#------------------------------------------------------------------------------ #$Date: 2021-08-05 03:36:52 +0300 (Thu, 05 Aug 2021) $ #$Revision: 267949 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564328.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_1564328 loop_ _publ_author_name 'Dong, Xinrui' 'Jiang, Wenhua' 'Hua, Dexiang' 'Wang, Xiaohui' 'Xu, Liang' 'Wu, Xiaoxing' _publ_section_title ; Radical-Mediated Vicinal Addition of Alkoxysulfonyl/Fluorosulfonyl and Trifluoromethyl Groups to Aryl Alkyl Alkynes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC03315H _journal_year 2021 _chemical_formula_moiety 'C19 H21 F3 O3 S Si' _chemical_formula_sum 'C19 H21 F3 O3 S Si' _chemical_formula_weight 414.51 _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 geom _atom_sites_solution_primary dual _audit_creation_date 2021-04-14 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-05-15 deposited with the CCDC. 2021-08-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.362(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.4060(3) _cell_length_b 15.9894(6) _cell_length_c 34.9562(12) _cell_measurement_reflns_used 9912 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 44.428 _cell_measurement_theta_min 3.264 _cell_volume 4127.4(3) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 193.0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_unetI/netI 0.0793 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 46817 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 55.092 _diffrn_reflns_theta_min 3.263 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.519 _exptl_absorpt_correction_T_max 0.7508 _exptl_absorpt_correction_T_min 0.5341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1557 before and 0.0794 after correction. The Ratio of minimum to maximum transmission is 0.6978. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.334 _exptl_crystal_description prism _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.271 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 495 _refine_ls_number_reflns 7828 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.1485 _refine_ls_R_factor_gt 0.0718 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+6.4085P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1544 _refine_ls_wR_factor_ref 0.1955 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4172 _reflns_number_total 7828 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc03315h2.cif _cod_data_source_block 2104122315_0m _cod_database_code 1564328 _shelx_shelxl_version_number 2016/6 _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_max 0.985 _shelx_estimated_absorpt_t_min 0.928 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C20(H20A, H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C) ; _shelx_res_file ; TITL 2104122315_0m_a.res in P2(1)/c 2104122315_0m.res created by SHELXL-2016/6 at 13:58:25 on 14-Apr-2021 REM Old TITL 2104122315_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.170, Rweak 0.008, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C38 O6 F6 S4 CELL 1.34139 7.406 15.9894 34.9562 90 94.362 90 ZERR 8 0.0003 0.0006 0.0012 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F O S Si DISP C 0.0148 0.007 57.7477 DISP F 0.0599 0.0411 317.6292 DISP H -0 0 0.6481 DISP O 0.0412 0.025 193.9543 DISP S 0.2924 0.4247 3241.7632 UNIT 152 168 24 24 8 8 L.S. 4 PLAN 20 SIZE 0.01 0.01 0.05 TEMP -80.15 BOND $H list 4 fmap 2 ACTA OMIT 1 3 5 OMIT -2 1 2 REM REM REM WGHT 0.068900 6.408500 FVAR 0.34581 S1 5 0.444443 0.954254 0.055627 11.00000 0.05062 0.05237 = 0.03864 0.00304 0.00997 0.00172 SI1 6 0.230047 0.794993 0.069886 11.00000 0.05749 0.04709 = 0.04064 -0.00586 0.00491 0.00067 F1 3 0.530428 1.029972 0.132735 11.00000 0.06039 0.06270 = 0.05270 -0.00232 0.00933 -0.01776 F2 3 0.366943 1.013397 0.179519 11.00000 0.08843 0.07209 = 0.04371 -0.01299 0.01323 -0.02670 F3 3 0.264000 1.083482 0.130351 11.00000 0.08284 0.04786 = 0.07474 -0.00852 0.01046 0.00874 O1 4 0.409077 1.049712 0.059552 11.00000 0.05532 0.04912 = 0.04992 0.00900 0.00707 0.00314 O2 4 0.632493 0.942606 0.065478 11.00000 0.03889 0.06931 = 0.06079 0.00793 0.01075 0.00617 O3 4 0.368803 0.927000 0.018758 11.00000 0.07270 