#------------------------------------------------------------------------------ #$Date: 2017-07-17 12:31:47 +0300 (Mon, 17 Jul 2017) $ #$Revision: 198757 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/21/2242106.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2242106 loop_ _publ_author_name 'Nur Adibah Binti Mohd Amin' 'Rusnah Syahila Duali Hussen' 'Lee, See Mun' 'Halcovitch, Nathan R.' 'Jotani, Mukesh M.' 'Tiekink, Edward R. T.' _publ_section_title ; trans-Dichloridobis(dimethyl sulfoxide-\kO)bis(4-fluorobenzyl-\kC^1^)tin(IV): crystal structure and Hirshfeld surface analysis ; _journal_coeditor_code WM5381 _journal_issue 5 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first 667 _journal_page_last 672 _journal_paper_doi 10.1107/S2056989017005072 _journal_volume 73 _journal_year 2017 _chemical_formula_iupac '[Sn (C7 H6 F)2 Cl2 (C2 H6 O S)2]' _chemical_formula_moiety 'C18 H24 Cl2 F2 O2 S2 Sn' _chemical_formula_sum 'C18 H24 Cl2 F2 O2 S2 Sn' _chemical_formula_weight 564.08 _chemical_name_systematic ; trans-Dichloridobis(dimethyl sulfoxide-\kO)bis(4-fluorobenzyl-\kC^1^)tin(IV) ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 110.391(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.23630(10) _cell_length_b 12.7020(2) _cell_length_c 11.40380(10) _cell_measurement_reflns_used 6127 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 76.3310 _cell_measurement_theta_min 5.3810 _cell_volume 1118.28(3) _computing_cell_refinement ; CrysAlis PRO (Rigaku Oxford Diffraction, 2015) ; _computing_data_collection ; CrysAlis PRO (Rigaku Oxford Diffraction, 2015) ; _computing_data_reduction ; CrysAlis PRO (Rigaku Oxford Diffraction, 2015) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS (Sheldrick, 2008) ; _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Agilent SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 7792 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.515 _diffrn_reflns_theta_min 5.409 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 13.281 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku Oxford Diffraction, 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.675 _exptl_crystal_description prism _exptl_crystal_F_000 564 _exptl_crystal_size_max 0.235 _exptl_crystal_size_mid 0.117 _exptl_crystal_size_min 0.104 _refine_diff_density_max 0.348 _refine_diff_density_min -0.758 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 126 _refine_ls_number_reflns 2292 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0182 _refine_ls_R_factor_gt 0.0176 _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^)+(0.0233P)^2^+0.7527P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0462 _reflns_number_gt 2228 _reflns_number_total 2292 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5381.cif _cod_data_source_block I _cod_database_code 2242106 _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 0.146 _shelx_estimated_absorpt_t_max 0.339 _shelx_hkl_file ; 0 0 1 62.5426 48.4463 2 0 0 1 115.136 53.9254 11 0 0 2 589440. 10181.0 2 0 0 2 584494. 10237.4 11 0 0 2 575065. 10355.4 12 0 0 3-41.7388 123.057 11 0 0 3 153.565 122.610 2 0 0 3-8.52027 134.980 12 0 0 -4 719103. 13398.3 10 0 0 4 730449. 13392.2 12 0 0 4 737012. 13097.6 2 0 0 4 722179. 