#------------------------------------------------------------------------------ #$Date: 2021-08-05 03:36:52 +0300 (Thu, 05 Aug 2021) $ #$Revision: 267949 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564327.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_1564327 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_absolute_configuration unk _chemical_formula_moiety 'C13 H14 F4 O2 S' _chemical_formula_sum 'C13 H14 F4 O2 S' _chemical_formula_weight 310.30 _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_Hall 'P -2yc' _space_group_name_H-M_alt 'P 1 c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-03-22 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-05-15 deposited with the CCDC. 2021-08-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.425(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.1315(7) _cell_length_b 8.3917(5) _cell_length_c 15.5384(10) _cell_measurement_reflns_used 7098 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 68.487 _cell_measurement_theta_min 4.212 _cell_volume 1368.85(15) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 273.15 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_unetI/netI 0.0321 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8209 _diffrn_reflns_point_group_measured_fraction_full 0.733 _diffrn_reflns_point_group_measured_fraction_max 0.726 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.482 _diffrn_reflns_theta_min 4.211 _diffrn_source 'sealed tube' _diffrn_source_current 0.64 _diffrn_source_power 0.0286272 _diffrn_source_voltage 44.73 _exptl_absorpt_coefficient_mu 2.556 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.6861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0654 before and 0.0388 after correction. The Ratio of minimum to maximum transmission is 0.9110. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.506 _exptl_crystal_description block _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.208 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.038 _refine_ls_abs_structure_details ; Flack x determined using 1114 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.056(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 367 _refine_ls_number_reflns 3662 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0246 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0171P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.0625 _reflns_Friedel_coverage 0.472 _reflns_Friedel_fraction_full 0.474 _reflns_Friedel_fraction_max 0.467 _reflns_number_gt 3604 _reflns_number_total 3662 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc03315h2.cif _cod_data_source_block ykd _cod_database_code 1564327 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.784 _shelx_estimated_absorpt_t_min 0.749 _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. Rigid bond restraints S1, O1 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002 3.a Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A) 3.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C1A(H1AA,H1AB,H1AC), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC) ; _shelx_res_file ; TITL ykd_a.res in Pc ykd.res created by SHELXL-2018/3 at 13:03:40 on 22-Mar-2021 REM Old TITL YKD in Pc REM SHELXT solution in Pc: R1 0.094, Rweak 0.025, Alpha 0.001 REM 0.722 for 179 systematic absences, Orientation as input REM Flack x = 0.105 ( 0.008 ) from 1117 Parsons' quotients REM Formula found by SHELXT: C26 O5 F7 S2 CELL 1.54178 11.1315 8.3917 15.5384 90 109.425 90 ZERR 4 0.0007 0.0005 0.001 0 0.003 0 LATT -1 SYMM +X,-Y,0.5+Z SFAC C H F O S UNIT 52 56 16 8 4 DELU 0.001 0.002 S1 O1 L.S. 10 0 0 PLAN 5 SIZE 0.1 0.11 0.12 TEMP 0 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.042600 0.017100 FVAR 0.59040 S1 5 0.126352 0.471827 0.500599 11.00000 0.04222 0.03863 = 0.02412 0.00301 0.00596 0.01044 F1 3 -0.004349 0.522239 0.499912 11.00000 0.03893 0.07027 = 0.05083 0.00189 0.00652 0.01511 F2 3 0.355287 0.323998 0.503943 11.00000 