#------------------------------------------------------------------------------ #$Date: 2022-11-24 12:12:12 +0200 (Thu, 24 Nov 2022) $ #$Revision: 279546 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/62/8106247.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_8106247 loop_ _publ_author_name 'Yeo, Chien Ing' 'Tiekink, Edward R.T.' _publ_section_title ; Crystal structure and molecular packing of O-ethyl (2-chlorophenyl)carbamothioate, C9H10ClNOS ; _journal_issue 4 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 651 _journal_page_last 653 _journal_paper_doi 10.1515/ncrs-2017-0422 _journal_volume 233 _journal_year 2018 _chemical_formula_moiety 'C9 H10 Cl N O S' _chemical_formula_sum 'C9 H10 Cl N O S' _chemical_formula_weight 215.69 _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 mixed _cell_angle_alpha 81.007(3) _cell_angle_beta 82.268(4) _cell_angle_gamma 73.210(3) _cell_formula_units_Z 4 _cell_length_a 7.2277(3) _cell_length_b 9.9791(3) _cell_length_c 14.7725(7) _cell_measurement_reflns_used 5271 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.5009 _cell_measurement_theta_min 2.4108 _cell_volume 1003.01(7) _computing_cell_refinement 'CrysAlis PRO [1]' _computing_data_collection 'CrysAlis PRO [1]' _computing_data_reduction 'CrysAlis PRO [1]' _computing_molecular_graphics 'ORTEP-3 for Windows [4]' _computing_publication_material 'SHELXL-2014/7 [3]' _computing_structure_refinement 'SHELXL-2014/7 [3]' _computing_structure_solution 'SHELXS-97 [2]' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.4041 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Agilent Technologies SuperNova Dual diffractometer with Atlas detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator Mirror _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_unetI/netI 0.0492 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 14831 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.561 _diffrn_reflns_theta_min 2.416 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro [1]' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.428 _exptl_crystal_description prism _exptl_crystal_F_000 448 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.384 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.069 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 243 _refine_ls_number_reflns 4637 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0364 _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^)+(0.0284P)^2^+0.3988P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.0828 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3653 _reflns_number_total 4637 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file suppl_ncrs-2017-0422_suppl.cif _cod_data_source_block shelx _cod_database_code 8106247 _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_min 0.875 _shelx_estimated_absorpt_t_max 0.922 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL 15 CELL 0.71073 7.2277 9.9791 14.7725 81.007 82.268 73.210 ZERR 4.00 0.0003 0.0003 0.0007 0.003 0.004 0.003 LATT 1 SFAC C H N O S CL UNIT 36 40 4 4 4 4 MERG 2 DFIX 0.88 0.01 N1 H1n N2 H2n FMAP 2 PLAN -1 SIZE 0.150 0.200 0.250 ACTA BOND $H CONF L.S. 36 MPLA S1 O1 N1 C1 MPLA C3 > C7 MPLA S2 O2 N2 C10 MPLA C11 > C16 TEMP -173.00 WGHT 0.028400 0.398800 FVAR 6.10356 CL1 6 0.231162 0.891329 0.550376 11.00000 0.01333 0.02159 = 0.02477 -0.00565 -0.00242 -0.00352 S1 5 0.725515 0.495781 0.392080 11.00000 0.01745 0.01851 = 0.02229 -0.00954 0.00162 -0.00797 O1 4 0.881235 0.692557 0.425034 11.00000 0.01456 0.01740 = 0.01818 -0.00523 0.00317 -0.00805 N1 3 0.609766 0.680176 0.513021 11.00000 0.01460 0.01638 = 0.01889 -0.00489 0.00191 -0.00809 H1N 2 0.516058 0.639480 0.527525 11.00000 -1.20000 C1 1 0.741236 0.627872 0.445024 11.00000 0.01301 0.01352 = 0.01540 0.00029 -0.00238 -0.00303 C2 1 0.617234 0.781605 0.569519 11.00000 0.01488 0.01172 = 0.01327 -0.00131 0.00323 -0.00670 C3 1 0.446474 0.883204 0.593694 11.00000 0.01133 0.01480 = 0.01329 0.00085 -0.00007 -0.00526 C4 1 0.444661 0.978118 0.653091 11.00000 0.01983 0.01383 = 0.01711 -0.00283 0.00348 -0.00439 AFIX 43 H4 2 0.327708 1.047192 0.668558 11.00000 -1.20000 AFIX 0 C5 1 0.612951 0.972225 0.689777 11.00000 0.02353 0.01933 = 0.01629 -0.00629 0.00144 -0.00983 AFIX 43 H5 2 0.612315 1.037098 0.730606 11.00000 -1.20000 AFIX 0 C6 1 0.783155 0.871092 0.666757 11.00000 0.01674 0.02386 = 0.01787 -0.00223 -0.00211 -0.00964 AFIX 43 H6 2 0.898751 0.866329 0.692546 11.00000 -1.20000 