13206.4 11 0 0 5 15.2279 145.110 11 0 0 -5 214.430 218.004 10 0 0 -6 85278.2 2936.44 10 0 0 6 84931.3 2659.24 2 0 0 6 84513.7 2717.15 11 0 0 -7-28.5329 208.100 10 0 0 7 1.23387 155.926 11 0 0 7 258.166 227.261 2 0 0 8 125249. 3951.49 2 0 0 8 129614. 3061.01 7 0 0 8 129933. 3030.49 14 0 0 -8 134304. 4491.27 10 0 0 -9 173.719 270.973 10 0 0 9 63.8211 128.710 14 0 0 9-106.656 172.437 7 0 0 10 12322.5 736.321 7 0 0 10 12643.3 739.171 14 0 0 11 103.043 140.662 14 0 0 12 100661. 2304.19 4 0 0 12 101330. 2334.86 14 0 0 -12 101813. 2326.05 9 0 0 -13 5.71634 78.7536 9 0 0 13 76.6966 75.5738 4 0 0 13-29.6979 75.5347 14 0 -1 0 67.3143 46.0823 1 0 1 0 46.3521 33.2795 11 0 -1 1 295195. 5282.29 12 0 -1 -1 285036. 5112.90 3 0 1 1 289142. 5091.56 12 0 1 1 300818. 5051.00 2 0 -1 -1 286089. 5082.26 1 0 -1 1 301394. 5076.34 1 0 -1 1 282181. 5204.38 2 0 1 2 296261. 5233.80 2 0 -1 2 288260. 5429.73 2 0 -1 2 305938. 5051.58 1 0 1 2 285872. 5520.07 11 0 -1 -2 293892. 5049.68 1 0 1 2 283710. 5390.73 12 0 -1 3 387727. 7198.12 2 0 1 3 380023. 7295.18 11 0 -1 3 388160. 7017.26 11 0 1 3 370828. 7181.99 12 0 1 3 383066. 6985.71 2 0 1 -4 1396.86 304.665 10 0 -1 4 1479.63 279.825 2 0 1 4 1405.06 227.066 2 0 1 4 1849.42 305.207 12 0 -1 4 1552.57 246.335 11 0 -1 4 1313.46 297.555 12 0 1 4 1557.28 305.555 11 0 -1 -4 1249.31 281.351 10 0 1 5 310483. 6790.51 11 0 -1 5 320040. 6467.89 11 0 1 5 317739. 6417.42 2 0 -1 5 330885. 6988.58 12 0 1 -5 308406. 6894.00 10 0 -1 -5 322762. 6851.19 10 0 -1 5 319353. 6677.17 2 0 1 6 309.278 204.597 11 0 -1 6-49.2528 153.497 2 0 1 6 383.691 186.721 2 0 -1 -6 176.900 223.358 10 0 -1 6 336.644 182.342 11 0 1 -6 180.941 247.809 10 0 1 -7 17164.5 1333.45 10 0 -1 -7 18208.6 1363.02 10 0 1 7 16818.3 1230.63 11 0 1 7 16963.8 1128.78 2 0 -1 7 16774.9 1196.39 2 0 1 -8 36220.7 2129.88 10 0 -1 8 37520.9 1298.25 14 0 1 8 38274.3 1994.85 11 0 1 -8 36616.0 1314.07 13 0 1 8 35250.5 1277.26 14 0 -1 -8 37639.4 2178.19 10 0 -1 8 38873.1 1331.66 7 0 -1 8 35277.9 1918.15 2 0 1 8 37398.8 1321.98 7 0 1 9 175075. 3975.91 7 0 -1 9 182106. 3967.49 14 0 -1 9 180613. 4004.07 7 0 1 9 179669. 3970.95 14 0 -1 -9 171955. 5271.50 3 0 -1 9 172022. 5129.25 2 0 1 -9 190500. 5791.11 10 0 -1 10 39279.7 1407.88 7 0 1 10 39613.5 1386.71 7 0 1 10 36690.0 1372.46 14 0 -1 10 39727.5 1393.35 14 0 -1 11 18737.4 859.372 14 0 -1 -11 18576.2 858.764 9 0 -1 11 17858.9 837.824 7 0 -1 11 18756.8 834.874 4 0 1 11 18626.4 867.857 14 0 1 12 54853.4 1529.95 14 0 1 12 55474.6 1501.82 4 0 -1 12 59456.5 1522.82 4 0 -1 12 57805.2 1524.46 14 0 1 -12 56732.3 1511.95 9 0 -1 -12 55782.5 1510.47 9 0 1 13 88478.8 1879.06 14 0 1 -13 88922.1 1851.78 9 0 -1 13 86630.3 1838.89 4 0 1 13 88659.2 1855.42 4 0 -1 -13 87773.4 1854.76 9 0 -1 13 89571.8 1852.57 14 0 -2 0 38993.1 775.532 12 0 2 0 36447.1 923.144 11 0 -2 0 38473.8 924.644 3 0 -2 0 40097.9 1024.65 1 0 -2 -1 88.7535 73.1589 1 0 -2 -1 181.216 85.0982 3 0 2 1 175.589 110.110 11 0 -2 1 200.786 95.3715 1 0 -2 1 160.898 96.8363 12 0 -2 1 141.486 107.884 2 0 -2 2 3972.56 363.113 12 0 2 2 4244.95 253.993 2 0 2 2 3669.04 252.014 12 0 -2 -2 3797.09 283.611 3 0 -2 2 4319.97 357.330 2 0 -2 -2 3510.55 251.025 1 0 -2 2 3833.90 254.237 1 0 2 -3 497.888 204.249 10 0 2 3 507.092 192.852 11 0 2 3 771.215 139.743 2 0 -2 3 652.850 208.924 12 0 -2 -3 832.222 118.711 1 0 -2 3 754.876 218.218 2 0 -2 3 750.554 127.582 11 0 2 3 708.632 161.339 12 0 -2 3 630.695 106.159 1 0 2 4 359759. 