#------------------------------------------------------------------------------ #$Date: 2022-11-08 20:40:22 +0100 (Tue, 08 Nov 2022) $ #$Revision: 279112 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022675.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_2022675 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 I2 N O2' _chemical_formula_sum 'C6 H3 I2 N O2' _chemical_formula_weight 374.89 _chemical_name_systematic ; 1,3-Diiodo-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 96.506(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 4.1810(5) _cell_length_b 15.0336(17) _cell_length_c 6.7970(8) _cell_measurement_reflns_used 4388 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.20 _cell_measurement_theta_min 2.71 _cell_volume 424.48(9) _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 0.999 _diffrn_measured_fraction_theta_max 0.998 _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 0.0190 _diffrn_reflns_av_unetI/netI 0.0131 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 5377 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.198 _diffrn_reflns_theta_min 2.710 _exptl_absorpt_coefficient_mu 7.358 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.4056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2014) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.933 _exptl_crystal_description trapezoidal _exptl_crystal_F_000 336 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.770 _refine_diff_density_min -0.751 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.345 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 982 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.345 _refine_ls_R_factor_all 0.0196 _refine_ls_R_factor_gt 0.0191 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+1.4021P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0404 _reflns_number_gt 974 _reflns_number_total 982 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file dv3019sup1.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 2022675--2022677.cif.' _cod_original_sg_symbol_H-M 'P 21/m' _cod_database_code 2022675 _cod_database_fobs_code 2022675 _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 0 545.85 11.30 1 0 0 523.35 11.50 2 0 0 1501.15 31.40 -2 0 0 1489.55 30.90 3 0 0 1972.10 41.40 -3 0 0 1941.81 42.00 3 0 0 1942.91 40.60 4 0 0 151.68 5.70 -4 0 0 152.98 6.20 4 0 0 143.69 4.80 -5 0 0 104.89 5.90 5 0 0 106.29 5.20 5 0 0 101.89 4.40 0 1 0 -1.30 0.10 0 1 0 -1.20 0.10 -1 -1 0 432.86 