#------------------------------------------------------------------------------ #$Date: 2022-11-08 20:40:22 +0100 (Tue, 08 Nov 2022) $ #$Revision: 279112 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022677.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_2022677 loop_ _publ_author_name 'Bosch, Eric' 'Bowling, Nathan P.' 'Speetzen, Erin D.' _publ_section_title ; A structural and computational comparison of close contacts and related intermolecular energies of interaction in the structures of 1,3-diiodo-5-nitrobenzene, 1,3-dibromo-5-nitrobenzene, and 1,3-dichloro-5-nitrobenzene ; _journal_coeditor_code DV3019 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 552 _journal_page_last 558 _journal_paper_doi 10.1107/S2053229622009275 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C6 H3 Cl2 N O2' _chemical_formula_sum 'C6 H3 Cl2 N O2' _chemical_formula_weight 191.99 _chemical_name_systematic ; 1,3-Dichloro-5-nitrobenzene ; _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 94.6320(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 3.8115(3) _cell_length_b 13.6452(11) _cell_length_c 6.8976(5) _cell_measurement_reflns_used 2128 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.90 _cell_measurement_theta_min 2.96 _cell_volume 357.56(5) _computing_cell_refinement ; SMART (Bruker, 2014) ; _computing_data_collection ; SMART (Bruker, 2014) ; _computing_data_reduction ; SAINT (Bruker, 2014) ; _computing_molecular_graphics ; X-SEED (Barbour, 2020) ; _computing_publication_material ; X-SEED (Barbour, 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.3660 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_unetI/netI 0.0145 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 4560 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.061 _diffrn_reflns_theta_min 2.963 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.7019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2014) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.783 _exptl_crystal_description 'cut rod' _exptl_crystal_F_000 192 _exptl_crystal_size_max 0.367 _exptl_crystal_size_mid 0.128 _exptl_crystal_size_min 0.033 _refine_diff_density_max 0.372 _refine_diff_density_min -0.215 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 813 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.117 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0275 _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^)+(0.0398P)^2^+0.1267P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.0705 _reflns_number_gt 747 _reflns_number_total 813 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file dv3019sup1.cif _cod_data_source_block 3 _cod_depositor_comments 'Adding full bibliography for 2022675--2022677.cif.' _cod_original_sg_symbol_H-M 'P 21/m' _cod_database_code 2022677 _cod_database_fobs_code 2022677 _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_hkl_file ; 1 0 0 3.60 1.20 1 0 0 3.30 1.00 -1 0 0 4.40 1.00 2 0 0 422.46 10.30 2 0 0 432.96 9.60 -2 0 0 443.56 9.20 3 0 0 270.17 8.90 3 0 0 275.37 9.80 -3 0 0 278.17 8.60 4 0 0 550.34 16.80 4 0 0 554.44 15.60 -4 0 0 545.05 14.70 0 -1 0 -0.80 0.20 0 1 0 -0.40 0.20 0 1 0 -0.70 0.10 1 -1 0 868.81 12.90 1 -1 0 861.81 12.70 1 1 0 847.32 11.00 -1 1 0 869.71 12.10 1 1 0 848.82 12.80 1 1 0 836.92 12.00 1 1 0 872.01 12.10 -2 -1 0 677.03 12.20 2 -1 0 667.53 13.40 2 -1 0 665.53 12.90 2 1 0 671.43 12.40 -2 1 0 657.03 12.10 2 1 0 682.83 13.50 -3 -1 0 11.70 2.50 3 -1 0 11.60 2.80 3 -1 0 12.70 3.10 3 1 0 9.20 2.50 -3 1 0 10.30 2.40 3 1 0 10.30 2.70 4 -1 0 95.49 8.90 4 -1 0 94.39 6.90 -4 -1 0 79.99 6.80 4 1 0 81.69 8.10 -4 1 0 81.49 6.90 4 1 0 86.29 6.40 0 -2 0 539.75 7.40 0 -2 0 522.75 7.10 0 2 0 538.05 7.40 0 2 0 526.75 6.90 1 -2 0 2847.71 34.60 1 -2 0 2816.02 34.40 1 2 0 2824.22 33.30 1 2 0 2758.42 33.00 -1 2 0 2837.12 33.70 1 2 0 2773.82 34.40 1 2 0 2850.41 33.80 2 -2 0 0.00 1.10 -2 -2 0 0.70 1.00 2 -2 0 -0.50 1.30 2 2 0 -0.10 1.10 -2 2 0 0.90 1.10 2 2 0 -0.20 1.20 3 -2 0 381.16 11.20 3 -2 0 397.96 12.00 -3 -2 0 379.16 10.30 3 2 0 374.06 10.40 3 2 0 374.86 11.70 -3 2 0 378.86 10.20 -4 -2 0 68.89 6.50 4 -2 0 68.59 7.10 4 -2 0 73.69 8.20 -4 2 0 71.39 6.70 4 2 0 60.59 6.20 4 2 0 65.99 7.20 0 -3 0 -0.40 0.70 0 -3 0 0.20 0.70 0 3 0 -1.10 0.60 0 3 0 -0.30 0.70 1 -3 0 1380.16 19.40 1 3 0 1368.76 18.60 1 3 0 1353.36 17.70 1 3 0 1376.96 18.30 1 3 0 1405.36 18.90 -1 3 0 1382.46 18.50 2 -3 0 391.16 9.80 2 -3 0 399.96 10.00 -2 3 0 397.46 8.90 2 3 0 398.86 8.70 2 3 0 399.96 9.90 2 3 0 395.26 9.00 -3 -3 0 108.89 5.60 3 -3 0 124.19 6.60 -3 -3 0 111.89 4.40 3 -3 0 105.49 6.40 3 3 0 97.79 6.20 3 3 0 110.39 5.60 -3 3 0 100.69 5.60 -4 -3 0 2.80 2.40 4 -3 0 0.30 3.10 4 -3 0 6.60 3.30 4 3 0 4.00 2.80 4 3 0 4.30 2.80 -4 3 0 3.40 2.80 0 -4 0 85.79 2.80 0 -4 0 83.99 3.10 0 4 0 89.39 2.60 0 4 0 87.29 3.10 1 -4 0 117.69 3.20 1 -4 0 115.49 4.30 -1 4 0 108.79 