#------------------------------------------------------------------------------ #$Date: 2021-09-21 01:13:53 +0300 (Tue, 21 Sep 2021) $ #$Revision: 269217 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/46/1564693.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_1564693 loop_ _publ_author_name 'Chen, Ya' 'Zhu, Kun' 'Huang, Qingqin' 'Lu, Yixin' _publ_section_title ; Regiodivergent Sulfonylarylations of 1,3-Enynes via Nickel/Photoredox Dual Catalysis ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC04320J _journal_year 2021 _chemical_formula_sum 'C23 H16 Cl2 O3 S' _chemical_formula_weight 443.32 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary 'Dual Space' _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-12-27 deposited with the CCDC. 2021-09-20 downloaded from the CCDC. ; _cell_angle_alpha 97.717(2) _cell_angle_beta 95.887(2) _cell_angle_gamma 105.087(2) _cell_formula_units_Z 2 _cell_length_a 7.3445(5) _cell_length_b 7.5430(5) _cell_length_c 18.6349(12) _cell_measurement_reflns_used 7685 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.30 _cell_measurement_theta_min 2.84 _cell_volume 977.50(11) _computing_cell_refinement 'APEX3 v2016.1-0 (Bruker AXS)' _computing_data_collection 'APEX3 (Bruker AXS)' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL--2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXT--(Sheldrick 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0899 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 8693 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.313 _diffrn_reflns_theta_min 2.903 _diffrn_source 'Microfocus Sealed Tube' _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_T_max 0.862105 _exptl_absorpt_correction_T_min 0.702817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2012)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not Measured' _exptl_crystal_description Rod _exptl_crystal_F_000 456 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.058 _exptl_crystal_size_min 0.028 _refine_diff_density_max 0.708 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 8693 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0639 _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^)+(0.0455P)^2^+1.3720P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1422 _refine_ls_wR_factor_ref 0.1727 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6021 _reflns_number_total 8693 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc04320j2.cif _cod_data_source_block K433 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. data item '_exptl_crystal_density_meas' value 'Not Measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 1564693 _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. ; _computing_bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)' _shelx_res_file ; TITL K433.res in P-1 K433.res created by SHELXL-2016/6 at 16:10:35 on 11-Nov-2020 CELL 0.71073 7.3445 7.5430 18.6349 97.717 95.887 105.087 ZERR 2.000 0.0005 0.0005 0.0012 0.002 0.002 0.002 LATT 1 SFAC C H CL O S UNIT 46 32 4 6 2 MERG 0 ACTA TEMP -173.090 L.S. 10 BOND $H LIST 4 FMAP 2 CONF PLAN 20 WGHT 0.045500 1.372000 BASF 0.42563 FVAR 0.68333 C1 1 0.314665 0.395982 0.788700 11.00000 0.03368 0.01581 = 0.02799 0.00666 0.00552 0.00914 O1 4 -0.052483 0.283927 0.746747 11.00000 0.02892 0.03043 = 0.03886 0.00801 0.00502 0.00108 CL1 3 0.822796 0.678345 0.957345 11.00000 0.03662 0.04091 = 0.04732 0.00506 -0.00476 0.00485 S1 5 0.122703 0.318729 0.716323 11.00000 0.03301 0.01656 = 0.02861 0.00300 0.00306 0.00583 C2 1 0.494739 0.389886 0.773421 11.00000 0.03731 0.02455 = 0.03083 0.01027 0.00757 0.01369 AFIX 43 H2 2 0.510114 0.329453 0.727241 11.00000 -1.20000 AFIX 0 O2 4 0.154774 0.172172 0.666253 11.00000 0.04865 0.01755 = 0.02996 0.00081 0.00158 0.01124 CL2 3 0.752582 1.174856 0.938672 11.00000 0.04711 0.03030 = 0.04098 -0.00124 -0.00706 0.00815 C3 1 0.651594 0.473447 0.826678 11.00000 0.02960 0.03345 = 0.03940 0.01214 0.01030 0.01429 AFIX 43 H3 2 0.775774 0.470126 0.817701 11.00000 -1.20000 AFIX 0 O3 4 0.321021 1.156403 0.404013 11.00000 0.03547 0.02509 = 0.03956 0.01026 -0.00043 0.00820 C4 1 