AFIX 0 C7 1 0.786070 0.777091 0.606569 11.00000 0.01247 0.01537 = 0.01683 -0.00196 0.00096 -0.00372 AFIX 43 H7 2 0.903895 0.709248 0.590527 11.00000 -1.20000 AFIX 0 C8 1 1.036860 0.644334 0.353948 11.00000 0.01488 0.01898 = 0.01499 -0.00614 0.00320 -0.00511 AFIX 23 H8A 2 0.982825 0.647366 0.295299 11.00000 -1.20000 H8B 2 1.112483 0.546295 0.372766 11.00000 -1.20000 AFIX 0 C9 1 1.163579 0.742734 0.342782 11.00000 0.02132 0.02583 = 0.02104 -0.00819 0.00327 -0.01224 AFIX 137 H9A 2 1.085497 0.839749 0.326765 11.00000 -1.50000 H9B 2 1.267874 0.716838 0.293665 11.00000 -1.50000 H9C 2 1.219996 0.735783 0.400636 11.00000 -1.50000 AFIX 0 CL2 6 1.288957 0.215588 0.849076 11.00000 0.01382 0.02312 = 0.03038 -0.01084 0.00074 -0.00555 S2 5 0.758354 0.652212 0.927063 11.00000 0.01957 0.01403 = 0.02341 -0.00532 -0.00548 -0.00449 O2 4 0.665774 0.475956 0.832977 11.00000 0.01827 0.01431 = 0.01704 -0.00374 -0.00756 -0.00110 N2 3 0.899710 0.377101 0.924272 11.00000 0.01412 0.01465 = 0.01852 -0.00570 -0.00535 -0.00237 H2N 2 0.984498 0.387581 0.957437 11.00000 -1.20000 C10 1 0.772812 0.497357 0.892684 11.00000 0.01331 0.01727 = 0.01341 -0.00493 0.00326 -0.00463 C11 1 0.909028 0.239077 0.905905 11.00000 0.01816 0.01306 = 0.01124 -0.00185 -0.00468 -0.00263 C12 1 1.086195 0.151442 0.874176 11.00000 0.01330 0.01813 = 0.01368 -0.00207 -0.00292 -0.00582 C13 1 1.102883 0.013328 0.862311 11.00000 0.02032 0.01595 = 0.01477 -0.00190 -0.00226 -0.00155 AFIX 43 H13 2 1.224907 -0.046100 0.841917 11.00000 -1.20000 AFIX 0 C14 1 0.942432 -0.037398 0.880130 11.00000 0.02543 0.01235 = 0.01814 -0.00151 -0.00584 -0.00530 AFIX 43 H14 2 0.953272 -0.131839 0.871538 11.00000 -1.20000 AFIX 0 C15 1 0.763913 0.049279 0.910761 11.00000 0.02003 0.01938 = 0.01686 0.00284 -0.00446 -0.01029 AFIX 43 H15 2 0.652876 0.014204 0.922426 11.00000 -1.20000 AFIX 0 C16 1 0.747971 0.186721 0.924263 11.00000 0.01396 0.01915 = 0.01348 -0.00239 -0.00106 -0.00190 AFIX 43 H16 2 0.626463 0.245165 0.946138 11.00000 -1.20000 AFIX 0 C17 1 0.524553 0.594107 0.787291 11.00000 0.01911 0.01547 = 0.01593 0.00121 -0.00690 -0.00165 AFIX 23 H17A 2 0.517943 0.575720 0.724026 11.00000 -1.20000 H17B 2 0.566866 0.681019 0.782851 11.00000 -1.20000 AFIX 0 C18 1 0.327008 0.615478 0.839296 11.00000 0.02115 0.02238 = 0.03099 -0.00458 -0.00348 -0.00162 AFIX 137 H18A 2 0.291084 0.526443 0.849551 11.00000 -1.50000 H18B 2 0.231794 0.687260 0.803542 11.00000 -1.50000 H18C 2 0.329209 0.646681 0.898739 11.00000 -1.50000 AFIX 0 HKLF 4 REM 15 REM R1 = 0.0364 for 3653 Fo > 4sig(Fo) and 0.0544 for all 4637 data REM 243 parameters refined using 2 restraints END WGHT 0.0269 0.4206 REM Highest difference peak 0.384, deepest hole -0.339, 1-sigma level 0.069 Q1 1 0.7957 0.5667 0.9052 11.00000 0.05 0.38 ; _shelx_res_checksum 62859 _shelx_hkl_file ; 0 0 2 110638. 1533.99 5 0 0 -2 113765. 1525.93 2 0 0 -3 86608.9 1645.35 2 0 0 3 88803.7 1684.38 5 0 0 -4 684338. 5357.51 2 0 0 4 686431. 5284.62 2 0 0 4 697606. 5447.23 5 0 0 -5 18840.0 1013.90 2 0 0 5 19457.0 682.352 3 0 0 5 19484.3 1036.73 5 0 0 5 17597.1 965.832 2 0 0 -6 32465.2 1450.08 2 0 0 6 31452.3 936.464 3 0 0 6 32436.2 1466.48 5 0 0 6 31841.7 1412.64 2 0 0 7 3315.26 554.833 5 0 0 7 2225.61 450.299 2 0 0 -7 3348.22 534.257 2 0 0 7 3649.78 351.442 3 0 0 8 29406.2 1639.04 5 0 0 8 27813.1 999.749 3 0 0 -8 27479.5 1556.66 2 0 0 8 26934.4 1519.86 2 0 0 -9 801.828 339.459 2 0 0 9 61.8804 248.991 5 0 0 9 286.853 151.720 3 0 0 9 345.193 269.575 2 0 0 -10 9162.85 1045.11 2 0 0 10 8073.23 605.599 3 0 0 10 7607.56 966.750 2 0 0 10 8294.58 1017.39 5 0 0 11 542.840 386.342 5 0 0 11 694.527 202.840 3 0 0 -11 1169.11 512.918 2 0 0 12 14535.7 857.479 3 0 0 -12 15125.3 1480.34 2 0 0 12 14929.3 1476.43 5 0 0 13 31306.6 2245.91 5 0 0 13 28310.0 1226.39 3 0 0 -14 6668.52 1125.51 2 0 0 14 6640.66 1165.44 5 0 0 15 5476.52 1090.02 5 0 0 -15 4989.55 1048.36 2 0 0 -16 2807.52 819.785 2 0 0 16 2890.45 857.324 5 0 0 17 6469.72 1325.88 5 0 0 -17 8698.66 1392.10 2 0 0 -18 2753.65 938.022 2 0 0 18 2763.62 1003.92 5 0 1 -18-460.834 619.225 2 0 -1 18-859.059 884.360 5 0 1 -17 307.232 498.094 2 0 -1 17-628.348 570.613 5 0 -1 16 2561.89 966.486 5 0 1 -16 2474.65 819.758 2 0 1 -15 4898.47 927.774 2 0 -1 15 5075.19 1128.28 5 0 -1 14 674.819 570.795 5 0 1 -14-173.168 263.836 2 0 1 -13 3201.03 814.796 2 0 -1 13 1944.44 699.703 5 0 -1 13 1762.41 402.267 3 0 1 -12 8312.87 1069.74 2 0 -1 12 8778.31 785.330 3 0 -1 12 9020.10 1198.37 5 0 -1 11 3213.00 707.344 5 0 -1 