C27 119.62(15) . . ? C14 C15 C27 119.84(16) . . ? C15 C16 C17 121.30(16) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 118.40(15) . . ? C16 C17 C22 122.13(16) . . ? C18 C17 C22 119.39(15) . . ? C17 C18 C13 119.08(15) . . ? C17 C18 C19 119.81(17) . . ? C13 C18 C19 121.06(17) . . ? C20 C19 C18 119.82(19) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 122.19(18) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C22 C21 C26 119.6(2) . . ? C22 C21 C20 119.47(17) . . ? C26 C21 C20 120.87(19) . . ? C21 C22 C23 118.34(17) . . ? C21 C22 C17 117.61(17) . . ? C23 C22 C17 123.93(16) . . ? C24 C23 C22 116.96(11) . 2 ? C24 C23 C22 116.96(11) . . ? C22 C23 C22 126.1(2) 2 . ? C23 C24 C25 119.51(13) . 2 ? C23 C24 C25 119.51(13) . . ? C25 C24 C25 121.0(3) 2 . ? C26 C25 C24 120.64(19) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C21 120.6(2) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C15 176.4(2) . . ? C27 C28 C29 176.9(2) . . ? C30 C29 C34 118.95(18) . . ? C30 C29 C28 120.96(18) . . ? C34 C29 C28 120.06(19) . . ? C31 C30 C29 121.0(2) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C32 C31 C30 119.9(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 119.7(2) . . ? C31 C32 C35 119.7(2) . . ? C33 C32 C35 120.6(2) . . ? C32 C33 C34 120.4(2) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C29 C34 C33 119.9(2) . . ? C29 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? N1 C35 C32 178.4(4) . . ? 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 Si1 O1 1.701(19) . ? Si1 C3 1.75(3) . ? Si1 C1 1.83(3) . ? Si1 C2 1.90(3) . ? Si2 O2 1.60(3) . ? Si2 O1 1.69(2) . ? Si2 C5 1.80(3) . ? Si2 C4 1.80(3) . ? Si3 O2 1.60(2) . ? Si3 C7 1.81(3) . ? Si3 C6 1.84(3) . ? Si3 C8 2.01(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.57(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.38(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.58(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.49(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O3 1.50(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O3 C13 1.412(16) . ? Si1B O1B 1.570(10) . ? Si1B C1B 1.739(18) . ? Si1B C3B 1.81(2) . ? Si1B C2B 1.89(2) . ? Si2B O1B 1.578(15) . ? Si2B O2B 1.63(3) . ? Si2B C4B 1.73(4) . ? Si2B C5B 1.83(3) . ? Si3B O2B 1.70(3) . ? Si3B C6B 1.78(4) . ? Si3B C8B 1.80(3) . ? Si3B C7B 1.92(4) . ? C1B H1D 0.9800 . ? C1B H1E 0.9800 . ? C1B H1F 0.9800 . ? C2B H2D 0.9800 . ? C2B H2E 0.9800 . ? C2B H2F 0.9800 . ? C3B H3D 0.9800 . ? C3B H3E 0.9800 . ? C3B H3F 0.9800 . ? C4B H4D 0.9800 . ? C4B H4E 0.9800 . ? C4B H4F 0.9800 . ? C5B H5D 0.9800 . ? C5B H5E 0.9800 . ? C5B H5F 0.9800 . ? C6B H6D 0.9800 . ? C6B H6E 0.9800 . ? C6B H6F 0.9800 . ? C7B H7D 0.9800 . ? C7B H7E 0.9800 . ? C7B H7F 0.9800 . ? C8B C9B 1.59(4) . ? C8B H8C 0.9900 . ? C8B H8D 0.9900 . ? C9B C10B 1.48(7) . ? C9B H9C 0.9900 . ? C9B H9D 0.9900 . ? C10B C11B 1.56(5) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11B C12B 1.41(4) . ? C11B H11C 0.9900 . ? C11B H11D 0.9900 . ? C12B O3B 1.32(4) . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? O3B C13 1.38(2) . ? Si1C O1C 1.591(17) . ? Si1C C2C 1.74(2) . ? Si1C C1C 1.86(2) . ? Si1C C3C 2.02(2) . ? Si2C O1C 1.563(16) . ? Si2C O2C 1.65(2) . ? Si2C C5C 1.89(2) . ? Si2C C4C 1.92(3) . ? Si3C O2C 1.63(2) . ? Si3C C8C 1.72(2) . ? Si3C C7C 1.83(3) . ? Si3C C6C 1.90(3) . ? C1C H1G 0.9800 . ? C1C H1H 0.9800 . ? C1C H1I 0.9800 . ? C2C H2G 0.9800 . ? C2C H2H 0.9800 . ? C2C H2I 0.9800 . ? C3C H3G 0.9800 . ? C3C H3H 0.9800 . ? C3C H3I 0.9800 . ? C4C H4G 0.9800 . ? C4C H4H 0.9800 . ? C4C H4I 0.9800 . ? C5C H5G 0.9800 . ? C5C H5H 0.9800 . ? C5C H5I 0.9800 . ? C6C H6G 0.9800 . ? C6C H6H 0.9800 . ? C6C H6I 0.9800 . ? C7C H7G 0.9800 . ? C7C H7H 0.9800 . ? C7C H7I 0.9800 . ? C8C C9C 1.46(3) . ? C8C H8E 0.9900 . ? C8C H8F 0.9900 . ? C9C C10C 1.67(3) . ? C9C H9E 0.9900 . ? C9C H9F 0.9900 . ? C10C C11C 1.45(3) . ? C10C H10E 0.9900 . ? C10C H10F 0.9900 . ? C11C C12C 1.61(4) . ? C11C H11E 0.9900 . ? C11C H11F 0.9900 . ? C12C O3C 1.49(3) . ? C12C H12E 0.9900 . ? C12C H12F 0.9900 . ? O3C C13 1.368(14) . ? N1 C35 1.140(3) . ? C13 C14 1.367(2) . ? C13 C18 1.422(3) . ? C14 C15 1.414(2) . ? C14 H14 0.9500 . ? C15 C16 1.371(2) . ? C15 C27 1.437(2) . ? C16 C17 1.408(2) . ? C16 H16 0.9500 . ? C17 C18 1.413(2) . ? C17 C22 1.454(2) . ? C18 C19 1.428(2) . ? C19 C20 1.348(3) . ? C19 H19 0.9500 . ? C20 C21 1.424(3) . ? C20 H20 0.9500 . ? C21 C22 1.413(3) . ? C21 C26 1.419(3) . ? C22 C23 1.447(2) . ? C23 C24 1.417(4) . ? C24 C25 1.425(3) 2 ? C24 C25 1.425(3) . ? C25 C26 1.352(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.193(2) . ? C28 C29 1.433(2) . ? C29 C30 1.379(3) . ? C29 C34 1.380(3) . ? C30 C31 1.378(3) . ? C30 H30 0.9500 . ? C31 C32 1.367(3) . ? C31 H31 0.9500 . ? C32 C33 1.379(4) . ? C32 C35 1.443(3) . ? C33 C34 1.384(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? 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 O2 Si2 O1 Si1 102(3) . . . . ? C5 Si2 O1 Si1 -16(4) . . . . ? C4 Si2 O1 Si1 -143(3) . . . . ? C3 Si1 O1 Si2 -70(3) . . . . ? C1 Si1 O1 Si2 165(3) . . . . ? C2 Si1 O1 Si2 52(3) . . . . ? C7 Si3 O2 Si2 -135(2) . . . . ? C6 Si3 O2 Si2 -14(3) . . . . ? C8 Si3 O2 Si2 111(2) . . . . ? O1 Si2 O2 Si3 87(2) . . . . ? C5 Si2 O2 Si3 -154(2) . . . . ? C4 Si2 O2 Si3 -23(3) . . . . ? Si3 C8 C9 C10 152(2) . . . . ? C8 C9 C10 C11 -179(2) . . . . ? C9 C10 C11 C12 -173(2) . . . . ? C10 C11 C12 O3 -167.5(17) . . . . ? C11 C12 O3 C13 175.4(15) . . . . ? C1B Si1B O1B Si2B 64(2) . . . . ? C3B Si1B O1B Si2B -163.8(18) . . . . ? C2B Si1B O1B Si2B -55(2) . . . . ? O2B Si2B O1B Si1B -125.7(17) . . . . ? C4B Si2B O1B Si1B -9(3) . . . . ? C5B Si2B O1B Si1B 117.5(19) . . . . ? O1B Si2B O2B Si3B 24(3) . . . . ? C4B Si2B O2B Si3B -99(3) . . . . ? C5B Si2B O2B Si3B 134(3) . . . . ? C6B Si3B O2B Si2B 59(3) . . . . ? C8B Si3B O2B Si2B -171(2) . . . . ? C7B Si3B O2B Si2B -59(3) . . . . ? O2B Si3B C8B C9B -49(3) . . . . ? C6B Si3B C8B C9B 72(3) . . . . ? C7B Si3B C8B C9B -164.4(19) . . . . ? Si3B C8B C9B C10B 179(3) . . . . ? C8B C9B C10B C11B -176(3) . . . . ? C9B C10B C11B C12B 144(3) . . . . ? C10B