0.623919 0.561393 0.892872 11.00000 0.03542 0.02226 = 0.03472 0.00844 -0.00195 0.00735 C5 1 0.446057 0.561330 0.909534 11.00000 0.03341 0.02304 = 0.02738 -0.00096 0.00243 0.01086 AFIX 43 H5 2 0.430976 0.617450 0.956508 11.00000 -1.20000 AFIX 0 C6 1 0.289193 0.478137 0.856739 11.00000 0.03181 0.02161 = 0.03218 0.00808 0.00567 0.01092 AFIX 43 H6 2 0.164943 0.477280 0.867007 11.00000 -1.20000 AFIX 0 C7 1 0.264185 0.811064 0.770504 11.00000 0.03611 0.01341 = 0.03063 0.00410 0.00529 0.00765 C8 1 0.453056 0.843797 0.756832 11.00000 0.03163 0.01794 = 0.03557 0.00648 0.00522 0.00975 AFIX 43 H8 2 0.479425 0.786151 0.712050 11.00000 -1.20000 AFIX 0 C9 1 0.601847 0.958818 0.807549 11.00000 0.03115 0.02400 = 0.03854 0.00616 0.00582 0.00855 AFIX 43 H9 2 0.729281 0.980868 0.797456 11.00000 -1.20000 AFIX 0 C10 1 0.563626 1.041746 0.873267 11.00000 0.04031 0.01968 = 0.03477 0.00394 0.00300 0.00815 C11 1 0.379134 1.015726 0.887787 11.00000 0.04598 0.02477 = 0.03073 0.00576 0.01035 0.01513 AFIX 43 H11 2 0.353684 1.075226 0.932387 11.00000 -1.20000 AFIX 0 C12 1 0.230905 0.901042 0.836134 11.00000 0.03630 0.01836 = 0.03218 0.00254 0.00530 0.00861 AFIX 43 H12 2 0.103498 0.883535 0.845835 11.00000 -1.20000 AFIX 0 C13 1 0.105547 0.681846 0.717288 11.00000 0.03847 0.01789 = 0.02890 0.00890 0.00628 0.00655 C14 1 -0.069649 0.704400 0.709478 11.00000 0.02898 0.02695 = 0.04352 0.00231 0.00445 0.00946 AFIX 93 H14A 2 -0.095882 0.805815 0.738542 11.00000 -1.20000 H14B 2 -0.167886 0.619008 0.674867 11.00000 -1.20000 AFIX 0 C15 1 0.143777 0.519491 0.672335 11.00000 0.02452 0.01743 = 0.02934 0.00243 -0.00119 0.00506 C16 1 0.185861 0.499660 0.604309 11.00000 0.02559 0.01507 = 0.02942 0.00107 -0.00095 0.00428 AFIX 43 H16 2 0.199570 0.380590 0.586298 11.00000 -1.20000 AFIX 0 C17 1 0.214472 0.632366 0.552676 11.00000 0.02036 0.02005 = 0.02826 0.00272 0.00132 0.00526 C18 1 0.177440 0.807595 0.564033 11.00000 0.02758 0.01882 = 0.03095 -0.00050 0.00461 0.00823 AFIX 43 H18 2 0.126074 0.844779 0.606450 11.00000 -1.20000 AFIX 0 C19 1 0.216032 0.924704 0.513379 11.00000 0.02720 0.01482 = 0.03688 0.00366 0.00095 0.00771 AFIX 43 H19 2 0.190539 1.042441 0.521261 11.00000 -1.20000 AFIX 0 C20 1 0.291814 0.873445 0.450782 11.00000 0.02610 0.01902 = 0.02886 0.00352 -0.00025 0.00511 C21 1 0.327018 0.699666 0.439275 11.00000 0.02860 0.01736 = 0.02934 -0.00335 0.00137 0.00413 AFIX 43 H21 2 0.378646 0.662773 0.396887 11.00000 -1.20000 AFIX 0 C22 1 0.286692 0.580852 0.489666 11.00000 0.02388 0.01996 = 0.02835 0.00118 -0.00165 0.00839 AFIX 43 H22 2 0.308921 0.461774 0.480908 11.00000 -1.20000 AFIX 0 C23 1 0.339486 0.999476 0.397375 11.00000 0.03314 0.01825 = 0.02924 0.00632 -0.00125 0.00400 AFIX 43 H23 2 0.387632 0.955608 0.355124 11.00000 -1.20000 AFIX 0 HKLF 5 REM K433.res in P-1 REM R1 = 0.0639 for 6021 Fo > 4sig(Fo) and 0.1045 for all 8693 data REM 263 parameters refined using 0 restraints END WGHT 0.0455 1.3720 REM Highest difference peak 0.708, deepest hole -0.663, 1-sigma level 0.101 Q1 1 0.8116 1.0684 0.9118 11.00000 0.05 0.71 Q2 1 0.8255 0.5570 0.9615 11.00000 0.05 0.66 Q3 1 0.4127 0.4169 0.7907 11.00000 0.05 0.41 Q4 1 -0.1175 0.9248 0.7524 11.00000 0.05 0.40 Q5 1 0.7610 1.0382 0.8406 11.00000 0.05 0.39 Q6 1 0.2699 0.7200 0.7266 11.00000 0.05 0.39 Q7 1 0.8739 1.1022 0.8649 11.00000 0.05 0.38 Q8 1 0.1794 0.8197 0.7258 11.00000 0.05 0.38 Q9 1 0.2610 0.3382 0.7665 11.00000 0.05 0.37 Q10 1 0.2629 0.3724 0.6719 11.00000 0.05 0.37 Q11 1 0.2929 0.4417 0.7730 11.00000 0.05 0.36 Q12 1 0.3056 0.6514 0.4012 11.00000 0.05 0.36 Q13 1 0.4411 0.6382 0.3881 11.00000 0.05 0.35 Q14 1 0.5813 1.1625 0.9748 11.00000 0.05 0.35 Q15 1 0.2991 0.6191 0.5344 11.00000 0.05 0.35 Q16 1 -0.0616 0.3090 0.6881 11.00000 0.05 0.35 Q17 1 0.1545 0.9791 0.8807 11.00000 0.05 0.34 Q18 1 0.0068 0.2130 0.8605 11.00000 0.05 0.34 Q19 1 0.2081 0.8800 0.4650 11.00000 0.05 0.33 Q20 1 0.8844 0.9672 0.8608 11.00000 0.05 0.33 ; _shelx_res_checksum 52105 _shelx_hkl_file ; -1 0 0 5.73236 0.84605 -2 1 0 0 5.73236 0.84605 1 2 0 0 4008.72 159.073 -2 -2 0 0 4008.72 159.073 1 -2 0 0 4136.24 160.009 -2 2 0 0 4136.24 160.009 1 3 0 0 414.538 14.5270 -2 -3 