0.04653 0.05438 = 0.03069 0.00299 0.02175 0.00620 F3 3 0.468965 0.183535 0.614712 11.00000 0.03474 0.06201 = 0.03508 -0.00363 0.01246 0.01658 F4 3 0.284283 0.099470 0.534936 11.00000 0.05162 0.03526 = 0.04103 -0.01366 0.01227 0.00411 O1 4 0.185033 0.604951 0.473607 11.00000 0.05486 0.04667 = 0.03528 0.01212 0.01260 0.00301 O2 4 0.109141 0.331321 0.446192 11.00000 0.04942 0.04504 = 0.02742 -0.00489 0.00022 0.00143 C1 1 0.271542 0.538711 0.782455 11.00000 0.05078 0.04389 = 0.02918 -0.01065 0.00904 0.01096 AFIX 137 H1A 2 0.278165 0.437250 0.812220 11.00000 -1.50000 H1B 2 0.250350 0.619118 0.818956 11.00000 -1.50000 H1C 2 0.351459 0.564538 0.774900 11.00000 -1.50000 AFIX 0 C2 1 0.166908 0.531069 0.688448 11.00000 0.03273 0.03175 = 0.02956 -0.00567 0.01205 0.00466 C3 1 0.207491 0.427826 0.619488 11.00000 0.02749 0.02766 = 0.02056 -0.00195 0.00698 -0.00023 C4 1 0.294528 0.310803 0.638905 11.00000 0.02626 0.02688 = 0.02207 -0.00354 0.00856 -0.00232 C5 1 0.348545 0.230450 0.571359 11.00000 0.03260 0.03584 = 0.02530 -0.00246 0.00919 0.00750 C6 1 0.145425 0.706013 0.656434 11.00000 0.05215 0.03281 = 0.04358 -0.00383 0.01468 0.01158 AFIX 137 H6A 2 0.127856 0.769143 0.702386 11.00000 -1.50000 H6B 2 0.074540 0.711965 0.600645 11.00000 -1.50000 H6C 2 0.220513 0.745778 0.646353 11.00000 -1.50000 AFIX 0 C7 1 0.045949 0.462860 0.701567 11.00000 0.04435 0.05542 = 0.05411 -0.01087 0.03003 -0.00270 AFIX 137 H7A 2 0.061138 0.354682 0.722463 11.00000 -1.50000 H7B 2 -0.022894 0.465806 0.644529 11.00000 -1.50000 H7C 2 0.024089 0.525510 0.745898 11.00000 -1.50000 AFIX 0 C8 1 0.344872 0.231643 0.730320 11.00000 0.02696 0.02496 = 0.02541 -0.00103 0.01053 0.00327 C9 1 0.268389 0.118344 0.752449 11.00000 0.02732 0.03401 = 0.02862 -0.00170 0.00806 -0.00076 AFIX 43 H9 2 0.187882 0.095630 0.711511 11.00000 -1.20000 AFIX 0 C10 1 0.312205 0.039617 0.835328 11.00000 0.03794 0.03666 = 0.03588 0.00533 0.01550 -0.00141 AFIX 43 H10 2 0.261178 -0.036544 0.849666 11.00000 -1.20000 AFIX 0 C11 1 0.431128 0.073377 0.896851 11.00000 0.04029 0.04279 = 0.02746 0.00811 0.01404 0.00709 AFIX 43 H11 2 0.459789 0.021028 0.952750 11.00000 -1.20000 AFIX 0 C12 1 0.507973 0.186060 0.874900 11.00000 0.02683 0.04108 = 0.02880 0.00047 0.00621 0.00394 AFIX 43 H12 2 0.587757 0.209927 0.916505 11.00000 -1.20000 AFIX 0 C13 1 0.466056 0.262552 0.791479 11.00000 0.02634 0.03268 = 0.02940 -0.00079 0.01021 0.00022 AFIX 43 H13 2 0.518926 0.334878 0.776136 11.00000 -1.20000 AFIX 0 S1A 5 0.845978 0.003317 0.510552 11.00000 0.03160 0.04330 = 0.02594 0.00791 0.00513 -0.00043 F1A 3 0.729799 0.042568 0.538314 11.00000 0.04348 0.06331 = 0.03471 0.00748 0.01789 0.00041 F2A 3 0.783116 0.330367 0.528168 11.00000 0.04517 0.05212 = 0.03034 -0.01304 0.01038 0.00246 F3A 3 0.689912 0.480093 0.416568 11.00000 0.07932 0.03514 = 0.04836 -0.00541 0.02219 0.01627 F4A 3 0.585313 0.291416 0.450986 11.00000 0.03650 0.07751 = 0.05006 -0.01262 0.02315 0.00600 O1A 4 0.955668 0.069699 0.573680 11.00000 0.03942 0.06382 = 0.03241 0.00617 -0.00059 -0.00333 O2A 4 0.839128 -0.166257 0.498805 11.00000 0.04167 0.03745 = 0.04679 0.01519 0.01037 0.00297 C1A 1 0.886995 0.107345 0.262368 11.00000 0.04304 0.04142 = 0.03623 -0.00458 0.02519 0.00034 AFIX 137 H1AA 2 0.806046 0.130021 0.217080 11.00000 -1.50000 H1AB 2 0.940996 0.055072 0.234136 11.00000 -1.50000 H1AC 2 0.926141 0.205104 0.289866 11.00000 -1.50000 AFIX 0 C2A 1 0.867470 -0.001755 0.336033 11.00000 0.02661 0.02803 = 0.03310 -0.00581 0.01193 -0.00027 C3A 1 0.807335 0.090889 0.398849 11.00000 0.02309 0.02789 = 0.02292 -0.00042 0.00672 -0.00244 C4A 1 0.733529 0.221435 0.377210 11.00000 0.02521 0.02839 = 0.02648 -0.00290 0.01082 -0.00267 C5A 1 0.698128 0.329334 0.444200 11.00000 0.03588 0.03933 = 0.03228 -0.00392 0.01222 0.00814 C6A 1 1.002752 -0.060003 0.392607 11.00000 0.02960 0.04069 = 0.05143 -0.00241 0.01549 0.00544 AFIX 137 H6AA 2 1.044773 -0.100285 0.352242 11.00000 -1.50000 H6AB 2 0.996477 -0.143104 0.433360 11.00000 -1.50000 H6AC 2 