#------------------------------------------------------------------------------ #$Date: 2022-10-01 03:02:04 +0100 (Sat, 01 Oct 2022) $ #$Revision: 278296 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244186.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_2244186 loop_ _publ_author_name 'Tinapple, Elizabeth' 'Farrar, Sam' 'Johnston, Dean H.' _publ_section_title ; Crystal structures and hydrogen-bonding analysis of a series of benzamide complexes of zinc(II) chloride ; _journal_coeditor_code ZL5023 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 880 _journal_page_last 886 _journal_paper_doi 10.1107/S2056989021008264 _journal_volume 77 _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_iupac '[Zn Cl2 (C8 H9 N O)2]' _chemical_formula_moiety 'C16 H18 Cl2 N2 O2 Zn' _chemical_formula_sum 'C16 H18 Cl2 N2 O2 Zn' _chemical_formula_weight 406.59 _chemical_name_systematic ; Dichloridobis(2-methylbenzamide-\kO)zinc(II) ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _cell_angle_alpha 90 _cell_angle_beta 97.8520(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.3802(3) _cell_length_b 8.2491(3) _cell_length_c 14.5953(5) _cell_measurement_reflns_used 9884 _cell_measurement_temperature 100 _cell_measurement_theta_max 30.512 _cell_measurement_theta_min 2.79 _cell_volume 880.23(6) _computing_cell_refinement ; SAINT (Bruker, 2020) ; _computing_data_collection ; BIS (Bruker, 2020) ; _computing_data_reduction ; SAINT (Bruker, 2020) ; _computing_molecular_graphics ; CrystalMaker (Palmer, 2020) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.03 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_unetI/netI 0.0357 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 20749 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.512 _diffrn_reflns_theta_min 2.786 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.708 _exptl_absorpt_correction_T_max 0.6802 _exptl_absorpt_correction_T_min 0.4783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.534 _exptl_crystal_description needle _exptl_crystal_F_000 416 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.111 _refine_diff_density_max 0.307 _refine_diff_density_min -0.237 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.016(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 223 _refine_ls_number_reflns 5348 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.003 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0179 _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^)+(0.0078P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0386 _reflns_number_gt 5135 _reflns_number_total 5348 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zl5023sup1.cif _cod_data_source_block 2 _cod_database_code 2244186 _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 0.482 _shelx_estimated_absorpt_t_max 0.833 _shelx_hkl_file ; 1 0 0 656.43 29.00 2 0 0 565.74 27.40 -3 0 0 92.59 6.40 3 0 0 93.19 6.70 3 0 0 92.59 8.50 -3 0 0 80.69 6.50 3 0 0 90.59 6.10 4 0 0 470.95 23.20 -4 0 0 449.36 22.50 4 0 0 446.16 24.10 4 0 0 464.55 22.20 -4 0 0 466.55 23.50 4 0 0 448.26 26.30 5 0 0 264.37 19.50 -5 0 0 253.67 15.00 5 0 0 255.67 14.70 5 0 0 258.07 16.90 -5 0 0 252.37 16.10 5 0 0 250.77 15.60 6 0 0 1401.86 70.69 6 0 0 1470.35 65.69 6 0 0 1407.96 67.19 -6 0 0 1454.45 64.49 -6 0 0 1422.56 65.89 7 0 0 339.57 23.30 -7 0 0 361.06 21.40 -7 0 0 335.57 22.50 7 0 0 326.17 25.80 7 0 0 353.26 21.80 -8 0 0 -2.00 4.10 8 0 0 1.80 4.20 -8 0 0 0.60 4.90 8 0 0 1.80 5.30 9 0 0 42.60 10.10 -9 0 0 44.60 10.80 -9 0 0 55.49 10.10 10 0 0 144.99 18.10 -10 0 0 169.68 19.40 0 -1 0 1.90 0.90 0 1 0 2.60 1.00 1 -1 0 978.90 44.90 1 1 0 1126.59 45.70 2 -1 0 711.83 30.20 2 1 0 562.24 30.70 -3 -1 0 95.59 7.10 3 -1 0 99.69 8.50 3 -1 0 94.49 6.70 3 -1 0 102.59 7.50 3 1 0 93.19 8.10 3 1 0 95.09 9.30 -3 1 0 112.69 7.30 4 -1 0 1047.20 48.30 4 -1 0 1160.88 49.60 -4 -1 0 1088.19 46.80 4 -1 0 1059.19 47.40 4 -1 0 1083.19 51.19 -4 -1 0 1079.99 48.10 4 1 0 992.50 49.60 -4 1 0 1083.39 47.90 -4 1 0 1002.30 48.10 4 1 0 1036.00 52.49 4 1 0 1063.99 46.50 4 1 0 1086.89 48.10 5 -1 0 925.11 43.00 -5 -1 0 918.51 41.10 5 -1 0 918.91 41.80 5 -1 0 946.91 44.00 -5 -1 0 914.81 42.80 5 -1 0 924.31 46.60 5 1 0 870.11 47.20 -5 1 0 908.11 42.30 5 1 0 889.61 42.20 -5 1 0 890.51 42.90 5 1 0 795.92 43.80 -6 -1 0 418.46 23.00 -6 -1 0 449.86 25.10 6 -1 0 415.76 24.60 6 -1 0 401.66 27.90 6 -1 0 422.06 25.40 6 1 0 441.26 29.30 -6 1 0 447.66 25.20 6 1 0 413.36 26.00 6 1 0 474.25 24.60 -6 1 0 456.15 24.40 -7 -1 0 145.49 12.70 -7 -1 0 168.28 14.60 