11 3629.68 510.229 3 0 -1 11 2738.28 576.373 2 0 1 -11 2051.92 536.942 2 0 -1 10 22773.6 1660.09 5 0 -1 10 26447.3 1627.74 2 0 -1 10 27558.2 1282.40 3 0 1 -10 26361.0 1669.48 2 0 -1 9 28944.6 1761.59 5 0 -1 9 29811.8 1288.53 3 0 -1 9 29463.0 1604.55 2 0 1 -9 30689.0 1694.28 2 0 -1 8 8384.00 666.735 3 0 -1 8 6730.73 747.787 2 0 -1 8 7832.37 876.981 5 0 1 -8 7629.46 816.439 2 0 -1 7 50715.4 2016.77 5 0 1 -7 51970.6 1897.29 2 0 -1 7 48076.3 1502.27 3 0 -1 7 52043.4 1847.26 2 0 -1 6 33384.1 1354.39 2 0 -1 6 31148.3 1143.07 3 0 -1 6 31128.2 1460.25 5 0 1 -6 31623.5 1353.64 2 0 -1 5 480.450 242.912 5 0 -1 5 297.207 149.418 3 0 1 -5 255.310 180.654 2 0 -1 5 424.248 202.210 2 0 1 -4 16411.5 762.828 2 0 -1 4 16662.7 898.759 5 0 -1 4 15133.0 722.706 2 0 -1 4 15121.5 703.439 3 0 -1 3 16.7149 94.5655 2 0 -1 3 173.376 125.527 3 0 1 -3 458.133 171.707 3 0 1 -3-41.8056 114.957 2 0 -1 3 10.3136 152.611 5 0 1 -2 102843. 1201.73 2 0 1 -2 104268. 1521.48 4 0 -1 2 99324.2 1581.32 5 0 -1 2 100676. 1160.02 2 0 1 -2 99710.7 1523.62 3 0 -1 1 29541.3 681.196 5 0 1 -1 29697.6 652.234 4 0 1 -1 28252.3 750.841 3 0 1 1 1718.62 169.414 3 0 -1 -1 1950.72 189.476 2 0 1 1 1686.53 177.999 6 0 1 1 1315.72 174.381 7 0 1 2 61722.9 1110.11 5 0 -1 -2 59414.4 1278.40 2 0 1 2 60157.5 1126.09 6 0 1 2 59731.3 928.819 3 0 1 3 5292.83 413.123 5 0 -1 -3 5257.72 469.020 2 0 1 4 16606.6 834.900 5 0 -1 -4 17463.8 938.270 2 0 -1 -5 291517. 4173.36 2 0 1 5 288242. 3870.43 5 0 -1 -6 1728.95 397.709 2 0 1 6 1850.56 358.429 5 0 1 7 22327.5 1301.26 5 0 1 7 20928.0 1304.46 2 0 -1 -7 23354.0 1396.69 2 0 -1 -7 21957.3 1287.41 5 0 1 8 3618.46 615.148 5 0 -1 -8 3596.92 601.120 5 0 -1 -8 4841.09 718.270 2 0 1 8 4936.31 715.741 2 0 1 9 121075. 1881.60 3 0 -1 -9 122432. 3588.66 2 0 -1 -9 127852. 3509.18 5 0 1 9 122319. 3453.13 5 0 1 9 124110. 3568.12 2 0 -1 -10 6840.71 943.181 2 0 1 10 8004.40 1008.50 2 0 1 10 7290.73 490.180 3 0 -1 -10 8696.37 999.063 5 0 1 10 6560.69 867.535 5 0 1 11 11525.2 623.913 3 0 -1 -11 10738.9 1223.41 2 0 1 11 11697.0 1219.05 5 0 1 12 747.617 393.082 5 0 1 12 485.603 178.170 3 0 -1 -12 798.348 509.951 2 0 1 13 4414.45 405.335 3 0 -1 -13 4118.50 845.657 2 0 1 13 5457.04 993.788 5 0 1 14 1911.19 623.369 5 0 -1 -14 2116.56 769.993 2 0 1 14 677.672 174.776 3 0 1 15 7339.76 1271.53 5 0 -1 -15 8757.69 1343.43 2 0 -1 -16-8.42590 189.534 2 0 1 16 1074.76 588.581 5 0 1 17 5.95341 526.184 5 0 -1 -17-100.397 573.972 2 0 -1 -18 9996.79 1582.30 2 0 1 18 11096.0 1656.34 5 0 1 19 6333.35 1475.41 5 0 -1 -19 4095.97 1266.85 2 0 -2 18 8646.48 1551.58 5 0 2 -18 8184.63 1400.60 2 0 2 -18 9059.82 1492.36 4 0 2 -17 1778.39 766.603 2 0 -2 17 2658.37 984.194 5 0 2 -16-621.713 616.771 2 0 -2 16-418.003 476.701 5 0 -2 15 7509.10 1346.77 5 0 2 -15 7402.06 1121.90 2 0 -2 14 16658.9 1812.49 5 0 2 -14 13668.9 1447.55 2 0 -2 13-473.829 322.294 3 0 -2 13 185.943 429.221 5 0 2 -13-737.820 392.095 2 0 2 -12 2535.46 610.083 2 0 -2 12 89.0555 91.0434 3 0 -2 12 1546.06 628.327 5 0 -2 12 2250.55 667.586 2 0 -2 11-315.525 473.987 5 0 -2 11-578.035 325.267 2 0 2 -11 55.6998 275.224 2 0 -2 11 105.931 129.667 3 0 -2 10 57231.0 2270.32 2 0 -2 10 58238.9 2696.64 5 0 2 -10 53267.6 2270.50 2 0 -2 10 52836.8 2034.78 3 0 2 -9 388.831 301.871 2 0 -2 9 384.227 252.751 3 0 -2 9 215.364 303.724 5 0 -2 9 454.802 296.008 2 0 2 -9-28.4559 248.845 5 0 -2 8 5847.10 656.183 3 0 2 -8 5054.39 635.266 2 0 -2 8 5911.45 655.812 2 0 -2 8 5863.02 795.755 5 0 -2 7 11931.8 1041.33 5 0 -2 7 12029.5 836.182 2 0 2 -7 11253.0 846.609 2 0 -2 7 11866.8 881.143 3 0 -2 6 6838.89 585.057 2 0 2 -6 7966.92 655.162 2 0 2 -6 5715.73 679.130 5 0 -2 6 6450.45 720.644 5 0 -2 6 6974.75 655.115 3 0 -2 5 20022.3 854.608 2 0 2 -5 19516.5 1110.46 5 0 2 -5 19596.1 1041.62 4 0 2 -5 19954.1 890.156 2 0 2 -5 19034.5 1006.02 3 0 -2 5 18909.6 1017.45 3 0 -2 5 17560.2 1052.68 5 0 -2 4 80442.4 2037.72 5 0 -2 4 77397.4 1416.13 2 0 2 -4 81653.8 1507.88 2 0 2 -4 75158.5 1959.94 5 0 2 -4 78340.1 1880.22 4 0 -2 4 74631.4 1921.52 3 0 2 -4 75913.6 1905.93 3 0 2 -3 45689.3 1300.54 4 0 -2 3 45791.9 860.673 2 0 2 -3 47426.8 1440.75 3 0 -2 3 48013.6 1418.50 5 0 -2 3 45745.8 1439.68 3 0 2 -3 46728.6 907.556 2 0 2 -3 46190.1 1385.51 5 0 2 -2 653242. 5109.53 3 0 -2 2 641091. 4333.98 4 0 -2 2 649414. 4538.76 5 0 2 -2 647100. 4300.21 4 0 2 -2 636722. 