1.050857 0.027276 0.427285 11.00000 -1.50000 AFIX 0 C7A 1 0.785689 -0.144466 0.290167 11.00000 0.03846 0.03729 = 0.05040 -0.01464 0.01849 -0.00519 AFIX 137 H7AA 2 0.702048 -0.108294 0.254676 11.00000 -1.50000 H7AB 2 0.779512 -0.217617 0.336012 11.00000 -1.50000 H7AC 2 0.824177 -0.197062 0.251024 11.00000 -1.50000 AFIX 0 C8A 1 0.667416 0.274524 0.280975 11.00000 0.03197 0.02640 = 0.02756 0.00243 0.01361 0.00476 C9A 1 0.563294 0.187917 0.227971 11.00000 0.03449 0.03283 = 0.02911 0.00163 0.01012 0.00345 AFIX 43 H9A 2 0.537220 0.098021 0.252005 11.00000 -1.20000 AFIX 0 C10A 1 0.497536 0.234898 0.138883 11.00000 0.04614 0.05059 = 0.03083 -0.00353 0.00430 0.01011 AFIX 43 H10A 2 0.427583 0.176497 0.103405 11.00000 -1.20000 AFIX 0 C11A 1 0.536268 0.368582 0.103077 11.00000 0.07595 0.05317 = 0.02950 0.01092 0.01634 0.02464 AFIX 43 H11A 2 0.493402 0.399082 0.043143 11.00000 -1.20000 AFIX 0 C12A 1 0.638607 0.456527 0.156473 11.00000 0.08461 0.03753 = 0.04316 0.01584 0.03586 0.01267 AFIX 43 H12A 2 0.663419 0.547352 0.132464 11.00000 -1.20000 AFIX 0 C13A 1 0.704778 0.411491 0.245178 11.00000 0.05230 0.02935 = 0.04328 0.00199 0.02399 -0.00032 AFIX 43 H13A 2 0.773519 0.471686 0.280752 11.00000 -1.20000 AFIX 0 HKLF 4 REM ykd_a.res in Pc REM wR2 = 0.0625, GooF = S = 1.068, Restrained GooF = 1.071 for all data REM R1 = 0.0246 for 3604 Fo > 4sig(Fo) and 0.0249 for all 3662 data REM 367 parameters refined using 3 restraints END WGHT 0.0426 0.0171 REM Highest difference peak 0.208, deepest hole -0.242, 1-sigma level 0.038 Q1 1 0.1703 0.4404 0.5663 11.00000 0.05 0.21 Q2 1 0.8147 0.0444 0.4473 11.00000 0.05 0.18 Q3 1 0.8398 -0.1342 0.5124 11.00000 0.05 0.18 Q4 1 0.1793 0.6167 0.4952 11.00000 0.05 0.16 Q5 1 0.4978 0.3413 0.1341 11.00000 0.05 0.16 ; _shelx_res_checksum 69774 _shelx_hkl_file ; 1 0 0 57.29 2.20 2 0 0 1620.04 50.19 -2 0 0 1723.43 52.99 -3 0 0 474.45 15.10 3 0 0 467.65 14.70 -4 0 0 335.97 11.70 4 0 0 266.87 10.70 5 0 0 348.37 13.00 -5 0 0 332.07 13.40 6 0 0 958.80 31.00 7 0 0 570.04 21.70 -8 0 0 216.88 6.50 -8 0 0 214.88 6.10 8 0 0 200.28 12.10 -9 0 0 42.30 1.70 -9 0 0 39.90 1.90 -10 0 0 10.20 0.80 -10 0 0 10.90 1.00 11 0 0 28.70 2.20 -11 0 0 33.90 1.40 -11 0 0 32.00 1.60 -12 0 0 26.60 1.30 12 0 0 30.80 1.90 -12 0 0 28.90 1.20 0 1 0 21.30 1.40 -1 1 0 1977.80 59.89 -1 1 0 1795.32 50.79 1 1 0 1973.40 58.39 -2 1 0 8440.26 230.48 2 1 0 8291.47 328.47 -2 1 0 8934.41 367.06 -3 1 0 728.13 22.00 3 1 0 676.63 21.10 4 -1 0 659.73 20.80 4 1 0 652.13 20.70 -4 1 0 643.24 21.40 5 -1 0 554.84 19.00 5 1 0 549.25 19.00 -5 1 0 546.55 19.80 6 -1 0 18.10 2.80 6 1 0 18.10 2.80 7 -1 0 92.49 7.00 -7 1 0 86.69 7.30 7 1 0 92.69 7.00 -8 -1 0 104.19 3.70 -8 -1 0 111.59 3.50 -8 1 0 109.39 3.40 -8 1 0 112.79 3.80 -9 -1 0 225.48 7.10 -9 -1 0 242.78 6.90 -9 1 0 241.58 7.30 -9 1 0 235.48 6.80 -10 -1 0 63.59 2.30 -10 -1 0 58.99 2.40 10 -1 0 60.99 3.40 -10 1 0 66.29 2.60 -10 1 0 65.89 2.30 11 -1 0 9.00 1.40 -11 -1 0 8.00 0.70 -11 1 0 7.30 0.70 -11 1 0 7.00 0.80 -12 -1 0 21.80 1.00 -12 1 0 21.30 1.10 -12 1 0 20.70 0.90 0 2 0 760.22 22.20 -1 2 0 4535.05 234.08 1 2 0 4676.93 137.09 -2 2 0 336.57 12.00 2 2 0 330.57 11.30 -2 2 0 317.67 8.80 -3 2 0 118.39 6.60 3 2 0 127.09 6.00 -4 2 0 195.98 9.80 4 2 0 237.98 9.50 5 2 0 248.38 11.10 -5 2 0 261.97 12.10 6 -2 0 70.69 5.80 -6 2 0 65.89 6.20 6 2 0 70.49 5.60 7 -2 0 733.13 26.70 -7 2 0 678.13 27.40 -7 2 0 704.13 19.60 7 2 0 726.13 26.50 -8 -2 0 21.60 1.10 -8 2 0 20.10 1.40 -8 2 0 20.90 1.10 -8 2 0 21.20 4.30 -9 -2 0 128.29 4.00 9 -2 0 130.49 5.30 -9 2 0 130.39 4.00 -9 2 0 129.19 4.40 10 -2 0 53.89 3.20 -10 -2 0 61.19 2.20 -10 2 0 61.39 2.60 -10 2 0 62.39 2.10 -11 -2 0 8.10 0.70 -11 2 0 7.30 0.90 -11 2 0 8.30 0.70 12 -2 0 10.60 1.50 -12 -2 0 10.70 0.60 -12 2 0 10.10 0.80 0 3 0 19.70 2.40 1 3 0 97.89 5.30 -1 3 0 86.99 4.90 -1 3 0 93.89 5.70 -2 3 0 481.65 16.80 -2 3 0 459.35 12.10 2 3 0 418.46 15.60 3 3 0 4.90 1.70 4 3 0 383.46 14.70 -4 3 0 363.76 15.70 5 3 0 10.70 2.40 6 -3 0 131.39 8.50 -6 3 0 