#------------------------------------------------------------------------------ #$Date: 2020-05-13 02:19:55 +0300 (Wed, 13 May 2020) $ #$Revision: 251998 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/83/4038353.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_4038353 loop_ _publ_author_name 'Ruggeri, Michele' 'Dombrowski, Amanda W.' 'Djuric, Stevan W.' 'Baxendale, Ian R.' _publ_section_title ; A rearrangement of 3-hydroxyazetidines into 2-oxazolines. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.0c00656 _journal_year 2020 _chemical_formula_moiety 'C17 H18 Cl N O2 S' _chemical_formula_sum 'C17 H18 Cl N O2 S' _chemical_formula_weight 335.83 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2019-07-23 _audit_creation_method ; Olex2 1.3-alpha (compiled 2019.07.11 svn.r3635 for OlexSys, GUI svn.r5848) ; _cell_angle_alpha 90 _cell_angle_beta 93.482(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.0972(4) _cell_length_b 10.3026(4) _cell_length_c 16.9599(7) _cell_measurement_reflns_used 9983 _cell_measurement_temperature 120 _cell_measurement_theta_max 30.37 _cell_measurement_theta_min 2.31 _cell_volume 1586.63(11) _computing_cell_refinement 'SAINT v8.38A (Bruker, 2017)' _computing_data_collection 'APEX3 v.2016.1-0 (Bruker, 2016)' _computing_data_reduction 'SAINT v8.38A (Bruker, 2017)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 multi-CPU (Sheldrick, 2015a)' _computing_structure_solution 'ShelXT 2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 120 _diffrn_detector 'Bruker PHOTON 100 CMOS' _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'CMOS sensor' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device '3-circle area detector diffractometer' _diffrn_measurement_device_type 'Bruker D8 venture' _diffrn_measurement_method \w-scan _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_unetI/netI 0.0371 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 40547 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.142 _diffrn_reflns_theta_min 2.314 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\mS microsource' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.378 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Krause et al., 2015) was used for absorption correction. wR2(int) was 0.0722 before and 0.0454 after correction. The Ratio of minimum to maximum transmission is 0.9684. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.406 _exptl_crystal_description irregular _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.355 _exptl_crystal_size_mid 0.208 _exptl_crystal_size_min 0.199 _refine_diff_density_max 0.488 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 251 _refine_ls_number_reflns 6043 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0371 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.5351P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0870 _refine_ls_wR_factor_ref 0.0958 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4563 _reflns_number_total 6043 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 5.cif _cod_data_source_block 5_19s225 _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 4038353 _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 0.928 _shelx_estimated_absorpt_t_min 0.877 _olex2_refinement_description ; 1. Others Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1) Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1) Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2) Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2) Uiso(H10A)=Uiso(H10B)=Uiso(H10C)=Uiso(H10D)=Uiso(H10E)=Uiso(H10F)=FVAR(3) Uiso(H17A)=Uiso(H17B)=Uiso(H17C)=Uiso(H17D)=Uiso(H17E)=Uiso(H17F)=FVAR(4) 2.a Disordered Me refined with riding coordinates: C10(H10A,H10B,H10C,H10D,H10E,H10F), C17(H17A,H17B,H17C,H17D,H17E,H17F) ; _shelx_res_file ; TITL 19srv225_a.res in P2(1)/n 19srv225.res created by SHELXL-2018/3 at 16:18:51 on 23-Jul-2019 REM Old TITL 19srv225 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.101, Rweak 0.004, Alpha 0.019 REM 0.546 for 194 systematic absences, Orientation as input REM Formula found by SHELXT: C17 N O2 S Cl CELL 0.71073 9.0972 10.3026 16.9599 90 93.482 90 ZERR 4 0.0004 0.0004 0.0007 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl N O S UNIT 68 72 4 4 8 4 L.S. 7 0 0 PLAN 6 SIZE 0.199 0.208 0.355 TEMP -153.15 BOND list 4 fmap 2 53 acta OMIT -4 1 2 REM REM REM WGHT 0.044100 0.535100 FVAR 0.71254 0.28669 0.42913 0.04086 0.03217 CL 3 0.653338 0.534783 0.931836 11.00000 0.02084 0.02738 = 0.02063 -0.00856 0.00269 -0.00854 S 6 0.262329 0.211852 0.839136 11.00000 0.01577 0.01694 = 0.01418 -0.00141 0.00219 -0.00428 O1 5 0.289300 0.087861 0.875557 11.00000 0.03330 0.01836 = 0.01899 0.00249 0.00261 -0.00769 O2 5 0.118038 0.267952 0.835310 11.00000 0.01439 0.03172 = 0.02142 -0.00525 0.00381 -0.00359 N 4 0.368588 0.314630 0.889131 11.00000 0.01503 0.01584 = 0.01622 -0.00189 0.00019 -0.00251 C1 1 0.559623 0.424323 0.862649 11.00000 0.01471 0.01531 = 0.01572 -0.00197 -0.00049 -0.00206 C2 1 0.530553 0.290418 0.900300 11.00000 0.01503 0.01907 = 0.01904 0.00263 0.00004 -0.00239 H2A 2 0.562383 0.281782 0.956463 11.00000 0.01933 H2B 2 0.562515 0.216398 0.871857 11.00000 0.01514 C3 1 0.391331 0.447981 0.856922 11.00000 0.01514 0.01591 = 0.02169 -0.00204 0.00178 -0.00065 H3A 2 0.350461 0.460307 0.803606 11.00000 0.02096 H3B 2 0.354091 0.514280 0.888813 11.00000 0.01951 C4 1 0.637964 0.422631 0.786913 11.00000 0.01539 0.01440 = 0.01463 -0.00045 0.00037 -0.00095 C5 1 0.760812 0.343680 0.780325 11.00000 0.01642 0.02063 = 0.01603 0.00221 0.00029 0.00202 H5 2 0.792533 0.294163 0.824926 11.00000 0.02237 C6 1 0.833457 0.340613 0.710732 11.00000 0.01755 0.02324 = 0.01989 -0.00126 0.00254 0.00094 H6 2 0.916947 0.285230 0.707445 11.00000 0.02788 C7 1 0.786260 0.416552 0.646041 11.00000 0.02480 0.02134 = 0.01520 -0.00241 0.00227 -0.00692 C8 1 0.664492 0.495605 0.653370 11.00000 0.02947 0.02408 = 0.01781 0.00636 -0.00047 -0.00067 H8 2 0.629838 0.549534 0.610558 11.00000 0.02960 C9 1 0.590995 0.499136 0.722944 11.00000 0.02238 0.01995 = 0.02233 0.00455 0.00161 0.00391 H9 2 0.505179 0.554719 0.726050 11.00000 0.03066 C10 1 0.867192 0.412473 0.571008 11.00000 0.03687 0.03368 = 0.01932 -0.00193 0.00913 -0.00674 AFIX 123 H10A 2 0.949476 0.351224 0.577389 21.00000 41.00000 H10B 2 0.799627 0.384376 0.527105 21.00000 41.00000 H10C 2 0.905033 0.499169 0.559799 21.00000 41.00000 H10D 2 0.819948 0.471955 0.532140 -21.00000 41.00000 H10E 2 0.969797 0.438804 0.582424 -21.00000 41.00000 H10F 2 0.864391 0.324010 0.549730 -21.00000 41.00000 AFIX 0 C11 1 0.321386 0.204329 0.742331 11.00000 0.01638 0.01473 = 0.01387 -0.00185 0.00105 -0.00177 C12 1 0.431188 0.116842 0.724256 11.00000 0.01835 0.01728 = 0.01700 0.00069 -0.00111 0.00257 H12 2 0.468816 0.061514 0.760852 11.00000 0.02437 C13 1 0.481258 0.115966 0.648674 11.00000 0.01856 0.02208 = 0.02004 -0.00150 0.00256 0.00468 H13 2 0.557669 0.056742 0.635992 11.00000 0.03079 C14 1 0.425009 0.201528 0.591039 11.00000 0.02036 0.02241 = 0.01587 -0.00125 0.00252 -0.00051 C15 1 0.314082 0.287502 0.610076 11.00000 0.02493 0.01918 = 0.01592 0.00174 -0.00095 0.00306 H15 2 0.271134 0.345011 0.570449 11.00000 0.02698 C16 1 0.261324 0.289102 0.685143 11.00000 0.01934 0.01686 = 0.01729 -0.00124 -0.00004 0.00303 H16 2 0.188532 0.349385 0.696773 11.00000 0.01597 C17 1 0.484167 0.203435 0.509850 11.00000 0.03482 0.03864 = 0.01738 0.00126 0.00734 0.00542 AFIX 123 H17A 2 0.431748 0.269398 0.477392 31.00000 51.00000 H17B 2 0.589504 0.224067 0.514334 31.00000 51.00000 H17C 2 0.469677 0.118078 0.485085 31.00000 51.00000 H17D 2 