7 -1 0 169.68 17.40 7 -1 0 132.59 14.10 7 -1 0 157.58 14.00 -7 1 0 192.48 14.30 -7 1 0 204.08 16.10 7 1 0 207.28 16.00 7 1 0 190.78 19.00 8 -1 0 190.58 16.80 -8 -1 0 170.78 16.90 8 -1 0 169.38 16.90 8 -1 0 175.08 19.80 -8 1 0 237.48 17.50 8 1 0 207.58 18.20 8 1 0 213.58 21.30 -8 1 0 223.68 18.20 9 -1 0 99.69 14.10 -9 -1 0 113.69 15.10 -9 1 0 112.39 15.70 -9 1 0 85.49 12.90 9 1 0 94.29 15.20 10 -1 0 90.19 15.50 -10 -1 0 93.19 15.20 -10 1 0 80.89 14.60 10 1 0 74.39 13.70 -10 1 0 101.19 14.50 0 -2 0 9695.03 409.66 0 2 0 9999.00 411.36 1 -2 0 2277.67 90.69 1 2 0 2004.40 90.39 2 -2 0 78.39 6.00 2 -2 0 80.59 5.70 2 -2 0 76.79 6.20 2 -2 0 86.39 7.10 2 2 0 79.39 7.60 -2 2 0 83.79 5.90 3 -2 0 2106.79 95.89 3 -2 0 2168.18 97.79 3 -2 0 2304.37 95.59 -3 -2 0 2281.87 95.49 3 -2 0 2269.17 96.69 -3 -2 0 2263.97 95.29 3 2 0 2406.76 97.49 3 2 0 2247.08 98.09 -3 2 0 2289.17 95.89 3 2 0 2237.88 100.59 -3 2 0 2322.27 95.99 -4 -2 0 -0.80 2.20 4 -2 0 1.10 1.80 -4 -2 0 -1.00 1.60 -4 -2 0 -0.70 1.70 4 -2 0 1.90 2.40 4 -2 0 0.90 2.60 4 -2 0 -0.90 1.70 -4 2 0 8.70 3.10 -4 2 0 9.30 3.20 4 2 0 11.90 3.30 4 2 0 12.30 4.30 4 2 0 14.00 5.10 -5 -2 0 1333.97 58.79 5 -2 0 1355.26 61.69 -5 -2 0 1319.17 58.19 -5 -2 0 1311.57 60.19 5 -2 0 1295.47 59.69 5 -2 0 1349.77 64.59 5 -2 0 1316.87 61.39 -5 2 0 1311.27 60.79 5 2 0 1421.06 67.39 -5 2 0 1302.57 60.39 5 2 0 1380.96 60.49 5 2 0 1340.57 63.29 -6 -2 0 241.48 16.20 6 -2 0 259.87 17.60 6 -2 0 251.87 17.00 6 -2 0 258.17 20.00 -6 2 0 207.08 16.20 6 2 0 214.58 14.90 6 2 0 203.88 17.40 6 2 0 207.48 19.50 -6 2 0 194.18 14.90 7 -2 0 672.43 36.90 7 -2 0 671.83 36.20 7 -2 0 658.73 40.40 -7 -2 0 672.93 35.50 -7 2 0 675.53 35.30 7 2 0 621.04 37.20 -7 2 0 635.64 35.90 7 2 0 618.74 41.00 8 -2 0 247.98 20.10 8 -2 0 231.58 23.00 8 -2 0 263.87 20.20 -8 -2 0 233.48 19.40 8 2 0 257.07 24.50 -8 2 0 252.07 19.40 8 2 0 230.88 20.50 -8 2 0 261.97 20.40 -9 -2 0 229.78 20.90 9 -2 0 210.48 20.40 9 -2 0 244.08 20.70 9 2 0 249.28 22.10 -9 2 0 222.58 20.00 -9 2 0 262.27 21.60 -10 -2 0 277.17 24.10 10 -2 0 260.47 23.70 -10 2 0 270.77 24.40 -10 2 0 214.78 21.50 10 2 0 283.17 25.00 0 -3 0 0.20 1.80 0 -3 0 0.10 1.40 0 -3 0 -0.40 1.40 0 3 0 0.40 1.60 0 3 0 0.70 1.40 1 -3 0 1091.39 45.50 1 -3 0 1069.19 46.70 -1 -3 0 1001.30 45.10 -1 -3 0 978.90 44.90 1 -3 0 1050.59 45.10 1 3 0 995.10 46.30 -1 3 0 1016.90 45.20 1 3 0 968.60 44.80 -1 3 0 1028.20 46.50 -2 -3 0 2184.28 93.89 -2 -3 0 2276.17 93.59 2 -3 0 2206.18 92.39 2 -3 0 2228.38 91.99 2 -3 0 2201.58 95.29 2 -3 0 2253.77 93.89 2 -3 0 2281.57 93.49 -2 3 0 2063.89 92.39 -2 3 0 2266.97 93.39 2 3 0 2173.78 93.69 2 3 0 2104.19 95.49 -2 3 0 2116.49 93.69 -3 -3 0 1182.98 51.39 -3 -3 0 1136.89 52.49 3 -3 0 1155.58 52.89 3 -3 0 1145.39 53.39 3 -3 0 1164.58 51.99 -3 3 0 1208.78 52.59 3 3 0 1217.98 52.69 3 3 0 1191.28 54.29 3 3 0 1179.38 56.89 -3 3 0 1227.68 52.19 4 -3 0 685.83 33.70 4 -3 0 642.94 35.10 -4 -3 0 696.33 32.40 -4 -3 0 669.23 31.70 4 -3 0 686.23 32.20 4 -3 0 675.93 33.10 4 3 0 663.13 32.50 4 3 0 612.74 34.60 4 3 0 650.43 37.80 -4 3 0 685.63 32.70 -4 3 0 646.94 32.20 5 -3 0 752.42 35.80 5 -3 0 779.22 39.20 -5 -3 0 724.03 34.00 5 -3 0 734.13 36.00 5 -3 0 736.63 34.30 -5 -3 0 728.93 33.70 5 3 0 603.64 36.30 -5 3 0 607.34 34.00 5 3 0 652.33 40.20 -5 3 0 606.64 33.80 5 3 0 629.04 33.80 6 -3 0 139.79 14.50 6 -3 0 140.99 12.60 6 -3 0 138.09 12.50 -6 -3 0 140.29 11.70 6 3 0 108.19 14.50 6 3 0 102.69 12.70 -6 3 0 85.69 10.80 -6 3 0 96.79 10.70 7 -3 0 39.20 10.40 7 -3 0 26.40 7.60 -7 -3 0 31.50 7.60 7 -3 0 35.80 8.10 7 3 0 34.70 10.70 -7 3 0 32.10 8.20 -7 3 0 29.60 7.60 7 3 0 48.20 10.40 8 -3 0 185.98 17.60 -8 -3 0 179.58 16.90 8 -3 0 178.08 20.70 8 -3 0 195.68 18.30 -8 3 0 203.98 18.50 8 3 0 201.08 22.40 -8 3 0 211.28 17.50 8 3 0 210.68 19.30 9 -3 0 215.68 20.30 -9 -3 0 243.18 21.00 9 -3 0 193.58 20.20 9 3 0 248.68 22.50 -9 3 0 255.67 22.30 -9 3 0 245.48 21.10 -10 -3 0 13.10 8.80 10 -3 0 -1.60 6.10 -10 3 0 11.90 8.60 -10 3 0 12.70 9.30 10 3 0 13.50 8.50 0 -4 0 4044.40 165.18 0 -4 0 4142.49 167.48 0 -4 0 3933.91 165.18 0 -4 0 4054.39 165.48 0 4 0 3880.91 165.08 0 4 0 3940.91 165.18 0 4 0 3750.82 166.58 -1 -4 0 732.23 32.30 1 -4 0 724.23 32.50 1 -4 0 732.93 32.30 1 -4 0 717.33 30.20 1 -4 0 714.03 31.50 1 -4 0 673.03 33.60 1 4 0 594.84 30.90 -1 4 0 637.94 30.20 1 4 0 623.44 31.40 1 4 0 607.74 33.00 -2 -4 0 318.57 17.50 2 -4 0 320.97 15.90 2 -4 0 336.97 18.10 2 -4 0 313.77 15.90 -2 -4 0 321.77 17.70 2 -4 0 315.27 15.30 2 -4 0 306.57 18.80 2 -4 0 322.37 17.30 -2 4 0 288.07 17.40 -2 4 0 286.27 18.50 2 4 0 283.77 