0 0 414.538 14.5270 1 -3 0 0 410.054 25.9204 -2 3 0 0 410.054 25.9204 1 4 0 0 64.0489 3.66563 -2 -4 0 0 64.0489 3.66563 1 -4 0 0 74.4040 8.14017 -2 4 0 0 74.4040 8.14017 1 5 0 0 8.64805 2.01665 -2 -5 0 0 8.64805 2.01665 1 -5 0 0 17.4060 3.80225 -2 5 0 0 17.4060 3.80225 1 6 0 0 24.5808 2.99417 -2 -6 0 0 24.5808 2.99417 1 -6 0 0 22.6371 5.12152 -2 6 0 0 22.6371 5.12152 1 7 0 0 7.48567 3.18136 -2 -7 0 0 7.48567 3.18136 1 -7 0 0 1.41457 5.06921 -2 7 0 0 1.41457 5.06921 1 -8 0 0 1.51975 4.32546 -2 8 0 0 1.51975 4.32546 1 -9 0 0 1.30124 4.65399 -2 9 0 0 1.30124 4.65399 1 9 -1 0 0.46565 3.28632 1 8 -1 0 9.78596 3.42393 1 -8 1 0 10.1098 2.66675 1 7 -1 0 2.46062 3.15352 1 -7 1 0 -3.2140 1.84685 1 6 -1 0 119.771 9.95529 1 -6 1 0 111.456 6.29296 1 5 -1 0 248.273 14.9254 1 -5 1 0 240.765 11.1081 1 4 -1 0 20.7164 4.65329 1 -4 1 0 14.4964 2.09616 1 3 -1 0 659.363 39.9112 1 -3 1 0 671.255 22.8213 1 2 -1 0 224.212 15.4710 1 -2 1 0 231.875 15.6401 1 1 -1 0 565.804 17.8179 1 -1 1 0 486.253 21.4721 1 -1 -1 0 8.64713 1.12684 1 1 1 0 10.4687 1.14188 1 -2 -1 0 369.393 20.3172 1 2 1 0 368.249 20.3917 1 -3 -1 0 48.7303 2.43233 1 3 1 0 50.2247 3.13355 1 -4 -1 0 102.025 4.44686 1 4 1 0 103.116 9.97567 1 5 1 0 594.440 28.8094 1 6 1 0 13.5060 3.92575 1 7 1 0 16.3645 4.95065 1 8 1 0 0.97812 2.38433 1 9 1 0 15.0688 3.68841 1 -8 -2 1 -2.5816 6.54501 -2 9 -2 0 -2.5816 6.54501 1 8 2 -1 -8.4505 7.11119 -2 -9 2 0 -8.4505 7.11119 1 -7 -2 1 2.53006 5.96896 -2 8 -2 0 2.53006 5.96896 1 7 2 -1 0.29746 6.31673 -2 -8 2 0 0.29746 6.31673 1 -6 -2 1 17.8817 8.09622 -2 7 -2 0 17.8817 8.09622 1 6 2 -1 7.83131 4.40567 -2 -7 2 0 7.83131 4.40567 1 -5 -2 1 170.438 17.5813 -2 6 -2 0 170.438 17.5813 1 5 2 -1 180.105 17.1733 -2 -6 2 0 180.105 17.1733 1 -4 -2 1 102.794 12.3505 -2 5 -2 0 102.794 12.3505 1 4 2 -1 122.809 8.49251 -2 -5 2 0 122.809 8.49251 1 4 -2 0 51.4686 5.54243 1 -4 2 0 47.8574 4.69980 1 3 -2 0 670.584 29.1568 1 -3 2 0 608.559 22.2862 1 2 -2 0 273.990 9.57399 1 -2 2 0 265.248 10.6671 1 1 -2 0 4464.19 125.370 1 -1 2 0 4735.42 175.372 1 0 -2 0 23.7737 1.72238 1 0 2 0 25.0569 1.57397 1 -1 -2 0 63.5798 5.60650 1 2 -2 1 399.476 23.8862 -2 -1 -2 0 399.476 23.8862 1 1 2 0 65.6169 3.86183 1 -2 -2 0 154.362 9.88506 1 -3 2 -1 424.575 17.9212 -2 2 2 0 424.575 17.9212 1 -4 2 -1 0.38252 2.81552 -2 3 2 0 0.38252 2.81552 1 3 2 0 1.61007 0.76381 1 -5 2 -1 121.211 7.63083 -2 4 2 0 121.211 7.63083 1 -6 2 -1 74.8436 5.64783 -2 5 2 0 74.8436 5.64783 1 -7 2 -1 19.3322 3.77735 -2 6 2 0 19.3322 3.77735 1 -8 2 -1 13.3617 6.83000 -2 7 2 0 13.3617 6.83000 1 -9 2 -1 -2.2318 5.33698 -2 8 2 0 -2.2318 5.33698 1 9 -3 0 6.12884 4.92171 1 -9 3 0 3.33981 4.25360 1 8 -3 0 -0.0380 2.89329 1 -8 3 0 2.37426 3.00451 1 7 -3 0 10.6305 3.36825 1 -7 3 0 7.75155 2.80117 1 6 -3 0 29.2491 4.23697 1 -6 3 0 22.0498 3.46957 1 5 -3 0 10.4415 2.64052 1 -5 3 0 8.65003 2.64074 1 4 -3 0 60.6442 5.00387 1 -4 3 0 56.4801 4.53986 1 3 -3 0 3.99853 1.71774 1 -3 3 0 3.64678 1.52928 1 2 -3 0 169.354 6.93882 1 -2 3 0 164.730 7.97566 1 1 -3 0 23.9126 2.06567 1 -1 3 0 20.3480 2.42647 1 0 -3 0 1.13921 0.65954 1 0 3 0 1.23671 0.63183 1 -1 -3 0 199.622 9.41869 1 1 3 0 180.618 7.30568 1 -2 -3 0 591.733 23.9562 1 2 3 0 561.940 23.8116 1 3 3 0 55.6614 3.55680 1 4 3 0 403.219 15.8535 1 5 3 0 4.92272 1.82247 1 6 3 0 0.89006 1.60307 1 7 3 0 5.20423 2.66701 1 8 3 0 2.64129 2.61491 1 -7 -4 3 -2.6508 7.65900 -2 9 -4 0 -2.6508 7.65900 1 7 4 -3 -0.2342 8.17438 -2 -9 4 0 -0.2342 8.17438 1 -6 -4 3 8.16473 6.61150 -2 8 -4 0 8.16473 6.61150 1 6 4 -3 5.83380 7.87239 -2 -8 4 0 5.83380 7.87239 1 -5 -4 3 29.6970 7.16933 -2 7 -4 0 29.6970 7.16933 1 5 4 -3 17.8163 8.11215 -2 -7 4 0 17.8163 8.11215 1 -4 -4 3 79.0889 8.97591 -2 6 -4 0 79.0889 8.97591 1 4 4 -3 69.0570 8.12321 -2 -6 4 0 69.0570 8.12321 1 5 -4 0 42.4905 8.96854 1 -3 -4 3 99.1772 12.8686 -2 5 -4 0 99.1772 12.8686 1 3 4 -3 110.286 8.94439 -2 -5 4 0 110.286 8.94439 1 -2 -4 3 611.993 42.6829 -2 4 -4 0 611.993 42.6829 1 4 -4 0 425.901 32.3889 1 2 4 -3 671.121 30.5323 -2 -4 4 0 671.121 30.5323 1 3 -4 0 40.7024 6.89171 1 1 4 -3 50.1274 8.55411 -2 -3 4 0 50.1274 8.55411 1 -3 4 0 46.5875 7.27409 1 2 -4 0 433.635 