4526.42 5 0 2 -1 498.633 133.466 5 0 2 -1 407.139 143.341 4 0 -2 1 398.292 145.669 5 0 -2 1 265.452 121.457 4 0 2 -1 376.693 199.612 3 0 -2 0 205.595 75.3679 2 0 2 0 154.133 76.8459 2 0 2 0 114.589 161.864 6 0 -2 0 355.717 128.238 4 0 2 0 41.8175 155.929 3 0 2 0 291.663 128.362 4 0 -2 0 160.802 98.7564 5 0 2 0 271.962 95.6859 5 0 -2 -1 492.349 157.291 2 0 2 1 307.466 145.229 3 0 2 1 643.202 201.675 7 0 2 1 228.012 113.638 2 0 2 1 358.279 191.264 6 0 2 2 264986. 3048.45 6 0 2 2 270113. 2865.94 3 0 2 2 273275. 3323.14 7 0 -2 -2 270779. 3044.47 2 0 -2 -2 266965. 2943.37 3 0 -2 -3 7304.47 488.515 3 0 2 3 7224.48 473.011 3 0 -2 -3 7322.47 543.626 6 0 2 3 7157.26 543.565 6 0 -2 -3 7169.71 594.609 2 0 2 3 6093.24 562.634 7 0 -2 -3 6532.71 451.771 5 0 2 4 11405.8 717.958 6 0 2 4 11857.2 592.734 3 0 -2 -4 12714.8 864.354 2 0 2 4 10966.8 797.280 7 0 2 4 12386.8 717.086 5 0 -2 -4 11886.7 694.117 5 0 2 5 3592.13 329.031 3 0 2 5 4185.24 496.121 5 0 -2 -5 3831.56 456.039 5 0 -2 -5 4215.27 561.749 2 0 2 5 3596.76 444.341 6 0 2 6 21227.6 790.452 3 0 2 6 23373.7 1206.75 5 0 -2 -6 21739.7 1327.87 2 0 -2 -6 22721.9 1182.59 5 0 2 7 12639.2 975.853 5 0 2 7 11735.8 612.475 3 0 -2 -7 12033.9 1062.75 2 0 -2 -7 13834.0 1007.69 5 0 -2 -8 13108.0 1055.96 5 0 -2 -8 12738.3 1153.33 2 0 2 8 12752.8 647.724 3 0 2 8 12725.7 1051.68 5 0 2 9-1.68617 95.0638 3 0 -2 -9-203.673 280.523 2 0 2 9 231.150 265.444 5 0 -2 -9 62.2892 310.822 5 0 -2 -10 311.741 396.144 2 0 2 10 608.116 383.654 5 0 2 10 684.029 169.748 3 0 -2 -10 801.178 430.951 5 0 2 11 2102.97 264.365 3 0 2 11 3393.00 666.505 5 0 -2 -11 2116.15 610.280 2 0 -2 -12 86262.9 3638.28 2 0 2 12 84566.0 3386.15 5 0 2 12 84843.1 1416.47 3 0 2 13 1627.61 208.687 3 0 2 13 1937.25 630.258 5 0 -2 -13 1989.87 681.637 2 0 -2 -14 41387.2 2785.73 2 0 2 14 42241.1 2661.66 5 0 2 15 18334.3 1922.52 5 0 -2 -15 18821.9 1962.80 2 0 2 16 1996.04 726.342 5 0 -2 -16 556.912 683.097 2 0 -2 -17 10038.7 1575.99 2 0 2 17 11431.8 1644.09 5 0 2 18-31.9900 270.139 5 0 -2 -18 807.584 721.601 2 0 -2 -19 636.911 627.157 2 0 2 19 830.290 581.778 5 0 3 -17 899.171 750.450 4 0 3 -17 2105.12 668.419 2 0 3 -16 8903.78 1265.22 2 0 -3 16 7805.05 1493.21 5 0 3 -16 7762.37 1323.88 4 0 -3 15 322.205 591.674 5 0 3 -15-260.100 431.851 4 0 3 -15 569.640 439.393 2 0 -3 14 31792.5 2524.53 5 0 3 -14 35558.2 2206.17 2 0 3 -14 31673.7 2237.98 4 0 -3 13 5590.36 1023.06 5 0 -3 13 4750.93 807.666 3 0 3 -13 5651.40 883.972 2 0 3 -13 4819.42 919.045 4 0 3 -12 1685.03 523.827 2 0 -3 12 1434.77 626.299 5 0 3 -12 1135.12 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2 -1 7 11 971.818 333.390 3 -1 7 11 168.811 468.374 6 1 -7 -11 149.827 452.863 2 -1 7 10 1465.92 657.569 6 -1 7 10 1503.63 414.961 3 1 -7 -10 414.935 496.795 2 -1 7 9 41354.1 2012.82 3 1 -7 -9 40353.1 2612.20 2 -1 7 9 44639.1 2701.36 6 1 -7 -9 40217.3 1857.75 5 -1 7 8 8877.01 955.776 3 -1 7 8 7339.65 1179.97 6 1 -7 -8 7324.53 1020.40 3 1 -7 -8 8370.58 1265.94 2 1 -7 -8 8538.85 823.874 5 1 -7 -7 42340.0 2473.99 2 1 -7 -7 44473.3 1663.74 5 1 -7 -7 45461.3 2789.04 7 -1 7 7 43472.6 2605.87 6 -1 7 7 43538.6 2163.74 3 1 -7 -7 41249.4 2258.65 3 1 -7 -6 2252.71 385.037 5 -1 7 6 2836.12 788.279 6 1 -7 -6 3176.35 713.338 3 1 -7 -6 2313.77 671.252 2 1 -7 -6 2163.07 730.738 7 -1 7 6 2542.19 584.317 3 1 -7 -5 32383.2 2328.44 7 -1 7 5 39103.6 2109.13 3 1 -7 -5 31059.7 1901.54 2 1 -7 -5 35291.8 1230.71 5 1 -7 -5 34174.8 1263.03 5 -1 7 5 29077.2 2128.97 6 1 -7 -4 18178.2 835.055 5 1 -7 -4 17147.1 771.573 5 1 -7 -4 16175.7 1638.96 7 -1 7 4 18346.3 1491.88 3 -1 7 4 18612.5 1701.51 6 1 -7 -4 16710.3 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2490.84 5 -1 6 10 61806.6 2087.20 3 1 -6 -10 57242.5 3133.34 2 -1 6 10 58263.1 1530.09 1 -1 6 10 55317.2 2904.64 6 1 -6 -9 486.295 606.411 2 -1 6 9 419.725 414.352 6 -1 6 9 1280.22 407.564 3 1 -6 -9 762.943 337.462 5 -1 6 9 659.246 145.182 1 1 -6 -8 45202.1 2081.77 3 1 -6 -8 45400.6 1842.07 5 -1 6 8 46310.3 1955.36 3 -1 6 8 44027.3 2490.53 6 1 -6 -8 44589.7 2529.29 2 -1 6 8 41795.2 743.040 1 -1 6 7 187462. 4011.69 3 1 -6 -7 174831. 4805.04 2 -1 6 7 190679. 5065.85 6 1 -6 -7 184378. 4265.53 3 1 -6 -7 174044. 