108.29 8.70 6 3 0 128.39 8.50 7 -3 0 2.00 0.70 -7 -3 0 1.40 0.40 -7 3 0 1.60 0.50 -7 3 0 2.00 1.90 7 3 0 1.40 1.70 -8 -3 0 82.29 2.80 8 -3 0 84.79 4.00 -8 3 0 81.59 3.10 -9 -3 0 80.19 2.70 -9 3 0 79.09 3.10 10 -3 0 1.50 1.00 -10 -3 0 1.00 0.40 -10 3 0 1.70 0.50 -11 -3 0 14.20 0.80 11 -3 0 17.20 2.00 -11 3 0 13.80 1.10 -12 3 0 21.20 1.00 0 4 0 671.03 22.40 1 4 0 79.39 5.50 -1 4 0 85.99 5.50 -2 4 0 90.29 6.60 2 4 0 88.79 6.10 -3 4 0 96.19 7.20 3 4 0 73.99 5.90 4 4 0 230.38 11.50 -4 4 0 211.68 12.10 -5 4 0 49.00 5.80 5 4 0 49.50 5.30 6 -4 0 233.38 13.30 6 -4 0 235.78 8.30 -6 4 0 241.78 7.20 6 4 0 241.98 13.20 7 -4 0 125.39 5.30 -7 4 0 111.79 4.00 8 -4 0 203.48 7.70 -8 4 0 213.38 6.50 -9 -4 0 2.40 0.50 9 -4 0 1.50 1.10 -9 4 0 1.80 0.60 10 -4 0 84.19 4.20 -10 -4 0 81.79 3.00 -10 4 0 89.39 3.10 11 -4 0 46.30 3.00 -11 4 0 49.20 1.90 0 5 0 218.38 10.90 1 5 0 219.68 11.10 2 5 0 233.48 11.80 -4 5 0 1.20 0.60 5 -5 0 57.29 3.50 5 5 0 60.99 3.10 -5 5 0 62.89 2.90 6 -5 0 369.06 12.40 -6 5 0 384.56 11.00 6 5 0 396.56 12.00 7 -5 0 45.60 3.30 -7 5 0 48.10 2.10 7 5 0 45.70 2.70 8 -5 0 204.98 7.80 -8 5 0 193.68 6.20 8 5 0 207.38 7.20 9 -5 0 116.49 5.30 -9 5 0 110.69 3.80 9 5 0 108.39 4.50 10 -5 0 37.50 2.90 -10 5 0 44.20 1.70 10 5 0 37.80 2.10 0 -6 0 173.28 6.20 0 6 0 158.88 9.90 0 6 0 158.18 5.80 0 6 0 151.78 5.50 0 6 0 157.58 5.80 1 -6 0 255.97 8.10 -1 -6 0 224.18 7.80 -1 6 0 231.08 7.40 -1 6 0 225.98 7.60 1 6 0 223.08 12.40 1 6 0 213.68 7.20 -1 6 0 221.68 7.60 1 6 0 217.28 7.50 -2 -6 0 5.90 1.20 2 -6 0 7.90 1.50 2 6 0 6.80 1.00 -2 6 0 6.60 1.00 -2 6 0 6.00 1.10 2 6 0 6.70 1.20 2 6 0 8.30 3.20 3 -6 0 225.28 7.90 3 6 0 197.48 6.90 -3 6 0 220.58 7.30 3 6 0 200.08 7.20 4 -6 0 209.38 7.90 4 6 0 193.28 7.10 -4 6 0 218.78 7.20 5 -6 0 13.70 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35.10 2.20 2 8 0 35.10 2.10 2 8 0 35.30 2.30 -2 8 0 35.70 2.30 3 -8 0 27.70 2.80 -3 8 0 28.50 2.00 3 8 0 30.40 2.10 3 8 0 27.90 1.90 -3 8 0 27.90 1.90 4 -8 0 22.20 2.40 4 8 0 21.50 1.80 -4 8 0 18.60 1.60 -4 8 0 18.20 1.50 5 -8 0 18.90 2.20 -5 8 0 17.10 1.40 5 8 0 16.40 1.60 6 -8 0 28.70 2.40 6 8 0 30.40 1.90 -6 8 0 25.30 1.60 7 -8 0 6.80 1.30 7 8 0 5.90 1.00 0 9 0 42.30 2.20 0 9 0 43.10 2.30 1 9 0 6.90 1.00 1 9 0 6.20 1.10 -1 9 0 5.20 0.90 -1 9 0 4.80 0.90 -2 9 0 86.69 3.40 -2 9 0 82.19 3.30 2 9 0 81.59 3.50 2 9 0 77.99 3.20 3 -9 0 1.30 1.00 -3 9 0 1.10 0.60 -3 9 0 1.30 0.50 3 9 0 1.70 0.70 4 -9 0 55.09 2.70 -4 9 0 59.19 2.50 4 9 0 57.99 2.70 5 -9 0 16.60 1.40 -5 9 0 16.10 1.10 5 9 0 18.50 1.40 0 10 0 11.20 1.00 -1 10 0 6.50 0.80 1 10 0 5.70 0.80 -2 10 0 15.00 1.10 -12 0 1 -0.30 0.30 -12 0 1 0.00 0.30 -12 0 1 -0.10 0.20 -11 0 1 0.00 0.30 -11 0 1 0.10 0.40 -10 0 1 0.10 0.40 -10 0 1 0.40 0.40 -9 0 1 0.10 0.40 -9 0 1 0.30 0.40 -8 0 1 0.30 0.30 -8 0 1 -0.10 0.40 7 0 -1 0.20 0.90 6 0 -1 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2.80 9 1 1 68.49 3.50 -9 1 -1 67.99 2.40 10 -1 1 19.70 1.90 -10 -1 -1 20.50 1.10 -10 -1 -1 18.50 1.20 10 1 1 19.80 1.90 -10 1 -1 19.00 1.10 -10 1 -1 19.40 1.30 -11 -1 -1 6.50 1.00 -11 -1 -1 6.60 0.70 11 -1 1 7.30 1.30 11 1 1 6.00 1.10 -11 1 -1 6.30 0.80 -11 1 -1 6.40 0.60 12 -1 1 36.90 2.20 -12 -1 -1 43.90 1.50 12 1 1 42.40 2.20 -12 1 -1 42.70 1.70 -12 1 -1 43.00 1.40 12 -2 -1 41.00 2.50 -12 -2 1 39.40 1.30 -12 -2 1 40.30 1.50 -12 2 1 40.40 1.40 -12 2 1 42.80 1.70 -11 -2 1 7.10 0.50 -11 -2 1 8.20 0.70 -11 2 1 7.30 0.90 -11 2 1 7.30 0.70 -10 -2 1 23.90 1.00 -10 -2 1 25.40 1.20 -10 2 1 25.10 1.60 -10 2 1 23.70 1.20 -9 -2 1 31.90 1.40 -9 -2 1 28.70 1.10 -9 2 1 29.70 1.70 -9 2 1 28.80 1.30 -8 -2 1 16.40 0.80 -8 -2 1 16.00 1.00 -8 2 1 16.60 1.20 -8 2 1 15.90 3.70 -8 2 1 16.60 0.90 7 -2 -1 14.10 2.90 -7 2 1 13.70 1.80 -7 2 1 11.80 3.00 6 -2 -1 95.49 6.50 6 2 -1 93.99 6.30 -6 2 1 87.89 6.80 5 2 -1 52.99 4.20 -5 2 1 51.19 4.70 -4 2 1 688.63 18.90 -4 2 1 755.82 23.90 4 2 -1 681.13 22.20 -3 2 1 888.51 22.90 -3 2 1 884.31 26.80 -3 2 1 817.12 22.90 3 2 -1 851.51 25.60 -2 2 1 120.19 3.60 2 2 -1 136.29 5.50 1 2 -1 