17.1799 1 -2 4 0 446.090 21.2882 1 1 -4 0 251.695 10.6816 1 -1 4 0 270.753 19.1041 1 0 -4 0 35.4255 5.04062 1 0 4 0 38.1807 5.49742 1 -2 4 -3 47.3903 7.20327 -2 0 4 0 47.3903 7.20327 1 3 -4 3 353.530 22.7459 -2 -1 -4 0 353.530 22.7459 1 1 4 0 142.591 6.90342 1 -3 4 -3 351.441 23.5389 -2 1 4 0 351.441 23.5389 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7.92564 1 -2 -5 0 45.6478 5.63242 1 2 5 0 44.1230 4.43436 1 3 5 0 125.145 4.64003 1 4 5 0 32.7929 2.13173 1 5 5 0 15.8467 2.80668 1 6 5 0 17.0233 3.18477 1 -6 -6 4 -7.6614 11.0031 -2 9 -6 0 -7.6614 11.0031 1 6 6 -4 4.62232 5.87299 -2 -9 6 0 4.62232 5.87299 1 -5 -6 4 -1.3438 8.55475 -2 8 -6 0 -1.3438 8.55475 1 -4 -6 4 98.2004 16.6399 -2 7 -6 0 98.2004 16.6399 1 4 6 -4 103.219 10.8389 -2 -7 6 0 103.219 10.8389 1 -3 -6 4 176.228 19.9429 -2 6 -6 0 176.228 19.9429 1 3 6 -4 148.279 13.0119 -2 -6 6 0 148.279 13.0119 1 -2 -6 4 125.599 15.5701 -2 5 -6 0 125.599 15.5701 1 2 6 -4 130.113 11.2563 -2 -5 6 0 130.113 11.2563 1 -1 -6 4 29.5960 7.46762 -2 4 -6 0 29.5960 7.46762 1 1 6 -4 31.4560 4.53443 -2 -4 6 0 31.4560 4.53443 1 0 -6 4 178.559 11.6118 -2 3 -6 0 178.559 11.6118 1 0 6 -4 157.388 9.85766 -2 -3 6 0 157.388 9.85766 1 1 -6 4 339.469 17.5085 -2 2 -6 0 339.469 17.5085 1 -1 6 -4 328.279 15.4069 -2 -2 6 0 328.279 15.4069 1 -2 6 -4 37.9657 4.31927 -2 -1 6 0 37.9657 4.31927 1 3 -6 4 605.807 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14.0132 8.99316 1 3 -4 -21 16.2017 5.10885 1 -3 4 21 53.1617 13.1205 1 2 -4 -21 3.46897 4.69324 1 -2 4 21 2.08861 7.31330 1 1 -4 -21 8.75552 4.37098 1 -1 4 21 -0.2355 7.16746 1 2 5 -22 2.67500 3.92250 1 -2 -5 22 7.31030 5.23425 1 1 5 -22 18.3791 5.25659 1 0 5 -22 2.43802 4.89163 1 0 -5 22 0.53207 5.62775 1 -1 5 -22 15.0129 7.46647 1 1 -5 22 10.0541 3.81468 1 -2 5 -22 2.06789 4.44259 1 2 -5 22 -1.5976 3.95578 1 -5 4 19 19.8450 7.17131 -2 3 4 -22 19.8450 7.17131 1 5 -4 -19 7.59776 8.55617 -2 -3 -4 22 7.59776 8.55617 1 -4 4 19 19.0628 11.6419 -2 2 4 -22 19.0628 11.6419 1 4 -4 -19 -2.7812 8.82686 -2 -2 -4 22 -2.7812 8.82686 1 -3 4 19 45.7473 9.84911 -2 1 4 -22 45.7473 9.84911 1 3 -4 -19 32.5174 11.4070 -2 -1 -4 22 32.5174 11.4070 1 -2 4 19 14.7568 6.87574 -2 0 4 -22 14.7568 6.87574 1 2 -4 -19 14.4102 4.80071 -2 0 -4 22 14.4102 4.80071 1 -1 4 19 10.6393 7.44870 -2 -1 4 -22 10.6393 7.44870 1 1 -4 -19 -1.6915 6.64358 -2 1 -4 22 -1.6915 6.64358 1 0 4 19 -1.9044 10.9415 -2 -2 4 -22 -1.9044 10.9415 1 0 -4 -19 0.55956 7.28797 -2 2 -4 22 0.55956 7.28797 1 -1 -4 -19 2.23751 12.2954 -2 3 -4 22 2.23751 12.2954 1 4 3 -22 8.01789 3.36841 1 -4 -3 22 0.58639 4.85783 1 3 3 -22 18.4114 4.31261 1 2 3 -22 15.6192 4.34587 1 -2 -3 22 2.86212 4.16224 1 1 3 -22 5.15068 3.49689 1 -1 -3 22 1.99899 1.65728 1 0 3 -22 9.91111 4.54359 1 0 -3 22 6.46645 3.54239 1 -1 3 -22 9.79738 4.08625 1 1 -3 22 4.88308 3.15516 1 -2 3 -22 11.9870 5.10935 1 2 -3 22 7.44365 4.40339 1 -3 3 -22 25.1697 6.53447 1 3 -3 22 17.5004 5.68428 1 -5 2 21 -1.4834 7.48316 -2 4 2 -22 -1.4834 7.48316 1 -4 2 21 2.02330 7.07197 -2 3 2 -22 2.02330 7.07197 1 4 -2 -21 20.0638 8.70874 -2 -3 -2 22 20.0638 8.70874 1 -3 2 21 101.931 11.2293 -2 2 2 -22 101.931 11.2293 1 -2 2 21 20.6665 7.61976 -2 1 2 -22 20.6665 7.61976 1 2 -2 -21 5.68963 4.93422 -2 -1 -2 22 5.68963 4.93422 1 -1 2 21 29.8038 8.23980 -2 0 2 -22 29.8038 8.23980 1 1 -2 -21 16.4987 6.90746 -2 0 -2 22 16.4987 6.90746 1 0 2 21 4.95056 7.66596 -2 -1 2 -22 4.95056 7.66596 1 0 -2 -21 23.2705 7.38736 -2 1 -2 22 23.2705 7.38736 1 1 2 21 3.87702 10.1869 -2 -2 2 -22 3.87702 10.1869 1 -1 -2 -21 9.66446 6.54435 -2 2 -2 22 9.66446 6.54435 1 -2 -2 -21 33.4238 9.19685 -2 3 -2 22 33.4238 9.19685 1 5 1 -22 4.48925 3.62898 1 -5 -1 22 -3.3239 5.03279 1 4 1 -22 8.82407 3.65182 1 -4 -1 22 -0.0519 4.22363 1 3 1 -22 51.9107 6.75468 1 2 1 -22 27.4055 5.28607 1 -2 -1 22 24.4279 4.02384 1 1 1 -22 3.91098 3.38378 1 -1 -1 22 3.73603 2.95702 1 0 1 -22 52.7893 7.98757 1 0 -1 22 41.5283 6.93694 1 -1 1 -22 5.62069 4.02923 1 1 -1 22 -0.2345 4.20358 1 -2 1 -22 12.7043 5.38748 1 2 -1 22 4.47243 3.78501 1 -3 1 -22 57.6511 10.3717 1 3 -1 22 19.5208 6.42158 1 -5 0 22 7.99157 6.46538 -2 5 0 -22 7.99157 6.46538 1 