3.70 -1 4 0 115.19 3.90 1 4 0 115.99 3.80 1 4 0 117.19 3.40 2 -4 0 92.09 4.70 -2 -4 0 98.79 4.00 2 -4 0 108.29 5.20 2 4 0 98.99 4.50 2 4 0 99.39 4.10 -2 4 0 101.99 4.50 2 4 0 98.49 4.80 3 -4 0 167.28 7.70 3 -4 0 176.58 8.20 -3 -4 0 174.08 7.10 -3 -4 0 171.28 5.80 -3 4 0 175.68 7.10 3 4 0 166.38 7.80 3 4 0 173.38 6.90 -4 -4 0 34.10 4.70 4 -4 0 42.80 6.20 -4 4 0 34.60 5.00 -4 4 0 43.40 6.00 4 4 0 27.20 5.30 4 4 0 40.00 5.20 0 -5 0 -5.00 0.90 0 -5 0 -3.60 1.00 0 5 0 -5.20 0.70 0 5 0 -4.90 0.90 1 -5 0 975.10 16.00 -1 -5 0 1000.80 14.30 1 -5 0 993.50 14.20 -1 -5 0 1001.00 15.60 -1 5 0 1033.20 15.50 1 5 0 988.70 15.60 -1 5 0 986.70 14.90 1 5 0 980.10 15.10 2 -5 0 1574.14 25.00 -2 -5 0 1521.45 22.50 -2 5 0 1497.95 23.90 2 5 0 1513.45 24.00 2 5 0 1542.75 23.50 -2 5 0 1572.04 23.20 2 5 0 1526.95 22.00 3 -5 0 193.18 8.60 -3 -5 0 197.18 6.70 -3 -5 0 201.38 8.00 3 5 0 201.78 8.70 -3 5 0 189.18 8.30 -3 5 0 205.58 7.80 3 5 0 201.08 7.20 4 -5 0 16.00 4.20 -4 -5 0 12.20 3.30 4 5 0 14.20 4.10 -4 5 0 15.10 4.20 4 5 0 14.60 3.40 -4 5 0 15.30 3.80 0 -6 0 19.30 2.30 0 -6 0 23.10 2.30 0 6 0 24.70 2.50 0 6 0 22.80 1.90 1 -6 0 357.56 8.70 -1 -6 0 346.57 8.20 -1 -6 0 357.86 7.10 1 -6 0 354.26 7.40 1 6 0 349.87 8.20 -1 6 0 356.46 8.10 -1 6 0 350.86 7.50 1 6 0 345.47 7.60 -2 -6 0 262.37 7.60 2 -6 0 261.77 8.60 -2 6 0 248.18 7.70 2 6 0 269.07 8.10 2 6 0 261.87 6.90 -2 6 0 271.97 8.10 2 6 0 278.27 8.10 -3 -6 0 384.36 10.10 3 -6 0 386.16 12.30 3 6 0 385.66 11.30 -3 6 0 371.36 11.90 3 6 0 390.66 10.30 3 6 0 398.46 12.30 -3 6 0 369.16 10.70 4 -6 0 57.69 7.40 -4 -6 0 62.39 6.60 -4 6 0 59.99 6.20 -4 6 0 47.60 6.50 4 6 0 64.49 7.40 0 -7 0 -0.20 1.10 0 -7 0 1.10 1.10 0 7 0 0.50 1.10 0 7 0 -1.10 0.80 1 -7 0 386.26 9.40 -1 -7 0 381.66 7.70 -1 -7 0 382.36 9.20 1 -7 0 374.46 8.20 1 7 0 381.96 9.10 -1 7 0 366.66 7.90 1 7 0 377.56 8.10 -1 7 0 380.76 9.00 2 -7 0 453.45 12.00 -2 -7 0 455.05 10.80 -2 -7 0 438.86 9.60 2 7 0 439.46 10.80 -2 7 0 446.96 10.90 -2 7 0 441.66 10.90 2 7 0 447.46 11.10 -3 -7 0 40.60 4.30 3 -7 0 34.10 5.30 -3 7 0 32.40 4.50 3 7 0 35.00 3.90 3 7 0 38.80 5.00 3 7 0 45.80 5.20 -3 7 0 41.00 5.10 4 -7 0 29.80 5.90 -4 -7 0 43.40 5.60 4 7 0 37.70 5.90 -4 7 0 29.60 4.80 -4 7 0 45.10 6.40 0 -8 0 1132.09 18.70 0 -8 0 1143.59 17.70 0 8 0 1138.29 16.30 0 8 0 1157.38 18.80 1 -8 0 454.15 10.80 -1 -8 0 458.55 9.00 1 -8 0 463.45 9.80 -1 -8 0 444.96 10.70 -1 8 0 452.75 10.40 1 8 0 450.55 10.60 -1 8 0 441.76 9.30 1 8 0 