0.562205 0.138297 0.507149 -31.00000 51.00000 H17E 2 0.404449 0.183628 0.470207 -31.00000 51.00000 H17F 2 0.524276 0.289617 0.499456 -31.00000 51.00000 AFIX 0 HKLF 4 REM 19srv225_a.res in P2(1)/n REM wR2 = 0.0958, GooF = S = 1.056, Restrained GooF = 1.056 for all data REM R1 = 0.0371 for 4563 Fo > 4sig(Fo) and 0.0614 for all 6043 data REM 251 parameters refined using 0 restraints END WGHT 0.0442 0.5347 REM Highest difference peak 0.488, deepest hole -0.363, 1-sigma level 0.066 Q1 1 0.7811 0.3438 0.7408 11.00000 0.05 0.49 Q2 1 0.6169 0.4640 0.7551 11.00000 0.05 0.43 Q3 1 0.3755 0.1600 0.7367 11.00000 0.05 0.43 Q4 1 0.6065 0.4193 0.8187 11.00000 0.05 0.42 Q5 1 0.2852 0.2800 0.6455 11.00000 0.05 0.41 Q6 1 0.6879 0.3719 0.7816 11.00000 0.05 0.41 ; _shelx_res_checksum 37881 _shelx_hkl_file ; -1 0 0 -0.40 0.40 -1 0 0 0.40 0.50 -1 0 0 0.20 0.40 2 0 0 3657.03 138.29 2 0 0 3650.53 138.29 -2 0 0 3629.04 138.29 -2 0 0 3809.52 138.29 -2 0 0 3703.23 138.19 -2 0 0 3706.33 138.19 -3 0 0 0.90 1.20 -3 0 0 1.50 1.40 3 0 0 1.90 1.40 3 0 0 1.20 1.30 -3 0 0 -2.40 1.80 -3 0 0 -1.50 1.40 -3 0 0 0.10 1.20 -4 0 0 284.87 11.70 -4 0 0 285.57 11.30 4 0 0 283.97 11.30 -4 0 0 280.07 11.20 4 0 0 277.17 11.20 -4 0 0 266.37 11.10 -4 0 0 287.77 11.20 5 0 0 0.00 2.20 -5 0 0 1.40 2.60 -5 0 0 2.00 2.20 -5 0 0 -2.30 2.60 -5 0 0 3.20 3.90 -5 0 0 0.90 3.10 5 0 0 4.80 2.80 -6 0 0 2.00 2.50 -6 0 0 5.50 4.30 6 0 0 -0.10 3.30 -6 0 0 -1.60 3.50 -6 0 0 7.90 3.40 -6 0 0 -6.30 5.70 -6 0 0 7.80 4.00 -7 0 0 5.30 4.60 -7 0 0 3.00 3.70 7 0 0 -6.10 4.20 -7 0 0 7.70 4.80 -7 0 0 3.60 5.10 7 0 0 4.20 4.60 -8 0 0 388.36 18.00 8 0 0 409.96 17.60 -8 0 0 412.06 18.10 -8 0 0 405.26 17.40 -8 0 0 411.86 18.80 8 0 0 415.46 18.20 -9 0 0 -0.40 8.00 -9 0 0 -2.00 5.90 -9 0 0 -0.20 6.30 9 0 0 3.90 6.30 -10 0 0 560.14 24.10 -10 0 0 537.95 23.30 10 0 0 500.65 23.60 11 0 0 11.50 10.00 -11 0 0 -8.70 10.10 -11 0 0 -4.50 8.70 -12 0 0 86.69 13.70 -12 0 0 101.89 12.30 -13 0 0 -2.40 13.90 -1 -1 0 906.61 33.50 1 -1 0 859.81 33.40 1 -1 0 887.41 33.50 -1 -1 0 944.51 33.60 1 -1 0 873.41 33.50 -1 -1 0 845.82 33.40 -1 -1 0 897.31 33.50 -1 1 0 886.81 33.40 -1 1 0 894.61 33.50 1 1 0 970.80 33.50 1 1 0 922.21 33.60 -1 1 0 861.61 33.50 1 1 0 885.21 33.50 1 1 0 855.21 33.40 -2 -1 0 4689.03 178.48 2 -1 0 4722.03 178.48 -2 -1 0 4711.23 178.38 2 -1 0 4783.52 178.48 -2 -1 0 4860.11 178.48 2 1 0 4861.21 178.48 2 1 0 4628.74 178.38 -2 1 0 4713.23 178.38 -2 1 0 4929.71 178.48 3 -1 0 1633.34 63.79 -3 -1 0 1778.52 63.69 3 -1 0 1638.34 63.69 -3 -1 0 1751.02 63.89 -3 -1 0 1654.43 63.49 -3 -1 0 1749.62 63.69 -3 1 0 1689.13 63.69 -3 1 0 1660.43 63.59 3 1 0 1631.04 63.49 -3 1 0 1719.43 63.79 3 1 0 1731.03 63.79 3 1 0 1678.13 63.69 -3 1 0 1711.83 63.69 -4 -1 0 2154.08 78.99 -4 -1 0 1952.80 79.09 -4 -1 0 2187.78 79.39 -4 -1 0 2163.68 79.19 4 -1 0 2084.89 79.19 4 -1 0 2032.00 79.19 -4 1 0 2087.79 79.19 -4 1 0 2165.48 79.19 -4 1 0 2113.29 78.99 -4 1 0 2167.58 79.29 -4 1 0 2147.89 79.19 4 1 0 2074.19 78.99 4 1 0 2023.50 79.19 -5 -1 0 962.80 37.50 -5 -1 0 1004.90 36.80 -5 -1 0 982.90 37.00 5 -1 0 942.31 37.30 -5 -1 0 982.20 37.20 5 -1 0 929.91 37.20 -5 1 0 947.61 36.80 -5 1 0 958.90 37.30 5 1 0 986.30 36.80 -5 1 0 1009.30 36.80 -5 1 0 975.60 37.20 -5 1 0 966.10 37.10 5 1 0 959.40 37.10 -5 1 0 974.30 37.20 -6 -1 0 735.23 27.30 6 -1 0 704.03 27.30 6 -1 0 653.73 27.40 -6 -1 0 713.33 27.30 -6 -1 0 724.63 27.00 -6 -1 0 683.13 27.50 -6 1 0 691.73 27.60 -6 1 0 712.63 27.00 -6 1 0 704.83 27.50 -6 1 0 689.63 28.00 6 1 0 662.63 27.30 6 1 0 694.23 26.90 -6 1 0 713.83 26.90 -6 1 0 701.83 27.50 7 -1 0 897.51 34.90 -7 -1 0 939.11 34.40 -7 -1 0 867.91 35.10 -7 -1 0 923.81 34.70 7 -1 0 923.71 34.80 -7 1 0 784.82 34.70 7 1 0 925.71 34.80 -7 1 0 899.91 34.60 -7 1 0 870.01 35.00 -7 1 0 899.31 34.90 8 -1 0 110.19 7.60 8 -1 0 104.59 7.80 -8 -1 0 122.39 