16.30 2 4 0 281.37 17.10 -2 4 0 292.17 16.10 -2 4 0 295.87 15.40 2 4 0 299.17 19.00 3 -4 0 437.06 25.40 -3 -4 0 418.56 24.50 3 -4 0 409.86 26.40 3 -4 0 440.56 24.70 -3 -4 0 445.66 22.80 3 -4 0 426.46 23.50 3 4 0 528.65 25.00 3 4 0 562.84 29.40 3 4 0 540.85 26.60 -3 4 0 520.85 24.70 -3 4 0 525.15 24.00 -3 4 0 530.65 26.30 -4 -4 0 625.94 32.40 -4 -4 0 604.84 30.60 4 -4 0 618.44 31.60 4 -4 0 615.24 35.20 4 -4 0 598.34 32.40 4 -4 0 603.24 33.20 4 4 0 685.33 32.50 -4 4 0 673.53 32.50 4 4 0 689.13 38.40 4 4 0 647.44 34.70 -4 4 0 727.83 34.40 -4 4 0 672.13 31.90 5 -4 0 44.00 8.30 5 -4 0 46.00 8.90 -5 -4 0 44.70 6.70 -5 -4 0 43.60 7.00 5 -4 0 42.50 7.00 5 -4 0 39.30 7.10 -5 4 0 47.80 7.50 5 4 0 37.00 8.10 -5 4 0 30.40 6.20 5 4 0 43.30 10.60 -6 -4 0 345.57 20.90 6 -4 0 356.06 23.40 6 -4 0 373.76 26.40 6 -4 0 352.86 23.00 6 4 0 336.47 24.50 -6 4 0 323.07 21.50 -6 4 0 321.67 21.60 6 4 0 345.57 27.80 7 -4 0 678.63 37.90 7 -4 0 664.63 37.70 -7 -4 0 656.83 35.00 7 -4 0 665.53 41.80 7 4 0 630.94 39.10 -7 4 0 618.84 35.50 -7 4 0 600.34 35.60 7 4 0 646.04 43.30 -8 -4 0 0.90 5.50 8 -4 0 5.70 5.70 8 -4 0 5.00 5.60 -8 4 0 2.10 6.20 8 4 0 5.80 6.30 -8 4 0 1.70 5.40 9 -4 0 217.88 20.80 9 -4 0 199.48 20.40 9 4 0 220.58 22.10 -9 4 0 198.08 19.20 -9 4 0 200.18 19.70 -9 4 0 210.58 20.50 0 -5 0 0.30 2.00 0 -5 0 -0.70 2.10 0 -5 0 -0.20 2.10 0 -5 0 0.70 2.30 0 5 0 0.30 2.10 0 5 0 1.00 2.60 0 5 0 -0.50 1.80 1 -5 0 1436.86 68.19 1 -5 0 1424.46 63.19 1 -5 0 1380.66 64.99 1 -5 0 1413.36 65.99 1 -5 0 1480.65 66.09 -1 -5 0 1396.76 65.69 -1 -5 0 1390.86 65.89 1 5 0 1583.64 65.59 1 5 0 1577.34 68.69 -1 5 0 1573.14 68.39 -1 5 0 1550.34 63.69 1 5 0 1544.95 65.99 -1 5 0 1520.85 66.29 2 -5 0 863.81 36.00 2 -5 0 835.12 40.50 -2 -5 0 820.12 38.20 2 -5 0 839.72 36.40 -2 -5 0 821.52 38.30 2 -5 0 852.21 38.10 2 -5 0 855.31 38.80 -2 5 0 706.63 35.60 2 5 0 716.13 36.50 -2 5 0 686.53 37.50 2 5 0 716.13 39.60 -2 5 0 717.53 39.50 2 5 0 715.03 37.50 -2 5 0 738.03 34.80 3 -5 0 26.40 6.10 3 -5 0 25.70 4.80 -3 -5 0 31.70 6.40 3 -5 0 25.80 5.50 3 -5 0 26.10 6.30 -3 5 0 30.00 6.70 -3 5 0 38.00 5.30 3 5 0 38.10 7.20 -3 5 0 31.60 6.10 3 5 0 36.10 5.90 -3 5 0 30.50 5.30 3 5 0 31.90 7.50 4 -5 0 9.60 3.70 -4 -5 0 7.90 4.00 4 -5 0 9.80 4.80 4 -5 0 7.90 4.10 4 -5 0 6.30 3.80 -4 5 0 3.30 2.80 -4 5 0 3.20 3.60 4 5 0 4.30 3.60 4 5 0 4.50 3.40 -4 5 0 2.10 2.80 4 5 0 7.50 5.30 5 -5 0 177.08 14.90 5 -5 0 185.68 15.90 -5 -5 0 180.68 14.70 5 -5 0 196.08 17.90 -5 5 0 205.08 15.00 -5 5 0 198.98 14.60 5 5 0 188.78 19.30 -5 5 0 196.78 15.90 5 5 0 191.48 16.90 6 -5 0 0.90 3.70 -6 -5 0 2.20 4.20 6 -5 0 -0.20 3.20 6 -5 0 0.60 4.70 6 5 0 1.40 5.00 -6 5 0 4.30 4.30 6 5 0 1.10 5.10 -6 5 0 2.20 4.10 -6 5 0 2.90 4.70 7 -5 0 503.95 31.90 7 -5 0 482.55 31.90 7 -5 0 500.05 35.80 7 5 0 522.05 38.60 -7 5 0 516.05 30.70 7 5 0 492.05 33.50 -7 5 0 504.65 32.50 -7 5 0 513.45 30.60 8 -5 0 268.17 23.80 8 -5 0 296.17 24.70 8 5 0 346.67 26.90 -8 5 0 315.77 25.00 -8 5 0 309.17 23.80 -8 5 0 314.77 23.90 9 -5 0 52.89 12.50 9 -5 0 71.19 14.60 -9 5 0 67.59 13.40 -9 5 0 67.59 13.50 -9 5 0 60.59 12.60 9 5 0 63.79 14.30 0 -6 0 375.46 21.10 0 -6 0 419.26 21.90 0 -6 0 368.26 23.20 0 -6 0 383.26 21.10 0 6 0 351.56 20.80 0 6 0 322.27 20.20 0 6 0 335.97 22.50 -1 -6 0 219.48 14.70 -1 -6 0 231.38 14.80 1 -6 0 218.28 14.60 1 -6 0 217.98 14.60 1 -6 0 222.68 14.00 1 -6 0 228.58 16.80 1 6 0 163.78 13.20 -1 6 0 187.18 14.20 -1 6 0 189.48 15.30 1 6 0 185.18 15.60 1 6 0 170.48 13.10 2 -6 0 145.59 13.50 -2 -6 0 148.69 12.60 2 -6 0 151.98 11.10 -2 -6 0 147.19 12.20 2 -6 0 146.89 12.30 2 -6 0 162.38 12.50 -2 6 0 153.38 12.50 -2 6 0 134.49 10.00 -2 6 0 152.08 13.90 2 6 0 145.79 11.30 2 6 0 141.19 13.90 -3 -6 0 611.04 31.10 3 -6 0 615.14 30.40 3 -6 0 613.64 31.40 3 -6 0 605.14 33.20 -3 -6 0 586.24 31.00 -3 6 0 505.35 27.60 -3 6 0 504.95 31.80 3 6 0 512.45 32.80 3 6 0 481.45 28.10 3 6 0 492.15 29.70 -3 6 0 479.65 29.70 -4 -6 0 984.40 49.50 4 -6 0 970.80 48.90 4 -6 0 947.11 49.99 4 -6 0 981.10 52.29 4 6 0 1045.80 54.89 -4 6 0 1001.00 52.59 4 6 0 999.70 50.49 -4 6 0 1019.60 50.49 -4 6 0 997.20 47.60 5 -6 0 124.89 14.70 5 -6 0 121.69 12.50 5 -6 0 118.29 12.90 -5 -6 0 137.59 13.30 5 6 0 92.29 12.90 -5 6 0 104.59 12.30 5 6 0 104.39 15.20 -5 6 0 119.99 11.60 6 -6 0 185.48 17.20 6 -6 0 182.08 19.80 -6 -6 0 212.78 17.30 6 -6 0 195.38 18.20 -6 6 0 217.38 18.80 6 6 0 207.38 22.70 6 6 0 212.18 19.70 -6 6 0 236.78 17.20 -6 6 0 212.78 17.20 7 -6 0 104.79 14.30 7 -6 0 123.49 14.60 -7 6 0 104.49 13.00 7 6 0 92.89 15.80 -7 6 0 90.29 13.40 -7 6 0 95.69 14.20 8 -6 0 165.78 