451.25 9.30 -2 -8 0 161.18 6.60 2 -8 0 148.89 7.20 2 -8 0 150.58 4.90 -2 -8 0 164.48 5.70 -2 8 0 162.88 6.40 -2 8 0 162.28 6.60 2 8 0 155.58 6.30 2 8 0 151.18 6.60 3 -8 0 93.09 6.90 -3 -8 0 86.09 5.70 3 8 0 84.29 5.90 -3 8 0 84.99 6.10 3 8 0 90.09 6.20 -3 8 0 98.69 6.30 -4 -8 0 110.59 7.80 4 -8 0 103.59 9.80 4 8 0 105.29 8.20 -4 8 0 98.59 8.00 -4 8 0 92.49 7.90 0 -9 0 1.90 1.40 0 -9 0 2.00 1.40 0 9 0 0.70 0.90 0 9 0 1.20 1.30 -1 -9 0 153.68 5.10 1 -9 0 151.78 5.70 -1 -9 0 166.18 6.60 1 -9 0 152.58 6.40 -1 9 0 156.78 6.30 1 9 0 144.89 6.10 1 9 0 156.78 5.20 -1 9 0 155.78 5.30 2 -9 0 36.60 4.90 2 -9 0 30.40 3.10 -2 -9 0 37.90 4.60 -2 -9 0 31.50 3.40 -2 9 0 37.30 4.40 -2 9 0 29.20 3.60 2 9 0 31.30 3.90 2 9 0 26.90 3.50 3 -9 0 0.40 2.80 -3 -9 0 2.00 2.30 3 9 0 -1.80 1.80 -3 9 0 1.10 2.10 -3 9 0 1.10 2.30 3 9 0 -0.60 2.30 -4 -9 0 11.60 3.80 4 -9 0 17.20 5.10 -4 9 0 12.90 4.30 -4 9 0 9.30 3.50 4 9 0 8.70 4.00 0 -10 0 3602.44 48.10 0 -10 0 3617.94 46.40 0 10 0 3619.94 44.10 0 10 0 3621.44 48.30 1 -10 0 86.19 4.90 1 -10 0 96.09 5.50 -1 -10 0 92.09 4.40 -1 -10 0 113.19 6.00 -1 10 0 100.89 4.60 1 10 0 101.99 5.50 1 10 0 106.99 4.50 -1 10 0 96.49 5.40 2 -10 0 49.90 4.10 -2 -10 0 41.40 5.00 2 -10 0 39.80 5.20 2 10 0 50.19 4.00 -2 10 0 44.10 4.70 2 10 0 53.29 5.30 -2 10 0 48.90 4.70 3 -10 0 280.77 11.90 -3 -10 0 268.67 10.10 3 10 0 269.77 10.50 -3 10 0 265.27 10.20 -3 10 0 255.27 10.10 3 10 0 263.57 10.60 0 -11 0 2.80 1.90 0 -11 0 5.30 2.10 0 11 0 2.20 1.80 0 11 0 1.80 1.20 -1 -11 0 307.17 10.20 1 -11 0 303.17 9.90 -1 -11 0 306.17 8.20 1 -11 0 310.27 9.30 -1 11 0 305.97 8.40 1 11 0 319.77 10.10 1 11 0 305.97 8.00 -1 11 0 307.77 9.90 2 -11 0 206.98 9.40 2 -11 0 211.68 7.20 -2 -11 0 229.98 9.30 -2 11 0 213.28 7.90 2 11 0 231.28 8.10 -2 11 0 188.78 8.40 2 11 0 219.98 8.90 3 -11 0 21.20 4.90 -3 -11 0 12.10 3.70 -3 11 0 13.00 3.50 3 11 0 11.00 3.20 3 11 0 22.00 4.50 -3 11 0 10.50 3.50 0 -12 0 109.09 5.70 0 -12 0 107.29 6.10 0 12 0 96.89 6.00 1 -12 0 486.05 13.00 1 -12 0 464.45 12.10 -1 -12 0 482.75 13.40 1 12 0 443.76 12.80 -1 12 0 464.75 13.00 2 -12 0 7.10 2.50 -2 -12 0 2.30 2.70 2 -12 0 8.00 3.50 2 12 0 6.10 2.90 -2 12 0 6.10 2.80 3 -12 0 170.08 10.30 -3 -12 0 158.58 8.90 3 12 0 159.98 9.10 -3 12 0 147.79 8.70 0 -13 0 0.20 2.10 0 -13 0 1.40 1.90 0 13 0 -3.20 1.50 -1 -13 0 226.08 9.60 1 -13 0 219.98 8.60 1 -13 0 238.48 9.30 -1 13 0 225.98 9.60 1 13 0 229.08 9.50 2 -13 0 163.68 9.10 -2 -13 0 162.68 