9.20 -1 -1 0 442.76 9.70 1 -1 0 456.45 9.80 -1 1 0 443.76 9.80 1 1 0 438.06 9.40 -1 1 0 444.56 9.40 1 1 0 446.26 9.50 -2 -1 0 269.77 6.00 -2 -1 0 278.57 7.20 2 -1 0 273.87 7.10 -2 1 0 277.87 7.30 2 1 0 276.57 6.50 2 1 0 283.77 6.90 -2 1 0 275.27 6.60 3 -1 0 10.10 1.80 -3 -1 0 10.30 1.80 -3 1 0 9.20 1.30 3 1 0 9.80 1.70 3 1 0 8.80 1.40 -3 1 0 14.30 1.70 4 -1 0 138.89 4.70 4 -1 0 138.69 5.50 -4 -1 0 141.79 6.00 4 1 0 135.09 4.70 4 1 0 139.99 5.30 -4 1 0 137.39 5.90 5 -1 0 16.80 2.40 -5 -1 0 18.40 3.50 5 -1 0 16.30 3.20 5 1 0 12.80 2.20 -5 1 0 16.00 3.20 0 -2 0 1178.18 23.80 0 2 0 1077.19 23.90 0 2 0 1210.28 24.10 1 -2 0 1566.04 32.20 -1 -2 0 1487.15 31.60 -1 -2 0 1559.44 32.00 -1 2 0 1541.55 31.70 1 2 0 1578.14 31.70 -1 2 0 1599.54 32.10 1 2 0 1565.84 31.70 -2 -2 0 302.17 7.00 2 -2 0 326.07 8.10 -2 -2 0 311.07 8.00 -2 2 0 316.27 7.40 2 2 0 330.37 7.70 -2 2 0 319.97 8.10 2 2 0 314.97 7.40 -3 -2 0 1200.28 25.70 3 -2 0 1260.77 27.70 -3 -2 0 1243.88 27.90 -3 2 0 1269.17 28.00 3 2 0 1270.97 27.20 3 2 0 1266.37 26.70 -3 2 0 1257.47 26.70 4 -2 0 218.78 7.40 -4 -2 0 199.58 7.50 4 2 0 220.68 6.40 4 2 0 216.68 6.90 -4 2 0 220.18 7.80 5 -2 0 91.19 5.10 5 -2 0 92.69 4.30 -5 -2 0 86.29 5.40 -5 2 0 90.69 5.50 5 2 0 86.99 4.10 0 -3 0 0.50 0.30 0 3 0 1.30 0.50 0 3 0 1.30 0.50 -1 -3 0 2622.04 56.29 1 -3 0 2776.02 57.59 1 -3 0 2741.53 55.79 -1 -3 0 2831.52 56.29 1 3 0 2774.92 56.09 1 3 0 2800.42 56.09 -1 3 0 2759.02 56.09 -1 3 0 2876.81 57.49 -2 -3 0 1266.07 26.50 -2 -3 0 1275.17 27.50 2 -3 0 1290.57 27.80 -2 3 0 1287.47 26.90 2 3 0 1289.17 26.80 2 3 0 1291.47 27.00 -2 3 0 1307.57 27.70 3 -3 0 5.20 1.60 -3 -3 0 2.70 1.10 -3 3 0 1.50 0.70 3 3 0 3.20 1.20 -3 3 0 6.10 1.40 3 3 0 1.50 0.80 -4 -3 0 380.56 11.50 4 -3 0 400.66 11.40 4 3 0 392.26 10.70 4 3 0 400.66 10.20 -4 3 0 388.46 10.10 -4 3 0 417.96 11.90 5 -3 0 263.37 8.10 -5 -3 0 241.98 9.40 5 -3 0 260.87 9.30 5 3 0 264.37 8.00 -5 3 0 252.97 9.80 0 -4 0 656.83 14.00 0 4 0 664.73 14.30 -1 -4 0 112.39 3.10 1 -4 0 107.59 3.60 1 -4 0 115.09 2.80 -1 -4 0 117.09 3.20 1 4 0 116.29 3.20 -1 4 0 117.69 3.30 1 4 0 113.59 3.10 -1 4 0 110.79 3.10 -2 -4 0 59.99 2.10 2 -4 0 63.99 2.90 -2 -4 0 61.49 2.60 2 4 0 59.19 2.20 -2 4 0 61.29 2.30 -2 4 0 58.59 2.60 2 4 0 61.39 2.30 3 -4 0 190.78 6.50 -3 -4 0 180.18 6.10 -3 -4 0 186.58 4.90 3 4 0 194.48 5.70 -3 4 0 192.38 5.50 -3 4 0 200.18 6.40 3 4 0 191.58 5.40 -4 -4 0 23.20 2.60 4 -4 0 26.80 2.90 4 4 0 23.50 2.70 4 4 0 24.90 2.10 -4 4 0 25.80 2.10 -4 4 0 32.00 2.90 5 -4 0 20.60 