0.06851 = 0.03455 -0.00294 0.00747 -0.00409 C1 1 0.247582 1.085404 0.039208 11.00000 0.07477 0.07074 = 0.07378 0.01108 0.00083 0.02387 AFIX 137 H1A 2 0.260211 1.083595 0.011515 11.00000 -1.50000 H1B 2 0.233211 1.143561 0.047288 11.00000 -1.50000 H1C 2 0.140948 1.053008 0.045166 11.00000 -1.50000 AFIX 0 C2 1 0.312913 0.903015 0.089199 11.00000 0.04487 0.04688 = 0.03959 0.00395 0.00723 0.00624 C3 1 0.174971 0.721366 0.108633 11.00000 0.08224 0.04472 = 0.05689 -0.00015 0.01240 -0.00190 AFIX 137 H3A 2 0.274726 0.720683 0.128727 11.00000 -1.50000 H3B 2 0.157547 0.665030 0.097941 11.00000 -1.50000 H3C 2 0.063668 0.739655 0.119611 11.00000 -1.50000 AFIX 0 C4 1 0.424455 0.745750 0.047638 11.00000 0.07733 0.05894 = 0.06162 -0.00591 0.01193 0.00835 AFIX 137 H4A 2 0.453604 0.778411 0.025198 11.00000 -1.50000 H4B 2 0.392146 0.688580 0.039666 11.00000 -1.50000 H4C 2 0.529919 0.744346 0.066343 11.00000 -1.50000 AFIX 0 C5 1 0.028052 0.809837 0.036299 11.00000 0.06134 0.07087 = 0.05050 -0.00781 0.00116 0.00059 AFIX 137 H5A 2 -0.074243 0.827449 0.050590 11.00000 -1.50000 H5B 2 -0.001814 0.757071 0.023026 11.00000 -1.50000 H5C 2 0.052944 0.852873 0.017444 11.00000 -1.50000 AFIX 0 C6 1 0.279400 0.936346 0.123566 11.00000 0.04435 0.04018 = 0.04049 -0.00067 0.00557 -0.00422 C7 1 0.362432 1.016016 0.141027 11.00000 0.05364 0.04921 = 0.04179 0.00050 0.01281 -0.00403 C8 1 0.137702 0.898070 0.146286 11.00000 0.04923 0.03829 = 0.03686 -0.00474 0.00912 -0.00025 C9 1 0.179154 0.859878 0.182352 11.00000 0.04494 0.04417 = 0.03955 -0.00048 0.00458 -0.00161 AFIX 43 H9 2 0.299480 0.861455 0.193879 11.00000 -1.20000 AFIX 0 C10 1 0.046361 0.820742 0.200615 11.00000 0.04731 0.04279 = 0.03560 0.00214 0.00680 0.00150 AFIX 43 H10 2 0.077249 0.793728 0.224421 11.00000 -1.20000 AFIX 0 C11 1 -0.133469 0.819148 0.185416 11.00000 0.04499 0.03732 = 0.04358 0.00049 0.00937 -0.00082 C12 1 -0.174442 0.860167 0.150508 11.00000 0.04533 0.03787 = 0.04767 0.00024 0.00283 0.00165 AFIX 43 H12 2 -0.296177 0.861368 0.139775 11.00000 -1.20000 AFIX 0 C13 1 -0.041354 0.898944 0.131349 11.00000 0.04970 0.04326 = 0.03992 0.00612 0.00777 0.00360 AFIX 43 H13 2 -0.072635 0.926515 0.107696 11.00000 -1.20000 AFIX 0 C14 1 -0.274417 0.775114 0.205133 11.00000 0.04512 0.02979 = 0.05276 0.00017 0.00793 0.00241 C15 1 -0.278930 0.778020 0.244940 11.00000 0.05432 0.03481 = 0.05392 -0.00180 0.01265 0.00245 AFIX 43 H15 2 -0.190175 0.809391 0.259828 11.00000 -1.20000 AFIX 0 C16 1 -0.411735 0.735547 0.262926 11.00000 0.06752 0.03970 = 0.06140 0.00315 0.02471 -0.00076 AFIX 43 H16 2 -0.414377 0.738932 0.290010 11.00000 -1.20000 AFIX 0 C17 1 -0.539421 0.688684 0.242141 11.00000 0.05639 0.04099 = 0.07687 0.00863 0.02253 -0.00445 AFIX 43 H17 2 -0.629439 0.659307 0.254705 11.00000 -1.20000 AFIX 0 C18 1 -0.535846 0.684681 0.203203 11.00000 0.05457 0.04264 = 0.07205 0.00876 0.00556 -0.00910 AFIX 43 H18 2 -0.623225 0.651768 0.188710 11.00000 -1.20000 AFIX 0 C19 1 -0.406362 0.728023 0.184541 11.00000 0.05058 0.03823 = 0.05682 0.00528 0.00209 0.00282 AFIX 43 H19 2 -0.407775 0.725527 0.157367 11.00000 -1.20000 AFIX 0 S2 5 0.941142 0.298232 0.072841 11.00000 0.06399 0.05769 = 0.05208 -0.01529 0.01803 -0.00896 SI2 6 0.725910 0.459713 0.081671 11.00000 0.08467 0.05247 = 0.04355 0.00396 0.01436 -0.00380 F4 3 1.036275 0.238563 0.152544 11.00000 0.06280 0.06840 = 0.07043 -0.00905 0.00367 0.01559 F5 3 0.874490 0.263297 0.199048 11.00000 0.09838 0.06517 = 0.04497 -0.00074 0.00074 0.02050 F6 3 0.770619 0.183783 0.153538 11.00000 0.09098 0.04270 = 0.07051 0.00317 0.00374 -0.00828 O4 4 0.912584 0.203114 0.081173 11.00000 0.06545 0.05336 = 0.06506 -0.02142 0.01368 -0.00959 O5 4 0.859265 0.316778 0.035553 11.00000 0.09331 0.08185 = 0.04168 -0.01152 0.01413 -0.00369 O6 4 1.128649 0.313109 0.080862 11.00000 0.05713 0.08478 = 0.08119 -0.02632 0.02300 -0.01943 C20 1 0.741403 0.164378 0.067359 11.00000 0.08458 0.07963 = 0.07094 -0.02213 0.00801 -0.03061 AFIX 137 H20A 2 0.723904 0.170443 0.039426 11.00000 -1.50000 H20B 2 0.641585 0.191826 0.079304 11.00000 -1.50000 H20C 2 0.743799 0.104861 0.074074 11.00000 -1.50000 AFIX 0 C21 1 0.810245 0.355578 0.104939 11.00000 0.05180 0.04777 = 0.04364 -0.01142 0.00559 -0.00603 C22 1 0.680179 0.539557 