8.80 2 13 0 166.68 8.50 -2 13 0 148.79 8.10 3 -13 0 91.09 9.70 -3 -13 0 70.89 7.70 -3 13 0 72.19 7.60 3 13 0 68.09 7.50 0 -14 0 233.18 9.80 0 14 0 231.68 9.90 -1 -14 0 14.90 3.70 1 -14 0 20.30 3.80 1 -14 0 9.80 3.40 1 14 0 10.10 3.20 -1 14 0 9.90 3.50 -2 -14 0 1.40 3.30 2 -14 0 6.00 3.70 -2 14 0 2.10 2.90 2 14 0 3.00 2.80 0 -15 0 0.80 2.60 0 15 0 -3.60 2.10 -1 -15 0 115.39 7.80 1 -15 0 116.59 7.70 1 -15 0 116.59 7.40 -1 15 0 106.69 7.60 1 15 0 105.59 7.60 -2 -15 0 542.15 16.90 2 -15 0 561.84 17.20 2 15 0 512.65 16.10 -2 15 0 513.95 16.20 0 -16 0 84.79 8.60 0 16 0 64.39 7.20 1 -16 0 41.20 6.80 1 -16 0 44.50 6.10 -1 -16 0 67.49 7.70 -1 16 0 69.79 7.50 1 16 0 49.20 6.60 0 -17 0 8.10 3.90 0 17 0 1.60 3.40 1 -17 0 167.88 9.50 -1 17 0 141.09 9.40 1 17 0 138.69 9.40 -4 0 1 46.30 5.20 4 0 -1 32.70 5.30 4 0 -1 41.50 5.60 3 0 -1 65.59 4.80 -3 0 1 60.19 4.00 3 0 -1 67.49 6.30 2 0 -1 1471.65 22.40 2 0 -1 1444.36 22.90 -2 0 1 1445.26 20.30 2 0 -1 1485.15 19.10 -1 0 1 5941.01 67.59 -1 0 1 5838.72 65.29 1 0 -1 5884.81 67.49 1 0 -1 5846.11 67.59 0 0 1 222.48 4.00 0 0 -1 221.68 3.40 0 0 1 218.58 4.20 1 0 1 9999.00 114.29 1 0 1 9848.62 110.09 -1 0 -1 9885.31 110.89 -2 0 -1 994.90 16.70 2 0 1 994.70 16.30 2 0 1 994.60 17.70 3 0 1 91.49 5.30 3 0 1 90.89 6.00 -3 0 -1 91.69 5.50 4 0 1 67.79 6.60 -4 0 -1 63.99 6.50 4 0 1 65.19 7.60 4 -1 -1 0.70 2.40 -4 -1 1 1.60 2.20 -4 1 1 2.10 3.00 4 1 -1 3.20 2.60 4 1 -1 1.70 2.60 -4 1 1 3.00 2.40 3 -1 -1 554.44 13.90 3 -1 -1 531.45 14.20 -3 -1 1 567.64 12.20 -3 1 1 565.54 12.00 3 1 -1 560.74 14.40 3 1 -1 555.84 13.50 2 -1 -1 132.59 5.60 2 -1 -1 147.79 5.60 -2 -1 1 146.39 4.50 -2 1 1 145.89 4.50 2 1 -1 144.39 5.40 2 1 -1 142.89 4.10 2 1 -1 141.99 5.60 1 -1 -1 62.69 2.90 1 -1 -1 60.69 2.30 -1 1 1 60.09 2.90 1 1 -1 58.69 2.70 -1 1 1 62.79 2.00 1 1 -1 63.09 2.80 1 1 -1 62.89 2.10 1 1 -1 61.59 2.40 0 -1 1 36.70 1.50 0 -1 1 33.70 1.70 0 -1 -1 35.60 1.20 0 -1 -1 35.80 1.60 0 1 -1 35.50 1.40 0 1 1 31.60 1.90 0 1 -1 34.20 1.60 0 1 1 34.70 1.20 1 -1 1 6848.71 78.69 -1 -1 -1 6818.62 78.29 -1 -1 -1 6870.41 76.49 1 -1 1 6832.02 78.29 -1 1 -1 6924.31 78.49 1 1 1 7015.40 79.19 1 1 1 6912.31 76.99 -2 -1 -1 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6.10 0 7 7 69.79 8.70 -1 -7 -7 131.29 9.00 1 -7 7 120.29 9.00 -1 7 -7 135.89 8.00 -1 7 -7 141.39 8.20 1 7 7 116.99 9.20 -2 -8 7 23.50 6.20 2 -8 -7 30.70 5.50 -2 8 7 23.50 7.00 2 8 -7 20.60 4.80 1 -8 -7 0.90 3.10 -1 -8 7 -2.10 