3.60 -5 -4 0 13.70 3.00 5 -4 0 12.70 2.30 5 4 0 14.00 2.20 -5 4 0 17.10 3.30 0 5 0 -2.10 0.70 0 5 0 0.00 1.00 -1 -5 0 3008.10 61.69 1 -5 0 3005.50 61.19 -1 -5 0 3066.39 61.59 -1 5 0 3024.10 61.79 1 5 0 3062.89 61.79 -1 5 0 3041.50 61.79 1 5 0 3047.30 61.79 -2 -5 0 2851.81 57.99 -2 -5 0 2747.82 57.29 2 -5 0 2859.51 58.69 -2 5 0 2809.32 57.49 -2 5 0 2834.52 58.09 2 5 0 2732.73 57.49 2 5 0 2824.52 57.39 3 -5 0 10.20 2.20 -3 -5 0 8.80 1.60 -3 -5 0 11.70 1.30 3 5 0 10.50 1.30 -3 5 0 8.00 1.20 -3 5 0 7.70 1.50 3 5 0 9.20 1.30 -4 -5 0 708.03 18.50 4 -5 0 748.73 19.00 -4 5 0 742.13 17.30 4 5 0 744.03 17.20 -4 5 0 740.03 18.80 5 -5 0 373.36 12.20 -5 -5 0 360.56 12.00 -5 5 0 367.26 10.40 5 5 0 368.76 10.30 -5 5 0 365.56 12.20 0 -6 0 146.89 3.80 0 6 0 130.99 4.00 0 6 0 120.19 4.40 1 -6 0 173.68 5.20 -1 -6 0 164.68 4.50 1 -6 0 159.38 4.10 -1 -6 0 166.18 4.30 -1 6 0 166.28 4.40 1 6 0 161.18 4.50 1 6 0 162.98 4.60 -1 6 0 161.78 4.60 2 -6 0 14.10 1.70 -2 -6 0 8.30 1.10 -2 -6 0 8.70 1.30 -2 6 0 8.50 1.20 2 6 0 8.40 1.10 2 6 0 8.40 1.30 -2 6 0 9.10 1.10 -3 -6 0 218.58 6.00 3 -6 0 225.58 7.60 -3 -6 0 228.18 7.00 -3 6 0 221.98 7.00 -3 6 0 230.68 6.40 3 6 0 227.18 6.30 3 6 0 230.48 6.50 -4 -6 0 44.20 3.30 4 -6 0 48.30 3.80 -4 6 0 42.00 2.70 4 6 0 46.50 2.70 -4 6 0 41.50 3.20 5 -6 0 16.50 3.60 -5 -6 0 14.90 3.00 -5 6 0 13.60 2.10 -5 6 0 16.50 3.30 5 6 0 14.70 2.20 0 -7 0 1.20 0.60 0 7 0 1.20 0.90 -1 -7 0 1619.94 33.40 1 -7 0 1665.63 34.90 1 -7 0 1609.24 33.20 -1 -7 0 1634.54 33.80 -1 7 0 1580.44 33.40 1 7 0 1605.34 34.00 1 7 0 1580.44 33.80 2 -7 0 798.32 19.00 -2 -7 0 797.72 17.60 2 -7 0 761.02 16.50 -2 -7 0 807.92 17.80 -2 7 0 798.32 17.70 2 7 0 798.62 17.60 2 7 0 798.12 17.60 -2 7 0 793.92 17.80 3 -7 0 11.10 2.50 -3 -7 0 9.90 1.40 -3 -7 0 10.50 1.90 -3 7 0 10.80 1.80 -3 7 0 11.10 1.60 3 7 0 10.80 1.50 3 7 0 13.10 1.40 -4 -7 0 378.96 11.10 4 -7 0 371.56 11.80 -4 7 0 368.86 10.00 -4 7 0 354.36 10.90 4 7 0 374.06 9.90 0 -8 0 2731.33 55.69 0 8 0 2725.83 56.29 0 8 0 2682.53 56.89 1 -8 0 484.65 11.00 -1 -8 0 513.05 11.10 1 -8 0 502.05 12.60 -1 -8 0 498.95 11.50 1 8 0 483.75 11.60 1 8 0 479.35 11.80 -1 8 0 488.65 12.00 -1 8 0 472.75 11.00 -2 -8 0 527.85 12.50 2 -8 0 539.75 13.80 -2 -8 0 540.15 12.50 2 -8 0 510.95 11.40 2 8 0 545.15 12.60 -2 8 0 515.35 12.40 2 8 0 525.85 12.50 -2 8 0 522.85 12.60 -3 -8 0 795.32 18.30 3 -8 0 781.82 19.60 -3 -8 0 758.02 17.60 3 8 0 767.12 17.70 -3 8 0 766.92 17.80 -3 8 0 766.82 18.30 -4 -8 0 100.19 4.80 4 -8 0 97.19 5.60 -4 8 