18.30 8 -6 0 152.98 17.90 -8 6 0 151.38 17.20 -8 6 0 150.88 17.30 -8 6 0 133.09 17.60 8 6 0 158.18 19.40 0 -7 0 -1.20 3.40 0 -7 0 -0.90 3.10 0 -7 0 2.30 3.60 0 -7 0 0.80 3.20 0 7 0 0.20 2.80 0 7 0 -1.50 2.80 0 7 0 1.00 2.90 1 -7 0 119.59 11.90 1 -7 0 134.89 14.30 -1 -7 0 126.29 11.90 -1 -7 0 119.99 11.90 1 -7 0 134.99 12.10 1 -7 0 135.79 11.80 1 7 0 156.98 14.60 -1 7 0 153.38 12.50 1 7 0 144.99 11.90 -1 7 0 149.39 13.90 1 7 0 150.18 12.40 -1 7 0 149.29 12.70 2 -7 0 1247.78 61.29 2 -7 0 1245.28 60.79 2 -7 0 1234.78 63.99 2 -7 0 1250.67 59.29 -2 -7 0 1304.87 61.49 -2 -7 0 1259.97 61.49 2 7 0 1351.16 61.59 -2 7 0 1277.07 63.59 2 7 0 1298.97 59.89 -2 7 0 1347.87 61.89 2 7 0 1311.47 64.99 3 -7 0 100.39 11.10 3 -7 0 89.99 11.40 -3 -7 0 93.89 11.30 -3 -7 0 91.99 11.60 3 -7 0 84.69 12.10 3 7 0 100.19 11.10 -3 7 0 119.49 12.30 -3 7 0 102.99 12.90 -3 7 0 100.59 9.80 3 7 0 100.99 13.00 4 -7 0 451.25 28.40 4 -7 0 428.26 31.00 -4 -7 0 451.55 29.30 4 -7 0 469.55 29.80 4 7 0 537.95 34.70 -4 7 0 524.95 33.00 -4 7 0 521.05 27.80 -4 7 0 490.75 30.10 4 7 0 504.55 30.40 5 -7 0 81.49 11.40 5 -7 0 66.79 12.80 5 -7 0 78.49 10.80 -5 -7 0 80.19 11.00 5 7 0 71.89 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39.80 10.10 2 0 18 39.70 9.90 3 0 18 2.90 6.40 3 0 18 11.10 8.00 -3 0 -18 16.20 8.20 3 0 18 12.10 7.40 -4 0 -18 121.09 17.40 4 0 18 120.79 15.50 4 0 18 121.49 15.80 4 0 18 123.79 18.50 -6 -1 18 211.98 21.60 6 -1 -18 189.08 20.30 -6 -1 18 217.68 20.30 -6 1 18 200.08 20.50 -6 1 18 215.68 20.50 6 1 -18 194.28 20.80 -5 -1 18 44.20 10.30 5 -1 -18 34.90 10.10 -5 -1 18 35.50 10.40 5 1 -18 18.80 8.20 -5 1 18 25.40 8.80 -5 1 18 21.60 8.40 -4 -1 18 13.00 7.80 4 -1 -18 10.60 7.60 -4 -1 18 6.70 6.90 -4 1 18 4.70 6.00 4 1 -18 7.20 7.10 -4 1 18 9.30 7.20 3 -1 -18 158.98 18.20 -3 -1 18 164.28 17.60 -3 -1 18 165.28 16.90 -3 1 18 178.18 17.40 -3 1 18 165.58 17.20 3 1 -18 176.48 18.60 -2 -1 18 140.39 16.20 -2 -1 18 165.88 16.70 2 -1 -18 172.08 18.30 -2 1 18 171.68 16.40 2 1 -18 193.58 18.70 -2 1 18 181.68 17.00 -1 -1 18 80.39 12.40 -1 -1 18 87.19 13.10 1 -1 -18 77.09 13.60 -1 1 18 80.49 12.20 -1 1 18 110.59 13.60 1 1 -18 78.19 14.40 0 -1 -18 133.09 16.50 0 -1 18 128.59 15.60 0 -1 18 141.79 15.60 0 1 18 163.78 15.80 0 1 18 146.69 15.60 0 1 -18 161.58 17.40 -1 -1 -18 36.80 9.40 1 -1 18 34.30 9.20 1 -1 18 21.50 7.50 -1 -1 -18 24.80 8.90 1 1 18 19.00 7.60 1 1 18 28.10 8.40 -1 1 -18 23.90 8.70 2 -1 18 41.10 10.10 -2 -1 -18 39.10 10.00 2 -1 18 34.70 9.50 -2 -1 -18 36.10 10.20 2 1 18 41.20 9.80 2 1 18 28.30 8.20 2 1 18 38.20 11.00 -2 1 -18 28.70 8.90 3 -1 18 502.95 35.90 3 -1 18 507.15 33.30 -3 -1 -18 502.85 33.40 3 -1 18 531.25 33.10 3 1 18 494.75 31.90 3 1 18 514.15 41.70 3 1 18 522.35 36.80 -3 1 -18 523.85 34.20 -6 -2 18 35.90 11.40 -6 -2 18 31.00 9.60 6 -2 -18 36.20 11.10 -6 2 18 34.80 10.40 -6 2 18 34.10 10.00 6 2 -18 33.10 10.60 -5 -2 18 26.20 8.60 5 -2 -18 20.60 9.10 -5 -2 18 24.10 9.10 -5 2 18 51.29 11.40 -5 2 18 58.59 11.70 5 2 -18 53.09 12.40 4 -2 -18 40.20 10.80 -4 -2 18 46.60 11.20 -4 -2 18 46.90 10.50 -4 2 18 49.99 11.40 -4 2 18 63.59 12.20 4 2 -18 50.79 11.80 -3 -2 18 69.19 12.10 -3 -2 18 66.19 12.00 3 -2 -18 58.29 12.10 -3 2 18 71.59 12.30 3 2 -18 49.30 11.10 -2 -2 18 125.29 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-2 -3 18 82.39 13.70 -2 3 18 87.19 13.20 2 3 -18 88.09 14.60 -1 -3 18 63.99 11.80 -1 -3 18 62.69 11.80 1 -3 -18 57.69 12.70 -1 3 18 41.10 9.40 1 3 -18 53.69 11.90 0 -3 -18 295.37 25.10 0 -3 18 336.87 24.60 0 -3 18 314.27 24.80 0 3 18 306.47 22.80 0 3 -18 312.47 24.90 0 3 18 336.47 36.40 -1 -3 -18 145.59 17.90 1 -3 18 131.19 16.10 1 -3 18 107.69 16.40 -1 3 -18 165.98 17.40 1 3 18 164.88 15.60 1 3 18 144.89 18.70 -2 -3 -18 60.79 12.80 2 -3 18 58.99 12.20 2 -3 18 54.39 12.20 -2 3 -18 43.30 11.20 2 3 18 54.39 13.80 3 -3 18 51.89 11.40 -3 -3 -18 59.19 12.90 3 -3 18 43.80 11.20 3 3 18 53.89 14.30 -3 3 -18 46.20 11.90 5 -4 -18 110.49 18.10 -5 -4 18 110.29 17.40 -5 4 18 169.68 18.80 5 4 -18 169.78 20.00 -4 -4 18 138.69 15.90 4 -4 -18 139.79 18.60 -4 -4 18 124.09 18.10 4 4 -18 199.48 20.90 -4 4 18 170.28 17.80 -3 -4 18 82.69 13.00 -3 -4 18 95.09 15.60 3 -4 -18 76.59 14.20 -3 4 18 88.49 13.40 3 4 -18 68.69 13.80 -2 -4 18 53.49 11.50 2 -4 -18 43.10 11.70 -2 -4 18 55.79 10.70 2 4 -18 48.30 11.90 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17.30 1 -5 18 132.79 16.50 -1 -5 -18 135.19 17.40 1 5 18 132.69 20.60 -1 5 -18 128.19 17.30 5 0 -19 23.20 9.70 -5 0 19 17.30 8.80 -5 0 19 19.90 9.30 -4 0 19 88.79 14.10 -4 0 19 107.79 15.60 4 0 -19 