5 0 -22 1.25313 4.01090 -2 -5 0 22 1.25313 4.01090 1 -4 0 22 12.1643 6.27755 -2 4 0 -22 12.1643 6.27755 1 4 0 -22 2.68872 4.06388 -2 -4 0 22 2.68872 4.06388 1 -3 0 22 112.822 10.9938 -2 3 0 -22 112.822 10.9938 1 -2 0 22 9.55079 5.48295 -2 2 0 -22 9.55079 5.48295 1 2 0 -22 -2.1730 4.21979 -2 -2 0 22 -2.1730 4.21979 1 -1 0 22 31.0674 6.69647 -2 1 0 -22 31.0674 6.69647 1 1 0 -22 27.0895 5.87998 -2 -1 0 22 27.0895 5.87998 1 0 0 22 9.20190 8.01783 -2 0 0 -22 9.20190 8.01783 1 0 0 -22 3.22279 4.41957 -2 0 0 22 3.22279 4.41957 1 1 0 22 9.93951 6.50833 -2 -1 0 -22 9.93951 6.50833 1 -1 0 -22 12.0328 6.90742 -2 1 0 22 12.0328 6.90742 1 2 0 22 8.69651 6.63487 -2 -2 0 -22 8.69651 6.63487 1 -2 0 -22 5.01773 4.42294 -2 2 0 22 5.01773 4.42294 1 -3 0 -22 12.3513 8.29541 -2 3 0 22 12.3513 8.29541 1 5 -1 -22 0.67583 3.58711 1 -5 1 22 3.63985 3.32616 1 4 -1 -22 4.84534 3.58583 1 -4 1 22 -0.0922 5.73182 1 3 -1 -22 8.68898 3.77907 1 -3 1 22 9.26837 3.84963 1 2 -1 -22 0.66694 3.16636 1 -2 1 22 -2.4291 3.31525 1 1 -1 -22 57.6329 7.16544 1 -1 1 22 39.1615 11.0017 1 0 -1 -22 3.30713 3.76275 1 -1 -1 -22 -0.2260 4.13779 1 1 1 22 1.15525 4.02830 1 -2 -1 -22 6.41993 4.85605 1 2 1 22 21.4164 6.61964 1 -3 -2 23 5.69631 7.32426 -2 4 -2 -22 5.69631 7.32426 1 -2 -2 23 33.3984 8.42760 -2 3 -2 -22 33.3984 8.42760 1 2 2 -23 41.6025 14.5021 -2 -3 2 22 41.6025 14.5021 1 -1 -2 23 -0.6748 8.96244 -2 2 -2 -22 -0.6748 8.96244 1 0 -2 23 -0.7103 13.2957 -2 1 -2 -22 -0.7103 13.2957 1 0 2 -23 15.9200 11.6495 -2 -1 2 22 15.9200 11.6495 1 1 -2 23 12.1651 6.84638 -2 0 -2 -22 12.1651 6.84638 1 -1 2 -23 4.71542 11.6756 -2 0 2 22 4.71542 11.6756 1 2 -2 23 7.47318 6.79136 -2 -1 -2 -22 7.47318 6.79136 1 -2 2 -23 -4.3460 12.1207 -2 1 2 22 -4.3460 12.1207 1 3 -3 -22 47.4765 7.35718 1 -3 3 22 32.3568 12.4359 1 2 -3 -22 5.39524 4.55646 1 -2 3 22 15.2227 10.5028 1 1 -3 -22 0.65137 3.71419 1 -1 3 22 12.6346 6.85878 1 0 5 -23 -0.9890 4.07250 1 0 -5 23 -9.3776 10.7511 1 -4 4 20 -4.7066 11.5651 -2 2 4 -23 -4.7066 11.5651 1 4 -4 -20 -11.003 11.3098 -2 -2 -4 23 -11.003 11.3098 1 -3 4 20 -0.6118 7.26666 -2 1 4 -23 -0.6118 7.26666 1 3 -4 -20 -3.2718 9.91297 -2 -1 -4 23 -3.2718 9.91297 1 -2 4 20 27.2082 13.2699 -2 0 4 -23 27.2082 13.2699 1 2 -4 -20 11.8002 5.30347 -2 0 -4 23 11.8002 5.30347 1 -1 4 20 0.32349 7.62989 -2 -1 4 -23 0.32349 7.62989 1 1 -4 -20 4.10004 7.07779 -2 1 -4 23 4.10004 7.07779 1 0 4 20 11.9600 9.03136 -2 -2 4 -23 11.9600 9.03136 1 0 -4 -20 0.67614 8.57975 -2 2 -4 23 0.67614 8.57975 1 3 3 -23 4.34429 3.49832 1 2 3 -23 24.0584 5.35004 1 -2 -3 23 9.81563 5.85666 1 1 3 -23 12.3013 4.60074 1 -1 -3 23 2.01773 1.29851 1 0 3 -23 4.53970 6.29115 1 0 -3 23 -5.8342 4.75464 1 -1 3 -23 2.82678 4.24142 1 1 -3 23 -1.0101 3.26189 1 -2 3 -23 -0.2722 4.45971 1 2 -3 23 5.11156 4.37798 1 4 2 -23 0.66758 4.95185 1 -4 -2 23 -0.2682 5.16386 1 -4 2 22 21.2491 7.79905 -2 3 2 -23 21.2491 7.79905 1 4 -2 -22 -1.1309 10.4540 -2 -3 -2 23 -1.1309 10.4540 1 -3 2 22 13.5820 8.01829 -2 2 2 -23 13.5820 8.01829 1 3 -2 -22 21.0541 10.7292 -2 -2 -2 23 21.0541 10.7292 1 -2 2 22 -4.7955 7.13771 -2 1 2 -23 -4.7955 7.13771 1 2 -2 -22 -1.7128 5.76518 -2 -1 -2 23 -1.7128 5.76518 1 -1 2 22 15.7877 8.05530 -2 0 2 -23 15.7877 8.05530 1 1 -2 -22 10.6263 6.31838 -2 0 -2 23 10.6263 6.31838 1 0 2 22 7.79266 8.06783 -2 -1 2 -23 7.79266 8.06783 1 0 -2 -22 11.1492 6.96715 -2 1 -2 23 11.1492 6.96715 1 1 2 22 5.89928 8.28549 -2 -2 2 -23 5.89928 8.28549 1 -1 -2 -22 6.19290 9.30825 -2 2 -2 23 6.19290 9.30825 1 4 1 -23 6.12945 4.14106 1 -4 -1 23 -5.3648 4.55214 1 3 1 -23 6.32406 4.79719 1 -3 -1 23 -1.9086 1.42348 1 2 1 -23 4.28335 4.28866 1 -2 -1 23 1.90440 2.12099 1 1 1 -23 30.4902 5.14813 1 -1 -1 23 20.6759 4.01090 1 0 1 -23 0.63339 3.65326 1 0 -1 23 -1.5000 2.98841 1 -1 1 -23 -2.0162 4.04339 1 1 -1 23 1.36339 3.83164 1 -2 1 -23 -1.5222 4.25625 1 2 -1 23 -1.5880 3.90382 1 -4 0 23 23.3499 7.07980 -2 4 0 -23 23.3499 7.07980 1 4 0 -23 3.78240 4.62826 -2 -4 0 23 3.78240 4.62826 1 -3 0 23 12.3558 5.94093 -2 3 0 -23 12.3558 5.94093 1 3 0 -23 -2.1779 5.31837 -2 -3 0 23 -2.1779 5.31837 1 -2 0 23 12.8865 8.73864 -2 2 0 -23 12.8865 8.73864 1 2 0 -23 2.16903 