7373.59 11 0 2 4 343303. 6789.35 2 0 -2 4 362795. 6727.37 11 0 -2 -4 376162. 7265.81 10 0 -2 4 363402. 7253.58 2 0 2 -4 345139. 7363.46 10 0 -2 4 383639. 7486.00 12 0 -2 5 22415.4 1206.85 2 0 -2 5 22618.8 1297.21 12 0 -2 5 22899.7 973.834 11 0 2 -5 20021.7 1235.82 10 0 2 5 21696.6 1250.47 11 0 2 5 21624.6 987.307 2 0 -2 -5 22498.2 1227.72 10 0 2 6 151799. 3815.50 2 0 2 6 156255. 4370.49 11 0 -2 6 159276. 4253.79 2 0 2 -6 157679. 4444.74 10 0 -2 -7 624.116 280.625 3 0 -2 7 67.2247 176.251 2 0 2 7 157.268 227.082 11 0 2 -7 160.687 193.384 10 0 2 8 351244. 8496.45 11 0 -2 8 347103. 8395.44 2 0 2 8 354079. 6908.01 14 0 2 8 350848. 6932.03 7 0 2 -8 372218. 8848.85 10 0 -2 8 361142. 6906.55 14 0 -2 8 368786. 6904.63 7 0 2 -8 350105. 6940.33 13 0 -2 -8 355877. 8366.31 3 0 2 9 4926.06 457.811 7 0 2 9 4976.79 463.518 14 0 2 -9 4522.73 454.579 13 0 2 -9 5440.92 876.938 10 0 -2 -9 4851.08 766.375 3 0 -2 9 5140.20 477.409 7 0 -2 9 5124.87 460.077 14 0 2 10 36015.5 1328.88 14 0 -2 -10 35948.9 1336.69 9 0 -2 10 36918.3 1314.37 14 0 -2 10 37738.9 1364.50 7 0 -2 11 1909.36 274.733 7 0 2 11 1766.72 265.112 14 0 -2 11 2062.11 279.622 4 0 -2 11 1624.65 253.062 14 0 -2 -11 2159.18 291.440 9 0 -2 12 76329.9 1804.27 4 0 -2 12 72850.7 1781.61 14 0 2 12 74481.0 1809.16 4 0 2 12 72688.7 1836.39 14 0 -2 -12 74246.3 1824.35 9 0 2 -12 74516.7 1809.05 9 0 -2 13 28.6170 67.1152 4 0 2 13 96.1911 79.1785 4 0 2 13 93.0041 70.9642 14 0 -2 13 78.0823 64.0545 14 0 -2 -13 278.650 89.5504 9 0 2 -13 127.370 74.2561 9 0 -3 0 132.495 119.304 1 0 3 0 79.9404 91.9733 11 0 -3 1 273301. 5238.30 1 0 3 -1 271422. 4892.34 11 0 -3 -1 268761. 5246.08 1 0 -3 -1 279292. 5103.73 3 0 3 1 277326. 5313.20 11 0 -3 1 285396. 5158.73 12 0 3 2 32573.7 893.494 2 0 -3 2 33109.3 1159.02 2 0 -3 -2 32065.9 1038.69 1 0 3 2 33375.8 1222.35 11 0 -3 -2 35035.5 1051.46 3 0 -3 2 33409.5 1038.33 1 0 -3 2 32591.0 1166.80 12 0 3 -2 32111.5 1218.73 10 0 -3 3 316989. 5822.22 1 0 3 -3 313650. 6470.38 10 0 3 3 313130. 5776.52 2 0 -3 3 306114. 5514.15 11 0 -3 -3 314398. 6029.82 3 0 -3 -3 316013. 5844.26 1 0 3 3 303587. 6419.84 11 0 -3 3 319026. 6413.69 12 0 -3 3 323591. 6324.33 2 0 -3 4 29771.1 878.755 11 0 -3 -4 29651.8 1197.46 3 0 3 4 31093.6 1449.92 11 0 -3 4 31947.1 1389.19 2 0 -3 4 31028.4 1430.83 12 0 3 4 30057.3 1043.34 2 0 3 -4 31242.1 1480.43 10 0 -3 5 247243. 5678.16 2 0 -3 5 248363. 5851.17 12 0 -3 -5 234212. 5344.97 3 0 3 5 246634. 5046.77 2 0 3 5 251742. 5878.52 11 0 3 -5 241691. 5850.93 10 0 3 6 5437.02 515.115 2 0 3 -6 5921.03 763.802 10 0 -3 6 5699.09 686.230 2 0 3 6 6122.57 761.445 11 0 -3 -6 6296.11 667.988 3 0 3 -7 62885.8 2776.89 10 0 -3 -7 62586.4 2511.36 3 0 3 7 60311.9 2691.43 11 0 -3 7 62657.1 2623.04 2 0 3 -8 16275.7 1440.82 10 0 3 -8 14174.2 793.201 13 0 -3 -8 14902.0 1248.72 3 0 3 8 15022.6 776.435 14 0 3 8 13735.6 1288.68 11 0 -3 8 15979.8 786.169 14 0 -3 8 14777.0 759.882 7 0 -3 -9 304132. 7682.02 3 0 -3 9 312899. 6129.86 7 0 -3 9 318498. 6100.39 14 0 -3 -9 285338. 6086.35 9 0 3 9 299025. 7924.47 11 0 3 9 307985. 6135.92 14 0 3 -9 309445. 