431.96 13.50 -1 2 1 430.16 13.50 0 2 -1 1258.37 41.80 0 2 -1 1227.38 38.50 0 2 1 1320.57 39.00 1 2 1 57.89 3.50 -1 2 -1 57.59 3.80 2 2 1 72.69 4.30 -2 2 -1 73.59 2.10 -2 2 -1 79.19 4.90 -3 2 -1 95.69 5.80 3 2 1 80.59 5.00 -4 2 -1 605.04 21.30 4 2 1 587.84 20.30 5 -2 1 53.29 4.70 -5 2 -1 53.59 5.20 5 2 1 51.89 4.60 6 -2 1 87.19 6.70 6 2 1 83.69 6.50 -6 2 -1 91.09 7.40 7 -2 1 124.89 8.90 7 -2 1 117.89 4.80 -7 2 -1 124.19 3.70 7 2 1 122.09 8.80 -7 2 -1 130.29 4.20 -7 2 -1 117.79 9.50 8 -2 1 30.60 2.30 8 2 1 29.90 2.20 -8 2 -1 34.10 1.40 -8 2 -1 34.50 1.80 9 -2 1 116.49 4.90 -9 -2 -1 119.09 3.70 -9 2 -1 117.09 4.10 -9 2 -1 114.19 3.60 9 2 1 111.19 4.80 10 -2 1 12.80 1.70 -10 -2 -1 14.10 0.90 -10 2 -1 12.50 0.80 -10 2 -1 13.00 1.20 10 2 1 12.60 1.60 -11 -2 -1 49.90 1.80 -11 2 -1 47.60 1.70 11 2 1 49.00 2.70 -11 2 -1 51.79 2.10 -12 -2 -1 20.40 0.80 12 -2 1 17.50 1.70 -12 2 -1 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1.20 -4 -3 17 24.20 1.20 -4 3 17 24.10 0.80 -4 3 17 25.20 1.20 -3 -3 17 38.40 1.10 -3 -3 17 38.40 1.50 -3 3 17 38.10 1.50 -3 3 17 37.80 1.20 -2 -3 17 12.20 0.50 -2 -3 17 11.30 0.80 -2 3 17 11.60 0.90 -2 3 17 12.00 0.50 -1 -3 17 7.60 0.40 -1 -3 17 8.00 0.60 -5 -4 17 3.30 0.60 -5 4 17 3.20 0.20 -4 4 17 18.70 0.60 -7 0 18 19.80 1.00 -6 0 18 53.59 1.90 -5 0 18 42.70 1.60 -4 0 18 117.49 3.60 -4 0 18 114.49 3.50 -3 0 18 51.59 1.90 -3 0 18 53.09 1.50 -2 0 18 14.90 0.80 -2 0 18 15.60 0.60 -7 -1 18 29.90 1.30 -6 -1 18 5.10 0.60 -6 1 18 5.20 0.60 -5 -1 18 73.39 2.40 -5 1 18 68.39 2.30 -5 1 18 67.69 2.30 -4 -1 18 48.60 1.80 -4 1 18 48.90 1.40 -4 1 18 52.29 1.80 -4 1 18 47.60 1.70 -3 -1 18 9.40 0.70 -3 -1 18 9.30 0.40 -3 1 18 8.90 0.80 -3 1 18 9.00 0.40 -3 1 18 8.80 0.80 -2 -1 18 106.99 2.90 -2 -1 18 106.99 3.30 -2 1 18 104.29 3.00 -6 -2 18 74.09 2.40 -5 -2 18 4.80 0.50 -4 -2 18 20.40 1.00 -4 2 18 20.80 0.60 -4 2 18 21.20 1.10 -3 -2 18 81.89 2.60 -3 2 18 83.49 3.00 -3 2 18 80.29 2.30 -2 -2 18 4.20 0.50 -2 -2 18 3.90 0.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 31542 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, 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 0.12635(5) 0.47183(7) 0.50060(3) 0.03625(15) Uani 1 1 d . U . . . F1 F -0.00435(15) 0.5222(2) 0.49991(12) 0.0554(4) Uani 1 1 d . . . . . F2 F 0.35529(14) 0.32400(18) 0.50394(9) 0.0416(3) Uani 1 1 d . . . . . F3 F 0.46897(13) 0.1835(2) 0.61471(9) 0.0437(3) Uani 1 1 d . . . . . F4 F 0.28428(14) 0.09947(17) 0.53494(10) 0.0434(3) Uani 1 1 d . . . . . O1 O 0.18503(19) 0.6050(2) 0.47361(12) 0.0462(4) Uani 1 1 d . U . . . O2 O 0.10914(18) 0.3313(2) 0.44619(12) 0.0438(4) Uani 1 1 d . . . . . C1 C 0.2715(3) 0.5387(3) 0.78246(16) 0.0423(6) Uani 1 1 d . . . . . H1A H 0.278165 0.437250 0.812220 0.064 Uiso 1 1 calc R U . . . H1B H 0.250350 0.619118 0.818956 0.064 Uiso 1 1 calc R U . . . H1C H 0.351459 0.564538 0.774900 0.064 Uiso 1 1 calc R U . . . C2 C 0.1669(2) 0.5311(3) 0.68845(15) 0.0309(4) Uani 1 1 d . . . . . C3 C 0.20749(19) 0.4278(2) 0.61949(13) 0.0255(4) Uani 1 1 d . . . . . C4 C 0.29453(18) 0.3108(2) 0.63890(13) 0.0249(4) Uani 1 1 d . . . . . C5 C 0.3485(2) 0.2304(3) 0.57136(14) 0.0314(4) Uani 1 1 d . . . . . C6 C 0.1454(3) 0.7060(3) 0.65643(19) 0.0432(5) Uani 1 1 d . . . . . H6A H 0.127856 0.769143 0.702386 0.065 Uiso 1 1 calc R U . . . H6B H 0.074540 0.711965 0.600645 0.065 Uiso 1 1 calc R U . . . H6C H 0.220513 0.745778 0.646353 0.065 Uiso 1 1 calc R U . . . C7 C 0.0459(3) 0.4629(4) 0.7016(2) 0.0479(6) Uani 1 1 d . . . . . H7A H 0.061138 0.354682 0.722463 0.072 Uiso 1 1 calc R U . . . H7B H -0.022894 0.465806 0.644529 0.072 Uiso 1 1 calc R U . . . H7C H 0.024089 0.525510 0.745898 0.072 Uiso 1 1 calc R U . . . C8 C 0.34487(18) 0.2316(2) 0.73032(14) 0.0253(4) Uani 1 1 d . . . . . C9 C 0.26839(19) 0.1183(3) 0.75245(14) 0.0303(4) Uani 1 1 d . . . . . H9 H 0.187882 0.095630 0.711511 0.036 Uiso 1 1 calc R U . . . C10 C 0.3122(2) 0.0396(3) 0.83533(17) 0.0360(5) Uani 1 1 d . . . . . H10 H 0.261178 -0.036544 