3.82244 -2 -2 0 23 2.16903 3.82244 1 -1 0 23 0.49844 5.24188 -2 1 0 -23 0.49844 5.24188 1 1 0 -23 4.17441 3.93091 -2 -1 0 23 4.17441 3.93091 1 0 0 23 14.9039 6.53417 -2 0 0 -23 14.9039 6.53417 1 0 0 -23 12.6742 5.62761 -2 0 0 23 12.6742 5.62761 1 1 0 23 16.7680 10.9928 -2 -1 0 -23 16.7680 10.9928 1 -1 0 -23 22.6724 6.86708 -2 1 0 23 22.6724 6.86708 1 2 0 23 4.03101 7.98187 -2 -2 0 -23 4.03101 7.98187 1 -2 0 -23 9.73362 5.81320 -2 2 0 23 9.73362 5.81320 1 4 -1 -23 10.1300 4.58756 1 -4 1 23 -1.0063 3.65764 1 3 -1 -23 19.5463 5.06793 1 -3 1 23 -0.9565 3.77510 1 2 -1 -23 -1.2309 3.76548 1 -2 1 23 5.82789 4.10075 1 1 -1 -23 17.8037 4.54043 1 -1 1 23 13.6477 5.32385 1 0 -1 -23 -10.500 6.98252 1 0 1 23 4.64107 4.29999 1 -1 -1 -23 -5.5462 4.38148 1 1 1 23 0.35766 4.33947 1 -2 -2 24 18.8501 7.96296 -2 3 -2 -23 18.8501 7.96296 1 2 2 -24 -3.9047 11.8124 -2 -3 2 23 -3.9047 11.8124 1 -1 -2 24 3.19854 8.21394 -2 2 -2 -23 3.19854 8.21394 1 1 2 -24 19.0480 12.0748 -2 -2 2 23 19.0480 12.0748 1 0 -2 24 22.5301 9.72082 -2 1 -2 -23 22.5301 9.72082 1 1 -2 24 0.28015 8.53872 -2 0 -2 -23 0.28015 8.53872 1 -1 2 -24 24.0909 13.8852 -2 0 2 23 24.0909 13.8852 1 2 3 -24 -0.3895 3.19203 1 -2 -3 24 -3.7749 5.36650 1 1 3 -24 68.1195 9.92257 1 0 3 -24 6.54120 4.70929 1 0 -3 24 13.7786 7.75996 1 -1 3 -24 7.35664 5.69857 1 1 -3 24 2.66251 4.58709 1 3 2 -24 -2.0759 3.46392 1 -3 -2 24 2.89295 5.01980 1 -3 2 23 14.9387 11.1599 -2 2 2 -24 14.9387 11.1599 1 3 -2 -23 -11.163 10.4450 -2 -2 -2 24 -11.163 10.4450 1 -2 2 23 27.7722 13.2044 -2 1 2 -24 27.7722 13.2044 1 2 -2 -23 -5.5781 6.13746 -2 -1 -2 24 -5.5781 6.13746 1 -1 2 23 36.9541 10.0344 -2 0 2 -24 36.9541 10.0344 1 1 -2 -23 -0.7517 7.30358 -2 0 -2 24 -0.7517 7.30358 1 0 2 23 -6.1882 11.3106 -2 -1 2 -24 -6.1882 11.3106 1 3 1 -24 3.64160 6.34397 1 -3 -1 24 9.35346 2.53337 1 2 1 -24 17.4623 4.77261 1 -2 -1 24 -1.4559 2.31312 1 1 1 -24 25.8392 6.27537 1 -1 -1 24 12.6655 3.64808 1 0 1 -24 3.36627 4.59931 1 0 -1 24 -5.3631 4.00448 1 -1 1 -24 16.6089 5.94958 1 1 -1 24 29.8770 6.58596 1 -3 0 24 3.29750 6.37231 -2 3 0 -24 3.29750 6.37231 1 3 0 -24 8.88085 5.59980 -2 -3 0 24 8.88085 5.59980 1 -2 0 24 134.004 12.6594 -2 2 0 -24 134.004 12.6594 1 2 0 -24 90.4976 9.90403 -2 -2 0 24 90.4976 9.90403 1 -1 0 24 43.8923 9.19615 -2 1 0 -24 43.8923 9.19615 1 1 0 -24 25.4748 7.05846 -2 -1 0 24 25.4748 7.05846 1 0 0 24 21.0110 7.81258 -2 0 0 -24 21.0110 7.81258 1 0 0 -24 11.4260 6.94745 -2 0 0 24 11.4260 6.94745 1 2 -1 -24 1.38145 3.81188 1 -2 1 24 6.46391 6.54919 1 1 -1 -24 0.02168 4.53166 1 -1 1 24 13.2820 5.52560 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 68955 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3147(6) 0.3960(5) 0.7887(2) 0.0250(9) Uani 1 1 d . . . . . O1 O -0.0525(4) 0.2839(4) 0.74675(17) 0.0339(7) Uani 1 1 d . . . . . Cl1 Cl 0.82280(18) 0.67834(18) 0.95735(7) 0.0438(3) Uani 1 1 d . . . . . S1 S 0.12270(16) 0.31873(14) 0.71632(6) 0.0264(3) Uani 1 1 d . . . . . C2 C 0.4947(6) 0.3899(6) 0.7734(2) 0.0292(10) Uani 1 1 d . . . . . H2 H 0.510114 0.329453 0.727241 0.035 Uiso 1 1 calc R U . . . O2 O 0.1548(4) 0.1722(4) 0.66625(16) 0.0323(7) Uani 1 1 d . . . . . Cl2 Cl 0.75258(18) 1.17486(17) 0.93867(7) 0.0416(3) Uani 1 1 d . . . . . C3 C 0.6516(6) 0.4734(6) 0.8267(2) 0.0321(10) Uani 1 1 d . . . . . H3 H 0.775774 0.470126 0.817701 0.039 Uiso 1 1 calc R U . . . O3 O 0.3210(4) 1.1564(4) 0.40401(17) 0.0334(7) Uani 1 1 d . . . . . C4 C 0.6239(7) 0.5614(6) 0.8929(2) 0.0311(10) Uani 1 1 d . . . . . C5 C 0.4461(6) 0.5613(6) 0.9095(2) 0.0280(9) Uani 1 1 d . . . . . H5 H 0.430976 0.617450 0.956508 0.034 Uiso 1 1 calc R U . . . C6 C 0.2892(6) 0.4781(6) 0.8567(2) 0.0274(9) Uani 1 1 d . . . . . H6 H 0.164943 0.477280 0.867007 0.033 Uiso 1 1 calc R U . . . C7 C 0.2642(6) 0.8111(5) 0.7705(2) 0.0265(9) Uani 1 1 d . . . . . C8 C 0.4531(6) 0.8438(6) 0.7568(2) 0.0276(9) Uani 1 1 d . . . . . H8 H 0.479425 0.786151 0.712050 0.033 Uiso 1 1 calc R U . . . C9 C 0.6018(6) 0.9588(6) 0.8075(2) 0.0309(10) Uani 1 1 d . . . . . H9 H 0.729281 0.980868 0.797456 0.037 Uiso 1 1 calc R U . . . C10 C 0.5636(7) 1.0417(6) 0.8733(2) 0.0319(10) Uani 1 1 d . . . . . C11 