6171.31 13 0 -3 10 30450.7 1197.76 7 0 -3 -10 28616.6 1161.61 9 0 -3 10 29980.6 1134.16 14 0 -3 10 31416.9 1145.70 4 0 3 10 28975.7 1164.15 14 0 -3 11 14881.1 701.181 14 0 -3 11 13578.8 706.384 7 0 -3 -11 14274.6 724.968 9 0 -3 11 15239.6 710.856 4 0 3 11 14380.4 731.198 14 0 3 12 11510.7 545.246 4 0 3 12 11205.7 557.632 14 0 -3 12 11058.4 508.800 14 0 -3 -12 11788.6 560.058 9 0 -3 12 11731.4 535.174 7 0 -3 12 12354.2 542.597 4 0 3 -13 137266. 2581.72 9 0 3 13 138546. 2624.65 14 0 -3 -13 135645. 2600.78 9 0 -3 13 136307. 2554.75 4 0 3 13 135201. 2581.13 4 0 -4 0 999999. 17022.2 3 0 4 0 966265. 16999.1 11 0 -4 0 977043. 17271.7 1 0 4 1 1131.54 221.775 11 0 -4 -1 1076.07 228.364 1 0 -4 1 991.464 207.654 1 0 -4 -1 942.559 175.187 3 0 4 -1 1184.04 154.711 11 0 4 2 23034.4 1065.06 11 0 -4 -2 26000.2 1014.16 1 0 4 -2 23084.6 1093.13 10 0 -4 2 22186.5 934.318 1 0 -4 -2 24080.5 915.274 3 0 -4 2 24298.4 1005.24 12 0 -4 -3 2172.68 278.699 1 0 4 3 2025.75 223.689 2 0 4 3 2255.04 386.245 11 0 -4 -3 2301.57 299.475 3 0 4 -3 2286.33 390.285 10 0 -4 3 2244.39 350.014 12 0 -4 3 2129.54 354.946 2 0 -4 4 249861. 5551.92 12 0 -4 4 242676. 5439.49 2 0 4 4 238462. 4724.48 2 0 -4 -4 232928. 5071.46 3 0 4 -4 232994. 5614.67 10 0 4 4 237345. 5592.35 11 0 -4 5 74668.3 2600.54 2 0 -4 -5 74302.9 2355.07 3 0 4 5 73591.7 2733.81 11 0 4 -5 76730.7 2795.88 10 0 -4 6 11208.3 997.846 2 0 -4 -6 9084.20 814.900 3 0 4 -6 10389.6 1017.22 10 0 4 6 10515.0 1045.67 11 0 4 7 813.663 338.167 11 0 4 -7 947.541 368.728 10 0 -4 -7 1110.51 336.236 3 0 -4 8 84884.3 2121.77 4 0 4 8 79299.8 3433.83 11 0 -4 8 80332.2 2155.20 7 0 -4 -8 77033.0 3079.15 3 0 4 -8 82284.2 3471.08 10 0 4 8 76762.3 2113.63 14 0 -4 -8 78439.1 2136.38 9 0 4 -8 78391.0 2195.61 13 0 -4 8 79595.3 2105.19 14 0 -4 9 16107.1 794.299 14 0 4 9 15681.1 822.685 14 0 -4 -9 16086.5 837.754 9 0 4 -9 16888.0 864.050 13 0 -4 9 17568.8 819.821 4 0 -4 9 16875.6 839.806 7 0 -4 10 12529.9 719.357 7 0 4 10 11794.9 690.132 14 0 4 -10 11181.3 664.331 13 0 -4 10 11635.5 649.990 4 0 -4 -10 10911.6 670.401 9 0 -4 10 11907.7 645.992 14 0 -4 11 3313.71 314.336 4 0 -4 11 3302.19 339.499 7 0 -4 11 3538.88 313.887 14 0 -4 -11 3181.18 327.794 9 0 4 11 3258.34 336.126 14 0 4 12 119150. 2535.30 14 0 -4 12 116772. 2481.97 7 0 4 12 120633. 2489.96 4 0 -4 12 117067. 2401.20 14 0 -4 -12 119498. 2519.50 9 0 -4 12 121129. 2449.38 4 0 -5 0 33.7678 132.408 1 0 -5 0-3.64832 106.210 3 0 5 0 71.4442 105.379 11 0 5 -1 417929. 7483.48 11 0 -5 1 401794. 8013.05 1 0 -5 -1 427344. 7781.01 3 0 5 1 398593. 7911.35 11 0 -5 -1 409068. 8063.33 1 0 -5 -2 115633. 2722.78 3 0 -5 2 110092. 2825.50 1 0 -5 -2 113003. 2889.89 1 0 5 2 106702. 2932.58 11 0 5 -2 110290. 3058.34 10 0 5 -3 206193. 5061.83 10 0 5 3 212814. 4205.02 2 0 -5 3 206590. 4561.87 1 0 -5 -3 218603. 4591.26 3 0 5 3 213699. 5019.09 11 0 -5 -3 209086. 4597.99 1 0 5 -4 25748.7 1477.77 10 0 5 4 23734.1 1397.29 11 0 -5 -4 25526.4 1184.75 3 0 5 -5 256372. 6352.34 10 0 -5 -5 244057. 5611.96 3 0 5 5 249230. 6261.14 11 0 5 -6 31730.7 1900.37 10 0 -5 -6 30532.2 1577.50 3 0 5 6 32796.8 1937.08 11 0 5 -7 66615.8 3012.73 10 0 -5 -7 61321.6 2539.12 3 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8 -6 2 94181.9 2045.48 14 -8 6 -2 94307.4 1954.78 6 8 -6 3 1602.21 144.294 14 8 -7 -9 28466.1 830.242 8 8 -7 -8 2320.61 240.255 8 -8 7 7 85910.2 1832.87 6 -8 -7 7 82376.3 1864.24 5 -8 7 6 9416.57 463.645 6 -8 -7 6 9124.18 479.055 5 8 -7 -6 9153.49 492.065 8 -8 7 5 66139.5 1632.15 6 -8 -7 5 65288.0 1688.00 5 -8 7 4 6030.12 401.597 6 -8 -7 4 6694.51 455.884 5 -8 7 3 40121.1 1193.92 6 -8 -7 3 40548.6 1272.16 5 -8 7 2 2078.36 245.125 6 -8 -7 2 2176.53 279.567 5 -8 7 1 34560.2 1043.76 6 -8 -7 1 34233.1 1117.09 5 -8 7 0 4464.94 310.272 6 -8 -7 0 4210.63 335.411 5 -8 7 -1 23244.5 713.989 6 -8 -7 -1 23012.1 764.931 5 8 -7 2 3288.77 227.281 14 -8 7 -2 3019.04 190.798 6 8 -8 -8 96020.7 2010.84 8 -8 8 7 6413.82 306.658 6 8 -8 -7 6104.03 359.967 8 -8 8 6 102475. 