0.118294 11.00000 0.09204 0.05426 = 0.06142 0.00390 0.01402 0.00563 AFIX 137 H22A 2 0.566797 0.525961 0.129642 11.00000 -1.50000 H22B 2 0.669750 0.594771 0.106157 11.00000 -1.50000 H22C 2 0.779858 0.540068 0.138407 11.00000 -1.50000 AFIX 0 C23 1 0.519206 0.440093 0.049547 11.00000 0.11400 0.09000 = 0.05707 0.01079 -0.01155 0.00279 AFIX 137 H23A 2 0.546467 0.399394 0.029831 11.00000 -1.50000 H23B 2 0.478410 0.492575 0.037254 11.00000 -1.50000 H23C 2 0.423545 0.417945 0.064587 11.00000 -1.50000 AFIX 0 C24 1 0.914102 0.503215 0.055469 11.00000 0.13836 0.07089 = 0.08451 0.00094 0.04638 -0.01868 AFIX 137 H24A 2 1.024014 0.506638 0.072873 11.00000 -1.50000 H24B 2 0.881231 0.559232 0.045928 11.00000 -1.50000 H24C 2 0.936217 0.466695 0.033800 11.00000 -1.50000 AFIX 0 C25 1 0.779820 0.328426 0.140657 11.00000 0.04784 0.04134 = 0.04085 -0.00725 0.00257 -0.00352 C26 1 0.864712 0.253389 0.160775 11.00000 0.06227 0.04762 = 0.05168 -0.00356 0.00923 0.00847 C27 1 0.640545 0.370455 0.161977 11.00000 0.04027 0.04024 = 0.03710 -0.00190 0.00928 -0.00502 C28 1 0.683762 0.412798 0.196852 11.00000 0.04565 0.03846 = 0.04310 -0.00191 0.00335 -0.00295 AFIX 43 H28 2 0.805440 0.413924 0.207621 11.00000 -1.20000 AFIX 0 C29 1 0.550219 0.452570 0.215391 11.00000 0.05050 0.03578 = 0.04185 -0.00498 0.00538 -0.00278 AFIX 43 H29 2 0.581927 0.481116 0.238776 11.00000 -1.20000 AFIX 0 C30 1 0.370268 0.451999 0.200754 11.00000 0.04813 0.03501 = 0.04182 0.00420 0.00759 -0.00550 C31 1 0.328356 0.408953 0.166621 11.00000 0.04905 0.04450 = 0.05050 0.00099 0.00410 0.00001 AFIX 43 H31 2 0.206487 0.407609 0.155973 11.00000 -1.20000 AFIX 0 C32 1 0.460206 0.368252 0.147975 11.00000 0.06074 0.04199 = 0.04100 -0.00283 0.00521 -0.00572 AFIX 43 H32 2 0.426999 0.338107 0.125096 11.00000 -1.20000 AFIX 0 C33 1 0.229179 0.495508 0.220995 11.00000 0.04158 0.02962 = 0.05964 0.00006 0.00802 -0.00617 C34 1 0.092323 0.540747 0.201184 11.00000 0.05048 0.03681 = 0.07385 -0.00192 0.00034 -0.00385 AFIX 43 H34 2 0.087119 0.543231 0.173969 11.00000 -1.20000 AFIX 0 C35 1 -0.037137 0.582439 0.220666 11.00000 0.05442 0.03830 = 0.09604 -0.00222 0.00083 0.00312 AFIX 43 H35 2 -0.129442 0.613780 0.206816 11.00000 -1.20000 AFIX 0 C36 1 -0.031659 0.578332 0.260079 11.00000 0.05758 0.04007 = 0.11006 -0.01207 0.03442 0.00035 AFIX 43 H36 2 -0.121112 0.606344 0.273378 11.00000 -1.20000 AFIX 0 C37 1 0.101439 0.534289 0.280018 11.00000 0.07482 0.03741 = 0.06991 -0.00616 0.02708 0.00058 AFIX 43 H37 2 0.104853 0.531901 0.307218 11.00000 -1.20000 AFIX 0 C38 1 0.231911 0.492937 0.260938 11.00000 0.05452 0.03508 = 0.06098 -0.00168 0.01714 0.00130 AFIX 43 H38 2 0.324375 0.462458 0.275183 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2104122315_0m_a.res in P2(1)/c REM R1 = 0.0718 for 4172 Fo > 4sig(Fo) and 0.1485 for all 7828 data REM 495 parameters refined using 0 restraints END WGHT 0.0762 5.5716 REM Highest difference peak 0.271, deepest hole -0.543, 1-sigma level 0.073 Q1 1 0.2980 1.0083 0.0744 11.00000 0.05 0.27 Q2 1 0.2488 0.8678 0.0780 11.00000 0.05 0.26 Q3 1 0.8672 0.6322 0.1069 11.00000 0.05 0.26 Q4 1 0.4224 0.9035 0.1907 11.00000 0.05 0.26 Q5 1 0.7957 0.9337 0.0421 11.00000 0.05 0.25 Q6 1 0.2548 0.5152 0.1487 11.00000 0.05 0.25 Q7 1 -0.3663 0.9221 0.1403 11.00000 0.05 0.25 Q8 1 0.5208 0.8833 0.0107 11.00000 0.05 0.24 Q9 1 0.6045 0.9496 0.0306 11.00000 0.05 0.23 Q10 1 -0.0276 0.7038 0.2511 11.00000 0.05 0.23 Q11 1 -0.7310 0.6776 0.2801 11.00000 0.05 0.23 Q12 1 0.3888 0.4189 0.3141 11.00000 0.05 0.23 Q13 1 0.1217 1.0422 0.1405 11.00000 0.05 0.22 Q14 1 0.4368 1.0443 0.0399 11.00000 0.05 0.22 Q15 1 1.2022 0.4839 0.0886 11.00000 0.05 0.22 Q16 1 0.3452 1.1222 -0.0264 11.00000 0.05 0.22 Q17 1 1.1231 0.4162 0.0701 11.00000 0.05 0.22 Q18 1 0.7616 0.9778 0.0519 11.00000 0.05 0.22 Q19 1 0.7429 0.8828 0.0606 11.00000 0.05 0.22 Q20 1 0.3715 1.0011 0.0152 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0 7 39 -13.469 7.57490 1 0 7 39 -1.5153 8.13023 4 1 -7 39 18.4933 9.63390 1 1 7 39 30.8137 14.0385 4 1 7 39 28.4326 10.0987 1 -3 0 40 36.3770 10.0658 1 -3 0 40 47.8869 10.5308 4 -2 0 40 17.4170 7.86062 4 -2 0 40 -7.4548 11.2820 1 -1 0 40 1.96772 7.31722 4 -1 0 40 -4.8268 6.74507 1 0 0 40 4.61433 8.03603 1 0 0 40 -2.7527 9.00630 4 1 0 40 34.7812 11.8631 4 1 0 40 39.1017 14.1946 1 2 0 40 16.6204 9.62705 1 -3 -1 40 3.65245 7.47315 1 -3 -1 40 10.3090 7.22372 4 -3 1 40 11.9854 8.39590 1 -3 1 40 16.5558 7.90090 4 -2 -1 40 3.81557 7.00795 4 -2 -1 40 26.8542 13.6749 1 -2 1 40 15.4845 8.14417 4 -1 -1 40 0.15444 7.52757 4 -1 -1 40 -8.2319 6.99440 1 -1 1 40 10.0678 7.73942 1 -1 1 40 3.48798 7.81606 4 0 -1 40 0.00016 7.73288 1 0 -1 40 -0.2576 9.09554 4 0 1 40 23.3062 9.86190 4 0 1 40 10.9395 8.48358 1 1 -1 40 -10.912 12.0529 4 1 -1 40 -3.4072 8.31156 1 1 1 40 -7.5496 10.2604 1 1 1 40 20.3063 11.8584 4 2 -1 40 27.4049 9.81791 1 2 1 40 18.6721 9.74191 1 -3 -2 40 -13.587 7.07082 1 -3 -2 40 4.95670 8.15971 4 -3 2 40 -0.3221 6.70549 4 -3 2 40 4.07201 8.11808 1 -2 -2 40 11.2495 11.2579 1 -2 -2 40 16.8611 11.2440 4 -2 2 40 10.0604 13.5481 1 -2 2 40 19.5032 13.1982 4 -1 -2 40 -5.1228 7.33934 1 -1 -2 40 -1.4007 7.15072 4 -1 2 40 -1.5725 7.65872 4 -1 2 40 -5.5108 7.17864 1 0 -2 40 8.00456 8.19953 1 0 2 40 -0.8580 7.73617 1 0 2 40 30.0462 10.4910 4 1 -2 40 25.5464 13.7510 4 1 -2 40 -1.3948 8.66180 1 1 2 40 -3.0863 14.0038 1 1 2 40 10.2818 10.9222 4 2 -2 40 8.81696 8.17606 1 2 2 40 -0.9290 9.09746 1 -3 -3 40 2.87986 7.65332 4 -3 -3 40 6.82059 7.21725 1 -3 3 40 17.7162 8.39707 4 -2 -3 40 20.3398 9.82611 1 -2 3 40 -6.8091 7.87518 1 -1 -3 40 -8.3257 7.91262 4 -1 -3 40 -3.8026 7.56403 1 -1 3 40 -1.5044 8.02608 1 -1 3 40 -0.2621 7.43579 4 0 -3 40 7.06727 9.69835 4 0 -3 40 -4.3090 7.45296 1 0 3 40 -1.7850 17.3883 4 0 3 40 -2.8243 8.04992 1 1 -3 40 -2.5691 7.40609 1 1 3 40 0.20091 9.14628 1 1 3 40 13.6644 11.7479 4 2 -3 40 0.71992 8.87615 1 2 3 40 5.03744 8.17476 1 -3 -4 40 52.5761 10.1485 4 -3 4 40 56.0703 11.7376 4 3 4 -40 89.5440 18.0030 2 -3 4 40 38.1715 12.3075 1 -2 -4 40 7.44087 7.98173 4 -2 -4 40 -7.6708 7.17638 1 -2 4 40 5.70375 8.48227 4 -2 4 40 9.74679 8.86955 1 -1 -4 40 -13.199 10.9558 1 -1 -4 40 7.30426 8.44371 4 -1 4 40 3.05994 9.27433 1 -1 4 40 -29.177 14.9087 4 0 -4 40 -5.4980 9.81628 4 0 -4 40 4.84433 12.2195 1 0 4 40 4.39462 9.24419 4 0 4 40 -9.1027 10.7254 1 1 -4 40 13.1521 9.17839 1 1 4 40 -0.2192 8.60926 1 1 4 40 -6.1793 11.8560 4 -2 -5 40 23.5077 9.32424 1 -2 -5 40 36.9332 10.4174 4 -2 5 40 54.1666 11.2511 4 -2 5 40 44.3954 11.4928 1 -1 -5 40 19.7224 9.21194 4 -1 -5 40 11.3939 9.13498 1 -1 5 40 10.9194 10.8465 1 -1 5 40 37.0267 10.6071 4 0 -5 40 15.2835 10.9843 4 0 -5 40 2.36365 8.67771 1 0 5 40 14.4101 8.98904 1 1 -5 40 -13.114 7.12009 1 1 5 40 6.92985 8.41717 1 1 5 40 25.0675 12.6146 4 -2 -6 40 -10.021 6.88649 1 -2 -6 40 4.09714 8.16233 4 -2 6 40 7.08657 8.84363 4 -2 6 40 -2.3737 9.31697 1 -1 -6 40 -5.3018 7.15817 1 -1 -6 40 -0.4109 9.29244 4 -1 6 40 -1.2068 8.95272 1 -1 6 40 4.79975 9.62527 4 0 -6 40 4.42029 7.95883 1 0 6 40 -3.7904 9.92834 4 0 6 40 -11.034 8.23951 1 -3 0 41 -3.0645 6.41794 4 -2 0 41 -0.5590 6.50232 1 -2 0 41 4.13933 7.34251 4 -1 0 41 15.8392 9.52685 4 -1 0 41 -11.682 8.96084 1 0 0 41 -3.7725 8.46650 4 0 0 41 -0.9766 11.1457 1 1 0 41 -14.902 7.41100 1 1 0 41 28.5609 13.1513 4 -3 -1 41 -11.597 6.42680 1 -3 -1 41 -1.6157 6.66122 4 -3 1 41 1.53933 7.59795 1 -3 1 41 -2.0276 7.01352 4 -2 -1 41 21.7273 7.93277 4 -2 -1 41 31.4341 10.0773 1 -2 1 41 42.9525 9.99831 4 -2 1 41 18.1386 8.33699 1 -1 -1 41 33.8987 11.6056 1 -1 -1 41 19.3573 8.73043 4 -1 1 41 10.9845 9.08711 4 -1 1 41 16.1334 13.0682 1 0 -1 41 1.48630 10.7232 1 0 -1 41 30.5319 10.7067 4 0 1 41 11.8505 9.38656 4 0 1 41 19.3490 10.3214 1 1 -1 41 -6.8150 7.79802 1 1 -1 41 26.9675 14.6454 4 1 1 41 -2.5796 11.9176 4 1 1 41 12.3916 9.12660 1 -3 -2 41 3.11821 6.37162 4 -3 2 41 -9.4442 7.55424 4 -2 -2 41 12.4887 8.09146 1 -2 -2 41 13.7543 8.23848 4 -2 2 41 -7.5192 7.66207 4 -2 2 41 2.57417 8.31503 1 -1 -2 41 10.5675 7.87928 4 -1 -2 41 -5.1995 6.82138 1 -1 2 41 15.9287 8.82085 4 -1 2 41 3.36138 7.81087 1 0 -2 41 5.16442 8.29550 1 0 2 41 -3.7244 8.39216 4 0 2 41 11.0144 7.81460 1 1 -2 41 15.9836 8.99291 1 1 2 41 -12.315 13.5243 4 1 2 41 -4.4037 8.96595 1 -2 -3 41 1.74171 7.01644 4 -2 -3 41 -6.3977 7.76541 1 -2 3 41 15.6628 8.33869 4 -2 3 41 1.25133 8.41028 1 -1 -3 41 40.0863 10.0853 1 -1 -3 41 47.8766 11.1729 4 -1 3 41 55.6034 10.7438 4 -1 3 41 62.5585 12.4993 1 0 -3 41 -9.0717 6.62206 1 0 -3 41 4.98718 10.2048 4 0 3 41 -0.6726 8.71056 4 0 3 41 -10.557 7.55242 1 1 -3 41 11.7224 7.74787 1 1 3 41 -5.6745 7.74345 1 1 3 41 -0.3673 12.3118 4 -2 -4 41 9.78974 7.72418 1 -2 -4 41 13.4627 7.61426 4 -2 4 41 6.63966 7.65735 4 -2 4 41 -0.4670 8.77717 1 -1 -4 41 14.4836 8.75238 1 -1 -4 41 10.7396 8.40459 4 -1 4 41 11.2048 8.71292 4 -1 4 41 15.8552 8.69916 1 0 -4 41 5.49647 11.5210 4 0 -4 41 -0.5860 8.24478 1 0 4 41 24.5375 10.2907 4 0 4 41 15.6452 8.73987 1 1 -4 41 2.40888 8.20013 1 -1 -5 41 17.6004 9.58457 4 -1 5 41 9.64554 8.56651 4 -1 5 41 16.8115 9.58667 1 0 -5 41 -2.1217 8.27806 1 0 5 41 -1.6827 7.11719 1 0 5 41 -9.5412 9.31224 4 -2 0 42 6.16480 8.10030 1 -2 0 42 7.12179 6.69600 4 -1 0 42 2.26217 8.16581 4 -1 0 42 -12.484 7.10606 1 0 0 42 15.4280 8.30937 1 0 0 42 9.83459 8.88180 4 -2 -1 42 -7.6413 6.69659 4 -2 -1 42 -11.483 6.03462 1 -2 1 42 -4.9054 7.40986 4 -1 -1 42 10.0989 7.25325 1 -1 -1 42 15.8570 9.26748 4 -1 1 42 8.08914 8.39024 1 -1 1 42 25.4509 9.46636 4 0 -1 42 0.51682 9.27009 4 0 -1 42 8.24498 8.23032 1 0 1 42 20.9672 9.47656 4 0 1 42 -0.3830 8.23804 1 -2 -2 42 5.72261 6.53823 4 -1 -2 42 16.7495 8.29128 4 -1 2 42 17.6865 8.83090 4 -1 2 42 11.6679 7.91530 1 0 -2 42 8.50599 7.84475 1 0 -2 42 2.54765 10.7155 4 0 2 42 1.69590 9.20225 4 0 2 42 25.8163 8.90409 1 -1 -3 42 1.23073 7.80962 1 -1 -3 42 16.1570 8.97294 4 -1 3 42 3.98070 8.55117 1 -1 3 42 -0.2116 8.25600 4 0 -3 42 1.39790 8.18028 1 0 3 42 7.26122 8.47586 1 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7508 _exptl_absorpt_correction_T_min 0.5341 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.34183 7.407 15.975 34.992 89.991 94.372 89.961 ) ; _shelx_hkl_checksum 78589 _olex2_submission_special_instructions 'No special instructions were received' 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 S1 S 0.44444(17) 0.95425(7) 0.05563(3) 0.0469(3) Uani 1 1 d . . . . . Si1 Si 0.23005(19) 0.79499(8) 0.06989(4) 0.0483(4) Uani 1 1 d . . . . . F1 F 0.5304(4) 1.02997(17) 0.13273(7) 0.0583(7) Uani 1 1 d . . . . . F2 F 0.3669(4) 1.01340(18) 0.17952(7) 0.0677(9) Uani 1 1 d . . . . . F3 F 0.2640(4) 1.08348(17) 0.13035(8) 0.0683(8) Uani 1 1 d . . . . . O1 O 0.4091(4) 1.04971(19) 0.05955(8) 0.0513(8) Uani 1 1 d . . . . . O2 O 0.6325(4) 0.9426(2) 0.06548(9) 0.0560(9) Uani 1 1 d . . . . . O3 O 0.3688(5) 0.9270(2) 0.01876(8) 0.0584(9) Uani 1 1 d . . . . . C1 C 0.2476(8) 1.0854(4) 0.03921(16) 0.0733(17) Uani 1 1 d . . . . . H1A H 0.260211 1.083595 0.011515 0.110 Uiso 1 1 calc GR . . . . H1B H 0.233211 1.143561 0.047288 0.110 Uiso 1 1 calc GR . . . . H1C H 0.140948 1.053008 0.045166 0.110 Uiso 1 1 calc GR . . . . C2 C 0.3129(6) 0.9030(3) 0.08920(12) 0.0436(11) Uani 1 1 d . . . . . C3 C 0.1750(8) 0.7214(3) 0.10863(14) 0.0609(14) Uani 1 1 d . . . . . H3A H 0.274726 0.720683 0.128727 0.091 Uiso 1 1 calc GR . . . . H3B H 0.157547 0.665030 0.097941 0.091 Uiso 1 1 calc GR . . . . H3C H 0.063668 0.739655 0.119611 0.091 Uiso 1 1 calc GR . . . . C4 C 0.4245(8) 0.7458(3) 0.04764(15) 0.0656(15) Uani 1 1 d . . . . . H4A H 0.453604 0.778411 0.025198 0.098 Uiso 1 1 calc GR . . . . H4B H 0.392146 0.688580 0.039666 0.098 Uiso 1 1 calc GR . . . . H4C H 0.529919 0.744346 0.066343 0.098 Uiso 1 1 calc GR . . . . C5 C 0.0281(7) 0.8098(3) 0.03630(14) 0.0611(14) Uani 1 1 d . . . . . H5A H -0.074243 0.827449 0.050590 0.092 Uiso 1 1 calc GR . . . . H5B H -0.001814 0.757071 0.023026 0.092 Uiso 1 1 calc GR . . . . H5C H 0.052944 0.852873 0.017444 0.092 Uiso 1 1 calc GR . . . . C6 C 0.2794(6) 0.9363(3) 0.12357(12) 0.0416(11) Uani 1 1 d . . . . . C7 C 0.3624(7) 1.0160(3) 0.14103(13) 0.0477(12) Uani 1 1 d . . . . . C8 C 0.1377(6) 0.8981(3) 0.14629(12) 0.0412(11) Uani 1 1 d . . . . . C9 C 0.1792(6) 0.8599(3) 0.18235(12) 0.0428(11) Uani 1 1 d . . . . . H9 H 0.299480 0.861455 0.193879 0.051 Uiso 1 1 calc R . . . . C10 C 0.0464(6) 0.8207(3) 0.20061(12) 0.0417(11) Uani 1 1 d . . . . . H10 H 0.077249 0.793728 0.224421 0.050 Uiso 1 1 calc R . . . . C11 C -0.1335(6) 0.8191(3) 0.18542(12) 0.0417(11) Uani 1 1 d . . . . . C12 C -0.1744(7) 0.8602(3) 0.15051(12) 0.0437(11) Uani 1 1 d . . . . . H12 H -0.296177 0.861368 0.139775 0.052 Uiso 1 1 calc R . . . . C13 C -0.0414(6) 0.8989(3) 0.13135(12) 0.0441(11) Uani 