C 0.3791(7) 1.0157(6) 0.8878(2) 0.0324(10) Uani 1 1 d . . . . . H11 H 0.353684 1.075226 0.932387 0.039 Uiso 1 1 calc R U . . . C12 C 0.2309(7) 0.9010(6) 0.8361(2) 0.0289(9) Uani 1 1 d . . . . . H12 H 0.103498 0.883535 0.845835 0.035 Uiso 1 1 calc R U . . . C13 C 0.1055(6) 0.6818(6) 0.7173(2) 0.0281(9) Uani 1 1 d . . . . . C14 C -0.0696(6) 0.7044(6) 0.7095(3) 0.0332(10) Uani 1 1 d . . . . . H14A H -0.095882 0.805815 0.738542 0.040 Uiso 1 1 calc R U . . . H14B H -0.167886 0.619008 0.674867 0.040 Uiso 1 1 calc R U . . . C15 C 0.1438(6) 0.5195(5) 0.6723(2) 0.0244(9) Uani 1 1 d . . . . . C16 C 0.1859(6) 0.4997(5) 0.6043(2) 0.0242(9) Uani 1 1 d . . . . . H16 H 0.199570 0.380590 0.586298 0.029 Uiso 1 1 calc R U . . . C17 C 0.2145(5) 0.6324(5) 0.5527(2) 0.0232(8) Uani 1 1 d . . . . . C18 C 0.1774(6) 0.8076(5) 0.5640(2) 0.0259(9) Uani 1 1 d . . . . . H18 H 0.126074 0.844779 0.606450 0.031 Uiso 1 1 calc R U . . . C19 C 0.2160(6) 0.9247(5) 0.5134(2) 0.0263(9) Uani 1 1 d . . . . . H19 H 0.190539 1.042441 0.521261 0.032 Uiso 1 1 calc R U . . . C20 C 0.2918(6) 0.8734(6) 0.4508(2) 0.0252(9) Uani 1 1 d . . . . . C21 C 0.3270(6) 0.6997(5) 0.4393(2) 0.0264(9) Uani 1 1 d . . . . . H21 H 0.378646 0.662773 0.396887 0.032 Uiso 1 1 calc R U . . . C22 C 0.2867(6) 0.5809(6) 0.4897(2) 0.0243(9) Uani 1 1 d . . . . . H22 H 0.308921 0.461774 0.480908 0.029 Uiso 1 1 calc R U . . . C23 C 0.3395(6) 0.9995(6) 0.3974(2) 0.0277(9) Uani 1 1 d . . . . . H23 H 0.387632 0.955608 0.355124 0.033 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 C1 0.034(2) 0.0158(18) 0.028(2) 0.0067(16) 0.0055(18) 0.0091(18) O1 0.0289(17) 0.0304(16) 0.0389(17) 0.0080(14) 0.0050(13) 0.0011(14) Cl1 0.0366(7) 0.0409(7) 0.0473(7) 0.0051(6) -0.0048(5) 0.0048(6) S1 0.0330(6) 0.0166(5) 0.0286(5) 0.0030(4) 0.0031(4) 0.0058(4) C2 0.037(3) 0.025(2) 0.031(2) 0.0103(18) 0.0076(19) 0.0137(19) O2 0.049(2) 0.0176(14) 0.0300(16) 0.0008(12) 0.0016(14) 0.0112(14) Cl2 0.0471(7) 0.0303(6) 0.0410(7) -0.0012(5) -0.0071(5) 0.0082(5) C3 0.030(2) 0.033(2) 0.039(3) 0.012(2) 0.0103(19) 0.014(2) O3 0.0355(18) 0.0251(16) 0.0396(18) 0.0103(14) -0.0004(14) 0.0082(14) C4 0.035(2) 0.022(2) 0.035(2) 0.0084(18) -0.0020(19) 0.0074(19) C5 0.033(2) 0.023(2) 0.027(2) -0.0010(18) 0.0024(18) 0.0109(19) C6 0.032(2) 0.022(2) 0.032(2) 0.0081(18) 0.0057(18) 0.0109(18) C7 0.036(2) 0.0134(18) 0.031(2) 0.0041(16) 0.0053(19) 0.0076(17) C8 0.032(2) 0.0179(19) 0.036(2) 0.0065(17) 0.0052(19) 0.0097(18) C9 0.031(2) 0.024(2) 0.039(2) 0.0062(19) 0.0058(19) 0.0086(19) C10 0.040(3) 0.020(2) 0.035(2) 0.0039(18) 0.003(2) 0.0082(19) C11 0.046(3) 0.025(2) 0.031(2) 0.0058(19) 0.010(2) 0.015(2) C12 0.036(2) 0.018(2) 0.032(2) 0.0025(17) 0.0053(19) 0.0086(18) C13 0.038(3) 0.0179(19) 0.029(2) 0.0089(18) 0.0063(19) 0.0066(19) C14 0.029(2) 0.027(2) 0.044(3) 0.002(2) 0.004(2) 0.0095(19) C15 0.025(2) 0.0174(19) 0.029(2) 0.0024(17) -0.0012(17) 0.0051(16) C16 0.026(2) 0.0151(18) 0.029(2) 0.0011(16) -0.0009(17) 0.0043(17) C17 0.020(2) 0.0200(19) 0.028(2) 0.0027(17) 0.0013(16) 0.0053(16) C18 0.028(2) 0.0188(19) 0.031(2) -0.0005(16) 0.0046(18) 0.0082(17) C19 0.027(2) 0.0148(18) 0.037(2) 0.0037(17) 0.0010(18) 0.0077(17) C20 0.026(2) 0.019(2) 0.029(2) 0.0035(17) -0.0002(17) 0.0051(17) C21 0.029(2) 0.0174(19) 0.029(2) -0.0034(16) 0.0014(18) 0.0041(17) C22 0.024(2) 0.0200(19) 0.028(2) 0.0012(16) -0.0016(17) 0.0084(17) C23 0.033(2) 0.018(2) 0.029(2) 0.0063(17) -0.0012(18) 0.0040(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' Cl Cl 0.1484 0.1585 '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' S S 0.1246 0.1234 '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 C6 C1 C2 121.1(4) . . ? C6 C1 S1 120.4(3) . . ? C2 C1 S1 118.1(3) . . ? O2 S1 O1 118.52(19) . . ? O2 S1 C1 109.04(19) . . ? O1 S1 C1 108.68(19) . . ? O2 S1 C15 108.55(18) . . ? O1 S1 C15 108.20(19) . . ? C1 S1 C15 102.70(19) . . ? C3 C2 C1 119.0(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 118.8(4) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 122.5(4) . . ? C5 C4 Cl1 118.9(3) . . ? C3 C4 Cl1 118.6(4) . . ? C4 C5 C6 118.9(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C5 C6 