2112.50 6 -8 -8 6 96987.4 2077.13 5 8 -8 -6 103292. 2186.76 8 -8 8 5 25948.6 823.854 6 -8 -8 5 25444.6 822.388 5 8 -8 -5 26067.1 818.539 8 -8 8 4 25441.4 828.939 6 -8 -8 4 24514.4 846.778 5 -8 -8 3 70.8767 107.068 5 -8 8 3 37.6548 89.6349 6 -8 8 2 61093.1 1479.05 6 -8 -8 2 59401.6 1554.32 5 -8 8 1 8348.06 415.871 6 -8 -8 1 8034.32 454.297 5 -8 8 0 4040.55 258.636 6 -8 -8 0 3757.23 290.180 5 8 -8 1 1817.19 172.604 14 -8 8 -1 2006.43 157.117 6 -8 9 6 13958.9 472.497 6 8 -9 -6 13819.5 494.554 8 -8 9 5 24294.0 701.614 6 -8 -9 5 21782.6 628.364 5 -8 9 4 6539.86 340.607 6 -8 -9 4 6533.27 335.404 5 -8 9 3 35300.1 950.358 6 -8 -9 3 36148.1 976.663 5 -8 9 2 13453.5 500.380 6 -8 -9 2 13809.5 540.013 5 -8 9 1 46361.7 1091.68 6 -8 -9 1 48026.2 1171.06 5 -8 9 0 1352.74 120.430 6 -8 10 4 14267.0 447.670 6 -8 10 3 3846.13 209.013 6 -9 0 10 78567.2 1745.33 5 -9 0 9 219.027 124.239 5 -9 0 8 102007. 2351.63 5 -9 0 7 203.302 148.614 5 -9 0 6 201839. 4135.58 5 -9 0 5 133.688 117.708 5 -9 0 4 33364.7 1087.39 5 -9 0 3 272.258 122.977 5 -9 0 2 46710.9 1235.43 5 -9 1 11 69433.4 1429.66 5 -9 -1 10 17569.0 608.429 5 -9 1 10 17463.1 617.584 5 -9 -1 9 32032.4 987.809 5 -9 1 9 31558.7 982.084 5 -9 -1 8 4504.73 359.492 5 -9 1 8 4142.76 343.495 5 -9 -1 7 74057.5 1906.11 5 -9 1 7 74280.2 1879.24 5 -9 -1 6 5431.66 428.651 5 -9 1 6 5586.88 418.098 5 -9 -1 5 16154.7 746.657 5 -9 1 5 17201.9 730.611 5 -9 -1 4 8453.55 509.138 5 -9 1 4 8806.83 487.826 5 -9 -1 3 58862.9 1563.04 5 -9 1 3 60341.8 1498.19 5 -9 -1 2 7681.56 434.213 5 -9 -1 1 48830.4 1226.89 5 -9 -2 10 82427.3 1741.14 5 -9 2 10 82379.5 1774.82 5 -9 -2 9 3984.47 301.088 5 -9 2 9 3558.49 284.292 5 -9 -2 8 1477.31 212.279 5 -9 2 8 1349.07 201.906 5 -9 -2 7 11753.3 609.171 5 -9 2 7 10916.7 558.790 5 -9 -2 6 75098.1 1932.36 5 -9 2 6 73731.9 1830.63 5 -9 -2 5 9521.83 563.350 5 -9 2 5 10304.5 525.159 5 -9 -2 4 12599.5 635.579 5 -9 2 4 12821.9 564.065 5 -9 -2 3 169.552 132.669 5 -9 2 2 140929. 2805.86 6 -9 -2 2 139878. 2935.81 5 -9 2 1 5892.22 337.781 6 -9 -2 1 5728.63 350.182 5 -9 -3 10 42023.3 979.486 5 -9 3 10 43878.7 1041.16 5 -9 -3 9 44844.8 1154.25 5 -9 3 9 44425.3 1147.21 5 -9 -3 8 5980.23 387.970 5 -9 3 8 6322.59 379.047 5 -9 -3 7 94214.6 2180.69 5 -9 3 7 89920.7 2057.70 5 -9 -3 6 1127.46 213.702 5 -9 3 6 1582.39 196.003 5 -9 -3 5 89874.6 2153.11 5 -9 3 5 85220.1 1937.98 5 -9 -3 4 7132.07 470.999 5 -9 3 3 78471.1 1768.69 6 -9 -3 3 81771.9 1965.68 5 -9 3 2 6443.66 360.892 6 -9 -3 2 5773.34 385.462 5 -9 3 1 36919.2 993.689 6 -9 -3 1 34897.3 1012.72 5 -9 -3 0 989.771 138.049 5 9 -3 0 751.337 128.586 14 -9 -4 9 91.2598 67.8702 5 -9 4 9 17.0729 69.0521 5 -9 -4 8 74707.9 1710.53 5 -9 4 8 73568.3 1635.99 5 -9 -4 7 2244.97 243.368 5 -9 4 7 2233.01 210.797 5 -9 -4 6 171285. 3428.21 5 -9 4 6 160215. 