3322.80 5 -1 6 6 7870.14 885.407 3 1 -6 -6 8160.69 1000.26 2 1 -6 -6 7732.24 937.371 3 -1 6 6 8442.02 1096.64 6 1 -6 -6 8363.30 679.117 5 1 -6 -6 7057.50 1069.34 7 -1 6 6 9533.83 1060.13 2 -1 6 5 36916.4 2193.36 6 1 -6 -5 38462.7 1289.21 5 1 -6 -5 39139.0 2046.90 3 1 -6 -5 40574.7 2337.71 7 1 -6 -5 36969.0 1994.99 2 -1 6 5 38734.1 1923.32 3 -1 6 4 1152.35 418.905 3 -1 6 4 410.962 427.267 6 1 -6 -4 761.758 194.052 5 1 -6 -4 1201.04 363.908 3 1 -6 -4 779.595 449.054 7 1 -6 -4 1122.66 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2904.75 748.571 4 1 -6 15 1017.57 814.476 5 -1 6 -15 454.874 293.360 4 1 -5 -17 409.321 676.479 2 -1 5 17 506.581 768.246 6 -1 5 16 10033.5 1533.10 6 1 -5 -16 13603.5 1958.97 2 -1 5 15 11946.2 1541.70 6 1 -5 -15 11313.6 1712.68 2 1 -5 -14 296.794 540.926 2 -1 5 14 345.579 487.126 6 -1 5 13 479.093 388.131 6 1 -5 -13 41.9863 513.667 2 -1 5 12 3325.08 827.752 6 -1 5 12 1360.56 392.035 1 1 -5 -12 3304.21 920.557 2 1 -5 -11 443.299 489.587 2 -1 5 11 60.4089 264.056 1 -1 5 11 286.810 439.684 6 -1 5 10 695.989 225.090 3 -1 5 10 744.801 445.864 6 -1 5 10 924.414 325.179 1 1 -5 -10 698.421 363.990 5 -1 5 9 64636.9 1918.80 3 -1 5 9 66935.4 1816.82 1 1 -5 -9 66063.7 2406.05 5 1 -5 -9 62922.1 3060.81 2 -1 5 9 65789.3 2938.46 6 -1 5 8 4109.99 541.375 3 1 -5 -8 4059.13 596.121 5 1 -5 -8 4851.14 844.549 2 -1 5 8 4662.49 828.298 6 -1 5 8 3504.25 385.240 1 -1 5 7 568.362 377.354 6 -1 5 7 357.822 268.490 2 1 -5 -7 854.384 470.822 2 -1 5 7 598.539 162.457 1 1 -5 -7 698.056 281.943 5 1 -5 -7 812.407 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1 -4 -3 139.668 115.407 5 1 -4 -3 71.0460 74.0875 1 -1 4 3 184.060 219.740 7 1 -4 -3 149.819 296.042 7 1 -4 -3-73.6297 215.585 2 -1 4 2 5073.75 605.271 3 1 -4 -2 5173.84 299.979 5 1 -4 -2 5312.21 620.554 4 -1 4 2 4456.62 642.591 6 1 -4 -2 5698.06 653.767 3 1 -4 -2 5437.73 294.626 5 1 -4 -2 4922.31 316.408 1 1 -4 -2 5655.72 583.579 2 1 -4 -2 4360.29 653.809 7 1 -4 -1 5937.75 411.891 1 -1 4 1 5437.73 639.407 4 1 -4 -1 5949.39 538.855 2 1 -4 -1 5614.95 625.137 4 1 -4 -1 5216.56 263.273 5 1 -4 -1 5599.69 731.067 7 -1 4 1 6223.44 684.062 3 1 -4 -1 5727.74 666.051 3 -1 4 1 5720.45 731.221 6 1 -4 0 2887.00 465.848 4 1 -4 0 2737.49 221.896 5 1 -4 0 2521.18 318.792 1 -1 4 0 3274.70 533.002 3 -1 4 0 2491.48 459.904 4 1 -4 0 2655.51 323.376 2 -1 4 0 3172.16 541.027 6 1 -4 0 2160.48 444.006 3 -1 4 -1 2329.56 517.197 6 1 -4 1 3380.03 299.199 5 1 -4 1 2858.55 383.143 1 -1 4 -1 2781.15 296.360 5 -1 4 -1 2624.44 497.079 3 1 -4 1 2450.85 419.098 4 1 -4 1 2219.11 249.262 2 -1 4 -1 2492.15 431.136 4 1 -4 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45225.3 2055.33 2 -4 3 -6 44865.6 2390.65 4 -4 3 -7 3646.47 786.775 4 4 -3 7 3485.62 632.664 2 4 -3 7 2377.08 683.028 1 4 -3 7 2927.81 644.192 6 -4 3 -8 5434.74 959.846 4 4 -3 8 5129.47 774.718 2 4 -3 8 6998.64 971.817 6 4 -3 8 6535.16 1064.59 1 -4 3 -8 5147.78 746.389 5 -4 3 -9 3021.96 766.861 4 4 -3 9 2767.76 613.773 2 4 -3 9 3158.67 676.993 6 4 -3 9 2838.00 758.175 1 -4 3 -10 852.458 459.158 4 4 -3 10 767.790 499.534 1 -4 3 -11 60.4474 351.481 4 4 -3 11-563.752 666.924 1 -4 3 -12 1483.28 750.900 4 4 -3 12 1755.87 809.872 1 -4 3 -13 11966.3 1593.14 4 4 -3 13 13863.8 1811.35 1 4 -3 14 4171.61 1043.00 1 -4 3 -14 3929.04 944.351 4 4 -3 15-30.2421 502.276 1 -4 3 -15-296.172 442.298 4 4 -2 -15 17431.7 2311.46 2 -4 2 15 18081.1 2017.92 5 4 -2 -14 878.415 728.443 2 -4 2 14-626.258 596.627 5 4 -2 -13 3629.01 1008.56 2 -4 2 13 1526.38 636.930 5 4 -2 -12 10788.8 1651.57 2 -4 2 12 9717.21 1267.04 5 -4 2 11 18643.8 1655.96 5 4 -2 -11 20223.8 2095.24 2 4 -2 -10-314.542 633.504 2 -4 2 10 368.445 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-8 -7 5 606.839 681.527 5 8 7 -4 1218.55 651.430 3 -8 -7 4 589.720 396.381 5 8 7 -3 960.689 484.123 3 -8 -7 3 941.472 626.692 5 8 7 -2 2412.34 984.521 3 8 7 -2 6041.60 1170.90 1 -8 -7 2 5582.96 1151.36 5 8 7 -1 4096.15 1049.51 1 8 7 -1 3617.23 1247.81 3 -8 -7 1 5926.15 1384.62 5 8 7 0 502.322 406.788 1 8 7 0 176.810 614.379 3 -8 -7 0-912.762 747.816 5 8 7 1 14016.5 1830.50 1 8 7 1 15395.1 2066.16 3 -8 -7 -1 13689.0 1819.51 5 8 7 2 1878.55 791.022 1 -8 -7 -2 2757.91 976.616 5 -8 -7 -3 33249.1 2808.43 5 8 7 3 34206.6 2719.23 1 8 7 4 1385.57 570.529 1 -8 -7 -4-177.535 494.335 5 8 7 5 7268.58 1276.85 1 -8 -7 -5 8854.83 1534.98 5 8 7 6-198.002 340.951 1 -8 -7 -6-937.119 762.836 5 -8 -7 -7 39490.1 3090.60 5 8 7 7 36484.1 2830.89 1 8 7 8 18629.4 1989.88 1 -8 -7 -8 14769.0 1943.66 5 8 7 9 2309.94 1023.56 1 8 7 10 266.634 445.981 1 8 7 11-209.806 476.127 1 8 8 -3 60545.5 4013.49 3 -8 -8 3 69425.8 4292.87 5 8 8 -2 334.423 522.584 3 -8 -8 2 725.488 556.002 5 8 8 -1 2851.61 1125.19 3 8 8 -1 5734.13 1297.30 1 -8 -8 1 4359.40 1162.99 5 8 8 0 4647.60 1164.98 1 8 8 0 5031.39 1266.29 3 -8 -8 0 3782.98 1112.60 5 8 8 1 6630.97 1387.40 1 8 8 1 11312.3 1894.78 3 -8 -8 -1 9108.67 1569.95 5 8 8 2 666.379 573.161 1 -8 -8 -2 158.351 351.373 