0.849666 0.043 Uiso 1 1 calc R U . . . C11 C 0.4311(2) 0.0734(3) 0.89685(15) 0.0362(5) Uani 1 1 d . . . . . H11 H 0.459789 0.021028 0.952750 0.043 Uiso 1 1 calc R U . . . C12 C 0.5080(2) 0.1861(3) 0.87490(15) 0.0330(4) Uani 1 1 d . . . . . H12 H 0.587757 0.209927 0.916505 0.040 Uiso 1 1 calc R U . . . C13 C 0.4661(2) 0.2626(3) 0.79148(15) 0.0292(4) Uani 1 1 d . . . . . H13 H 0.518926 0.334878 0.776136 0.035 Uiso 1 1 calc R U . . . S1A S 0.84598(5) 0.00332(7) 0.51055(4) 0.03472(14) Uani 1 1 d . . . . . F1A F 0.72980(15) 0.0426(2) 0.53831(10) 0.0460(4) Uani 1 1 d . . . . . F2A F 0.78312(14) 0.33037(19) 0.52817(10) 0.0431(3) Uani 1 1 d . . . . . F3A F 0.6899(2) 0.48009(19) 0.41657(12) 0.0540(4) Uani 1 1 d . . . . . F4A F 0.58531(15) 0.2914(2) 0.45099(12) 0.0525(4) Uani 1 1 d . . . . . O1A O 0.95567(18) 0.0697(3) 0.57368(12) 0.0483(4) Uani 1 1 d . . . . . O2A O 0.83913(17) -0.1663(2) 0.49881(13) 0.0430(4) Uani 1 1 d . . . . . C1A C 0.8870(2) 0.1073(3) 0.26237(16) 0.0372(5) Uani 1 1 d . . . . . H1AA H 0.806046 0.130021 0.217080 0.056 Uiso 1 1 calc R U . . . H1AB H 0.940996 0.055072 0.234136 0.056 Uiso 1 1 calc R U . . . H1AC H 0.926141 0.205104 0.289866 0.056 Uiso 1 1 calc R U . . . C2A C 0.8675(2) -0.0018(3) 0.33603(16) 0.0288(4) Uani 1 1 d . . . . . C3A C 0.80733(18) 0.0909(2) 0.39885(13) 0.0249(4) Uani 1 1 d . . . . . C4A C 0.73353(19) 0.2214(3) 0.37721(14) 0.0261(4) Uani 1 1 d . . . . . C5A C 0.6981(2) 0.3293(3) 0.44420(16) 0.0356(5) Uani 1 1 d . . . . . C6A C 1.0028(2) -0.0600(3) 0.39261(19) 0.0401(5) Uani 1 1 d . . . . . H6AA H 1.044773 -0.100285 0.352242 0.060 Uiso 1 1 calc R U . . . H6AB H 0.996477 -0.143104 0.433360 0.060 Uiso 1 1 calc R U . . . H6AC H 1.050857 0.027276 0.427285 0.060 Uiso 1 1 calc R U . . . C7A C 0.7857(2) -0.1445(3) 0.29017(18) 0.0411(5) Uani 1 1 d . . . . . H7AA H 0.702048 -0.108294 0.254676 0.062 Uiso 1 1 calc R U . . . H7AB H 0.779512 -0.217617 0.336012 0.062 Uiso 1 1 calc R U . . . H7AC H 0.824177 -0.197062 0.251024 0.062 Uiso 1 1 calc R U . . . C8A C 0.6674(2) 0.2745(3) 0.28098(15) 0.0277(4) Uani 1 1 d . . . . . C9A C 0.5633(2) 0.1879(3) 0.22797(15) 0.0323(4) Uani 1 1 d . . . . . H9A H 0.537220 0.098021 0.252005 0.039 Uiso 1 1 calc R U . . . C10A C 0.4975(3) 0.2349(4) 0.13888(17) 0.0446(6) Uani 1 1 d . . . . . H10A H 0.427583 0.176497 0.103405 0.054 Uiso 1 1 calc R U . . . C11A C 0.5363(3) 0.3686(4) 0.10308(18) 0.0532(7) Uani 1 1 d . . . . . H11A H 0.493402 0.399082 0.043143 0.064 Uiso 1 1 calc R U . . . C12A C 0.6386(4) 0.4565(3) 0.1565(2) 0.0515(7) Uani 1 1 d . . . . . H12A H 0.663419 0.547352 0.132464 0.062 Uiso 1 1 calc R U . . . C13A C 0.7048(3) 0.4115(3) 0.24518(18) 0.0396(5) Uani 1 1 d . . . . . H13A H 0.773519 0.471686 0.280752 0.048 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0422(3) 0.0386(3) 0.0241(3) 0.0030(2) 0.0060(2) 0.0104(2) F1 0.0389(8) 0.0703(11) 0.0508(10) 0.0019(8) 0.0065(7) 0.0151(7) F2 0.0465(7) 0.0544(8) 0.0307(6) 0.0030(6) 0.0217(6) 0.0062(7) F3 0.0347(6) 0.0620(9) 0.0351(7) -0.0036(6) 0.0125(5) 0.0166(6) F4 0.0516(8) 0.0353(7) 0.0410(7) -0.0137(6) 0.0123(6) 0.0041(6) O1 0.0549(10) 0.0467(10) 0.0353(8) 0.0121(8) 0.0126(8) 0.0030(8) O2 0.0494(9) 0.0450(10) 0.0274(7) -0.0049(7) 0.0002(7) 0.0014(8) C1 0.0508(14) 0.0439(14) 0.0292(11) -0.0106(9) 0.0090(10) 0.0110(11) C2 0.0327(10) 0.0318(11) 0.0296(11) -0.0057(8) 0.0120(9) 0.0047(9) C3 0.0275(9) 0.0277(10) 0.0206(8) -0.0020(8) 0.0070(7) -0.0002(8) C4 0.0263(8) 0.0269(9) 0.0221(9) -0.0035(8) 0.0086(7) -0.0023(8) C5 0.0326(10) 0.0358(11) 0.0253(9) -0.0025(8) 0.0092(9) 0.0075(9) C6 0.0522(13) 0.0328(12) 0.0436(13) -0.0038(10) 0.0147(11) 0.0116(11) C7 0.0444(13) 0.0554(16) 0.0541(15) -0.0109(13) 0.0300(12) -0.0027(12) C8 0.0270(9) 0.0250(9) 0.0254(9) -0.0010(7) 0.0105(8) 0.0033(7) C9 0.0273(9) 0.0340(11) 0.0286(10) -0.0017(8) 0.0081(8) -0.0008(8) C10 0.0379(12) 0.0367(11) 0.0359(12) 0.0053(9) 0.0155(10) -0.0014(10) C11 0.0403(11) 0.0428(12) 0.0275(10) 0.0081(9) 0.0140(9) 0.0071(10) C12 0.0268(9) 