98.89 16.70 -3 0 19 317.47 24.50 -3 0 19 320.57 24.90 3 0 -19 314.47 26.50 2 0 -19 294.17 25.20 -2 0 19 306.47 23.50 -2 0 19 312.47 24.10 -1 0 19 18.60 7.70 -1 0 19 17.10 7.80 1 0 -19 19.10 8.70 0 0 -19 56.89 11.80 0 0 19 52.89 11.20 0 0 19 54.49 10.60 -1 0 -19 12.20 7.40 -1 0 -19 4.10 7.10 1 0 19 9.10 6.40 1 0 19 14.50 7.50 -2 0 -19 7.60 7.10 -2 0 -19 1.80 7.90 2 0 19 5.90 6.60 2 0 19 7.40 7.00 -5 -1 19 4.30 7.30 -5 -1 19 10.10 7.80 5 -1 -19 3.40 6.90 5 1 -19 6.60 7.40 -5 1 19 2.70 7.40 -5 1 19 8.10 7.80 -4 -1 19 75.79 13.40 4 -1 -19 97.19 15.90 -4 -1 19 90.89 14.20 -4 1 19 62.59 12.20 -4 1 19 62.29 12.40 4 1 -19 83.79 15.40 3 -1 -19 51.69 12.30 -3 -1 19 45.40 11.00 -3 -1 19 52.19 11.30 -3 1 19 57.49 11.60 -3 1 19 66.59 12.60 3 1 -19 60.69 12.90 2 -1 -19 33.10 10.00 -2 -1 19 26.50 8.90 -2 -1 19 27.50 9.40 2 1 -19 32.70 9.90 -2 1 19 33.10 8.90 -2 1 19 25.80 8.90 -1 -1 19 44.20 10.50 1 -1 -19 34.40 10.60 -1 -1 19 42.10 10.60 -1 1 19 66.19 11.80 -1 1 19 46.40 10.40 1 1 -19 58.09 12.80 0 -1 19 206.28 19.60 0 -1 19 200.78 19.30 0 -1 -19 224.78 20.70 0 1 19 207.28 18.60 0 1 -19 216.38 20.70 0 1 19 204.38 18.60 1 -1 19 19.80 8.20 -1 -1 -19 14.90 8.40 -1 -1 -19 20.20 8.20 1 -1 19 22.60 8.20 1 1 19 30.60 8.90 -1 1 -19 29.90 9.30 1 1 19 25.10 8.70 -1 1 -19 25.80 8.90 -2 -1 -19 116.89 16.00 2 -1 19 108.69 15.40 -2 -1 -19 118.49 16.30 2 -1 19 107.69 15.70 2 1 19 101.29 14.80 -2 1 -19 88.09 14.70 -5 -2 19 326.77 25.60 -5 -2 19 321.47 27.00 5 -2 -19 320.17 27.50 -5 2 19 348.97 26.80 5 2 -19 322.67 27.60 4 -2 -19 146.99 18.50 -4 -2 19 142.29 17.20 -4 -2 19 142.59 16.50 4 2 -19 144.79 18.10 -4 2 19 127.39 16.70 3 -2 -19 405.16 30.10 -3 -2 19 376.06 27.30 -3 -2 19 379.36 28.20 -3 2 19 369.46 26.80 3 2 -19 334.87 28.20 2 -2 -19 40.70 11.30 -2 -2 19 60.69 11.80 -2 -2 19 40.40 10.20 -2 2 19 14.40 7.30 2 2 -19 21.60 8.70 -1 -2 19 30.70 9.40 1 -2 -19 25.30 9.90 -1 -2 19 20.10 8.60 1 2 -19 31.20 10.30 -1 2 19 37.70 9.20 0 -2 19 77.79 13.50 0 -2 19 85.29 13.60 0 -2 -19 81.09 14.40 0 2 19 120.39 14.00 0 2 -19 123.59 16.50 1 -2 19 161.48 17.60 -1 -2 -19 128.39 16.70 1 -2 19 133.59 16.40 1 2 19 169.38 16.90 -1 2 -19 166.98 18.20 -1 2 -19 177.18 18.70 2 -2 19 15.40 7.90 2 -2 19 14.00 8.00 -2 -2 -19 2.80 7.60 2 2 19 7.60 6.90 2 2 19 12.40 8.50 -2 2 -19 7.40 7.70 4 -3 -19 100.19 16.90 -4 -3 19 96.29 15.30 -4 -3 19 77.19 14.80 4 3 -19 120.49 17.00 -4 3 19 123.79 17.00 3 -3 -19 8.20 7.80 -3 -3 19 7.10 7.10 -3 -3 19 14.10 8.50 -3 3 19 5.90 7.00 3 3 -19 5.80 7.60 -2 -3 19 5.00 6.50 -2 -3 19 13.10 7.40 2 -3 -19 4.70 7.20 2 3 -19 2.90 6.20 -2 3 19 6.00 6.30 1 -3 -19 87.89 15.20 -1 -3 19 112.39 16.50 -1 -3 19 115.19 15.00 -1 3 19 112.19 14.60 1 3 -19 103.29 16.30 0 -3 19 179.78 19.40 0 -3 -19 195.38 20.70 0 -3 19 159.18 18.00 0 3 -19 185.58 19.60 0 3 19 198.18 18.00 1 -3 19 39.60 11.00 1 -3 19 41.00 10.70 -1 -3 -19 46.10 11.60 1 3 19 58.09 13.80 1 3 19 34.70 9.30 -1 3 -19 59.89 12.80 -1 3 -19 38.10 11.20 -2 -3 -19 45.60 12.00 2 -3 19 28.90 9.50 2 -3 19 39.30 11.20 2 3 19 20.90 10.60 -2 3 -19 31.50 10.30 3 -4 -19 92.99 16.60 -3 -4 19 92.09 14.00 -3 -4 19 96.59 15.80 3 4 -19 70.89 15.20 -3 4 19 61.39 12.50 2 -4 -19 154.08 18.40 -2 -4 19 140.19 16.40 -2 -4 19 128.19 16.40 2 4 -19 101.09 17.30 -2 4 19 105.59 15.10 -1 -4 19 9.20 6.20 1 -4 -19 5.10 7.70 -1 -4 19 3.50 6.90 1 4 -19 6.10 7.10 -1 4 19 7.30 6.90 0 -4 -19 178.48 20.60 0 -4 19 204.28 19.70 0 -4 19 186.08 19.80 0 4 -19 174.58 19.50 0 4 19 224.28 27.10 -1 -4 -19 132.59 18.60 1 -4 19 159.28 17.90 1 -4 19 137.09 18.30 1 4 19 202.88 22.50 -1 4 -19 181.18 20.00 4 0 -20 -1.30 6.20 -4 0 20 0.60 7.30 -4 0 20 6.40 7.70 3 0 -20 576.84 38.80 -3 0 20 613.84 37.50 -3 0 20 596.04 37.70 -2 0 20 62.59 11.80 2 0 -20 68.99 13.80 -2 0 20 62.79 12.00 -1 0 20 83.89 13.60 -1 0 20 81.09 13.60 1 0 -20 94.09 16.00 0 0 20 5.20 6.40 0 0 -20 7.60 7.80 0 0 20 6.10 6.60 -1 0 -20 3.90 7.20 1 0 20 2.40 6.40 1 0 20 3.30 6.80 -1 0 -20 6.70 7.30 -4 -1 20 42.80 11.50 -4 -1 20 49.30 11.20 4 -1 -20 51.09 12.60 -4 1 20 77.29 13.70 4 1 -20 68.79 14.30 -4 1 20 71.79 13.60 -3 -1 20 227.68 21.60 3 -1 -20 221.38 22.30 -3 -1 20 241.98 21.50 3 1 -20 199.88 22.10 -3 1 20 183.98 19.60 -3 1 20 200.08 19.90 -2 -1 20 168.58 18.70 -2 -1 20 189.48 19.10 2 -1 -20 179.78 20.40 -2 1 20 169.38 18.50 2 1 -20 176.38 19.80 -2 1 20 179.28 18.80 -1 -1 20 8.90 6.70 1 -1 -20 9.60 8.20 -1 -1 20 2.20 7.00 -1 1 20 9.80 7.40 -1 1 20 6.10 7.00 1 1 -20 11.70 8.60 0 -1 20 35.20 10.00 0 -1 -20 49.00 12.00 0 -1 20 60.29 12.00 0 1 -20 44.90 12.00 0 1 20 42.40 16.40 0 1 20 36.50 10.00 -1 -1 -20 228.38 22.60 1 -1 20 231.38 21.30 1 -1 20 256.27 22.50 -1 1 -20 234.68 22.10 1 1 20 237.88 21.20 -1 1 -20 214.78 21.80 -3 -2 20 243.58 23.00 3 -2 -20 237.28 22.90 -3 -2 20 258.57 22.10 3 2 -20 222.08 23.10 -3 2 20 213.68 20.50 2 -2 -20 14.00 8.50 -2 -2 20 18.50 8.90 -2 -2 20 6.40 7.20 -2 2 20 16.00 8.00 2 2 -20 14.00 9.30 1 -2 -20 50.89 12.30 -1 -2 20 70.29 13.70 -1 -2 20 70.39 13.30 -1 2 20 84.59 13.30 1 2 -20 94.79 15.70 0 -2 20 86.19 13.90 0 -2 20 93.99 15.10 0 -2 -20 81.99 15.60 0 2 20 117.49 15.00 0 2 -20 89.99 15.70 -2 -3 20 70.89 13.50 2 -3 -20 59.09 13.40 -2 -3 20 66.99 12.50 -2 3 20 52.59 11.30 2 3 -20 58.69 13.20 -1 -3 20 52.39 11.90 1 -3 -20 48.20 12.50 -1 -3 20 52.29 11.50 1 3 -20 49.50 12.60 -1 3 20 44.30 10.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 35897 _shelx_res_file ; TITL ot277_0m_a.res in P2(1) ot277_0m.res created by SHELXL-2018/3 at 23:02:13 on 08-Aug-2021 REM Old TITL OT277_0m in P2(1) REM SHELXT solution in P2(1) REM R1 0.046, Rweak 0.034, Alpha 0.008, Orientation as input REM Flack x = 0.028 ( 0.003 ) from Parsons' quotients REM Formula found by SHELXT: C16 O4 Cl2 Zn CELL 0.71073 7.3802 8.2491 14.5953 90 97.852 90 ZERR 2 0.0003 0.0003 0.0005 0 0.001 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O Cl Zn UNIT 32 36 4 4 4 2 EQIV $1 +X,-1+Y,+Z EQIV $2 -1+X,+Y,+Z DFIX 0.88 N1 H1a N1 H1b N2 H2a N2 H2b L.S. 10 PLAN 4 SIZE 0.111 0.16 0.5 TEMP -173.12 CONF HTAB N1 Cl1 HTAB N1 Cl2_$1 HTAB N2 Cl1 HTAB N2 O1_$2 BOND $H list 4 MORE -1 fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.007800 BASF 0.01568 FVAR 0.80409 ZN1 6 0.654483 0.681459 0.177553 11.00000 0.00830 0.01066 = 0.01290 0.00037 0.00197 0.00019 CL1 5 0.472298 0.603393 0.050277 11.00000 0.01314 0.02521 = 0.01136 0.00050 -0.00077 0.00219 CL2 5 0.813060 0.907295 0.191651 11.00000 0.01858 0.01049 = 0.02507 0.00124 0.00381 -0.00277 O1 4 0.851194 0.511614 0.204251 11.00000 0.01067 0.00975 = 0.01713 -0.00202 -0.00006 0.00071 O2 4 0.516771 0.667309 0.284427 11.00000 0.00825 0.02138 = 0.01428 -0.00054 0.00199 -0.00290 N1 3 0.709234 0.287599 0.140251 11.00000 0.01230 0.01129 = 0.03179 -0.00466 -0.00417 0.00078 H1A 2 0.719076 0.190446 0.128692 11.00000 -1.50000 H1B 2 0.616141 0.339552 0.113382 11.00000 -1.50000 N2 3 0.222771 0.648873 0.216914 11.00000 0.00940 0.02193 = 0.01173 0.00132 0.00211 -0.00157 H2A 2 0.253006 0.665058 0.163720 11.00000 -1.50000 H2B 2 0.113597 0.626877 0.220895 11.00000 -1.50000 C1 1 1.025853 0.268953 0.204864 11.00000 0.00933 0.00835 = 0.01356 -0.00007 0.00217 -0.00154 C2 1 1.113013 0.196631 0.135376 11.00000 0.01322 0.01344 = 0.01376 0.00058 0.00359 -0.00112 C3 1 1.272325 0.109212 0.162999 11.00000 0.01447 0.01713 = 0.02070 -0.00265 0.00769 0.00125 AFIX 43 H3 2 1.334536 0.060513 0.117218 11.00000 -1.20000 AFIX 0 C4 1 1.342864 0.091158 0.255458 11.00000 0.01271 0.01650 = 0.02366 0.00179 0.00120 0.00342 AFIX 43 H4 2 1.451212 0.029817 0.272382 11.00000 -1.20000 AFIX 0 C5 1 1.254792 0.162934 0.323270 11.00000 0.01567 0.01683 = 0.01530 0.00186 -0.00153 0.00163 AFIX 43 H5 2 1.301711 0.149691 0.386746 11.00000 -1.20000 AFIX 0 C6 1 1.097794 0.254175 0.297864 11.00000 0.01275 0.01234 = 0.01369 -0.00229 0.00303 -0.00156 AFIX 43 H6 2 1.039430 0.306526 0.343897 11.00000 -1.20000 AFIX 0 C7 1 0.853516 0.363410 0.181788 11.00000 0.01141 0.01067 = 0.01077 0.00161 0.00179 -0.00053 C8 1 1.040345 0.211053 0.033692 11.00000 0.02200 0.03196 = 0.01541 0.00013 0.00428 0.00302 AFIX 137 H8A 2 1.139556 0.190759 -0.003126 11.00000 -1.50000 H8B 2 0.991635 0.320424 0.020737 11.00000 -1.50000 H8C 2 0.942754 0.131322 0.017568 11.00000 -1.50000 AFIX 0 C9 1 0.290619 0.607397 0.380667 11.00000 0.00986 0.01225 = 0.01168 -0.00217 0.00170 -0.00359 C10 1 0.397458 0.509369 0.445748 11.00000 0.01260 0.01264 = 0.01471 -0.00093 -0.00114 -0.00185 C11 1 0.329630 0.475544 0.528210 11.00000 0.02205 0.01497 = 0.01494 0.00142 -0.00078 -0.00446 AFIX 43 H11 2 0.397722 0.406299 0.572177 11.00000 -1.20000 AFIX 0 C12 1 0.166106 0.539718 0.548047 11.00000 0.02241 0.01934 = 0.01369 -0.00150 0.00639 -0.00718 AFIX 43 H12 2 0.124588 0.515956 0.605376 11.00000 -1.20000 AFIX 0 C13 1 0.062760 0.638937 0.484000 11.00000 0.01399 0.01998 = 0.01642 -0.00410 0.00565 -0.00357 AFIX 43 H13 2 -0.049035 0.684050 0.497503 11.00000 -1.20000 AFIX 0 C14 1 0.124161 0.671712 0.400008 11.00000 0.01187 0.01384 = 0.01477 -0.00157 0.00148 -0.00134 AFIX 43 H14 2 0.053015 0.737965 0.355540 11.00000 -1.20000 AFIX 0 C15 1 0.349303 0.643200 0.289394 11.00000 0.01126 0.00978 = 0.01277 -0.00080 