0 98.09 4.30 -4 8 0 98.29 4.80 4 8 0 99.49 4.20 0 -9 0 0.40 0.60 0 9 0 0.10 0.80 1 -9 0 239.48 6.00 -1 -9 0 235.98 5.90 -1 -9 0 238.88 6.50 1 -9 0 215.48 7.30 1 9 0 235.58 6.90 -1 9 0 229.78 7.10 -1 9 0 242.88 5.90 1 9 0 237.28 6.60 -2 -9 0 179.28 5.40 -2 -9 0 185.58 5.60 2 -9 0 178.58 4.60 -2 9 0 184.68 5.40 2 9 0 179.38 5.60 -2 9 0 188.48 5.80 -3 -9 0 7.70 1.60 -3 -9 0 9.30 1.50 3 -9 0 9.00 2.40 -3 9 0 6.30 1.40 -3 9 0 8.90 1.60 3 9 0 8.40 1.40 -4 -9 0 65.89 3.40 4 -9 0 68.79 5.10 -4 -9 0 68.19 4.00 4 9 0 68.59 3.50 -4 9 0 73.89 4.00 -4 9 0 64.89 3.60 0 -10 0 3392.46 69.89 0 10 0 3422.96 71.29 1 -10 0 440.36 10.20 -1 -10 0 426.66 9.90 1 -10 0 422.66 11.80 -1 -10 0 447.96 10.70 -1 10 0 418.36 11.50 1 10 0 424.16 11.40 1 10 0 440.66 10.90 2 -10 0 412.86 12.00 -2 -10 0 421.96 10.70 2 -10 0 414.56 9.70 -2 -10 0 421.86 10.30 -2 10 0 429.76 11.10 2 10 0 419.86 10.90 -2 10 0 436.66 10.30 2 10 0 426.86 10.60 -3 -10 0 1162.08 26.00 -3 -10 0 1216.08 26.30 3 -10 0 1154.58 28.30 -3 10 0 1154.18 26.20 -3 10 0 1161.78 26.10 3 10 0 1150.98 26.10 -4 -10 0 134.39 5.70 4 -10 0 132.29 7.10 -4 -10 0 131.29 5.10 -4 10 0 143.69 5.80 -4 10 0 137.99 5.50 4 10 0 142.39 5.40 0 -11 0 7.70 1.30 0 -11 0 5.20 1.50 0 11 0 4.00 1.20 1 -11 0 204.78 5.70 1 -11 0 231.68 7.50 -1 -11 0 203.88 6.10 -1 -11 0 186.18 5.30 1 11 0 193.68 6.80 -1 11 0 196.78 7.00 1 11 0 206.08 6.30 2 -11 0 118.09 3.80 2 -11 0 130.89 5.80 -2 -11 0 119.99 4.20 -2 -11 0 124.79 4.60 -2 11 0 123.79 5.00 2 11 0 122.49 4.80 -2 11 0 126.69 4.10 3 -11 0 4.80 2.20 -3 -11 0 4.30 1.40 -3 -11 0 4.50 1.40 -3 11 0 4.20 1.20 3 11 0 4.80 1.40 -3 11 0 2.90 1.30 -4 -11 0 69.59 3.80 -4 -11 0 76.79 4.20 4 -11 0 74.19 5.60 -4 11 0 72.19 4.20 4 11 0 76.09 4.00 -4 11 0 75.19 4.10 0 -12 0 523.25 14.30 0 -12 0 537.95 12.90 0 12 0 550.74 14.10 1 -12 0 445.46 10.50 1 -12 0 415.96 12.30 -1 12 0 410.06 12.00 1 12 0 428.46 11.10 1 12 0 439.36 12.10 2 -12 0 139.89 6.30 -2 -12 0 141.69 5.10 2 -12 0 141.99 4.80 -2 -12 0 136.99 4.70 -2 12 0 147.69 5.80 2 12 0 139.49 5.50 -3 -12 0 582.94 14.60 3 -12 0 555.94 16.70 -3 -12 0 570.94 14.20 -3 12 0 580.64 15.00 3 12 0 577.14 14.80 4 -12 0 102.69 6.70 -4 -12 0 107.59 4.90 -4 -12 0 104.09 5.00 -4 12 0 101.39 5.00 4 12 0 117.59 5.20 0 -13 0 1.00 1.00 0 -13 0 10.30 2.20 0 13 0 1.20 1.10 -1 -13 0 748.13 17.60 1 -13 0 753.22 19.30 1 -13 0 763.82 17.10 1 13 0 725.03 17.80 1 13 0 746.73 18.90 -2 -13 0 617.14 15.20 2 13 0 609.04 16.10 -2 13 0 610.94 16.30 3 -13 0 2.80 2.30 -3 -13 0 1.60 1.30 -3 13 0 3.20 1.60 3 13 0 1.60 1.30 0 -14 0 364.86 11.60 0 -14 0 427.06 10.70 0 14 0 432.76 11.80 -1 -14 0 5.20 1.40 1 -14 0 4.60 1.20 1 -14 0 2.40 1.70 -1 14 0 3.80 1.60 1 14 0 5.80 1.70 2 -14 0 59.49 4.50 -2 -14 0 64.29 3.50 -2 14 0 55.99 4.00 2 14 0 63.19 4.10 -3 -14 0 54.09 3.60 3 -14 0 45.10 4.80 3 14 0 55.99 3.80 -3 14 0 57.49 4.00 0 -15 0 2.90 1.80 0 -15 0 1.10 1.20 0 15 0 1.80 1.30 -1 -15 0 782.72 18.80 1 -15 0 764.92 20.70 1 -15 0 815.42 18.40 -1 15 0 816.52 20.40 1 15 0 761.12 20.00 2 -15 0 721.53 20.50 -2 -15 0 752.12 18.40 2 15 0 760.32 19.90 3 -15 0 3.40 2.90 -3 -15 0 -1.30 1.50 3 15 0 2.10 1.60 -3 15 0 0.50 1.50 0 -16 0 214.78 8.00 0 -16 0 195.38 6.70 0 16 0 190.48 7.30 1 -16 0 23.70 2.30 -1 -16 0 19.70 2.50 1 -16 0 28.20 3.20 -1 16 0 23.20 3.30 1 16 0 26.30 2.80 2 -16 0 36.00 4.10 -2 -16 0 29.80 2.80 -2 16 0 29.00 3.90 2 16 0 33.60 3.50 3 -16 0 61.79 5.70 0 -17 0 0.40 1.60 0 -17 0 3.50 1.60 0 17 0 1.80 1.50 -1 -17 0 496.15 13.20 1 -17 0 437.96 14.50 1 -17 0 494.95 12.70 1 17 0 491.05 14.20 -1 17 0 511.85 14.40 2 -17 0 203.08 9.40 -2 -17 0 222.38 7.70 2 17 0 215.88 8.80 -2 17 0 209.18 8.80 0 -18 0 581.04 14.90 0 18 0 572.44 15.80 1 -18 0 88.09 5.70 1 -18 0 94.89 4.50 -1 -18 0 90.39 4.70 1 18 0 92.99 5.20 -1 18 0 97.09 5.40 0 -19 0 6.60 1.90 0 19 0 5.30 1.90 -5 0 1 459.35 14.00 5 0 -1 459.35 12.20 4 0 -1 513.35 12.40 4 0 -1 509.45 13.00 -4 0 1 499.25 13.70 -2 0 1 3610.14 74.89 -2 0 1 3739.63 75.59 -2 0 1 3787.32 76.29 2 0 -1 3787.42 75.89 -1 0 1 4632.24 98.99 1 0 -1 5425.56 101.39 -1 0 1 4770.82 101.29 -1 0 1 4743.13 100.19 0 0 1 29.40 1.20 0 0 -1 22.50 1.30 0 0 1 23.20 0.90 -1 0 -1 9999.00 187.88 -1 0 -1 8716.33 190.68 -1 0 -1 9152.48 187.58 1 0 1 9273.77 190.58 2 0 1 1181.68 25.30 -2 0 -1 1167.38 24.10 -2 0 -1 1169.98 25.70 3 0 1 127.09 3.80 3 0 1 122.09 4.60 -3 0 -1 114.89 4.80 -4 0 -1 731.23 19.30 4 0 1 760.52 17.10 4 0 1 765.82 18.70 5 0 1 237.68 8.60 -5 0 -1 221.38 9.30 5 0 1 236.98 7.20 -5 -1 1 11.50 2.80 5 -1 -1 4.30 1.60 5 1 -1 8.80 1.90 -5 1 1 10.90 2.50 -4 -1 1 35.80 2.80 4 -1 -1 33.40 2.20 4 -1 -1 30.90 2.60 4 1 -1 33.50 2.20 -4 1 1 29.80 2.70 4 1 -1 35.70 2.60 3 -1 -1 216.88 6.40 -3 -1 1 205.18 4.80 3 1 -1 217.68 6.00 -3 1 1 203.88 6.50 -3 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3.70 0 5 -7 29.30 3.40 -1 -5 -7 121.89 5.50 -1 -5 -7 128.29 5.30 1 -5 7 127.09 6.10 1 -5 7 131.99 4.90 1 5 7 133.69 7.00 -1 5 -7 138.39 7.10 -2 -5 -7 565.24 15.20 2 -5 7 561.04 16.90 2 -5 7 592.44 14.80 -2 -5 -7 557.64 