1 1 d . . . . . H13 H -0.072635 0.926515 0.107696 0.053 Uiso 1 1 calc R . . . . C14 C -0.2744(6) 0.7751(3) 0.20513(13) 0.0423(11) Uani 1 1 d . . . . . C15 C -0.2789(7) 0.7780(3) 0.24494(13) 0.0472(12) Uani 1 1 d . . . . . H15 H -0.190175 0.809391 0.259828 0.057 Uiso 1 1 calc R . . . . C16 C -0.4117(7) 0.7355(3) 0.26293(15) 0.0552(13) Uani 1 1 d . . . . . H16 H -0.414377 0.738932 0.290010 0.066 Uiso 1 1 calc R . . . . C17 C -0.5394(7) 0.6887(3) 0.24214(16) 0.0572(14) Uani 1 1 d . . . . . H17 H -0.629439 0.659307 0.254705 0.069 Uiso 1 1 calc R . . . . C18 C -0.5358(7) 0.6847(3) 0.20320(16) 0.0564(13) Uani 1 1 d . . . . . H18 H -0.623225 0.651768 0.188710 0.068 Uiso 1 1 calc R . . . . C19 C -0.4064(7) 0.7280(3) 0.18454(14) 0.0486(12) Uani 1 1 d . . . . . H19 H -0.407775 0.725527 0.157367 0.058 Uiso 1 1 calc R . . . . S2 S 0.94114(19) 0.29823(8) 0.07284(4) 0.0572(4) Uani 1 1 d . . . . . Si2 Si 0.7259(2) 0.45971(9) 0.08167(4) 0.0597(4) Uani 1 1 d . . . . . F4 F 1.0363(4) 0.23856(18) 0.15254(8) 0.0673(8) Uani 1 1 d . . . . . F5 F 0.8745(4) 0.26330(18) 0.19905(8) 0.0697(9) Uani 1 1 d . . . . . F6 F 0.7706(4) 0.18378(17) 0.15354(8) 0.0682(8) Uani 1 1 d . . . . . O4 O 0.9126(5) 0.2031(2) 0.08117(10) 0.0608(9) Uani 1 1 d . . . . . O5 O 0.8593(5) 0.3168(2) 0.03555(9) 0.0718(11) Uani 1 1 d . . . . . O6 O 1.1286(5) 0.3131(2) 0.08086(11) 0.0735(11) Uani 1 1 d . . . . . C20 C 0.7414(8) 0.1644(4) 0.06736(16) 0.0783(18) Uani 1 1 d . . . . . H20A H 0.723904 0.170443 0.039426 0.117 Uiso 1 1 calc GR . . . . H20B H 0.641585 0.191826 0.079304 0.117 Uiso 1 1 calc GR . . . . H20C H 0.743799 0.104861 0.074074 0.117 Uiso 1 1 calc GR . . . . C21 C 0.8102(7) 0.3556(3) 0.10494(13) 0.0476(12) Uani 1 1 d . . . . . C22 C 0.6802(8) 0.5396(3) 0.11829(15) 0.0688(16) Uani 1 1 d . . . . . H22A H 0.566797 0.525961 0.129642 0.103 Uiso 1 1 calc GR . . . . H22B H 0.669750 0.594771 0.106157 0.103 Uiso 1 1 calc GR . . . . H22C H 0.779858 0.540068 0.138407 0.103 Uiso 1 1 calc GR . . . . C23 C 0.5192(9) 0.4401(4) 0.04955(16) 0.088(2) Uani 1 1 d . . . . . H23A H 0.546467 0.399394 0.029831 0.132 Uiso 1 1 calc GR . . . . H23B H 0.478410 0.492575 0.037254 0.132 Uiso 1 1 calc GR . . . . H23C H 0.423545 0.417945 0.064587 0.132 Uiso 1 1 calc GR . . . . C24 C 0.9141(10) 0.5032(4) 0.05547(18) 0.096(2) Uani 1 1 d . . . . . H24A H 1.024014 0.506638 0.072873 0.144 Uiso 1 1 calc GR . . . . H24B H 0.881231 0.559232 0.045928 0.144 Uiso 1 1 calc GR . . . . H24C H 0.936217 0.466695 0.033800 0.144 Uiso 1 1 calc GR . . . . C25 C 0.7798(6) 0.3284(3) 0.14066(12) 0.0434(11) Uani 1 1 d . . . . . C26 C 0.8647(8) 0.2534(3) 0.16077(14) 0.0536(13) Uani 1 1 d . . . . . C27 C 0.6405(6) 0.3705(3) 0.16198(12) 0.0389(10) Uani 1 1 d . . . . . C28 C 0.6838(6) 0.4128(3) 0.19685(12) 0.0424(11) Uani 1 1 d . . . . . H28 H 0.805440 0.413924 0.207621 0.051 Uiso 1 1 calc R . . . . C29 C 0.5502(6) 0.4526(3) 0.21539(12) 0.0426(11) Uani 1 1 d . . . . . H29 H 0.581927 0.481116 0.238776 0.051 Uiso 1 1 calc R . . . . C30 C 0.3703(6) 0.4520(3) 0.20075(12) 0.0414(11) Uani 1 1 d . . . . . C31 C 0.3284(7) 0.4090(3) 0.16662(13) 0.0480(12) Uani 1 1 d . . . . . H31 H 0.206487 0.407609 0.155973 0.058 Uiso 1 1 calc R . . . . C32 C 0.4602(7) 0.3683(3) 0.14797(13) 0.0478(12) Uani 1 1 d . . . . . H32 H 0.426999 0.338107 0.125096 0.057 Uiso 1 1 calc R . . . . C33 C 0.2292(6) 0.4955(3) 0.22099(14) 0.0434(11) Uani 1 1 d . . . . . C34 C 0.0923(7) 0.5407(3) 0.20118(16) 0.0539(13) Uani 1 1 d . . . . . H34 H 0.087119 0.543231 0.173969 0.065 Uiso 1 1 calc R . . . . C35 C -0.0371(8) 0.5824(3) 0.22067(18) 0.0632(15) Uani 1 1 d . . . . . H35 H -0.129442 0.613780 0.206816 0.076 Uiso 1 1 calc R . . . . C36 C -0.0317(8) 0.5783(3) 0.2601(2) 0.0678(16) Uani 1 1 d . . . . . H36 H -0.121112 0.606344 0.273378 0.081 Uiso 1 1 calc R . . . . C37 C 0.1014(8) 0.5343(3) 0.28002(16) 0.0596(14) Uani 1 1 d . . . . . H37 H 0.104853 0.531901 0.307218 0.072 Uiso 1 1 calc R . . . . C38 C 0.2319(7) 0.4929(3) 0.26094(14) 0.0495(12) Uani 1 1 d . . . . . H38 H 0.324375 0.462458 0.275183 0.059 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0506(8) 0.0524(7) 0.0386(6) 0.0030(5) 0.0100(5) 0.0017(6) Si1 0.0575(9) 0.0471(8) 0.0406(7) -0.0059(6) 0.0049(6) 0.0007(7) F1 