3170.88 5 -9 -4 5 205.484 147.781 5 -9 -4 4 11543.6 594.210 5 -9 -4 3 237.338 119.836 5 -9 4 3 302.763 101.100 6 -9 4 2 32477.1 925.541 6 -9 -4 2 31384.0 996.026 5 -9 -4 1 299.413 107.808 5 -9 4 1 391.781 104.794 6 9 -4 0 1040.13 143.807 14 -9 4 0 1378.88 153.557 6 -9 -4 0 1321.86 150.880 5 -9 -5 8 15680.1 537.210 5 -9 5 8 14210.9 462.088 5 -9 -5 7 65627.4 1557.11 5 -9 -5 6 7459.00 433.203 5 -9 -5 5 23492.6 846.169 5 -9 5 4 26027.9 768.146 6 -9 -5 4 27466.9 931.059 5 -9 5 3 67118.2 1547.63 6 -9 -5 3 71086.1 1720.11 5 -9 5 2 9286.58 416.996 6 -9 -5 2 9224.92 477.342 5 -9 5 1 47457.5 1134.72 6 -9 -5 1 46102.1 1192.68 5 9 -5 0 6077.83 314.452 14 -9 5 0 6302.60 294.657 6 -9 -5 0 5990.40 300.803 5 -9 -6 7 2673.96 207.717 5 -9 -6 6 31440.0 907.137 5 -9 -6 5 189.206 105.546 5 -9 6 5 59.8839 44.1494 6 -9 6 4 22764.0 675.101 6 -9 -6 4 24802.5 822.309 5 -9 6 3 4698.63 273.551 6 -9 -6 3 4867.76 336.279 5 -9 6 2 157590. 3006.01 6 -9 -6 2 159656. 3145.47 5 -9 6 1 11792.5 421.517 6 -9 -6 1 11506.7 466.238 5 -9 -7 6 1577.63 148.312 5 -9 -7 5 26393.6 760.679 5 -9 7 4 6058.15 273.092 6 -9 -7 4 6789.96 351.040 5 -9 7 3 38537.0 922.634 6 -9 -7 3 41815.5 1050.64 5 -9 7 2 2205.08 159.357 6 -9 -7 2 2257.14 195.674 5 -10 0 8 48332.9 1099.94 5 -10 0 7 21.7357 68.4419 5 -10 0 6 193379. 3613.28 5 -10 0 5 88.7807 69.7408 5 -10 -1 8 7707.95 333.013 5 -10 -1 7 45627.3 1087.34 5 -10 1 7 42482.6 1015.85 5 -10 -1 6 375.930 102.012 5 -10 1 6 263.608 81.4390 5 -10 -1 5 28532.1 800.226 5 -10 -1 4 13494.7 468.478 5 -10 -2 8 8414.10 337.979 5 -10 -2 7 185.869 82.9725 5 -10 -2 6 2812.54 219.106 5 -10 -2 5 1380.52 162.146 5 -10 -2 4 1686.08 163.980 5 -10 -3 7 90257.7 1828.63 5 -10 -3 6 1938.03 176.917 5 -10 -3 5 12123.9 463.911 5 -10 -3 4 19781.3 603.545 5 -10 -4 6 128992. 2463.31 5 -10 -4 5 7009.84 320.548 5 -10 -4 4 34635.4 850.219 5 0 0 0 0.00 0.00 0 TITL ET147 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 8.236301 12.701947 11.403823 90.0000 110.3911 90.0000 ZERR 1.00 0.000127 0.000152 0.000137 0.0000 0.0015 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C N O F UNIT 36.00 10.00 10.00 12.00 TREF HKLF 4 END ; _shelx_hkl_checksum 26477 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL dib5 CELL 1.54184 8.2363 12.7020 11.4038 90.000 110.391 90.000 ZERR 2.00 0.0001 0.0002 0.0001 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H CL F O S SN UNIT 36 48 4 4 4 4 2 MERG 2 FMAP 2 PLAN -1 SIZE 0.104 0.117 0.235 ACTA BOND $H CONF SIZE 0.104 0.117 0.235 L.S. 24 TEMP -173 WGHT 0.023300 0.752700 FVAR 5.74502 SN 7 0.500000 0.500000 0.500000 10.50000 0.00785 0.00543 = 0.00565 -0.00080 0.00078 0.00005 CL1 3 0.446652 0.487624 0.265447 11.00000 0.02083 0.01534 = 0.00719 0.00013 0.00249 0.00143 S1 6 0.557778 0.246281 0.430153 11.00000 0.00860 0.00802 = 0.00877 -0.00157 0.00171 0.00079 F1 4 0.064562 0.032192 0.343472 11.00000 0.02503 0.00887 = 0.03283 -0.00140 0.00056 -0.00256 O1 5 0.603492 0.335827 0.527516 11.00000 0.01348 0.00667 = 0.00949 -0.00213 0.00124 0.00160 C1 1 0.233193 0.457143 0.465505 11.00000 0.00820 0.01308 = 0.01724 -0.00295 0.00394 -0.00066 AFIX 23 H1A 2 0.205365 0.474598 0.540986 11.00000 -1.20000 H1B 2 0.158270 0.501259 0.396162 11.00000 -1.20000 AFIX 0 C2 1 0.187766 0.344368 0.433394 11.00000 0.00591 0.01123 = 0.01225 -0.00120 0.00315 0.00004 C3 1 0.109258 0.312598 0.308712 11.00000 0.00874 0.01286 = 0.01052 0.00226 0.00184 0.00047 AFIX 43 H3 2 0.083782 0.363737 