5 8 8 3 341.537 563.623 1 8 8 3 709.292 858.154 3 -8 -8 -3 860.954 586.413 5 8 8 4 1181.46 703.493 1 8 8 4 625.312 837.619 3 -8 -8 -4 967.374 719.370 5 8 8 5 2147.76 868.097 1 8 8 5 1692.18 993.184 3 -8 -8 -5 2049.92 987.843 5 8 8 6 5060.63 1154.58 1 -8 -8 -6 5513.85 1333.80 5 8 8 7 4659.18 1097.35 1 -8 -8 -7 2221.98 980.355 5 8 8 8 694.024 431.631 1 -8 -8 -8-806.997 530.314 5 8 8 9 462.912 353.345 1 -8 -8 -9-1554.54 880.047 5 8 9 -1 75.0550 727.049 3 -8 -9 1-485.672 786.303 5 8 9 0 2218.06 994.830 3 -8 -9 0 1779.75 769.444 5 8 9 1 2685.69 784.175 1 8 9 1 1053.56 774.902 3 -8 -9 -1 1565.61 675.248 5 8 9 2 17604.0 2045.73 1 8 9 2 19835.2 2493.54 3 -8 -9 -2 17213.3 2222.59 5 8 9 3 9738.99 1590.01 1 8 9 3 10010.9 1827.64 3 -8 -9 -3 11425.3 1889.25 5 8 9 4-534.386 584.173 1 8 9 4-735.514 891.144 3 -8 -9 -4-1829.44 1076.19 5 8 9 5 30738.7 3027.76 3 -8 -9 -5 26294.4 2657.91 5 8 9 5 26545.2 2459.53 1 8 9 6-249.921 487.813 1 8 9 6-1168.41 997.726 3 -8 -9 -6 165.346 471.458 5 8 9 7 423.210 748.668 3 8 9 7 1225.24 749.739 1 -8 -9 -7 1825.54 753.827 5 -9 0 -1 1440.88 881.815 6 9 0 1 954.567 765.134 1 -9 0 -2 5253.08 1048.60 6 9 0 2 2310.45 1134.25 1 -9 -1 1 5700.24 1335.32 6 9 1 -1 7109.67 1393.46 1 -9 -1 0 4885.22 1128.18 6 9 1 0 4646.90 1206.02 1 -9 -1 -1 43410.6 3062.26 6 9 1 1 40726.6 3245.99 1 -9 -1 -2-837.659 801.710 6 9 1 2 883.600 767.654 1 -9 -1 -3 1733.16 745.269 6 -9 -1 -3 402.488 545.814 5 9 1 3 934.121 816.454 1 -9 -1 -3 262.178 502.329 4 9 1 4-711.299 735.300 1 -9 -1 -4 594.062 551.124 4 -9 -1 -5 17476.4 1836.30 5 -9 -1 -5 15630.9 1689.70 4 9 1 5 18878.9 2212.66 1 9 2 -2-154.780 634.506 1 -9 -2 2 525.472 546.041 5 -9 -2 1 9676.56 1673.86 6 9 2 -1 10641.8 1879.53 1 -9 -2 1 8306.87 1307.57 5 -9 -2 0 24782.2 2337.23 6 -9 -2 0 26433.6 2254.36 5 -9 -2 -1 4450.05 1043.67 6 9 2 1 6936.64 1430.25 1 -9 -2 -1 3529.81 997.068 5 -9 -2 -2 13510.8 1659.94 6 9 2 2 15280.8 1938.66 1 -9 -2 -2 11550.9 1556.46 5 -9 -2 -3 19643.5 1923.23 6 -9 -2 -3 21682.5 2071.77 5 9 2 3 26226.7 2587.23 1 -9 -2 -3 23988.4 1937.65 4 -9 -2 -4 451.136 697.815 5 9 2 4 2061.71 720.655 1 -9 -2 -4 1167.24 522.956 4 -9 -2 -5 16580.7 1844.05 5 -9 -2 -5 15598.2 1623.10 4 9 2 5 15649.6 1996.90 1 -9 -2 -6 1406.53 863.453 5 9 2 6 2434.44 917.443 1 -9 -2 -6 2501.98 831.086 4 9 2 7 83.3277 594.652 1 -9 -2 -7 874.131 628.467 5 -9 -2 -7-634.291 480.990 4 9 3 -3 7662.35 1521.22 1 -9 -3 3 5838.09 1262.19 5 9 3 -2 6896.56 1416.49 1 -9 -3 2 3594.73 893.439 5 9 3 -1 201.696 648.276 1 -9 -3 1-332.056 374.425 5 9 3 0 1106.81 666.444 1 -9 -3 0 981.284 537.695 5 -9 -3 -1 123.477 602.023 6 9 3 1-140.660 522.587 1 -9 -3 -1 223.659 310.638 5 -9 -3 -2 19387.7 1919.45 6 9 3 2 20408.7 2288.43 1 -9 -3 -2 16036.0 1842.37 5 -9 -3 -3 1674.01 722.267 6 9 3 3 351.268 703.729 1 -9 -3 -3 716.724 801.345 5 -9 -3 -4 3230.85 1090.77 5 9 3 4 2550.97 938.294 1 -9 -3 -5 7368.02 1335.24 5 9 3 5 5600.33 1331.19 1 -9 -3 -6 6796.54 1355.88 5 9 3 6 10098.4 1673.87 1 -9 -3 -6 6744.46 1084.41 4 -9 -3 -7 2020.95 716.394 5 9 3 7 1750.56 864.267 1 -9 -3 -7 1332.07 502.902 4 9 4 -2 11573.3 1739.48 1 -9 -4 2 13346.7 1836.57 5 9 4 -1-1444.86 653.257 1 -9 -4 1-301.833 711.595 5 -9 -4 0 29084.0 2572.28 5 9 4 0 32481.1 2906.70 1 9 4 1 1244.26 771.572 1 -9 -4 -1 643.194 605.820 5 9 4 2-446.079 444.345 1 -9 -4 -2-807.565 615.735 5 9 4 3 294.080 364.646 1 -9 -4 -3 856.018 648.154 5 -9 -4 -4 19770.5 2086.93 5 9 4 4 22456.0 2349.05 1 -9 -4 -5 1696.06 831.974 5 9 4 5 4717.81 1194.01 1 -9 -4 -6 7144.84 1426.66 5 9 4 6 5547.50 1268.26 1 -9 -4 -7 11932.5 1723.71 5 9 4 7 11720.2 1837.07 1 -9 -4 -8 3873.45 1015.78 5 9 4 8 5337.43 1313.80 1 9 5 -2 1068.52 639.166 1 -9 -5 2-59.3528 559.212 5 9 5 -1 1144.05 821.161 1 -9 -5 1 3233.87 944.604 5 9 5 0 314.929 668.500 1 -9 -5 0-76.9743 609.899 5 9 5 1 365.326 369.999 1 -9 -5 -1 57.4484 545.726 5 9 5 2 13.7264 469.613 1 -9 -5 -2-643.138 670.417 5 9 5 3 6136.94 1309.99 1 -9 -5 -3 8156.36 1436.09 5 9 5 4 2859.66 956.902 1 -9 -5 -4 894.542 710.885 5 9 5 5 2165.25 983.807 1 -9 -5 -5 2705.28 970.734 5 -9 -5 -6 1271.14 821.534 5 9 5 6 3798.11 1103.55 1 -9 -5 -7 21497.7 2396.84 5 9 5 7 25730.5 2595.56 1 9 6 -1 17028.5 2134.05 1 9 6 -1 20044.8 2460.34 3 9 6 0 1542.75 999.914 1 -9 -6 0 1673.20 715.333 5 9 6 1 7975.46 1496.01 1 -9 -6 -1 6134.81 1294.12 5 -9 -6 -2 29728.6 2795.72 5 9 6 2 30814.0 2804.09 1 9 6 3 8425.29 1485.78 1 -9 -6 -3 5938.55 1440.22 5 9 6 4 2688.58 942.209 1 -9 -6 -4 3693.73 1306.26 5 9 6 5 395.247 330.817 1 -9 -6 -5-1185.65 