0.060(2) 0.0627(18) 0.0527(16) -0.0023(13) 0.0093(14) -0.0178(15) F2 0.088(2) 0.0721(19) 0.0437(16) -0.0130(14) 0.0132(15) -0.0267(17) F3 0.083(2) 0.0479(17) 0.075(2) -0.0085(15) 0.0105(17) 0.0087(16) O1 0.055(2) 0.0491(19) 0.0499(19) 0.0090(15) 0.0071(16) 0.0031(16) O2 0.039(2) 0.069(2) 0.061(2) 0.0079(17) 0.0108(16) 0.0062(17) O3 0.073(3) 0.069(2) 0.0346(17) -0.0029(16) 0.0075(16) -0.0041(19) C1 0.075(4) 0.071(4) 0.074(4) 0.011(3) 0.001(3) 0.024(3) C2 0.045(3) 0.047(3) 0.040(3) 0.004(2) 0.007(2) 0.006(2) C3 0.082(4) 0.045(3) 0.057(3) 0.000(2) 0.012(3) -0.002(3) C4 0.077(4) 0.059(3) 0.062(3) -0.006(3) 0.012(3) 0.008(3) C5 0.061(4) 0.071(4) 0.051(3) -0.008(3) 0.001(3) 0.001(3) C6 0.044(3) 0.040(3) 0.040(2) -0.001(2) 0.006(2) -0.004(2) C7 0.054(3) 0.049(3) 0.042(3) 0.001(2) 0.013(2) -0.004(3) C8 0.049(3) 0.038(3) 0.037(2) -0.005(2) 0.009(2) 0.000(2) C9 0.045(3) 0.044(3) 0.040(2) 0.000(2) 0.005(2) -0.002(2) C10 0.047(3) 0.043(3) 0.036(2) 0.0021(19) 0.007(2) 0.001(2) C11 0.045(3) 0.037(2) 0.044(3) 0.000(2) 0.009(2) -0.001(2) C12 0.045(3) 0.038(3) 0.048(3) 0.000(2) 0.003(2) 0.002(2) C13 0.050(3) 0.043(3) 0.040(2) 0.006(2) 0.008(2) 0.004(2) C14 0.045(3) 0.030(2) 0.053(3) 0.000(2) 0.008(2) 0.002(2) C15 0.054(3) 0.035(2) 0.054(3) -0.002(2) 0.013(2) 0.002(2) C16 0.068(4) 0.040(3) 0.061(3) 0.003(2) 0.025(3) -0.001(3) C17 0.056(4) 0.041(3) 0.077(4) 0.009(3) 0.023(3) -0.004(3) C18 0.055(3) 0.043(3) 0.072(4) 0.009(3) 0.006(3) -0.009(2) C19 0.051(3) 0.038(3) 0.057(3) 0.005(2) 0.002(2) 0.003(2) S2 0.0640(10) 0.0577(8) 0.0521(8) -0.0153(6) 0.0180(6) -0.0090(7) Si2 0.0847(12) 0.0525(9) 0.0435(8) 0.0040(6) 0.0144(7) -0.0038(8) F4 0.063(2) 0.068(2) 0.0704(19) -0.0091(15) 0.0037(16) 0.0156(16) F5 0.098(3) 0.0652(19) 0.0450(17) -0.0007(14) 0.0007(15) 0.0205(17) F6 0.091(2) 0.0427(17) 0.0705(19) 0.0032(14) 0.0037(17) -0.0083(16) O4 0.065(2) 0.053(2) 0.065(2) -0.0214(17) 0.0137(18) -0.0096(18) O5 0.093(3) 0.082(3) 0.042(2) -0.0115(18) 0.0141(19) -0.004(2) O6 0.057(3) 0.085(3) 0.081(3) -0.026(2) 0.023(2) -0.019(2) C20 0.085(5) 0.080(4) 0.071(4) -0.022(3) 0.008(3) -0.031(4) C21 0.052(3) 0.048(3) 0.044(3) -0.011(2) 0.006(2) -0.006(2) C22 0.092(5) 0.054(3) 0.061(3) 0.004(3) 0.014(3) 0.006(3) C23 0.114(6) 0.090(5) 0.057(4) 0.011(3) -0.012(3) 0.003(4) C24 0.138(7) 0.071(4) 0.085(5) 0.001(3) 0.046(4) -0.019(4) C25 0.048(3) 0.041(3) 0.041(3) -0.007(2) 0.003(2) -0.004(2) C26 0.062(4) 0.048(3) 0.052(3) -0.004(2) 0.009(3) 0.008(3) C27 0.040(3) 0.040(2) 0.037(2) -0.0019(19) 0.009(2) -0.005(2) C28 0.046(3) 0.038(3) 0.043(3) -0.002(2) 0.003(2) -0.003(2) C29 0.050(3) 0.036(2) 0.042(2) -0.005(2) 0.005(2) -0.003(2) C30 0.048(3) 0.035(2) 0.042(3) 0.004(2) 0.008(2) -0.005(2) C31 0.049(3) 0.044(3) 0.050(3) 0.001(2) 0.004(2) 0.000(2) C32 0.061(4) 0.042(3) 0.041(3) -0.003(2) 0.005(2) -0.006(2) C33 0.042(3) 0.030(2) 0.060(3) 0.000(2) 0.008(2) -0.006(2) C34 0.050(3) 0.037(3) 0.074(3) -0.002(2) 0.000(3) -0.004(2) C35 0.054(4) 0.038(3) 0.096(5) -0.002(3) 0.001(3) 0.003(2) C36 0.058(4) 0.040(3) 0.110(5) -0.012(3) 0.034(3) 0.000(3) C37 0.075(4) 0.037(3) 0.070(3) -0.006(2) 0.027(3) 0.001(3) C38 0.055(3) 0.035(3) 0.061(3) -0.002(2) 0.017(2) 0.001(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0148 0.0070 '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' F F 0.0599 0.0411 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.2924 0.4247 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2153 0.2529 '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 S1 C2 106.79(19) . . ? O2 S1 O1 106.0(2) . . ? O2 S1 O3 119.1(2) . . ? O2 S1 C2 110.8(2) . . ? O3 S1 O1 108.69(19) . . ? O3 S1 C2 104.9(2) . . ? C3 Si1 C2 113.0(2) . . ? C4 Si1 C2 106.7(2) . . ? C4 Si1 C3 104.8(2) . . ? C5 Si1 C2 109.1(2) . . ? C5 Si1 C3 109.4(3) . . ? C5 Si1 C4 113.8(2) . . ? C1 O1 S1 118.5(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1 C2 Si1 110.8(2) . . ? C6 C2 S1 123.4(4) . . ? C6 C2 Si1 125.8(3) . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 C7 126.1(4) . . ? C2 C6 C8 119.6(4) . . ? C8 C6 C7 114.1(4) . . ? F1 C7 F2 105.9(4) . . ? F1 C7 F3 107.8(4) . . ? F1 C7 C6 114.4(4) . . ? F2 C7 C6 110.7(4) . . ? F3 C7 F2 106.0(4) . . ? F3 C7 C6 111.6(4) . . ? C9 C8 C6 122.5(4) . . ? C13 C8 C6 119.0(4) . . ? C13 C8 C9 118.5(4) . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120.0 . . ? C9 C10 H10 119.0 . . ? C9 C10 C11 122.1(4) . . ? C11 C10 H10 119.0 . . ? C10 C11 C12 117.5(4) . . ? C10 C11 C14 121.3(4) . . ? C12 C11 C14 121.2(4) . . ? C11 C12 H12 119.4 . . ? C13 C12 C11 121.2(4) . . ? C13 C12 H12 119.4 . . ? C8 C13 H13 119.7 . . ? C12 C13 C8 120.7(4) . . ? C12 C13 H13 119.7 . . ? C15 C14 C11 121.5(4) . . ? C19 C14 C11 120.8(4) . . ? C19 C14 C15 117.7(4) . . ? C14 C15 H15 119.7 . . ? C16 C15 C14 120.5(5) . . ? C16 C15 H15 119.7 . . ? C15 C16 H16 119.6 . . ? C17 C16 C15 120.8(5) . . ? C17 C16 H16 119.6 . . ? C16 C17 H17 120.4 . . ? C18 C17 C16 119.3(5) . . ? C18 C17 H17 120.4 . . ? C17 C18 H18 119.6 . . ? C17 C18 C19 120.8(5) . . ? C19 C18 H18 119.6 . . ? C14 C19 H19 119.6 . . ? C18 C19 C14 120.8(5) . . ? C18 C19 H19 119.6 . . ? O4 S2 C21 107.1(2) . . ? O5 S2 O4 108.5(2) . . ? O5 S2 C21 104.7(2) . . ? O6 S2 O4 105.7(2) . . ? O6 S2 O5 119.2(2) . . ? O6 S2 C21 111.1(2) . . ? C22 Si2 C21 111.8(2) . . ? C22 Si2 C24 105.4(3) . . ? C23 Si2 C21 109.5(2) . . ? C23 Si2 C22 110.4(3) . . ? C23 Si2 C24 112.3(3) . . ? C24 Si2 C21 107.4(3) . . ? C20 O4 S2 118.5(4) . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S2 C21 Si2 110.5(2) . . ? C25 C21 S2 123.3(4) . . ? C25 C21 Si2 126.2(4) . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 126.4(4) . . ? C21 C25 C27 119.3(4) . . ? C27 C25 C26 114.2(4) . . ? F4 C26 F5 104.7(4) . . ? F4 C26 C25 114.1(4) . . ? F5 C26 C25 111.1(4) . . ? F6 C26 F4 107.6(4) . . ? F6 C26 F5 106.0(4) . . ? F6 C26 C25 112.6(4) . . ? C28 C27 C25 122.2(4) . . ? C32 C27 C25 120.0(4) . . ? C32 C27 C28 117.8(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 C27 120.3(4) . . ? C29 C28 H28 119.9 . . ? C28 C29 H29 119.1 . . ? C28 C29 C30 121.7(4) . . ? C30 C29 H29 119.1 . . ? C29 C30 C31 117.6(4) . . ? C29 C30 C33 120.9(4) . . ? C31 C30 C33 121.5(4) . . ? C30 C31 H31 119.4 . . ? C32 C31 C30 121.3(5) . . ? C32 C31 H31 119.4 . . ? C27 C32 H32 119.4 . . ? C31 C32 C27 121.3(4) . . ? C31 C32 H32 119.4 . . ? C34 C33 C30 121.5(4) . . ? C34 C33 C38 118.0(5) . . ? C38 C33 C30 120.5(4) . . ? C33 C34 H34 119.6 . . ? C33 C34 C35 120.8(5) . . ? C35 C34 H34 119.6 . . ? C34 C35 H35 120.0 . . ? C36 C35 C34 119.9(5) . . ? C36 C35 H35 120.0 . . ? C35 C36 H36 119.9 . . ? C37 C36 C35 120.2(5) . . ? C37 C36 H36 119.9 . . ? C36 C37 H37 119.8 . . ? C36 C37 C38 120.4(5) . . ? C38 C37 H37 119.8 . . ? C33 C38 H38 119.6 . . ? C37 C38 C33 120.7(5) . . ? C37 C38 H38 119.6 . . ? 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 S1 O1 1.556(3) . ? S1 O2 1.421(3) . ? S1 O3 1.434(3) . ? S1 C2 1.781(5) . ? Si1 C2 1.937(5) . ? Si1 C3 1.863(5) . ? Si1 C4 1.862(5) . ? Si1 C5 1.845(5) . ? F1 C7 1.318(5) . ? F2 C7 1.344(5) . ? F3 C7 1.339(5) . ? O1 C1 1.460(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C6 1.354(6) . ? 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 C7 1.522(6) . ? C6 C8 1.494(6) . ? C8 C9 1.413(6) . ? C8 C13 1.388(6) . ? C9 H9 0.9500 . ? C9 C10 1.364(6) . ? C10 H10 0.9500 . ? C10 C11 1.396(6) . ? C11 C12 1.398(6) . ? C11 C14 1.473(6) . ? C12 H12 0.9500 . ? C12 C13 1.380(6) . ? C13 H13 0.9500 . ? C14 C15 1.395(6) . ? C14 C19 1.390(6) . ? C15 H15 0.9500 . ? C15 C16 1.385(6) . ? C16 H16 0.9500 . ? C16 C17 1.371(7) . ? C17 H17 0.9500 . ? C17 C18 1.365(7) . ? C18 H18 0.9500 . ? C18 C19 1.386(7) . ? C19 H19 0.9500 . ? S2 O4 1.566(4) . ? S2 O5 1.426(4) . ? S2 O6 1.416(4) . ? S2 C21 1.790(5) . ? Si2 C21 1.936(5) . ? Si2 C22 1.857(5) . ? Si2 C23 1.855(6) . ? Si2 C24 1.860(6) . ? F4 C26 1.345(6) . ? F5 C26 1.344(5) . ? F6 C26 1.327(6) . ? O4 C20 1.460(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.357(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.504(7) . ? C25 C27 1.479(6) . ? C27 C28 1.410(6) . ? C27 C32 1.388(6) . ? C28 H28 0.9500 . ? C28 C29 1.378(6) . ? C29 H29 0.9500 . ? C29 C30 1.391(6) . ? C30 C31 1.392(6) . ? C30 C33 1.479(6) . ? C31 H31 0.9500 . ? C31 C32 1.378(6) . ? C32 H32 0.9500 . ? C33 C34 1.387(6) . ? C33 C38 1.395(6) . ? C34 H34 0.9500 . ? C34 C35 1.388(7) . ? C35 H35 0.9500 . ? C35 C36 1.377(8) . ? C36 H36 0.9500 . ? C36 C37 1.360(8) . ? C37 H37 0.9500 . ? C37 C38 1.383(7) . ? C38 H38 0.9500 . ?