0.00174 -0.00001 C16 1 0.578029 0.434783 0.428761 11.00000 0.01459 0.02087 = 0.02118 0.00358 0.00082 0.00485 AFIX 137 H16A 2 0.563507 0.383911 0.367518 11.00000 -1.50000 H16B 2 0.615433 0.352757 0.476157 11.00000 -1.50000 H16C 2 0.671673 0.519549 0.431646 11.00000 -1.50000 AFIX 0 HKLF 4 REM ot277_0m_a.res in P2(1) REM wR2 = 0.0386, GooF = S = 1.001, Restrained GooF = 1.003 for all data REM R1 = 0.0179 for 5135 Fo > 4sig(Fo) and 0.0190 for all 5348 data REM 223 parameters refined using 5 restraints END WGHT 0.0078 0.0000 REM Highest difference peak 0.307, deepest hole -0.237, 1-sigma level 0.051 Q1 1 0.3126 0.6187 0.3382 11.00000 0.05 0.31 Q2 1 0.9467 0.3185 0.1817 11.00000 0.05 0.26 Q3 1 1.0781 0.1984 0.0912 11.00000 0.05 0.25 Q4 1 0.3534 0.4618 0.4790 11.00000 0.05 0.25 ; _shelx_res_checksum 10748 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' 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 Zn Zn1 0.65448(2) 0.68146(2) 0.17755(2) 0.01057(5) Uani d 1 . . Cl Cl1 0.47230(6) 0.60339(6) 0.05028(3) 0.01680(9) Uani d 1 . . Cl Cl2 0.81306(6) 0.90729(5) 0.19165(3) 0.01797(10) Uani d 1 . . O O1 0.85119(17) 0.51161(15) 0.20425(9) 0.0127(2) Uani d 1 . . O O2 0.51677(14) 0.66731(18) 0.28443(8) 0.0146(2) Uani d 1 . . N N1 0.7092(2) 0.28760(19) 0.14025(13) 0.0191(4) Uani d 1 . . H H1A 0.719(3) 0.190(3) 0.1287(15) 0.029 Uiso d 1 . . H H1B 0.616(3) 0.340(3) 0.1134(17) 0.029 Uiso d 1 . . N N2 0.2228(2) 0.64887(18) 0.21691(10) 0.0143(3) Uani d 1 . . H H2A 0.253(3) 0.665(3) 0.1637(13) 0.021 Uiso d 1 . . H H2B 0.114(3) 0.627(3) 0.2209(15) 0.021 Uiso d 1 . . C C1 1.0259(2) 0.2690(2) 0.20486(12) 0.0104(3) Uani d 1 . . C C2 1.1130(2) 0.1966(2) 0.13538(11) 0.0133(3) Uani d 1 . . C C3 1.2723(2) 0.1092(2) 0.16300(13) 0.0169(4) Uani d 1 . . H H3 1.334536 0.060513 0.117218 0.020 Uiso calc 1 . . C C4 1.3429(2) 0.0912(2) 0.25546(13) 0.0177(4) Uani d 1 . . H H4 1.451212 0.029817 0.272382 0.021 Uiso calc 1 . . C C5 1.2548(2) 0.1629(3) 0.32327(12) 0.0163(4) Uani d 1 . . H H5 1.301711 0.149691 0.386746 0.020 Uiso calc 1 . . C C6 1.0978(2) 0.2542(2) 0.29786(12) 0.0128(3) Uani d 1 . . H H6 1.039430 0.306526 0.343897 0.015 Uiso calc 1 . . C C7 0.8535(2) 0.3634(2) 0.18179(12) 0.0109(3) Uani d 1 . . C C8 1.0403(3) 0.2111(3) 0.03369(13) 0.0230(5) Uani d 1 . . H H8A 1.139556 0.190759 -0.003126 0.034 Uiso calc 1 . . H H8B 0.991635 0.320424 0.020737 0.034 Uiso calc 1 . . H H8C 0.942754 0.131322 0.017568 0.034 Uiso calc 1 . . C C9 0.2906(2) 0.6074(2) 0.38067(11) 0.0112(3) Uani d 1 . . C C10 0.3975(2) 0.5094(2) 0.44575(12) 0.0136(3) Uani d 1 . . C C11 0.3296(3) 0.4755(2) 0.52821(13) 0.0176(4) Uani d 1 . . H H11 0.397722 0.406299 0.572177 0.021 Uiso calc 1 . . C C12 0.1661(3) 0.5397(2) 0.54805(13) 0.0181(4) Uani d 1 . . H H12 0.124588 0.515956 0.605376 0.022 Uiso calc 1 . . C C13 0.0628(2) 0.6389(2) 0.48400(13) 0.0165(4) Uani d 1 . . H H13 -0.049035 0.684050 0.497503 0.020 Uiso calc 1 . . C C14 0.1242(2) 0.6717(3) 0.40001(11) 0.0135(3) Uani d 1 . . H H14 0.053015 0.737965 0.355540 0.016 Uiso calc 1 . . C C15 0.3493(2) 0.64320(19) 0.28939(12) 0.0113(3) Uani d 1 . . C C16 0.5780(3) 0.4348(2) 0.42876(14) 0.0190(4) Uani d 1 . . H H16A 0.563507 0.383911 0.367518 0.029 Uiso calc 1 . . H H16B 0.615433 0.352757 0.476157 0.029 Uiso calc 1 . . H H16C 0.671673 0.519549 0.431646 0.029 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 Zn1 0.00830(8) 0.01066(9) 0.01290(9) 0.00019(8) 0.00197(6) 0.00037(9) Cl1 0.01314(19) 0.0252(2) 0.01136(19) 0.00219(17) -0.00077(14) 0.00050(17) Cl2 0.0186(2) 0.01049(19) 0.0251(2) -0.00277(17) 0.00381(18) 0.00124(18) O1 0.0107(6) 0.0098(6) 0.0171(6) 0.0007(5) -0.0001(5) -0.0020(5) O2 0.0082(5) 0.0214(6) 0.0143(5) -0.0029(6) 0.0020(4) -0.0005(6) N1 0.0123(7) 0.0113(7) 0.0318(10) 0.0008(6) -0.0042(7) -0.0047(7) N2 0.0094(6) 0.0219(9) 0.0117(7) -0.0016(6) 0.0021(5) 0.0013(6) C1 0.0093(7) 0.0084(7) 0.0136(8) -0.0015(6) 0.0022(6) -0.0001(6) C2 0.0132(7) 0.0134(8) 0.0138(7) -0.0011(7) 0.0036(6) 0.0006(8) C3 0.0145(8) 0.0171(8) 0.0207(9) 0.0013(7) 0.0077(7) -0.0026(8) C4 0.0127(8) 0.0165(8) 0.0237(10) 0.0034(7) 0.0012(7) 0.0018(8) C5 0.0157(8) 0.0168(9) 0.0153(8) 0.0016(8) -0.0015(6) 0.0019(8) C6 0.0128(8) 0.0123(7) 0.0137(8) -0.0016(6) 0.0030(6) -0.0023(6) C7 0.0114(8) 0.0107(8) 0.0108(8) -0.0005(6) 0.0018(6) 0.0016(6) C8 0.0220(9) 0.0320(13) 0.0154(9) 0.0030(8) 0.0043(7) 0.0001(8) C9 0.0099(7) 0.0122(7) 0.0117(8) -0.0036(6) 0.0017(6) -0.0022(7) C10 0.0126(8) 0.0126(7) 0.0147(8) -0.0019(6) -0.0011(6) -0.0009(7) C11 0.0220(10) 0.0150(8) 0.0149(9) -0.0045(7) -0.0008(7) 0.0014(7) C12 0.0224(10) 0.0193(9) 0.0137(9) -0.0072(7) 0.0064(7) -0.0015(7) C13 0.0140(8) 0.0200(9) 0.0164(8) -0.0036(6) 0.0056(6) -0.0041(7) C14 0.0119(7) 0.0138(7) 0.0148(7) -0.0013(8) 0.0015(5) -0.0016(8) C15 0.0113(7) 0.0098(8) 0.0128(8) 0.0000(5) 0.0017(6) -0.0008(6) C16 0.0146(8) 0.0209(9) 0.0212(10) 0.0048(7) 0.0008(7) 0.0036(8) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 Cl2 Zn1 Cl1 . . 