855.149 5 9 6 6 4159.31 1083.02 1 -9 -6 -6 3216.18 1079.84 5 -9 -6 -7 2674.29 1019.91 5 9 6 7 2144.02 870.020 1 9 7 2 856.073 799.758 1 -9 -7 -2 276.129 667.776 5 9 7 3 4779.47 1242.21 1 -9 -7 -3 5332.72 1332.95 5 9 7 4 15958.4 2080.70 1 -9 -7 -4 14921.3 2079.45 5 9 7 5 2521.95 915.775 1 -9 -7 -5 3494.49 1021.12 5 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 33122 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 Cl1 Cl 0.23116(7) 0.89133(5) 0.55038(4) 0.01979(12) Uani 1 1 d . . . . . S1 S 0.72551(7) 0.49578(5) 0.39208(4) 0.01832(12) Uani 1 1 d . . . . . O1 O 0.88124(18) 0.69256(13) 0.42503(9) 0.0160(3) Uani 1 1 d . . . . . N1 N 0.6098(2) 0.68018(16) 0.51302(12) 0.0158(4) Uani 1 1 d D . . . . H1N H 0.516(2) 0.6395(19) 0.5275(14) 0.019 Uiso 1 1 d D U . . . C1 C 0.7412(3) 0.62787(18) 0.44502(13) 0.0142(4) Uani 1 1 d . . . . . C2 C 0.6172(3) 0.78160(18) 0.56952(13) 0.0131(4) Uani 1 1 d . . . . . C3 C 0.4465(3) 0.88320(18) 0.59369(13) 0.0132(4) Uani 1 1 d . . . . . C4 C 0.4447(3) 0.97812(19) 0.65309(14) 0.0174(4) Uani 1 1 d . . . . . H4 H 0.3277 1.0472 0.6686 0.021 Uiso 1 1 calc R U . . . C5 C 0.6130(3) 0.9722(2) 0.68978(14) 0.0187(4) Uani 1 1 d . . . . . H5 H 0.6123 1.0371 0.7306 0.022 Uiso 1 1 calc R U . . . C6 C 0.7832(3) 0.8711(2) 0.66676(14) 0.0186(4) Uani 1 1 d . . . . . H6 H 0.8988 0.8663 0.6925 0.022 Uiso 1 1 calc R U . . . C7 C 0.7861(3) 0.77709(19) 0.60657(13) 0.0151(4) Uani 1 1 d . . . . . H7 H 0.9039 0.7092 0.5905 0.018 Uiso 1 1 calc R U . . . C8 C 1.0369(3) 0.64433(19) 0.35395(14) 0.0162(4) Uani 1 1 d . . . . . H8A H 0.9828 0.6474 0.2953 0.019 Uiso 1 1 calc R U . . . H8B H 1.1125 0.5463 0.3728 0.019 Uiso 1 1 calc R U . . . C9 C 1.1636(3) 0.7427(2) 0.34278(15) 0.0214(5) Uani 1 1 d . . . . . H9A H 1.0855 0.8397 0.3268 0.032 Uiso 1 1 calc R U . . . H9B H 1.2679 0.7168 0.2937 0.032 Uiso 1 1 calc R U . . . H9C H 1.2200 0.7358 0.4006 0.032 Uiso 1 1 calc R U . . . Cl2 Cl 1.28896(7) 0.21559(5) 0.84908(4) 0.02177(13) Uani 1 1 d . . . . . S2 S 0.75835(7) 0.65221(5) 0.92706(4) 0.01836(12) Uani 1 1 d . . . . . O2 O 0.66577(19) 0.47596(13) 0.83298(9) 0.0165(3) Uani 1 1 d . . . . . N2 N 0.8997(2) 0.37710(16) 0.92427(11) 0.0153(3) Uani 1 1 d D . . . . H2N H 0.984(2) 0.388(2) 0.9574(13) 0.018 Uiso 1 1 d D U . . . C10 C 0.7728(3) 0.49736(19) 0.89268(13) 0.0147(4) Uani 1 1 d . . . . . C11 C 0.9090(3) 0.23908(18) 0.90591(13) 0.0141(4) Uani 1 1 d . . . . . C12 C 1.0862(3) 0.15144(19) 0.87418(13) 0.0145(4) Uani 1 1 d . . . . . C13 C 1.1029(3) 0.01333(19) 0.86231(14) 0.0177(4) Uani 1 1 d . . . . . H13 H 1.2249 -0.0461 0.8419 0.021 Uiso 1 1 calc R U . . . C14 C 0.9424(3) -0.03740(19) 0.88013(14) 0.0183(4) Uani 1 1 d . . . . . H14 H 0.9533 -0.1318 0.8715 0.022 Uiso 1 1 calc R U . . . C15 C 0.7639(3) 0.04928(19) 0.91076(14) 0.0180(4) Uani 1 1 d . . . . . H15 H 0.6529 0.0142 0.9224 0.022 Uiso 1 1 calc R U . . . C16 C 0.7480(3) 0.18672(19) 0.92426(13) 0.0161(4) Uani 1 1 d . . . . . H16 H 0.6265 0.2452 0.9461 0.019 Uiso 1 1 calc R U . . . C17 C 0.5246(3) 0.59411(19) 0.78729(14) 0.0173(4) Uani 1 1 d . . . . . H17A H 0.5179 0.5757 0.7240 0.021 Uiso 1 1 calc R U . . . H17B H 0.5669 0.6810 0.7829 0.021 Uiso 1 1 calc R U . . . C18 C 0.3270(3) 0.6155(2) 0.83930(16) 0.0255(5) Uani 1 1 d . . . . . H18A H 0.2911 0.5264 0.8496 0.038 Uiso 1 1 calc R U . . . H18B H 0.2318 0.6873 0.8035 0.038 Uiso 1 1 calc R U . . . H18C H 0.3292 0.6467 0.8987 0.038 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 Cl1 0.0133(2) 0.0216(2) 0.0248(3) -0.0057(2) -0.0024(2) -0.00352(19) S1 0.0175(3) 0.0185(2) 0.0223(3) -0.0095(2) 0.0016(2) -0.0080(2) O1 0.0146(7) 0.0174(7) 0.0182(7) -0.0052(5) 0.0032(6) -0.0080(5) N1 0.0146(8) 0.0164(8) 0.0189(9) -0.0049(7) 0.0019(7) -0.0081(7) C1 0.0130(9) 0.0135(9) 0.0154(10) 0.0003(7) -0.0024(8) -0.0030(7) C2 0.0149(9) 0.0117(9) 0.0133(10) -0.0013(7) 0.0032(8) -0.0067(7) C3 0.0113(9) 0.0148(9) 0.0133(10) 0.0009(7) -0.0001(8) -0.0053(7) C4 0.0198(10) 0.0138(9) 0.0171(11) -0.0028(8) 0.0035(8) -0.0044(8) C5 0.0235(11) 0.0193(10) 0.0163(10) -0.0063(8) 0.0014(9) -0.0098(8) C6 0.0167(10) 0.0239(10) 0.0179(11) -0.0022(8) -0.0021(8) -0.0096(8) C7 0.0125(9) 0.0154(9) 0.0168(10) -0.0020(8) 0.0010(8) -0.0037(7) C8 0.0149(9) 0.0190(10) 0.0150(10) -0.0061(8) 0.0032(8) -0.0051(8) C9 0.0213(11) 0.0258(11) 0.0210(11) -0.0082(9) 0.0033(9) -0.0122(9) Cl2 0.0138(2) 0.0231(3) 0.0304(3) -0.0108(2) 0.0007(2) -0.00555(19) S2 0.0196(3) 0.0140(2) 0.0234(3) -0.0053(2) -0.0055(2) -0.00449(19) O2 