0.0411(12) 0.0288(10) 0.0005(9) 0.0062(8) 0.0039(9) C13 0.0263(9) 0.0327(11) 0.0294(10) -0.0008(8) 0.0102(8) 0.0002(8) S1A 0.0316(2) 0.0433(3) 0.0259(2) 0.0079(2) 0.0051(2) -0.0004(2) F1A 0.0435(8) 0.0633(10) 0.0347(7) 0.0075(6) 0.0179(6) 0.0004(7) F2A 0.0452(7) 0.0521(8) 0.0303(6) -0.0130(6) 0.0104(6) 0.0025(7) F3A 0.0793(12) 0.0351(8) 0.0484(9) -0.0054(6) 0.0222(9) 0.0163(8) F4A 0.0365(7) 0.0775(11) 0.0501(8) -0.0126(8) 0.0232(7) 0.0060(7) O1A 0.0394(9) 0.0638(12) 0.0324(9) 0.0062(8) -0.0006(7) -0.0033(9) O2A 0.0417(8) 0.0375(9) 0.0468(9) 0.0152(8) 0.0104(7) 0.0030(8) C1A 0.0430(11) 0.0414(12) 0.0362(11) -0.0046(10) 0.0252(10) 0.0003(10) C2A 0.0266(9) 0.0280(10) 0.0331(11) -0.0058(8) 0.0119(9) -0.0003(8) C3A 0.0231(8) 0.0279(10) 0.0229(8) -0.0004(7) 0.0067(7) -0.0024(7) C4A 0.0252(8) 0.0284(10) 0.0265(10) -0.0029(8) 0.0108(7) -0.0027(8) C5A 0.0359(11) 0.0393(13) 0.0323(11) -0.0039(9) 0.0122(9) 0.0081(10) C6A 0.0296(11) 0.0407(12) 0.0514(14) -0.0024(11) 0.0155(10) 0.0054(10) C7A 0.0385(11) 0.0373(12) 0.0504(14) -0.0146(11) 0.0185(11) -0.0052(10) C8A 0.0320(9) 0.0264(10) 0.0276(10) 0.0024(8) 0.0136(8) 0.0048(8) C9A 0.0345(10) 0.0328(11) 0.0291(10) 0.0016(8) 0.0101(9) 0.0034(9) C10A 0.0461(12) 0.0506(15) 0.0308(11) -0.0035(10) 0.0043(10) 0.0101(11) C11A 0.0759(19) 0.0532(16) 0.0295(11) 0.0109(11) 0.0163(12) 0.0246(15) C12A 0.085(2) 0.0375(13) 0.0432(15) 0.0158(12) 0.0359(15) 0.0127(14) C13A 0.0523(13) 0.0294(11) 0.0433(13) 0.0020(10) 0.0240(11) -0.0003(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 F1 S1 C3 102.56(9) . . ? O1 S1 F1 108.22(12) . . ? O1 S1 O2 117.24(12) . . ? O1 S1 C3 109.83(11) . . ? O2 S1 F1 106.73(11) . . ? O2 S1 C3 111.14(10) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? C1 C2 C3 112.06(18) . . ? C1 C2 C6 104.7(2) . . ? C1 C2 C7 108.0(2) . . ? C6 C2 C3 110.91(19) . . ? C7 C2 C3 110.57(19) . . ? C7 C2 C6 110.4(2) . . ? C2 C3 S1 115.45(15) . . ? C4 C3 S1 117.28(15) . . ? C4 C3 C2 127.27(19) . . ? C3 C4 C5 126.01(19) . . ? C3 C4 C8 123.53(18) . . ? C8 C4 C5 110.30(17) . . ? F2 C5 F3 105.04(18) . . ? F2 C5 C4 114.72(18) . . ? F3 C5 C4 109.85(17) . . ? F4 C5 F2 108.39(17) . . ? F4 C5 F3 106.07(19) . . ? F4 C5 C4 112.19(18) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C4 118.03(18) . . ? C13 C8 C4 122.47(19) . . ? C13 C8 C9 119.45(19) . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 120.0(2) . . ? C10 C9 H9 120.0 . . ? C9 C10 H10 119.8 . . ? C11 C10 C9 120.4(2) . . ? C11 C10 H10 119.8 . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.7(2) . . ? C12 C11 H11 120.1 . . ? C11 C12 H12 119.9 . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.9 . . ? C8 C13 H13 119.9 . . ? C12 C13 C8 120.2(2) . . ? C12 C13 H13 119.9 . . ? F1A S1A C3A 103.34(9) . . ? O1A S1A F1A 109.78(12) . . ? O1A S1A O2A 118.71(13) . . ? O1A S1A C3A 112.67(11) . . ? O2A S1A F1A 103.63(11) . . ? O2A S1A C3A 107.27(11) . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? C1A C2A C3A 111.41(17) . . ? C1A C2A C6A 105.02(19) . . ? C6A C2A C3A 109.89(19) . . ? C7A C2A C1A 109.2(2) . . ? C7A C2A C3A 111.63(18) . . ? C7A C2A C6A 109.5(2) . . ? C2A C3A S1A 112.62(15) . . ? C4A C3A S1A 120.29(16) . . ? C4A C3A C2A 127.09(19) . . ? C3A C4A C5A 126.01(19) . . ? C3A C4A C8A 123.29(18) . . ? C8A C4A C5A 110.59(17) . . ? F2A C5A F4A 107.74(19) . . ? F2A C5A C4A 114.27(18) . . ? F3A C5A F2A 105.1(2) . . ? F3A C5A F4A 106.7(2) . . ? F3A C5A C4A 110.48(19) . . ? F4A C5A C4A 112.1(2) . . ? C2A C6A H6AA 109.5 . . ? C2A C6A H6AB 109.5 . . ? C2A C6A H6AC 109.5 . . ? H6AA C6A H6AB 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? C2A C7A H7AA 109.5 . . ? C2A C7A H7AB 109.5 . . ? C2A C7A H7AC 109.5 . . ? H7AA C7A H7AB 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? C9A C8A C4A 118.30(19) . . ? C9A C8A C13A 119.7(2) . . ? C13A C8A C4A 121.9(2) . . ? C8A C9A H9A 119.9 . . ? C8A C9A C10A 120.2(2) . . ? C10A C9A H9A 119.9 . . ? C9A C10A H10A 120.0 . . ? C11A C10A C9A 119.9(3) . . ? C11A