3.20 1 8 -7 -1.30 3.00 -1 8 7 0.50 3.90 0 -8 -7 50.99 7.20 0 -8 7 44.50 7.10 0 8 7 50.89 7.90 0 8 -7 51.19 6.80 1 -8 7 288.87 13.40 -1 -8 -7 280.17 12.60 1 8 7 228.68 12.60 -1 8 -7 298.57 11.50 -1 8 -7 277.57 11.30 1 -9 -7 6.10 3.90 -1 -9 7 8.90 4.40 -1 9 7 3.40 3.80 1 9 -7 7.60 3.90 0 -9 7 19.80 5.60 0 -9 -7 22.70 5.50 0 9 -7 26.40 5.20 0 9 7 38.70 6.90 -1 -9 -7 5.90 4.30 1 -9 7 4.10 4.10 1 9 7 13.00 4.60 -1 9 -7 6.20 3.80 -1 9 -7 11.70 3.80 -1 -10 7 32.50 6.70 1 -10 -7 39.00 6.60 -1 10 7 23.30 6.10 1 10 -7 30.90 5.80 0 -10 7 251.97 13.00 0 -10 -7 223.48 12.00 0 10 -7 251.57 11.80 0 10 7 261.07 13.30 -2 0 8 96.79 10.50 -2 0 8 115.29 11.00 2 0 -8 122.59 8.90 -1 0 8 255.07 12.20 -1 0 8 267.27 11.90 1 0 -8 270.17 12.10 0 0 -8 367.96 13.70 0 0 8 378.46 14.10 0 0 8 377.16 12.90 1 0 8 25.80 5.60 -1 0 -8 23.60 4.90 -2 -1 8 75.09 9.10 -2 -1 8 73.39 9.40 2 -1 -8 72.99 7.90 2 1 -8 63.69 7.60 -2 1 8 80.19 9.90 -2 1 8 77.19 8.80 1 -1 -8 0.80 3.60 -1 -1 8 1.30 3.60 -1 -1 8 -1.60 3.10 -1 1 8 0.80 3.30 -1 1 8 0.50 3.90 1 1 -8 -0.50 3.00 0 -1 8 16.50 4.40 0 -1 8 20.10 4.80 0 -1 -8 23.50 5.00 0 1 8 18.20 5.00 0 1 -8 16.90 4.50 1 -1 8 50.69 7.10 -1 -1 -8 51.99 6.80 -1 1 -8 55.49 6.60 1 1 8 44.90 6.80 2 -2 -8 89.39 8.60 -2 -2 8 70.49 9.00 -2 -2 8 83.69 9.80 -2 2 8 92.99 9.50 2 2 -8 68.09 8.10 -2 2 8 78.99 10.00 -1 -2 8 143.29 9.00 -1 -2 8 152.18 9.40 1 -2 -8 155.78 9.50 1 2 -8 159.58 9.80 -1 2 8 161.28 9.20 -1 2 8 152.08 10.20 0 -2 8 11.80 4.20 0 -2 -8 9.70 4.10 0 -2 8 20.10 4.90 0 2 8 10.20 4.30 0 2 -8 10.90 4.00 -1 -2 -8 -5.60 2.50 1 -2 8 5.80 4.00 1 -2 8 2.40 3.40 1 2 8 2.30 3.50 -1 2 -8 1.30 3.10 2 -3 -8 149.39 9.40 -2 -3 8 126.79 10.10 -2 3 8 114.79 12.20 2 3 -8 138.09 9.50 -2 3 8 149.79 10.00 -1 -3 8 18.00 5.20 1 -3 -8 10.60 4.30 1 3 -8 8.40 4.00 -1 3 8 17.90 4.70 -1 3 8 15.90 5.20 0 -3 -8 107.29 10.00 0 -3 8 124.09 8.50 0 3 8 107.09 8.60 0 3 -8 116.19 8.40 1 -3 8 88.49 8.50 -1 -3 -8 87.99 8.80 -1 3 -8 77.79 7.80 1 3 8 78.59 9.00 -2 -4 8 11.10 5.00 2 -4 -8 15.10 5.00 -2 4 8 19.10 5.30 2 4 -8 9.50 4.10 -2 4 8 14.50 6.10 1 -4 -8 54.69 7.30 -1 -4 8 55.19 7.20 -1 4 8 60.69 8.30 1 4 -8 60.69 7.60 0 -4 -8 4.70 4.00 0 -4 8 8.60 4.10 0 4 8 3.40 3.90 0 4 -8 2.80 3.50 -1 -4 -8 0.20 3.20 1 -4 8 -2.90 2.90 -1 4 -8 -0.30 3.30 1 4 8 0.40 3.50 -1 -5 8 64.69 7.90 1 -5 -8 56.69 7.50 1 5 -8 61.49 7.80 -1 5 8 52.89 8.00 0 -5 -8 78.69 8.30 0 -5 8 99.39 9.60 0 5 -8 76.49 8.40 0 5 8 96.49 10.40 -1 -5 -8 188.88 10.60 1 -5 8 228.88 11.60 1 5 8 191.78 11.60 -1 5 -8 210.08 10.40 1 -6 -8 138.59 9.40 -1 -6 8 123.09 9.70 1 6 -8 160.48 10.20 -1 6 8 130.49 10.50 0 -6 -8 2.80 3.60 0 -6 8 -0.40 3.60 0 6 8 0.10 3.60 0 6 -8 -0.80 3.20 -1 -7 8 33.00 6.50 1 -7 -8 26.80 5.70 1 7 -8 48.50 7.70 -1 7 8 46.50 8.10 0 -7 -8 95.19 9.30 0 -7 8 96.49 10.00 0 7 -8 65.59 7.60 0 7 8 73.89 9.