C1 119.5(4) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 117.8(4) . . ? C12 C7 C13 121.3(4) . . ? C8 C7 C13 120.9(4) . . ? C9 C8 C7 121.0(4) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.5(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.9(4) . . ? C11 C10 Cl2 120.0(4) . . ? C9 C10 Cl2 119.1(4) . . ? C10 C11 C12 118.9(4) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C7 121.7(4) . . ? C11 C12 H12 119.1 . . ? C7 C12 H12 119.1 . . ? C14 C13 C7 122.2(4) . . ? C14 C13 C15 119.4(4) . . ? C7 C13 C15 118.3(4) . . ? C13 C14 H14A 120.0 . . ? C13 C14 H14B 120.0 . . ? H14A C14 H14B 120.0 . . ? C16 C15 C13 129.9(4) . . ? C16 C15 S1 115.5(3) . . ? C13 C15 S1 114.5(3) . . ? C15 C16 C17 130.4(4) . . ? C15 C16 H16 114.8 . . ? C17 C16 H16 114.8 . . ? C22 C17 C18 118.8(4) . . ? C22 C17 C16 116.8(4) . . ? C18 C17 C16 124.4(4) . . ? C19 C18 C17 119.8(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 121.2(4) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 119.0(4) . . ? C21 C20 C23 119.2(4) . . ? C19 C20 C23 121.8(4) . . ? C22 C21 C20 120.0(4) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 121.3(4) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? O3 C23 C20 124.1(4) . . ? O3 C23 H23 118.0 . . ? C20 C23 H23 118.0 . . ? 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 C1 C6 1.387(6) . ? C1 C2 1.392(6) . ? C1 S1 1.766(4) . ? O1 S1 1.435(3) . ? Cl1 C4 1.744(5) . ? S1 O2 1.432(3) . ? S1 C15 1.796(4) . ? C2 C3 1.389(6) . ? C2 H2 0.9500 . ? Cl2 C10 1.737(5) . ? C3 C4 1.380(6) . ? C3 H3 0.9500 . ? O3 C23 1.218(5) . ? C4 C5 1.373(6) . ? C5 C6 1.384(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.393(6) . ? C7 C8 1.400(6) . ? C7 C13 1.484(6) . ? C8 C9 1.384(6) . ? C8 H8 0.9500 . ? C9 C10 1.388(6) . ? C9 H9 0.9500 . ? C10 C11 1.378(6) . ? C11 C12 1.390(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.337(6) . ? C13 C15 1.494(6) . ? C14 H14A 0.9500 . ? C14 H14B 0.9500 . ? C15 C16 1.334(6) . ? C16 C17 1.471(5) . ? C16 H16 0.9500 . ? C17 C22 1.387(6) . ? C17 C18 1.411(5) . ? C18 C19 1.378(6) . ? C18 H18 0.9500 . ? C19 C20 1.394(6) . ? C19 H19 0.9500 . ? C20 C21 1.394(6) . ? C20 C23 1.473(5) . ? C21 C22 1.385(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23 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 C6 C1 S1 O2 -154.2(3) . . . . ? C2 C1 S1 O2 32.4(4) . . . . ? C6 C1 S1 O1 -23.7(4) . . . . ? C2 C1 S1 O1 162.9(3) . . . . ? C6 C1 S1 C15 90.8(4) . . . . ? C2 C1 S1 C15 -82.6(3) . . . . ? C6 C1 C2 C3 -2.2(6) . . . . ? S1 C1 C2 C3 171.1(3) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C2 C3 C4 C5 3.4(7) . . . . ? C2 C3 C4 Cl1 -176.1(3) . . . . ? C3 C4 C5 C6 -3.3(6) . . . . ? Cl1 C4 C5 C6 176.2(3) . . . . ? C4 C5 C6 C1 0.4(6) . . . . ? C2 C1 C6 C5 2.3(6) . . . . ? S1 C1 C6 C5 -170.9(3) . . . . ? C12 C7 C8 C9 1.3(6) . . . . ? C13 C7 C8 C9 -177.6(4) . . . . ? C7 C8 C9 C10 0.6(6) . . . . ? C8 C9 C10 C11 -2.0(6) . . . . ? C8 C9 C10 Cl2 176.3(3) . . . . ? C9 C10 C11 C12 1.5(6) . . . . ? Cl2 C10 C11 C12 -176.8(3) . . . . ? C10 C11 C12 C7 0.4(6) . . . . ? C8 C7 C12 C11 -1.8(6) . . . . ? C13 C7 C12 C11 177.1(4) . . . . ? C12 C7 C13 C14 31.4(6) . . . . ? C8 C7 C13 C14 -149.7(4) . . . . ? C12 C7 C13 C15 -147.3(4) . . . . ? C8 C7 C13 C15 31.5(5) . . . . ? C14 C13 C15 C16 84.1(6) . . . . ? C7 C13 C15 C16 -97.2(5) . . . . ? C14 C13 C15 S1 -93.9(4) . . . . ? C7 C13 C15 S1 84.8(4) . . . . ? O2 S1 C15 C16 -0.7(4) . . . . ? O1 S1 C15 C16 -130.6(3) . . . . ? C1 S1 C15 C16 114.6(3) . . . . ? O2 S1 C15 C13 177.6(3) . . . . ? O1 S1 C15 C13 47.7(3) . . . . ? C1 S1 C15 C13 -67.1(3) . . . . ? C13 C15 C16 C17 2.3(8) . . . . ? S1 C15 C16 C17 -179.7(3) . . . . ? C15 C16 C17 C22 170.1(4) . . . . ? C15 C16 C17 C18 -8.5(7) . . . . ? C22 C17 C18 C19 -1.0(6) . . . . ? C16 C17 C18 C19 177.5(4) . . . . ? C17 C18 C19 C20 -0.1(6) . . . . ? C18 C19 C20 C21 0.6(6) . . . . ? C18 C19 C20 C23 -178.0(4) . . . . ? C19 C20 C21 C22 0.0(6) . . . . ? C23 C20 C21 C22 178.7(4) . . . . ? C20 C21 C22 C17 -1.2(6) . . . . ? C18 C17 C22 C21 1.7(6) . . . . ? C16 C17 C22 C21 -177.0(4) . . . . ? C21 C20 C23 O3 -177.0(4) . . . . ? C19 C20 C23 O3 1.6(7) . . . . ?