15.70 2 5 7 584.54 17.90 -2 5 -7 601.24 18.70 -3 -6 7 18.10 1.90 3 -6 -7 21.70 2.60 -3 6 7 30.60 5.30 3 6 -7 23.30 3.90 2 -6 -7 57.29 3.40 -2 -6 7 58.19 3.10 2 6 -7 55.79 4.50 -2 6 7 56.29 5.00 -1 -6 7 12.20 1.90 1 -6 -7 12.90 2.20 -1 6 7 17.60 3.90 1 6 -7 16.70 3.30 0 -6 7 62.89 3.20 0 -6 7 62.29 4.20 0 -6 -7 63.09 3.60 0 6 -7 60.29 4.60 0 6 7 67.39 5.00 1 -6 7 26.80 3.10 -1 -6 -7 24.50 2.60 1 -6 7 20.30 2.10 -1 6 -7 28.80 4.40 1 6 7 29.70 3.60 -2 -6 -7 4.60 1.80 2 -6 7 7.30 2.50 -2 6 -7 6.60 2.80 2 6 7 7.40 2.90 -3 -7 7 88.19 4.00 3 7 -7 79.19 5.40 -3 7 7 79.99 6.20 -2 -7 7 236.18 7.30 2 -7 -7 233.48 7.70 2 7 -7 231.68 9.70 -2 7 7 236.78 10.50 1 -7 -7 625.24 15.90 -1 -7 7 623.74 15.30 -1 7 7 632.54 19.00 1 7 -7 617.24 18.40 0 -7 7 56.99 3.10 0 -7 -7 52.79 3.40 0 7 7 58.89 4.90 0 7 -7 56.59 4.60 -1 -7 -7 383.06 11.40 1 -7 7 402.36 10.50 1 -7 7 385.26 12.30 -1 7 -7 389.56 13.80 1 7 7 401.56 13.90 2 -7 7 141.39 7.10 -2 -7 -7 142.29 6.20 2 7 7 145.29 7.90 2 -8 -7 142.59 5.80 -2 -8 7 144.49 5.40 -2 8 7 146.59 8.10 2 8 -7 136.99 7.40 1 -8 -7 50.49 3.40 -1 -8 7 47.30 2.90 1 8 -7 52.99 4.40 -1 8 7 50.79 4.60 0 -8 7 411.36 10.90 0 -8 -7 409.86 11.80 0 8 -7 402.86 13.80 0 8 7 410.76 14.30 1 -8 7 151.88 6.90 -1 -8 -7 149.88 6.30 1 -8 7 158.18 5.50 1 8 7 139.49 7.90 -1 8 -7 161.38 8.20 -2 -9 7 10.20 1.90 2 -9 -7 8.90 2.10 2 9 -7 13.40 3.20 -2 9 7 14.30 3.80 -1 -9 7 38.40 2.60 1 -9 -7 36.10 3.00 -1 9 7 34.90 4.20 1 9 -7 37.70 3.90 0 -9 7 10.70 1.90 0 -9 -7 12.00 2.40 0 9 -7 13.50 3.20 0 9 7 13.30 3.60 1 -9 7 1.90 1.20 -1 -9 -7 2.10 1.50 1 -9 7 4.40 2.40 -1 9 -7 5.10 2.30 1 9 7 2.90 2.40 -2 -10 7 312.87 9.20 2 -10 -7 317.67 9.80 2 10 -7 282.87 11.60 -2 10 7 311.37 12.70 1 -10 -7 20.40 2.90 -1 -10 7 19.10 2.10 1 10 -7 25.80 4.30 -1 10 7 32.40 5.40 0 -10 7 614.94 15.40 0 -10 -7 611.14 16.40 0 10 -7 625.34 18.80 0 10 7 618.94 19.30 -1 -10 -7 222.58 8.10 1 -10 7 220.98 7.10 -1 10 -7 218.48 10.00 1 10 7 217.08 10.10 1 -11 -7 51.69 3.70 -1 -11 7 54.29 3.30 -1 11 7 53.09 5.10 1 11 -7 55.49 4.70 0 -11 -7 2.10 1.70 0 -11 7 1.70 1.30 0 11 7 4.20 2.50 0 11 -7 2.70 1.90 2 0 -8 379.86 12.90 -2 0 8 385.16 10.70 -1 0 8 472.35 15.40 1 0 -8 486.15 14.50 -1 0 8 483.95 12.70 0 0 -8 28.50 3.90 0 0 8 19.50 2.90 0 0 8 20.60 2.50 1 0 8 352.86 10.20 -1 0 -8 358.86 12.00 1 0 8 339.97 12.40 -2 -1 8 34.70 2.60 2 -1 -8 37.30 3.70 -2 1 8 31.50 2.50 2 1 -8 30.40 3.60 -1 -1 8 13.60 2.00 1 -1 -8 11.70 2.60 1 1 -8 12.50 2.90 -1 1 8 18.70 3.90 -1 1 8 11.50 1.90 0 -1 -8 55.69 4.00 