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 19387 _shelx_res_file ; TITL eb831_a.res in P2(1)/m E:\SOLVED~1\EB801-~1\EB831_~1\eb831_a.res created by SHELXL-2018/3 at 12:44:31 on 15-Jul-2022 CELL 0.71073 3.8115 13.6452 6.8976 90.000 94.632 90.000 ZERR 2.0000 0.0003 0.0011 0.0005 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, -Z SFAC C H N O CL UNIT 12 6 2 4 4 BOND BOND $H EQIV $1 1-X, 1-Y, 1-Z EQIV $2 1+X, Y, Z-1 RTAB CLODST Cl1 O1_$1 RTAB CLOANG C3 Cl1 O1_$1 RTAB CHODST H4 O1_$2 RTAB CHOANG C4 H4 O1_$2 ACTA FMAP 2 1 53 PLAN 20 0 0 HTAB 2.0 LIST 4 1 TEMP -173 L.S. 16 WGHT 0.039800 0.126700 FVAR 1.09922 CL1 5 0.861151 0.447397 0.233133 11.00000 0.02635 0.01503 = 0.02403 0.00304 0.00686 -0.00205 O1 4 0.334610 0.329128 0.868163 11.00000 0.04416 0.02146 = 0.02300 -0.00115 0.01238 0.00699 N1 3 0.399425 0.250000 0.795394 10.50000 0.01671 0.02157 = 0.01541 0.00000 0.00097 0.00000 C4 1 0.844605 0.250000 0.253963 10.50000 0.01430 0.02129 = 0.01653 0.00000 0.00140 0.00000 AFIX 43 H4 2 0.942848 0.250000 0.131693 10.50000 -1.20000 AFIX 0 C1 1 0.560276 0.250000 0.607556 10.50000 0.01276 0.02005 = 0.01310 0.00000 0.00096 0.00000 C3 1 0.771631 0.337637 0.344784 11.00000 0.01410 0.01504 = 0.01944 0.00204 -0.00004 -0.00188 C2 1 0.626930 0.339735 0.523683 11.00000 0.01441 0.01613 = 0.01776 -0.00175 -0.00007 -0.00001 AFIX 43 H2 2 0.576278 0.399770 0.585345 11.00000 -1.20000 AFIX 0 HKLF 4 REM eb831_a.res in P2(1)/m REM wR2 = 0.0705, GooF = S = 1.117, Restrained GooF = 1.117 for all data REM R1 = 0.0275 for 747 Fo > 4sig(Fo) and 0.0303 for all 813 data REM 55 parameters refined using 0 restraints END WGHT 0.0398 0.1268 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.372, deepest hole -0.215, 1-sigma level 0.066 Q1 1 0.4967 0.2500 0.6592 10.50000 0.05 0.35 Q2 1 0.1596 0.3510 0.7736 11.00000 0.05 0.35 Q3 1 0.6961 0.3375 0.4189 11.00000 0.05 0.31 Q4 1 0.5632 0.2936 0.5542 11.00000 0.05 0.31 Q5 1 0.7658 0.3619 0.3225 11.00000 0.05 0.26 Q6 1 0.7764 0.2914 0.2978 11.00000 0.05 0.26 Q7 1 0.4158 0.3130 0.5863 11.00000 0.05 0.20 Q8 1 0.6955 