7.40 -8 -1 0 122.69 8.30 -8 -1 0 99.39 7.10 -8 1 0 127.79 8.10 -8 1 0 89.59 8.40 -8 1 0 126.69 7.90 8 1 0 111.19 7.60 -8 1 0 118.39 6.90 9 -1 0 256.17 14.10 -9 -1 0 269.47 13.60 -9 -1 0 231.18 13.70 -9 -1 0 265.57 14.30 9 -1 0 264.17 14.00 9 1 0 247.68 13.50 -9 1 0 227.78 13.10 -9 1 0 244.58 13.80 10 -1 0 15.40 8.20 10 -1 0 18.60 8.00 -10 -1 0 -0.90 8.10 -10 -1 0 29.60 7.70 10 1 0 12.40 8.30 -10 1 0 9.90 7.00 -10 1 0 9.60 7.60 -11 -1 0 1.40 9.10 -11 -1 0 6.40 9.60 -11 -1 0 -5.60 8.90 -11 1 0 2.10 8.50 11 1 0 4.50 16.10 -12 -1 0 111.09 12.90 -12 -1 0 107.39 13.30 -12 1 0 101.79 13.50 12 1 0 128.79 13.50 -12 1 0 117.99 12.70 -13 -1 0 -5.50 13.90 -13 1 0 -0.50 15.10 0 -2 0 999.80 38.20 0 -2 0 973.80 38.20 0 -2 0 1012.90 38.20 0 -2 0 1056.09 38.20 0 2 0 1002.30 38.20 0 2 0 1028.90 38.20 0 2 0 1038.40 38.20 0 2 0 1013.80 38.20 1 -2 0 4558.94 167.08 -1 -2 0 4579.44 166.98 1 -2 0 4448.06 166.88 1 -2 0 4309.87 166.88 -1 -2 0 4561.44 167.08 1 -2 0 4577.44 167.08 -1 -2 0 4532.35 167.08 -1 2 0 4367.36 166.88 1 2 0 4489.05 166.98 -1 2 0 4372.76 167.08 -1 2 0 4623.64 167.08 1 2 0 4161.88 167.08 1 2 0 4410.76 167.08 2 -2 0 338.47 13.80 -2 -2 0 350.76 13.30 2 -2 0 344.87 13.60 -2 -2 0 353.16 13.70 -2 -2 0 375.76 13.80 2 -2 0 342.97 13.40 2 2 0 386.36 13.80 2 2 0 363.86 13.40 -2 2 0 359.56 13.50 -2 2 0 350.26 13.80 -2 2 0 329.47 13.50 2 2 0 358.06 13.80 2 2 0 355.46 13.60 -3 -2 0 126.59 5.90 -3 -2 0 134.19 5.90 3 -2 0 133.19 6.10 3 -2 0 141.79 5.50 3 -2 0 136.99 6.00 -3 -2 0 133.49 5.30 -3 -2 0 144.09 6.50 -3 -2 0 129.29 5.30 -3 2 0 146.19 6.20 3 2 0 125.99 6.10 3 2 0 126.89 6.20 -3 2 0 139.79 5.70 -3 2 0 139.79 6.10 3 2 0 130.49 5.70 -3 2 0 140.59 5.50 -4 -2 0 2866.31 112.29 -4 -2 0 2912.81 111.89 -4 -2 0 3086.49 112.49 -4 -2 0 3019.30 111.89 -4 -2 0 3076.09 112.19 4 -2 0 2931.81 111.99 4 -2 0 2883.61 112.59 -4 2 0 3026.70 112.29 -4 2 0 3151.38 112.29 4 2 0 3042.90 112.29 4 2 0 2952.50 112.19 4 2 0 2890.81 112.49 -4 2 0 2964.20 112.19 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-23 125.99 19.70 -5 5 23 157.08 19.40 -4 -5 23 45.20 16.30 4 -5 -23 52.19 16.90 -4 5 23 65.59 17.20 4 5 -23 72.09 18.00 -3 -5 23 -12.30 14.80 3 -5 -23 4.00 15.60 3 5 -23 6.30 16.10 -3 5 23 21.20 14.50 2 -5 -23 24.60 15.40 -2 -5 23 16.80 13.30 2 5 -23 1.30 15.20 -2 5 23 -12.00 14.60 -2 5 23 -11.60 15.80 1 -5 -23 54.49 15.10 -1 -5 23 48.50 13.40 1 5 -23 60.09 15.50 -1 5 23 59.19 14.70 -1 5 23 46.00 13.80 0 -5 23 -11.30 12.90 0 -5 -23 16.70 15.50 0 5 -23 33.50 15.80 0 5 23 -9.70 13.70 0 5 23 16.40 12.80 1 -5 23 -2.30 14.00 -1 -5 -23 -32.10 15.80 1 5 23 3.30 12.30 -1 5 -23 -16.50 14.90 1 5 23 14.20 15.10 -2 -5 -23 -4.60 16.80 2 -5 23 18.00 14.20 2 5 23 2.10 14.30 2 5 23 -7.40 13.70 -2 5 -23 -8.60 15.80 -3 -5 -23 13.50 16.50 3 -5 23 5.90 16.90 -3 5 -23 42.10 17.70 3 5 23 -6.40 16.90 4 -5 23 83.19 17.70 -4 -5 -23 119.29 19.70 4 5 23 97.99 17.80 -4 5 -23 103.39 20.00 -4 -6 23 -10.40 17.80 -4 -6 23 4.30 17.00 4 -6 -23 -9.50 17.10 4 6 -23 1.70 18.80 -4 6 23 -10.00 16.40 -3 -6 23 9.80 16.40 -3 -6 23 13.30 14.90 3 -6 -23 12.80 17.40 -3 6 23 1.00 15.90 3 6 -23 9.90 17.40 2 -6 -23 21.40 16.00 -2 -6 23 41.70 16.00 -2 -6 23 -21.30 15.40 2 6 -23 -10.70 16.50 -2 6 23 -5.50 15.90 -2 6 23 5.30 14.90 -1 -6 23 8.70 14.50 1 -6 -23 -0.10 16.00 -1 -6 23 -2.80 14.70 -1 6 23 -15.20 16.10 -1 6 23 9.40 15.20 1 6 -23 18.00 17.70 0 -6 23 219.38 18.50 0 -6 -23 251.77 21.70 0 6 23 237.38 18.90 0 6 -23 248.58 20.20 0 6 23 244.18 18.70 -1 -6 -23 37.90 16.10 1 -6 23 45.50 15.10 1 6 23 16.10 14.60 1 6 23 24.40 16.90 -1 6 -23 72.19 17.10 -2 -6 -23 239.78 21.20 2 -6 23 200.48 18.60 2 6 23 166.78 19.10 -2 6 -23 184.38 19.60 -3 -6 -23 21.70 19.20 -3 6 -23 44.30 18.00 3 6 23 49.10 17.00 3 -7 -23 15.10 18.20 -3 -7 23 -7.20 16.90 3 7 -23 -1.70 19.20 -3 7 23 13.40 18.70 -3 7 23 37.40 27.70 -2 -7 23 75.99 17.10 2 -7 -23 36.00 18.30 -2 -7 23 13.90 17.50 2 7 -23 91.69 20.40 -2 7 23 37.80 17.90 -2 7 23 45.20 18.10 1 -7 -23 69.89 18.00 -1 -7 23 54.09 17.80 -1 7 23 64.49 16.00 1 7 -23 55.99 18.80 -1 7 23 15.30 17.60 0 -7 -23 50.59 18.70 0 7 -23 20.00 18.10 0 7 23 21.00 15.50 0 7 23 40.40 17.20 -1 -7 -23 54.69 20.10 1 7 23 20.20 18.50 -1 7 -23 60.19 18.40 6 0 -24 172.58 20.00 -5 0 24 4.40 14.80 5 0 -24 -21.60 17.20 4 0 -24 27.00 15.10 -4 0 24 -5.10 13.40 -3 0 24 -14.50 13.10 3 0 -24 -20.90 14.80 2 0 -24 4.30 13.70 2 0 -24 8.10 15.00 -2 0 24 37.00 12.70 1 0 -24 -16.10 14.50 -1 0 24 7.50 13.40 1 0 -24 -4.40 13.00 0 0 24 48.10 13.70 0 0 -24 24.60 13.00 0 0 -24 40.80 14.40 -1 0 -24 6.90 14.50 -1 0 -24 20.60 14.20 1 0 24 -13.90 13.60 -2 0 -24 24.50 14.80 -2 0 -24 44.90 15.00 2 0 24 39.30 12.90 -3 0 -24 22.40 15.50 -3 0 -24 6.90 14.80 3 0 24 -2.40 13.30 -4 0 -24 78.49 17.30 4 0 24 106.29 16.20 6 -1 -24 -14.50 17.60 6 1 -24 -11.10 19.30 -5 -1 24 5.60 14.90 5 -1 -24 -12.80 16.20 5 1 -24 17.60 17.90 -5 1 24 -9.30 15.40 -4 -1 24 23.60 13.80 4 -1 -24 13.80 16.00 4 1 -24 26.20 15.60 -4 1 24 3.70 14.10 -3 -1 24 76.89 14.10 3 -1 -24 75.19 15.20 3 1 -24 44.80 15.70 3 1 -24 88.29 14.80 -3 1 24 55.29 14.10 2 -1 -24 17.80 15.40 -2 -1 24 17.40 12.60 2 1 -24 36.20 15.10 -2 1 24 20.00 12.80 2 1 -24 1.60 14.10 -1 -1 24 -7.70 12.10 1 -1 -24 7.30 14.60 -1 1 24 19.30 12.50 1 1 -24 9.80 13.40 1 1 -24 7.20 13.30 0 -1 -24 18.30 15.00 0 -1 -24 3.70 12.90 0 -1 24 12.30 12.70 0 1 24 -4.60 12.40 0 1 -24 -11.40 14.00 0 1 -24 0.90 14.30 1 -1 24 25.40 13.20 -1 -1 -24 55.79 13.80 -1 -1 -24 30.20 14.60 -1 1 -24 52.19 14.40 1 1 24 49.30 13.30 -1 1 -24 47.30 14.90 2 -1 24 -28.00 13.70 -2 -1 -24 18.40 15.20 -2 -1 -24 -4.70 14.20 -2 1 -24 -8.50 15.00 -2 1 -24 12.20 14.60 2 1 24 31.10 14.00 3 -1 24 29.00 14.30 -3 -1 -24 58.59 15.80 -3 -1 -24 22.00 14.60 -3 1 -24 33.20 16.00 3 1 24 40.10 13.90 -4 -1 -24 55.49 16.10 4 -1 24 64.99 15.30 -4 1 -24 40.00 16.90 4 1 24 36.50 15.60 5 -2 -24 14.50 16.90 -5 -2 24 32.50 15.30 -5 2 24 25.30 15.20 -4 -2 24 26.60 14.60 4 -2 -24 42.80 16.20 -4 2 24 25.70 14.90 4 2 -24 62.19 16.30 4 2 -24 6.20 23.90 3 -2 -24 20.20 15.90 -3 -2 24 22.70 13.40 -3 2 24 30.60 14.60 3 2 -24 2.10 14.50 3 2 -24 2.80 15.60 2 -2 -24 98.49 15.50 -2 -2 24 90.39 13.90 2 2 -24 72.89 14.70 2 2 -24 76.59 15.90 -2 2 24 104.19 14.30 -1 -2 24 188.78 15.70 1 -2 -24 169.38 17.50 1 2 -24 131.39 16.50 -1 2 24 196.18 16.30 1 2 -24 188.48 17.40 0 -2 -24 149.49 17.00 0 -2 24 147.19 15.10 0 2 -24 147.49 15.80 0 2 24 123.89 15.20 0 2 -24 130.19 15.90 -1 -2 -24 -5.90 14.20 1 -2 24 8.90 13.20 -1 2 -24 -0.40 14.20 -1 2 -24 -13.50 13.80 1 2 24 2.80 13.60 -2 -2 -24 5.80 19.50 2 -2 24 0.50 14.00 -2 -2 -24 34.20 16.40 -2 2 -24 -13.80 17.00 2 2 24 6.20 14.40 -2 2 -24 17.80 15.40 -3 -2 -24 21.00 15.30 3 -2 24 10.30 15.70 -3 -2 -24 23.40 16.70 3 2 24 20.50 13.20 -3 2 -24 -1.10 16.30 3 2 24 35.10 16.50 -4 -2 -24 9.60 15.90 4 -2 24 -18.70 16.30 -4 -2 -24 15.60 17.90 -4 2 -24 16.80 17.80 4 2 24 2.10 17.00 4 2 24 10.60 15.00 -5 -3 24 35.90 17.40 5 -3 -24 1.50 17.40 -5 3 24 -4.50 16.90 5 3 -24 1.80 18.40 -4 -3 24 20.60 14.40 4 -3 -24 -30.70 22.80 4 3 -24 18.70 17.40 -4 3 24 -7.20 15.20 3 -3 -24 4.90 16.70 -3 -3 24 9.70 14.50 3 3 -24 -12.90 16.40 -3 3 24 -29.20 14.20 -2 -3 24 4.20 13.60 2 -3 -24 21.20 14.80 2 3 -24 2.10 14.40 2 3 -24 7.40 15.70 -2 3 24 8.20 14.10 1 -3 -24 10.40 15.50 -1 -3 24 -5.20 13.00 1 3 -24 -17.60 14.50 -1 3 24 -2.30 13.10 1 3 -24 2.10 14.10 0 -3 24 203.68 17.10 0 -3 -24 231.88 19.30 0 3 -24 231.38 17.90 0 3 -24 238.28 18.60 0 3 24 224.98 16.70 1 -3 24 2.90 13.30 -1 -3 -24 -1.60 16.00 -1 3 -24 9.80 15.90 1 3 24 -3.20 14.10 -1 3 -24 17.10 14.70 -2 -3 -24 57.79 16.60 2 -3 24 52.89 15.70 -2 3 -24 40.80 15.70 2 3 24 42.70 14.90 2 3 24 47.90 15.70 3 -3 24 26.70 15.60 -3 -3 -24 -3.90 17.50 3 3 24 28.20 14.10 -3 3 -24 0.80 17.60 3 3 24 29.10 16.20 -4 -3 -24 -6.50 18.90 4 -3 24 -23.90 18.20 4 3 24 10.80 17.50 -4 3 -24 -0.60 17.80 4 -4 -24 38.30 18.30 -4 -4 24 12.70 15.60 4 4 -24 22.00 18.10 -4 4 24 47.00 16.00 -3 -4 24 0.50 15.00 3 -4 -24 -5.50 16.10 -3 4 24 1.60 15.40 3 4 -24 1.30 17.30 2 -4 -24 18.50 16.30 -2 -4 24 17.40 13.90 2 4 -24 33.50 16.30 -2 4 24 45.30 15.10 -1 -4 24 17.60 14.00 1 -4 -24 4.80 16.80 1 4 -24 39.60 15.50 -1 4 24 28.30 14.00 0 -4 -24 -14.50 15.90 0 -4 24 -13.40 14.00 0 4 -24 -13.70 15.60 0 4 24 1.80 13.20 1 -4 24 38.50 14.40 -1 -4 -24 48.60 17.20 1 4 24 63.89 14.90 -1 4 -24 45.80 16.10 1 4 24 55.49 16.10 2 -4 24 -9.70 16.10 -2 -4 -24 13.60 17.70 2 4 24 -22.20 15.80 -2 4 -24 -2.30 16.20 2 4 24 -6.30 14.10 -3 -4 -24 149.49 20.20 3 -4 24 184.48 20.00 3 4 24 182.88 19.00 -3 4 -24 169.88 19.50 4 -5 -24 148.19 20.00 4 5 -24 227.48 23.00 -4 5 24 227.18 31.60 3 -5 -24 3.50 18.30 -3 -5 24 54.99 18.40 -3 5 24 55.49 17.10 3 5 -24 36.10 18.40 2 -5 -24 114.89 19.30 -2 -5 24 100.49 16.00 2 5 -24 74.69 18.00 -2 5 24 84.19 16.50 1 -5 -24 4.20 17.20 -1 -5 24 7.90 15.90 1 5 -24 34.90 17.40 -1 5 24 5.60 15.80 0 -5 24 -6.20 15.70 0 -5 -24 15.40 17.20 0 5 -24 29.40 17.70 0 5 24 21.70 16.90 0 5 24 15.20 15.20 -1 -5 -24 312.17 23.20 1 -5 24 278.17 20.50 -1 5 -24 322.17 23.50 1 5 24 300.37 21.00 1 5 24 290.67 19.30 -2 -5 -24 -19.10 17.50 2 -5 24 -8.40 17.60 2 5 24 39.40 18.10 -2 5 -24 1.60 18.60 2 -6 -24 5.60 19.80 -2 -6 24 7.30 16.50 -2 6 24 23.50 17.70 2 6 -24 14.80 19.10 1 -6 -24 338.27 24.60 1 6 -24 346.97 25.70 -1 6 24 374.56 23.30 0 -6 -24 22.50 19.60 0 6 24 19.70 16.20 0 6 24 31.20 18.20 0 6 -24 29.70 18.40 -4 0 25 11.90 17.60 4 0 -25 -4.70 16.80 -3 0 25 22.60 15.00 3 0 -25 26.60 15.90 -2 0 25 -11.60 13.70 2 0 -25 7.90 16.20 1 0 -25 -7.70 15.20 -1 0 25 20.30 15.40 0 0 -25 -18.80 16.50 0 0 -25 -8.50 14.70 0 0 25 -7.50 14.00 1 0 25 67.19 15.10 -1 0 -25 71.19 17.00 -1 0 -25 112.79 16.60 2 0 25 10.40 14.30 -2 0 -25 5.40 17.30 -2 0 -25 -12.50 16.30 -3 0 -25 -2.80 17.60 3 0 25 -3.70 15.60 -4 -1 25 12.50 25.10 4 -1 -25 -22.40 18.20 -4 1 25 9.30 17.50 4 1 -25 12.90 17.70 -3 -1 25 35.80 14.70 3 -1 -25 81.09 16.90 -3 1 25 53.09 15.80 3 1 -25 78.19 17.60 2 -1 -25 20.30 16.00 -2 -1 25 13.80 14.60 2 1 -25 20.30 16.60 2 1 -25 11.60 15.40 -2 1 25 18.30 14.20 1 -1 -25 87.29 16.50 -1 -1 25 91.69 15.40 1 1 -25 105.79 17.40 1 1 -25 93.59 16.50 -1 1 25 133.39 15.60 0 -1 -25 113.59 17.70 0 -1 25 91.19 16.50 0 1 -25 75.89 16.30 0 1 -25 69.29 16.30 0 1 25 109.19 16.50 -1 -1 -25 139.69 17.80 1 -1 25 119.59 16.00 -1 1 -25 162.68 17.50 1 1 25 154.58 17.60 -1 1 -25 121.29 17.50 2 -1 25 9.60 16.70 -2 -1 -25 -11.30 16.60 -2 -1 -25 0.70 19.00 2 1 25 17.90 14.50 -2 1 -25 -0.10 16.90 -2 1 -25 -0.60 23.60 -3 -1 -25 -32.30 17.30 3 -1 25 6.80 15.90 -3 -1 -25 -4.80 19.10 -3 1 -25 9.50 18.50 3 1 25 31.10 15.30 4 -2 -25 -32.80 19.20 4 2 -25 -21.90 18.70 3 -2 -25 -8.80 16.70 -3 -2 25 14.90 14.40 -3 2 25 4.30 16.50 3 2 -25 9.90 16.40 3 2 -25 34.10 16.80 -2 -2 25 20.60 14.70 2 -2 -25 47.60 17.70 2 2 -25 19.70 16.70 2 2 -25 8.60 16.30 -2 2 25 5.20 14.90 1 -2 -25 108.09 18.40 -1 -2 25 39.00 15.50 1 2 -25 71.49 16.50 1 2 -25 98.19 16.00 -1 2 25 77.19 16.70 0 -2 -25 6.10 17.30 0 -2 25 -2.90 14.30 0 2 -25 29.70 15.40 0 2 -25 8.70 16.10 0 2 25 -7.00 14.50 1 -2 25 67.29 15.70 -1 -2 -25 74.79 16.70 -1 2 -25 71.89 16.30 1 2 25 48.00 15.90 -1 2 -25 107.79 17.10 2 -2 25 -22.60 15.80 -2 -2 -25 7.20 17.70 2 2 25 18.70 14.90 -2 2 -25 49.90 18.00 3 -3 -25 355.66 24.70 3 3 -25 406.36 25.10 2 -3 -25 52.09 18.60 -2 -3 25 40.20 15.20 -2 3 25 58.39 16.20 2 3 -25 43.30 16.50 1 -3 -25 44.80 16.90 -1 -3 25 55.99 16.10 1 3 -25 81.39 18.20 -1 3 25 80.59 15.70 0 -3 -25 29.50 17.70 0 -3 25 29.90 15.10 0 3 25 15.40 14.90 0 3 -25 19.20 17.40 0 3 -25 17.30 17.40 -1 -3 -25 -4.80 18.90 1 -3 25 9.00 15.50 1 3 25 16.00 16.00 -1 3 -25 32.60 16.60 -2 -3 -25 92.19 19.20 2 -3 25 124.09 18.50 -2 3 -25 95.29 18.60 2 3 25 100.79 17.00 2 -4 -25 -3.90 17.90 -2 4 25 -9.40 16.70 2 4 -25 -44.20 19.00 1 -4 -25 -0.90 19.10 1 4 -25 19.90 18.70 -1 4 25 -13.00 16.50 0 -4 -25 85.09 20.20 0 4 25 127.59 16.70 0 4 -25 127.19 19.50 -1 -4 -25 68.79 20.20 -1 4 -25 61.59 19.90 1 4 25 40.90 16.90 2 0 -26 -3.70 18.40 1 0 -26 -9.60 18.70 -1 0 26 -6.40 16.20 0 0 -26 -23.50 18.20 0 0 26 1.00 17.50 1 -1 -26 -20.10 18.60 1 1 -26 36.50 18.20 -1 1 26 -10.90 17.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 36072 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl 0.65334(3) 0.53478(3) 0.93184(2) 0.02289(8) Uani 1 1 d . . . . . S S 0.26233(3) 0.21185(3) 0.83914(2) 0.01558(7) Uani 1 1 d . . . . . O1 O 0.28930(11) 0.08786(9) 0.87556(5) 0.0235(2) Uani 1 1 d . . . . . O2 O 0.11804(9) 0.26795(10) 0.83531(5) 0.02240(19) Uani 1 1 d . . . . . N N 0.36859(11) 0.31463(10) 0.88913(6) 0.01573(19) Uani 1 1 d . . . . . C1 C 0.55962(12) 0.42432(11) 0.86265(7) 0.0153(2) Uani 1 1 d . . . . . C2 C 0.53055(13) 0.29042(12) 0.90030(7) 0.0178(2) Uani 1 1 d . . . . . H2A H 0.5624(17) 0.2818(14) 0.9565(9) 0.019(4) Uiso 1 1 d . . . . . H2B H 0.5625(16) 0.2164(14) 0.8719(9) 0.015(4) Uiso 1 1 d . . . . . C3 C 0.39133(13) 0.44798(12) 0.85692(7) 0.0175(2) Uani 1 1 d . . . . . H3A H 0.3505(18) 0.4603(15) 0.8036(9) 0.021(4) Uiso 1 1 d . . . . . H3B H 0.3541(17) 0.5143(15) 0.8888(9) 0.020(4) Uiso 1 1 d . . . . . C4 C 0.63796(13) 0.42263(11) 0.78691(6) 0.0148(2) Uani 1 1 d . . . . . C5 C 0.76081(13) 0.34368(12) 0.78033(7) 0.0177(2) Uani 1 1 d . . . . . H5 H 0.7925(17) 0.2942(15) 0.8249(9) 0.022(4) Uiso 1 1 d . . . . . C6 C 0.83346(14) 0.34061(13) 0.71073(7) 0.0202(2) Uani 1 1 d . . . . . H6 H 0.9169(19) 0.2852(16) 0.7074(10) 0.028(4) Uiso 1 1 d . . . . . C7 C 0.78626(14) 0.41655(12) 0.64604(7) 0.0204(2) Uani 1 1 d . . . . . C8 C 0.66449(16) 0.49561(13) 0.65337(7) 0.0239(3) Uani 1 1 d . . . . . H8 H 0.6298(19) 0.5495(17) 0.6106(10) 0.030(4) Uiso 1 1 d . . . . . C9 C 0.59100(15) 0.49914(13) 0.72294(8) 0.0215(2) Uani 1 1 d . . . . . H9 H 0.5052(19) 0.5547(17) 0.7260(10) 0.031(4) Uiso 1 1 d . . . . . C10 C 0.86719(17) 0.41247(15) 0.57101(8) 0.0297(3) Uani 1 1 d . . . . . H10A H 0.949476 0.351224 0.577389 0.041(4) Uiso 0.29(2) 1 calc R U P . . H10B H 0.799627 0.384376 0.527105 0.041(4) Uiso 0.29(2) 1 calc R U P . . H10C H 0.905033 0.499169 0.559799 0.041(4) Uiso 0.29(2) 1 calc R U P . . H10D H 0.819948 0.471955 0.532140 0.041(4) Uiso 0.71(2) 1 calc R U P . . H10E H 0.969797 0.438804 0.582424 0.041(4) Uiso 0.71(2) 1 calc R U P . . H10F H 0.864391 0.324010 0.549730 0.041(4) Uiso 0.71(2) 1 calc R U P . . C11 C 0.32139(13) 0.20433(11) 0.74233(6) 0.0150(2) Uani 1 1 d . . . . . C12 C 0.43119(13) 0.11684(12) 0.72426(7) 0.0176(2) Uani 1 1 d . . . . . H12 H 0.4688(18) 0.0615(16) 0.7609(9) 0.024(4) Uiso 1 1 d . . . . . C13 C 0.48126(14) 0.11597(13) 0.64867(7) 0.0202(2) Uani 1 1 d . . . . . H13 H 0.558(2) 0.0567(17) 0.6360(10) 0.031(4) Uiso 1 1 d . . . . . C14 C 0.42501(14) 0.20153(12) 0.59104(7) 0.0195(2) Uani 1 1 d . . . . . C15 C 0.31408(14) 0.28750(12) 0.61008(7) 0.0201(2) Uani 1 1 d . . . . . H15 H 0.2711(18) 0.3450(16) 0.5704(10) 0.027(4) Uiso 1 1 d . . . . . C16 C 0.26132(14) 0.28910(12) 0.68514(7) 0.0179(2) Uani 1 1 d . . . . . H16 H 0.1885(16) 0.3494(15) 0.6968(8) 0.016(4) Uiso 1 1 d . . . . . C17 C 0.48417(17) 0.20343(16) 0.50985(8) 0.0300(3) Uani 1 1 d . . . . . H17A H 0.431748 0.269398 0.477392 0.032(4) Uiso 0.429(18) 1 calc R U P . . H17B H 0.589504 0.224067 0.514334 0.032(4) Uiso 0.429(18) 1 calc R U P . . H17C H 0.469677 0.118078 0.485085 0.032(4) Uiso 0.429(18) 1 calc R U P . . H17D H 0.562205 0.138297 0.507149 0.032(4) Uiso 0.571(18) 1 calc R U P . . H17E H 0.404449 0.183628 0.470207 0.032(4) Uiso 0.571(18) 1 calc R U P . . H17F H 0.524276 0.289617 0.499456 0.032(4) Uiso 0.571(18) 1 calc R U P . . 