0 -1 8 52.89 4.30 0 -1 8 51.99 3.10 0 1 8 50.99 3.10 0 1 -8 51.79 4.00 0 1 8 56.49 4.50 1 -1 8 27.70 3.60 -1 -1 -8 29.10 4.00 1 -1 8 24.60 2.40 1 1 8 22.80 2.40 -1 1 -8 28.20 4.20 1 1 8 28.80 3.80 -2 -2 8 322.87 9.40 2 -2 -8 321.87 11.10 2 2 -8 318.87 11.80 -2 2 8 318.87 9.40 -1 -2 8 380.66 10.50 1 -2 -8 381.96 11.90 -1 2 8 377.76 10.70 1 2 -8 377.76 12.70 -1 2 8 391.26 13.50 0 -2 8 2.20 1.10 0 -2 8 3.50 2.00 0 -2 -8 2.10 1.70 0 2 -8 2.30 1.90 0 2 8 1.60 1.00 0 2 8 2.80 1.90 1 -2 8 185.78 8.40 1 -2 8 178.88 6.40 -1 -2 -8 199.58 6.90 -1 -2 -8 189.38 7.80 1 2 8 186.28 8.80 -1 2 -8 193.78 8.50 -2 -3 8 138.99 5.40 2 -3 -8 139.89 6.60 -2 3 8 141.39 5.50 -2 3 8 139.29 8.10 2 3 -8 135.39 7.30 1 -3 -8 97.69 5.10 -1 -3 8 98.29 4.40 -1 3 8 105.19 4.60 1 3 -8 98.69 5.90 -1 3 8 100.89 6.30 0 -3 8 383.36 10.70 0 -3 8 385.86 12.70 0 -3 -8 400.96 12.10 0 3 8 396.86 13.70 0 3 -8 411.76 13.30 0 3 8 390.96 11.10 -1 -3 -8 84.19 4.30 1 -3 8 73.79 3.80 1 -3 8 79.79 5.30 -1 -3 -8 84.09 5.00 -1 3 -8 82.79 5.50 1 3 8 83.99 5.90 -2 -4 8 19.90 2.10 -2 4 8 29.40 5.40 -2 4 8 20.00 2.10 2 4 -8 22.10 4.10 -1 -4 8 55.59 3.20 1 -4 -8 46.70 4.30 -1 4 8 51.59 3.20 1 4 -8 55.49 4.50 -1 4 8 51.19 4.70 0 -4 8 5.10 2.10 0 -4 -8 3.50 1.50 0 -4 8 4.40 1.40 0 -4 -8 4.30 1.80 0 4 8 5.60 2.50 0 4 -8 2.40 1.90 -1 -4 -8 28.30 3.20 1 -4 8 22.30 2.30 1 -4 8 25.30 3.30 -1 -4 -8 25.40 2.70 1 4 8 24.90 3.70 -1 4 -8 32.90 4.80 -2 -5 8 89.59 4.20 2 -5 -8 80.39 4.30 -2 5 8 93.09 6.70 2 5 -8 84.09 5.80 1 -5 -8 63.09 3.80 -1 -5 8 69.19 3.60 1 5 -8 67.49 5.10 -1 5 8 71.09 5.50 0 -5 -8 473.75 13.20 0 -5 8 493.45 12.80 0 5 -8 486.85 15.60 0 5 8 479.05 16.00 1 -5 8 106.19 6.10 1 -5 8 105.69 4.60 -1 -5 -8 101.89 5.00 1 5 8 109.79 6.80 -1 5 -8 109.69 6.70 -1 -6 8 48.20 3.10 1 -6 -8 47.30 3.40 -1 6 8 47.20 4.70 1 6 -8 53.79 4.60 0 -6 -8 4.40 1.80 0 -6 8 6.10 1.50 0 6 -8 6.90 2.50 0 6 8 4.70 2.50 1 -7 -8 92.29 4.70 -1 -7 8 89.29 4.30 1 7 -8 85.19 5.90 -1 7 8 91.59 6.40 0 -7 -8 374.26 11.30 0 -7 8 374.06 10.50 0 7 -8 367.06 13.40 0 7 8 374.46 13.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 31028 _shelx_res_file ; TITL eb752_a.res in P2(1)/m E:\SOLVED~1\EB751-~1\EB752_~1\eb752_a.res created by SHELXL-2018/3 at 12:17:43 on 15-Jul-2022 CELL 0.71073 4.1810 15.0336 6.7970 90.000 96.506 90.000 ZERR 2.0000 0.0005 0.0017 0.0008 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, -Z SFAC C H N O I UNIT 12 6 2 4 4 BOND BOND $H RTAB IODIST I1 O1_$1 RTAB IOANG C3 I1 O1_$1 RTAB IIDIST I1 I1_$2 RTAB