0.4529 0.1404 11.00000 0.05 0.20 Q9 1 1.0714 0.4455 0.1797 11.00000 0.05 0.20 Q10 1 1.0568 0.4550 0.3520 11.00000 0.05 0.19 Q11 1 0.4003 0.4488 0.2988 11.00000 0.05 0.18 Q12 1 0.5052 0.3355 0.8386 11.00000 0.05 0.17 Q13 1 0.3606 0.4742 0.5020 11.00000 0.05 0.15 Q14 1 0.1132 0.3454 0.9419 11.00000 0.05 0.14 Q15 1 0.7852 0.5028 0.3199 11.00000 0.05 0.13 Q16 1 0.1432 0.2500 0.8982 10.50000 0.05 0.12 Q17 1 0.9411 0.3267 0.6642 11.00000 0.05 0.11 Q18 1 0.9972 0.3805 0.2678 11.00000 0.05 0.11 Q19 1 0.4143 0.4400 0.7826 11.00000 0.05 0.11 Q20 1 0.8486 0.2500 0.7027 10.50000 0.05 0.11 ; _shelx_res_checksum 56955 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-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 Cl Cl1 0.86115(10) 0.44740(3) 0.23313(5) 0.02154(16) Uani d 1 . . O O1 0.3346(3) 0.32913(8) 0.86816(17) 0.0290(3) Uani d 1 . . N N1 0.3994(5) 0.250000 0.7954(3) 0.0179(4) Uani d 1 . . C C4 0.8446(5) 0.250000 0.2540(3) 0.0174(4) Uani d 1 . . H H4 0.942848 0.250000 0.131693 0.021 Uiso calc 1 . . C C1 0.5603(5) 0.250000 0.6076(3) 0.0153(4) Uani d 1 . . C C3 0.7716(4) 0.33764(10) 0.3448(2) 0.0163(3) Uani d 1 . . C C2 0.6269(4) 0.33974(11) 0.5237(2) 0.0162(3) Uani d 1 . . H H2 0.576278 0.399770 0.585345 0.019 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 Cl1 0.0264(2) 0.0150(2) 0.0240(2) -0.00205(13) 0.00686(15) 0.00304(13) O1 0.0442(8) 0.0215(6) 0.0230(6) 0.0070(5) 0.0124(5) -0.0011(5) N1 0.0167(9) 0.0216(9) 0.0154(9) 0.000 0.0010(6) 0.000 C4 0.0143(10) 0.0213(11) 0.0165(10) 0.000 0.0014(8) 0.000 C1 0.0128(9) 0.0200(10) 0.0131(9) 0.000 0.0010(7) 0.000 C3 0.0141(7) 0.0150(7) 0.0194(7) -0.0019(5) 0.0000(5) 0.0020(6) C2 0.0144(7) 0.0161(7) 0.0178(7) 0.0000(5) -0.0001(5) -0.0017(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 O1 N1 O1 . 4_565 123.75(18) ? O1 N1 C1 . . 118.12(9) ? O1 N1 C1 4_565 . 118.12(9) ? C3 C4 C3 4_565 . 118.91(19) ? C3 C4 H4 4_565 . 120.5 ? C3 C4 H4 . . 120.5 ? C2 C1 C2 4_565 . 124.05(19) ? C2 C1 N1 4_565 . 117.96(10) ? C2 C1 N1 . . 117.96(10) ? C4 C3 C2 . . 121.72(14) ? C4 C3 Cl1 . . 119.39(12) ? C2 C3 Cl1 . . 118.89(11) ? C1 C2 C3 . . 116.80(14) ? C1 C2 H2 . . 121.6 ? C3 C2 H2 . . 121.6 ? 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 Cl1 C3 . 1.7306(15) ? O1 N1 . 1.2242(14) ? N1 C1 . 1.477(3) ? C4 C3 4_565 1.3885(18) ? C4 C3 . 1.3885(18) ? C4 H4 . 0.9500 ? C1 C2 4_565 1.3864(17) ? C1 C2 . 1.3865(17) ? C3 C2 . 1.392(2) ? C2 H2 . 0.9500 ?