C10A H10A 120.0 . . ? C10A C11A H11A 120.1 . . ? C12A C11A C10A 119.8(2) . . ? C12A C11A H11A 120.1 . . ? C11A C12A H12A 119.6 . . ? C11A C12A C13A 120.9(3) . . ? C13A C12A H12A 119.6 . . ? C8A C13A H13A 120.3 . . ? C12A C13A C8A 119.4(3) . . ? C12A C13A H13A 120.3 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 F1 1.5118(17) . ? S1 O1 1.426(2) . ? S1 O2 1.4262(19) . ? S1 C3 1.804(2) . ? F2 C5 1.331(3) . ? F3 C5 1.343(3) . ? F4 C5 1.331(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 C2 1.537(3) . ? C2 C3 1.557(3) . ? C2 C6 1.543(3) . ? C2 C7 1.538(3) . ? C3 C4 1.342(3) . ? C4 C5 1.529(3) . ? C4 C8 1.498(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.393(3) . ? C8 C13 1.392(3) . ? C9 H9 0.9300 . ? C9 C10 1.384(3) . ? C10 H10 0.9300 . ? C10 C11 1.380(4) . ? C11 H11 0.9300 . ? C11 C12 1.391(3) . ? C12 H12 0.9300 . ? C12 C13 1.381(3) . ? C13 H13 0.9300 . ? S1A F1A 1.5291(16) . ? S1A O1A 1.402(2) . ? S1A O2A 1.4335(19) . ? S1A C3A 1.800(2) . ? F2A C5A 1.333(3) . ? F3A C5A 1.329(3) . ? F4A C5A 1.333(3) . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9600 . ? C1A H1AC 0.9600 . ? C1A C2A 1.537(3) . ? C2A C3A 1.562(3) . ? C2A C6A 1.549(3) . ? C2A C7A 1.529(3) . ? C3A C4A 1.343(3) . ? C4A C5A 1.527(3) . ? C4A C8A 1.498(3) . ? C6A H6AA 0.9600 . ? C6A H6AB 0.9600 . ? C6A H6AC 0.9600 . ? C7A H7AA 0.9600 . ? C7A H7AB 0.9600 . ? C7A H7AC 0.9600 . ? C8A C9A 1.384(3) . ? C8A C13A 1.399(3) . ? C9A H9A 0.9300 . ? C9A C10A 1.390(3) . ? C10A H10A 0.9300 . ? C10A C11A 1.383(5) . ? C11A H11A 0.9300 . ? C11A C12A 1.379(5) . ? C12A H12A 0.9300 . ? C12A C13A 1.382(4) . ? C13A H13A 0.9300 . ? 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 S1 C3 C4 C5 11.4(3) . . . . ? S1 C3 C4 C8 -163.57(15) . . . . ? F1 S1 C3 C2 -32.54(18) . . . . ? F1 S1 C3 C4 147.07(17) . . . . ? O1 S1 C3 C2 82.34(18) . . . . ? O1 S1 C3 C4 -98.04(19) . . . . ? O2 S1 C3 C2 -146.27(16) . . . . ? O2 S1 C3 C4 33.3(2) . . . . ? C1 C2 C3 S1 -156.28(18) . . . . ? C1 C2 C3 C4 24.1(3) . . . . ? C2 C3 C4 C5 -169.1(2) . . . . ? C2 C3 C4 C8 16.0(3) . . . . ? C3 C4 C5 F2 31.1(3) . . . . ? C3 C4 C5 F3 149.1(2) . . . . ? C3 C4 C5 F4 -93.1(3) . . . . ? C3 C4 C8 C9 77.5(3) . . . . ? C3 C4 C8 C13 -105.2(2) . . . . ? C4 C8 C9 C10 178.55(19) . . . . ? C4 C8 C13 C12 -179.88(19) . . . . ? C5 C4 C8 C9 -98.2(2) . . . . ? C5 C4 C8 C13 79.2(2) . . . . ? C6 C2 C3 S1 -39.7(2) . . . . ? C6 C2 C3 C4 140.8(2) . . . . ? C7 C2 C3 S1 83.1(2) . . . . ? C7 C2 C3 C4 -96.4(3) . . . . ? C8 C4 C5 F2 -153.38(17) . . . . ? C8 C4 C5 F3 -35.4(2) . . . . ? C8 C4 C5 F4 82.4(2) . . . . ? C8 C9 C10 C11 0.5(3) . . . . ? C9 C8 C13 C12 -2.6(3) . . . . ? C9 C10 C11 C12 -0.7(4) . . . . ? C10 C11 C12 C13 -0.7(4) . . . . ? C11 C12 C13 C8 2.4(3) . . . . ? C13 C8 C9 C10 1.1(3) . . . . ? S1A C3A C4A C5A 13.7(3) . . . . ? S1A C3A C4A C8A -162.26(16) . . . . ? F1A S1A C3A C2A -149.41(15) . . . . ? F1A S1A C3A C4A 30.3(2) . . . . ? O1A S1A C3A C2A 92.16(17) . . . . ? O1A S1A C3A C4A -88.2(2) . . . . ? O2A S1A C3A C2A -40.31(17) . . . . ? O2A S1A C3A C4A 139.37(17) . . . . ? C1A C2A C3A S1A -154.14(16) . . . . ? C1A C2A C3A C4A 26.2(3) . . . . ? C2A C3A C4A C5A -166.7(2) . . . . ? C2A C3A C4A C8A 17.4(3) . . . . ? C3A C4A C5A F2A 26.9(3) . . . . ? C3A C4A C5A F3A 145.2(2) . . . . ? C3A C4A C5A F4A -96.0(3) . . . . ? C3A C4A C8A C9A 72.8(3) . . . . ? C3A C4A C8A C13A -109.9(3) . . . . ? C4A C8A C9A C10A 178.7(2) . . . . ? C4A C8A C13A C12A -178.7(2) . . . . ? C5A C4A C8A C9A -103.7(2) . . . . ? C5A C4A C8A C13A 73.6(2) . . . . ? C6A C2A C3A S1A -38.2(2) . . . . ? C6A C2A C3A C4A 142.2(2) . . . . ? C7A C2A C3A S1A 83.5(2) . . . . ? C7A C2A C3A C4A -96.2(3) . . . . ? C8A C4A C5A F2A -156.7(2) . . . . ? C8A C4A C5A F3A -38.5(3) . . . . ? C8A C4A C5A F4A 80.4(2) . . . . ? C8A C9A C10A C11A 0.0(4) . . . . ? C9A C8A C13A C12A -1.4(4) . . . . ? C9A C10A C11A C12A -1.2(4) . . . . ? C10A C11A C12A C13A 1.1(4) . . . . ? C11A C12A C13A C8A 0.2(4) . . . . ? C13A C8A C9A C10A 1.3(3) . . . . ?