0.244010 11.00000 -1.20000 AFIX 0 C4 1 0.067914 0.207717 0.277828 11.00000 0.01153 0.01525 = 0.01166 -0.00284 0.00200 -0.00043 AFIX 43 H4 2 0.014713 0.186814 0.193022 11.00000 -1.20000 AFIX 0 C5 1 0.105752 0.134870 0.372802 11.00000 0.01099 0.00780 = 0.02110 -0.00179 0.00295 -0.00144 C6 1 0.182209 0.161923 0.497473 11.00000 0.01168 0.01507 = 0.01522 0.00648 0.00315 0.00153 AFIX 43 H6 2 0.206240 0.110091 0.561331 11.00000 -1.20000 AFIX 0 C7 1 0.222927 0.267275 0.526676 11.00000 0.00885 0.01763 = 0.00900 0.00003 0.00218 -0.00060 AFIX 43 H7 2 0.275764 0.287330 0.611815 11.00000 -1.20000 AFIX 0 C8 1 0.637134 0.132856 0.524662 11.00000 0.02279 0.00803 = 0.01413 0.00022 0.00490 0.00268 AFIX 137 H8A 2 0.757625 0.144701 0.578588 11.00000 -1.50000 H8B 2 0.631188 0.071785 0.470805 11.00000 -1.50000 H8C 2 0.566241 0.119686 0.576582 11.00000 -1.50000 AFIX 0 C9 1 0.718084 0.254816 0.358755 11.00000 0.01663 0.01754 = 0.01669 -0.00187 0.00965 0.00048 AFIX 137 H9A 2 0.703535 0.320862 0.311778 11.00000 -1.50000 H9B 2 0.705490 0.195238 0.301652 11.00000 -1.50000 H9C 2 0.833505 0.253046 0.423516 11.00000 -1.50000 AFIX 0 HKLF 4 REM dib5 REM R1 = 0.0176 for 2228 Fo > 4sig(Fo) and 0.0182 for all 2292 data REM 126 parameters refined using 0 restraints END WGHT 0.0231 0.7634 REM Highest difference peak 0.348, deepest hole -0.758, 1-sigma level 0.073 Q1 1 0.7754 0.5995 0.5498 11.00000 0.05 0.35 ; _shelx_res_checksum 43526 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn 0.5000 0.5000 0.5000 0.00673(6) Uani d 1 . . Cl Cl1 0.44665(6) 0.48762(3) 0.26545(4) 0.01508(10) Uani d 1 . . S S1 0.55778(5) 0.24628(3) 0.43015(3) 0.00881(9) Uani d 1 . . F F1 0.06456(15) 0.03219(9) 0.34347(11) 0.0248(2) Uani d 1 . . O O1 0.60349(15) 0.33583(9) 0.52752(10) 0.0106(2) Uani d 1 . . C C1 0.2332(2) 0.45714(13) 0.46551(16) 0.0130(3) Uani d 1 . . H H1A 0.2054 0.4746 0.5410 0.016 Uiso calc 1 . . H H1B 0.1583 0.5013 0.3962 0.016 Uiso calc 1 . . C C2 0.1878(2) 0.34437(13) 0.43339(15) 0.0098(3) Uani d 1 . . C C3 0.1093(2) 0.31260(13) 0.30871(15) 0.0111(3) Uani d 1 . . H H3 0.0838 0.3637 0.2440 0.013 Uiso calc 1 . . C C4 0.0679(2) 0.20772(14) 0.27783(15) 0.0134(3) Uani d 1 . . H H4 0.0147 0.1868 0.1930 0.016 Uiso calc 1 . . C C5 0.1058(2) 0.13487(13) 0.37280(16) 0.0140(3) Uani d 1 . . C C6 0.1822(2) 0.16192(14) 0.49747(16) 0.0144(3) Uani d 1 . . H H6 0.2062 0.1101 0.5613 0.017 Uiso calc 1 . . C C7 0.2229(2) 0.26727(14) 0.52668(15) 0.0121(3) Uani d 1 . . H H7 0.2758 0.2873 0.6118 0.014 Uiso calc 1 . . C C8 0.6371(2) 0.13286(13) 0.52466(15) 0.0154(3) Uani d 1 . . H H8A 0.7576 0.1447 0.5786 0.023 Uiso calc 1 . . H H8B 0.6312 0.0718 0.4708 0.023 Uiso calc 1 . . H H8C 0.5662 0.1197 0.5766 0.023 Uiso calc 1 . . C C9 0.7181(2) 0.25482(14) 0.35875(16) 0.0159(3) Uani d 1 . . H H9A 0.7035 0.3209 0.3118 0.024 Uiso calc 1 . . H H9B 0.7055 0.1952 0.3017 0.024 Uiso calc 1 . . H H9C 0.8335 0.2530 0.4235 0.024 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn 0.00785(9) 0.00543(9) 0.00565(8) 0.00005(4) 0.00078(6) -0.00080(4) Cl1 0.0208(2) 0.0153(2) 0.00719(18) 0.00143(14) 0.00249(16) 0.00013(13) S1 0.00860(18) 0.00802(18) 0.00877(16) 0.00079(13) 0.00171(14) -0.00157(13) F1 0.0250(6) 0.0089(5) 0.0328(6) -0.0026(4) 0.0006(5) -0.0014(5) O1 0.0135(6) 0.0067(5) 0.0095(5) 0.0016(4) 0.0012(4) -0.0021(4) C1 