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 Cl 0.02084(14) 0.02738(15) 0.02063(14) -0.00856(11) 0.00269(10) -0.00854(11) S 0.01577(13) 0.01694(13) 0.01418(12) -0.00141(10) 0.00219(9) -0.00428(10) O1 0.0333(5) 0.0184(4) 0.0190(4) 0.0025(3) 0.0026(4) -0.0077(4) O2 0.0144(4) 0.0317(5) 0.0214(4) -0.0053(4) 0.0038(3) -0.0036(3) N 0.0150(4) 0.0158(4) 0.0162(4) -0.0019(3) 0.0002(3) -0.0025(3) C1 0.0147(5) 0.0153(5) 0.0157(5) -0.0020(4) -0.0005(4) -0.0021(4) C2 0.0150(5) 0.0191(5) 0.0190(5) 0.0026(4) 0.0000(4) -0.0024(4) C3 0.0151(5) 0.0159(5) 0.0217(5) -0.0020(4) 0.0018(4) -0.0007(4) C4 0.0154(5) 0.0144(5) 0.0146(5) -0.0005(4) 0.0004(4) -0.0010(4) C5 0.0164(5) 0.0206(5) 0.0160(5) 0.0022(4) 0.0003(4) 0.0020(4) C6 0.0175(5) 0.0232(6) 0.0199(5) -0.0013(5) 0.0025(4) 0.0009(5) C7 0.0248(6) 0.0213(6) 0.0152(5) -0.0024(4) 0.0023(4) -0.0069(5) C8 0.0295(7) 0.0241(6) 0.0178(5) 0.0064(5) -0.0005(5) -0.0007(5) C9 0.0224(6) 0.0199(6) 0.0223(6) 0.0046(5) 0.0016(5) 0.0039(5) C10 0.0369(8) 0.0337(7) 0.0193(6) -0.0019(5) 0.0091(5) -0.0067(6) C11 0.0164(5) 0.0147(5) 0.0139(5) -0.0019(4) 0.0010(4) -0.0018(4) C12 0.0184(5) 0.0173(5) 0.0170(5) 0.0007(4) -0.0011(4) 0.0026(4) C13 0.0186(6) 0.0221(6) 0.0200(5) -0.0015(4) 0.0026(4) 0.0047(5) C14 0.0204(6) 0.0224(6) 0.0159(5) -0.0012(4) 0.0025(4) -0.0005(5) C15 0.0249(6) 0.0192(5) 0.0159(5) 0.0017(4) -0.0010(4) 0.0031(5) C16 0.0193(5) 0.0169(5) 0.0173(5) -0.0012(4) 0.0000(4) 0.0030(4) C17 0.0348(8) 0.0386(8) 0.0174(6) 0.0013(5) 0.0073(5) 0.0054(6) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 -1.00 1.00 0.1150 1.00 1.00 -1.00 0.1120 1.00 -1.00 0.00 0.1110 1.00 1.00 1.00 0.0770 -2.00 -1.00 -1.00 0.0970 -1.00 -1.00 -2.00 0.1340 -1.00 1.00 2.00 0.1720 1.00 -1.00 -2.00 0.1430 -2.00 0.00 1.00 0.1360 -1.00 2.00 -1.00 0.1130 1.00 2.00 -2.00 0.1070 -1.00 -2.00 2.00 0.1230 -2.00 -1.00 2.00 0.1240 0.00 -1.00 2.00 0.0810 0.00 1.00 -2.00 0.0990 -2.00 1.00 -1.00 0.0990 0.00 0.00 -1.00 0.0940 1.00 0.00 -2.00 0.1470 -1.00 0.00 2.00 0.1520 0.00 0.00 1.00 0.1060 -1.00 0.00 -1.00 0.0820 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 S N 105.86(5) . . ? O1 S C11 107.98(6) . . ? O2 S O1 120.77(6) . . ? O2 S N 105.87(5) . . ? O2 S C11 107.84(5) . . ? N S C11 107.93(5) . . ? C2 N S 120.30(8) . . ? C2 N C3 92.43(9) . . ? C3 N S 119.69(8) . . ? C2 C1 Cl 112.21(8) . . ? C3 C1 Cl 111.52(8) . . ? C3 C1 C2 88.46(9) . . ? C4 C1 Cl 109.35(8) . . ? C4 C1 C2 116.26(10) . . ? C4 C1 C3 117.76(10) . . ? N C2 C1 89.47(9) . . ? N C3 C1 89.47(9) . . ? C5 C4 C1 119.92(10) . . ? C9 C4 C1 121.40(10) . . ? C9 C4 C5 118.67(11) . . ? C6 C5 C4 120.51(11) . . ? C5 C6 C7 121.12(12) . . ? C6 C7 C10 120.36(12) . . ? C8 C7 C6 117.95(11) . . ? C8 C7 C10 121.69(12) . . ? C7 C8 C9 121.26(12) . . ? C4 C9 C8 120.48(12) . . ? C12 C11 S 119.82(9) . . ? C16 C11 S 119.55(9) . . ? C16 C11 C12 120.59(11) . . ? C13 C12 C11 119.20(11) . . ? C12 C13 C14 121.22(11) . . ? C13 C14 C15 118.70(11) . . ? C13 C14 C17 120.89(12) . . ? C15 C14 C17 120.40(11) . . ? C16 C15 C14 121.01(11) . . ? C15 C16 C11 119.26(11) . . ? 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 Cl C1 1.8103(11) . ? S O1 1.4336(9) . ? S O2 1.4321(9) . ? S N 1.6356(10) . ? S C11 1.7599(11) . ? N C2 1.4950(15) . ? N C3 1.4975(16) . ? C1 C2 1.5496(16) . ? C1 C3 1.5475(16) . ? C1 C4 1.5064(16) . ? C4 C5 1.3922(16) . ? C4 C9 1.3873(16) . ? C5 C6 1.3876(17) . ? C6 C7 1.3939(18) . ? C7 C8 1.387(2) . ? C7 C10 1.5090(17) . ? C8 C9 1.3916(18) . ? C11 C12 1.3933(16) . ? C11 C16 1.3920(16) . ? C12 C13 1.3862(17) . ? C13 C14 1.3905(17) . ? C14 C15 1.3953(18) . ? C14 C17 1.5087(17) . ? C15 C16 1.3877(17) . ?