0.0183(7) 0.0143(6) 0.0170(7) -0.0037(5) -0.0076(6) -0.0011(5) N2 0.0141(8) 0.0146(8) 0.0185(9) -0.0057(7) -0.0053(7) -0.0024(6) C10 0.0133(9) 0.0173(9) 0.0134(10) -0.0049(8) 0.0033(8) -0.0046(8) C11 0.0182(10) 0.0131(9) 0.0112(10) -0.0019(7) -0.0047(8) -0.0026(7) C12 0.0133(9) 0.0181(9) 0.0137(10) -0.0021(8) -0.0029(8) -0.0058(7) C13 0.0203(10) 0.0160(9) 0.0148(10) -0.0019(8) -0.0023(8) -0.0015(8) C14 0.0254(11) 0.0124(9) 0.0181(11) -0.0015(8) -0.0058(9) -0.0053(8) C15 0.0200(10) 0.0194(10) 0.0169(10) 0.0028(8) -0.0045(8) -0.0103(8) C16 0.0140(9) 0.0192(10) 0.0135(10) -0.0024(8) -0.0011(8) -0.0019(8) C17 0.0191(10) 0.0155(9) 0.0159(10) 0.0012(8) -0.0069(8) -0.0017(8) C18 0.0212(11) 0.0224(11) 0.0310(13) -0.0046(9) -0.0035(10) -0.0016(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 C1 O1 C8 118.86(14) . . C1 N1 C2 127.78(16) . . C1 N1 H1N 114.7(14) . . C2 N1 H1N 117.1(14) . . O1 C1 N1 112.88(16) . . O1 C1 S1 124.60(14) . . N1 C1 S1 122.51(15) . . C7 C2 C3 118.66(17) . . C7 C2 N1 122.18(16) . . C3 C2 N1 119.01(17) . . C4 C3 C2 120.93(18) . . C4 C3 Cl1 118.75(14) . . C2 C3 Cl1 120.31(14) . . C5 C4 C3 119.89(18) . . C5 C4 H4 120.1 . . C3 C4 H4 120.1 . . C4 C5 C6 119.68(18) . . C4 C5 H5 120.2 . . C6 C5 H5 120.2 . . C7 C6 C5 120.60(18) . . C7 C6 H6 119.7 . . C5 C6 H6 119.7 . . C6 C7 C2 120.22(17) . . C6 C7 H7 119.9 . . C2 C7 H7 119.9 . . O1 C8 C9 106.42(15) . . O1 C8 H8A 110.4 . . C9 C8 H8A 110.4 . . O1 C8 H8B 110.4 . . C9 C8 H8B 110.4 . . H8A C8 H8B 108.6 . . C8 C9 H9A 109.5 . . C8 C9 H9B 109.5 . . H9A C9 H9B 109.5 . . C8 C9 H9C 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . C10 O2 C17 120.55(14) . . C10 N2 C11 125.83(16) . . C10 N2 H2N 115.0(13) . . C11 N2 H2N 119.1(13) . . O2 C10 N2 111.77(15) . . O2 C10 S2 126.09(14) . . N2 C10 S2 122.14(15) . . C16 C11 C12 119.04(17) . . C16 C11 N2 121.36(17) . . C12 C11 N2 119.48(17) . . C13 C12 C11 120.80(18) . . C13 C12 Cl2 119.37(14) . . C11 C12 Cl2 119.83(14) . . C14 C13 C12 119.77(18) . . C14 C13 H13 120.1 . . C12 C13 H13 120.1 . . C13 C14 C15 120.14(17) . . C13 C14 H14 119.9 . . C15 C14 H14 119.9 . . C16 C15 C14 120.09(18) . . C16 C15 H15 120.0 . . C14 C15 H15 120.0 . . C15 C16 C11 120.15(17) . . C15 C16 H16 119.9 . . C11 C16 H16 119.9 . . O2 C17 C18 110.98(16) . . O2 C17 H17A 109.4 . . C18 C17 H17A 109.4 . . O2 C17 H17B 109.4 . . C18 C17 H17B 109.4 . . H17A C17 H17B 108.0 . . C17 C18 H18A 109.5 . . C17 C18 H18B 109.5 . . H18A C18 H18B 109.5 . . C17 C18 H18C 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cl1 C3 1.7369(19) . S1 C1 1.6718(19) . O1 C1 1.329(2) . O1 C8 1.458(2) . N1 C1 1.343(2) . N1 C2 1.425(2) . N1 H1N 0.873(9) . C2 C7 1.390(3) . C2 C3 1.397(2) . C3 C4 1.384(3) . C4 C5 1.379(3) . C4 H4 0.9500 . C5 C6 1.387(3) . C5 H5 0.9500 . C6 C7 1.384(3) . C6 H6 0.9500 . C7 H7 0.9500 . C8 C9 1.503(3) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . Cl2 C12 1.7368(19) . S2 C10 1.6717(18) . O2 C10 1.327(2) . O2 C17 1.459(2) . N2 C10 1.343(2) . N2 C11 1.426(2) . N2 H2N 0.872(9) . C11 C16 1.387(3) . C11 C12 1.394(3) . C12 C13 1.385(3) . C13 C14 1.373(3) . C13 H13 0.9500 . C14 C15 1.392(3) . C14 H14 0.9500 . C15 C16 1.386(3) . C15 H15 0.9500 . C16 H16 0.9500 . C17 C18 1.501(3) . C17 H17A 0.9900 . C17 H17B 0.9900 . C18 H18A 0.9800 . C18 H18B 0.9800 . C18 H18C 0.9800 . 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 C8 O1 C1 N1 178.51(15) . . . . C8 O1 C1 S1 -1.8(2) . . . . C2 N1 C1 O1 -7.3(3) . . . . C2 N1 C1 S1 172.99(15) . . . . C1 N1 C2 C7 -43.0(3) . . . . C1 N1 C2 C3 141.49(19) . . . . C7 C2 C3 C4 0.2(3) . . . . N1 C2 C3 C4 175.91(17) . . . . C7 C2 C3 Cl1 -179.11(14) . . . . N1 C2 C3 Cl1 -3.4(2) . . . . C2 C3 C4 C5 -0.5(3) . . . . Cl1 C3 C4 C5 178.82(15) . . . . C3 C4 C5 C6 0.1(3) . . . . C4 C5 C6 C7 0.7(3) . . . . C5 C6 C7 C2 -1.0(3) . . . . C3 C2 C7 C6 0.5(3) . . . . N1 C2 C7 C6 -175.01(17) . . . . C1 O1 C8 C9 176.33(16) . . . . C17 O2 C10 N2 -177.28(15) . . . . C17 O2 C10 S2 2.7(3) . . . . C11 N2 C10 O2 -6.6(3) . . . . C11 N2 C10 S2 173.39(15) . . . . C10 N2 C11 C16 -54.7(3) . . . . C10 N2 C11 C12 129.3(2) . . . . C16 C11 C12 C13 -1.0(3) . . . . N2 C11 C12 C13 175.13(17) . . . . C16 C11 C12 Cl2 179.02(15) . . . . N2 C11 C12 Cl2 -4.9(3) . . . . C11 C12 C13 C14 1.4(3) . . . . Cl2 C12 C13 C14 -178.63(16) . . . . C12 C13 C14 C15 -0.5(3) . . . . C13 C14 C15 C16 -0.6(3) . . . . C14 C15 C16 C11 1.0(3) . . . . C12 C11 C16 C15 -0.2(3) . . . . N2 C11 C16 C15 -176.25(17) . . . . C10 O2 C17 C18 -93.4(2) . . . .