0.0082(7) 0.0131(9) 0.0172(8) -0.0007(6) 0.0039(6) -0.0030(6) C2 0.0059(7) 0.0112(8) 0.0122(7) 0.0000(6) 0.0032(6) -0.0012(6) C3 0.0087(7) 0.0129(8) 0.0105(7) 0.0005(6) 0.0018(6) 0.0023(6) C4 0.0115(8) 0.0152(9) 0.0117(7) -0.0004(6) 0.0020(6) -0.0028(6) C5 0.0110(8) 0.0078(8) 0.0211(8) -0.0014(6) 0.0030(6) -0.0018(6) C6 0.0117(8) 0.0151(8) 0.0152(8) 0.0015(6) 0.0032(6) 0.0065(6) C7 0.0089(8) 0.0176(8) 0.0090(7) -0.0006(6) 0.0022(6) 0.0000(6) C8 0.0228(9) 0.0080(8) 0.0141(8) 0.0027(6) 0.0049(7) 0.0002(6) C9 0.0166(9) 0.0175(9) 0.0167(8) 0.0005(6) 0.0097(7) -0.0019(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn 0.0259 5.4591 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 Sn C1 . 3_666 180.0 ? C1 Sn O1 . . 95.99(5) y C1 Sn Cl1 . . 90.05(5) y C1 Sn Cl1 . 3_666 89.95(5) ? C1 Sn O1 . 3_666 84.01(5) y C1 Sn Cl1 . 3_666 89.95(5) y O1 Sn Cl1 . . 90.44(3) y O1 Sn Cl1 . 3_666 89.56(3) y C1 Sn O1 3_666 . 84.01(5) ? C1 Sn O1 3_666 3_666 95.99(5) ? O1 Sn O1 . 3_666 180.0 ? C1 Sn Cl1 3_666 3_666 90.05(5) ? O1 Sn Cl1 3_666 3_666 90.44(3) ? O1 Sn Cl1 3_666 . 89.56(3) ? Cl1 Sn Cl1 3_666 . 180.000(18) ? O1 S1 C9 . . 104.51(8) ? O1 S1 C8 . . 102.41(7) ? C9 S1 C8 . . 98.73(8) ? S1 O1 Sn . . 127.03(6) ? C2 C1 Sn . . 115.97(11) ? C2 C1 H1A . . 108.3 ? Sn C1 H1A . . 108.3 ? C2 C1 H1B . . 108.3 ? Sn C1 H1B . . 108.3 ? H1A C1 H1B . . 107.4 ? C7 C2 C3 . . 118.03(15) ? C7 C2 C1 . . 121.12(14) ? C3 C2 C1 . . 120.85(15) ? C4 C3 C2 . . 121.27(15) ? C4 C3 H3 . . 119.4 ? C2 C3 H3 . . 119.4 ? C5 C4 C3 . . 118.50(15) ? C5 C4 H4 . . 120.8 ? C3 C4 H4 . . 120.8 ? F1 C5 C4 . . 118.88(15) ? F1 C5 C6 . . 118.46(15) ? C4 C5 C6 . . 122.66(16) ? C5 C6 C7 . . 118.07(15) ? C5 C6 H6 . . 121.0 ? C7 C6 H6 . . 121.0 ? C6 C7 C2 . . 121.47(15) ? C6 C7 H7 . . 119.3 ? C2 C7 H7 . . 119.3 ? S1 C8 H8A . . 109.5 ? S1 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? S1 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? S1 C9 H9A . . 109.5 ? S1 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? S1 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn C1 . 2.1628(16) y Sn C1 3_666 2.1628(16) ? Sn O1 . 2.2332(11) y Sn O1 3_666 2.2332(11) ? Sn Cl1 3_666 2.5599(4) ? Sn Cl1 . 2.5599(4) y S1 O1 . 1.5417(11) ? S1 C9 . 1.7796(17) ? S1 C8 . 1.7815(17) ? F1 C5 . 1.360(2) ? C1 C2 . 1.494(2) ? C1 H1A . 0.9900 ? C1 H1B . 0.9900 ? C2 C7 . 1.400(2) ? C2 C3 . 1.401(2) ? C3 C4 . 1.390(2) ? C3 H3 . 0.9500 ? C4 C5 . 1.375(2) ? C4 H4 . 0.9500 ? C5 C6 . 1.383(2) ? C6 C7 . 1.392(2) ? C6 H6 . 0.9500 ? C7 H7 . 0.9500 ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C8 H8C . 0.9800 ? C9 H9A . 0.9800 ? C9 H9B . 0.9800 ? C9 H9C . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C3 H3 F1 2_555 0.95 2.49 3.333(2) 147 C6 H6 Cl1 4_555 0.95 2.77 3.6129(18) 148 C8 H8B Cl1 2_645 0.98 2.76 3.6379(17) 150 C9 H9C Cg1 1_655 0.98 2.67 3.3887(19) 130 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion C9 S1 O1 Sn . . . . 92.64(10) C8 S1 O1 Sn . . . . -164.80(9) Sn C1 C2 C7 . . . . 81.29(17) Sn C1 C2 C3 . . . . -98.42(16) C7 C2 C3 C4 . . . . -0.3(2) C1 C2 C3 C4 . . . . 179.42(15) C2 C3 C4 C5 . . . . 0.0(2) C3 C4 C5 F1 . . . . 179.52(15) C3 C4 C5 C6 . . . . 0.4(3) F1 C5 C6 C7 . . . . -179.60(15) C4 C5 C6 C7 . . . . -0.5(3) C5 C6 C7 C2 . . . . 0.1(3) C3 C2 C7 C6 . . . . 0.2(2) C1 C2 C7 C6 . . . . -179.50(15)