C11B C12B O3B -178(3) . . . . ? C11B C12B O3B C13 -175(2) . . . . ? O2C Si2C O1C Si1C -80(3) . . . . ? C5C Si2C O1C Si1C 166(2) . . . . ? C4C Si2C O1C Si1C 50(3) . . . . ? C2C Si1C O1C Si2C -133(2) . . . . ? C1C Si1C O1C Si2C -12(3) . . . . ? C3C Si1C O1C Si2C 105(2) . . . . ? C8C Si3C O2C Si2C 142(2) . . . . ? C7C Si3C O2C Si2C -94(3) . . . . ? C6C Si3C O2C Si2C 26(3) . . . . ? O1C Si2C O2C Si3C 71(3) . . . . ? C5C Si2C O2C Si3C -171(2) . . . . ? C4C Si2C O2C Si3C -56(3) . . . . ? O2C Si3C C8C C9C -53(3) . . . . ? C7C Si3C C8C C9C -175(3) . . . . ? C6C Si3C C8C C9C 66(3) . . . . ? Si3C C8C C9C C10C 170(2) . . . . ? C8C C9C C10C C11C -171(3) . . . . ? C9C C10C C11C C12C 164(2) . . . . ? C10C C11C C12C O3C 167(2) . . . . ? C11C C12C O3C C13 156.5(18) . . . . ? C12C O3C C13 C14 11.7(18) . . . . ? C12C O3C C13 C18 -179.5(15) . . . . ? C12B O3B C13 C14 -4(3) . . . . ? C12B O3B C13 C18 177(2) . . . . ? C12 O3 C13 C14 -33.3(17) . . . . ? C12 O3 C13 C18 158.1(13) . . . . ? O3C C13 C14 C15 168.7(6) . . . . ? O3B C13 C14 C15 -178.6(15) . . . . ? O3 C13 C14 C15 -167.4(8) . . . . ? C18 C13 C14 C15 0.4(3) . . . . ? C13 C14 C15 C16 1.3(3) . . . . ? C13 C14 C15 C27 178.56(17) . . . . ? C14 C15 C16 C17 0.9(3) . . . . ? C27 C15 C16 C17 -176.39(16) . . . . ? C15 C16 C17 C18 -4.7(2) . . . . ? C15 C16 C17 C22 178.69(16) . . . . ? C16 C17 C18 C13 6.3(2) . . . . ? C22 C17 C18 C13 -176.99(16) . . . . ? C16 C17 C18 C19 -171.36(16) . . . . ? C22 C17 C18 C19 5.4(3) . . . . ? C14 C13 C18 C17 -4.3(3) . . . . ? O3C C13 C18 C17 -173.2(6) . . . . ? O3B C13 C18 C17 174.8(14) . . . . ? O3 C13 C18 C17 164.6(7) . . . . ? C14 C13 C18 C19 173.32(18) . . . . ? O3C C13 C18 C19 4.3(6) . . . . ? O3B C13 C18 C19 -7.6(14) . . . . ? O3 C13 C18 C19 -17.8(7) . . . . ? C17 C18 C19 C20 4.7(3) . . . . ? C13 C18 C19 C20 -172.93(19) . . . . ? C18 C19 C20 C21 -5.7(3) . . . . ? C19 C20 C21 C22 -3.6(3) . . . . ? C19 C20 C21 C26 174.0(2) . . . . ? C26 C21 C22 C23 11.9(3) . . . . ? C20 C21 C22 C23 -170.46(16) . . . . ? C26 C21 C22 C17 -164.33(18) . . . . ? C20 C21 C22 C17 13.3(3) . . . . ? C16 C17 C22 C21 162.40(16) . . . . ? C18 C17 C22 C21 -14.2(2) . . . . ? C16 C17 C22 C23 -13.6(3) . . . . ? C18 C17 C22 C23 169.82(15) . . . . ? C21 C22 C23 C24 -23.76(17) . . . . ? C17 C22 C23 C24 152.19(13) . . . . ? C21 C22 C23 C22 156.24(17) . . . 2 ? C17 C22 C23 C22 -27.81(13) . . . 2 ? C22 C23 C24 C25 19.27(13) 2 . . 2 ? C22 C23 C24 C25 -160.73(13) . . . 2 ? C22 C23 C24 C25 -160.74(13) 2 . . . ? C22 C23 C24 C25 19.27(13) . . . . ? C23 C24 C25 C26 -2.5(2) . . . . ? C25 C24 C25 C26 177.5(2) 2 . . . ? C24 C25 C26 C21 -10.2(3) . . . . ? C22 C21 C26 C25 5.3(3) . . . . ? C20 C21 C26 C25 -172.3(2) . . . . ? C34 C29 C30 C31 1.3(3) . . . . ? C28 C29 C30 C31 -176.77(19) . . . . ? C29 C30 C31 C32 -0.6(3) . . . . ? C30 C31 C32 C33 -0.5(4) . . . . ? C30 C31 C32 C35 179.7(2) . . . . ? C31 C32 C33 C34 0.9(4) . . . . ? C35 C32 C33 C34 -179.4(3) . . . . ? C30 C29 C34 C33 -0.9(4) . . . . ? C28 C29 C34 C33 177.2(2) . . . . ? C32 C33 C34 C29 -0.2(5) . . . . ?