125.120(19) ? O1 Zn1 Cl1 . . 107.22(4) ? O1 Zn1 Cl2 . . 102.18(4) ? O2 Zn1 Cl1 . . 108.84(3) ? O2 Zn1 Cl2 . . 107.52(4) ? O2 Zn1 O1 . . 103.91(5) ? C7 O1 Zn1 . . 130.95(12) ? C15 O2 Zn1 . . 131.79(10) ? H1A N1 H1B . . 119(2) ? C7 N1 H1A . . 118.0(15) ? C7 N1 H1B . . 121.5(16) ? H2A N2 H2B . . 118(2) ? C15 N2 H2A . . 119.8(14) ? C15 N2 H2B . . 121.5(15) ? C2 C1 C7 . . 121.28(15) ? C6 C1 C2 . . 120.96(16) ? C6 C1 C7 . . 117.75(16) ? C1 C2 C8 . . 122.60(16) ? C3 C2 C1 . . 117.57(15) ? C3 C2 C8 . . 119.84(16) ? C2 C3 H3 . . 119.1 ? C4 C3 C2 . . 121.86(17) ? C4 C3 H3 . . 119.1 ? C3 C4 H4 . . 120.1 ? C3 C4 C5 . . 119.86(17) ? C5 C4 H4 . . 120.1 ? C4 C5 H5 . . 120.2 ? C4 C5 C6 . . 119.70(16) ? C6 C5 H5 . . 120.2 ? C1 C6 H6 . . 120.0 ? C5 C6 C1 . . 120.02(16) ? C5 C6 H6 . . 120.0 ? O1 C7 N1 . . 122.80(17) ? O1 C7 C1 . . 119.18(15) ? N1 C7 C1 . . 118.01(16) ? C2 C8 H8A . . 109.5 ? C2 C8 H8B . . 109.5 ? C2 C8 H8C . . 109.5 ? H8A C8 H8B . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C10 C9 C15 . . 121.02(15) ? C14 C9 C10 . . 120.54(16) ? C14 C9 C15 . . 118.44(15) ? C9 C10 C16 . . 123.15(16) ? C11 C10 C9 . . 117.69(17) ? C11 C10 C16 . . 119.12(16) ? C10 C11 H11 . . 119.0 ? C12 C11 C10 . . 122.04(17) ? C12 C11 H11 . . 119.0 ? C11 C12 H12 . . 120.0 ? C11 C12 C13 . . 119.91(18) ? C13 C12 H12 . . 120.0 ? C12 C13 H13 . . 120.2 ? C12 C13 C14 . . 119.52(18) ? C14 C13 H13 . . 120.2 ? C9 C14 H14 . . 119.9 ? C13 C14 C9 . . 120.27(16) ? C13 C14 H14 . . 119.9 ? O2 C15 N2 . . 122.81(16) ? O2 C15 C9 . . 119.34(14) ? N2 C15 C9 . . 117.86(15) ? C10 C16 H16A . . 109.5 ? C10 C16 H16B . . 109.5 ? C10 C16 H16C . . 109.5 ? H16A C16 H16B . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 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 Zn1 Cl1 . 2.2340(4) ? Zn1 Cl2 . 2.1947(5) ? Zn1 O1 . 2.0169(13) ? Zn1 O2 . 1.9781(11) ? O1 C7 . 1.266(2) ? O2 C15 . 1.2637(19) ? N1 H1A . 0.82(2) ? N1 H1B . 0.858(19) ? N1 C7 . 1.310(2) ? N2 H2A . 0.847(18) ? N2 H2B . 0.836(18) ? N2 C15 . 1.313(2) ? C1 C2 . 1.406(2) ? C1 C6 . 1.394(2) ? C1 C7 . 1.490(2) ? C2 C3 . 1.391(2) ? C2 C8 . 1.512(2) ? C3 H3 . 0.9500 ? C3 C4 . 1.386(3) ? C4 H4 . 0.9500 ? C4 C5 . 1.389(3) ? C5 H5 . 0.9500 ? C5 C6 . 1.389(2) ? C6 H6 . 0.9500 ? C8 H8A . 0.9800 ? C8 H8B . 0.9800 ? C8 H8C . 0.9800 ? C9 C10 . 1.405(2) ? C9 C14 . 1.402(2) ? C9 C15 . 1.486(2) ? C10 C11 . 1.393(3) ? C10 C16 . 1.519(3) ? C11 H11 . 0.9500 ? C11 C12 . 1.384(3) ? C12 H12 . 0.9500 ? C12 C13 . 1.389(3) ? C13 H13 . 0.9500 ? C13 C14 . 1.390(2) ? C14 H14 . 0.9500 ? C16 H16A . 0.9800 ? C16 H16B . 0.9800 ? C16 H16C . 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 _geom_hbond_publ_flag N1 H1A Cl2 1_545 0.82(2) 2.57(2) 3.2916(17) 146.9(19) yes N1 H1B Cl1 . 0.858(19) 2.54(2) 3.3077(17) 150(2) yes N2 H2A Cl1 . 0.847(18) 2.520(19) 3.2667(16) 148(2) yes N2 H2B O1 1_455 0.836(18) 2.141(19) 2.949(2) 163(2) yes 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 _geom_torsion_publ_flag Zn1 O1 C7 N1 . . . . -6.3(3) ? Zn1 O1 C7 C1 . . . . 174.92(12) ? Zn1 O2 C15 N2 . . . . -11.9(3) ? Zn1 O2 C15 C9 . . . . 168.30(12) ? C1 C2 C3 C4 . . . . 0.9(3) ? C2 C1 C6 C5 . . . . -1.9(3) ? C2 C1 C7 O1 . . . . -119.46(19) ? C2 C1 C7 N1 . . . . 61.7(2) ? C2 C3 C4 C5 . . . . -0.7(3) ? C3 C4 C5 C6 . . . . -0.8(3) ? C4 C5 C6 C1 . . . . 2.1(3) ? C6 C1 C2 C3 . . . . 0.5(3) ? C6 C1 C2 C8 . . . . -179.44(18) ? C6 C1 C7 O1 . . . . 60.7(2) ? C6 C1 C7 N1 . . . . -118.08(19) ? C7 C1 C2 C3 . . . . -179.36(16) ? C7 C1 C2 C8 . . . . 0.7(3) ? C7 C1 C6 C5 . . . . 177.87(16) ? C8 C2 C3 C4 . . . . -179.24(17) ? C9 C10 C11 C12 . . . . -2.2(3) ? C10 C9 C14 C13 . . . . -0.1(3) ? C10 C9 C15 O2 . . . . -38.3(2) ? C10 C9 C15 N2 . . . . 141.92(17) ? C10 C11 C12 C13 . . . . 1.1(3) ? C11 C12 C13 C14 . . . . 0.6(3) ? C12 C13 C14 C9 . . . . -1.1(3) ? C14 C9 C10 C11 . . . . 1.7(3) ? C14 C9 C10 C16 . . . . 179.43(17) ? C14 C9 C15 O2 . . . . 142.68(18) ? C14 C9 C15 N2 . . . . -37.1(2) ? C15 C9 C10 C11 . . . . -177.30(16) ? C15 C9 C10 C16 . . . . 0.4(3) ? C15 C9 C14 C13 . . . . 178.94(16) ? C16 C10 C11 C12 . . . . 179.92(17) ? _cod_database_fobs_code 2244186