IIANG C3 I1 I1_$2 EQIV $1 1-X,1-Y,1-Z EQIV $2 2-X,1-Y,-Z HTAB C2 I1_$1 ACTA FMAP 2 1 53 PLAN 20 0 0 HTAB 2.0 LIST 4 1 TEMP -173 L.S. 16 WGHT 0.000000 1.402100 FVAR 0.41149 I1 5 0.833162 0.449772 0.220233 11.00000 0.02045 0.01361 = 0.01868 0.00277 0.00633 -0.00068 O1 4 0.266961 0.321771 0.856275 11.00000 0.04471 0.01972 = 0.02635 -0.00617 0.02025 0.00074 N1 3 0.336464 0.250000 0.787910 10.50000 0.01738 0.01704 = 0.01537 0.00000 0.00188 0.00000 C1 1 0.503233 0.250000 0.606638 10.50000 0.01153 0.01764 = 0.01202 0.00000 0.00091 0.00000 C2 1 0.575457 0.331248 0.525617 11.00000 0.01418 0.01341 = 0.01574 -0.00087 0.00086 0.00082 AFIX 43 H2 2 0.524333 0.385788 0.585351 11.00000 -1.20000 AFIX 0 C3 1 0.725515 0.329562 0.353656 11.00000 0.01343 0.01201 = 0.01612 0.00199 0.00092 -0.00180 C4 1 0.803291 0.250000 0.267185 10.50000 0.01159 0.02126 = 0.01228 0.00000 0.00189 0.00000 AFIX 43 H4 2 0.908365 0.250000 0.150367 10.50000 -1.20000 AFIX 0 HKLF 4 REM eb752_a.res in P2(1)/m REM wR2 = 0.0404, GooF = S = 1.345, Restrained GooF = 1.345 for all data REM R1 = 0.0191 for 974 Fo > 4sig(Fo) and 0.0196 for all 982 data REM 55 parameters refined using 0 restraints END WGHT 0.0000 1.4021 REM Instructions for potential hydrogen bonds HTAB C2 I1_$1 REM Highest difference peak 0.770, deepest hole -0.751, 1-sigma level 0.108 Q1 1 0.4958 0.3503 0.6680 11.00000 0.05 0.77 Q2 1 0.7130 0.4393 0.1021 11.00000 0.05 0.58 Q3 1 0.1481 0.3469 0.7624 11.00000 0.05 0.57 Q4 1 0.4967 0.4545 0.3409 11.00000 0.05 0.49 Q5 1 0.9629 0.4743 0.3586 11.00000 0.05 0.41 Q6 1 0.8849 0.4351 0.3425 11.00000 0.05 0.40 Q7 1 0.4173 0.2500 0.6836 10.50000 0.05 0.39 Q8 1 0.5986 0.3360 0.4212 11.00000 0.05 0.37 Q9 1 0.1776 0.3278 0.9430 11.00000 0.05 0.36 Q10 1 0.3772 0.2500 0.2803 10.50000 0.05 0.35 Q11 1 0.5223 0.2155 0.5578 11.00000 0.05 0.34 Q12 1 0.8715 0.2500 0.3790 10.50000 0.05 0.33 Q13 1 0.9450 0.4218 0.1227 11.00000 0.05 0.30 Q14 1 1.0929 0.4791 0.5005 11.00000 0.05 0.30 Q15 1 0.6757 0.3422 0.2476 11.00000 0.05 0.29 Q16 1 1.1691 0.2500 0.0976 10.50000 0.05 0.28 Q17 1 0.5154 0.4485 -0.0181 11.00000 0.05 0.28 Q18 1 0.6557 0.2248 0.3241 11.00000 0.05 0.28 Q19 1 0.2458 0.2830 0.8240 11.00000 0.05 0.27 Q20 1 0.3985 0.3389 0.9016 11.00000 0.05 0.27 ; _shelx_res_checksum 36604 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 I I1 0.83316(5) 0.44977(2) 0.22023(3) 0.01726(8) Uani d 1 . . O O1 0.2670(7) 0.32177(18) 0.8563(4) 0.0290(6) Uani d 1 . . N N1 0.3365(10) 0.250000 0.7879(6) 0.0166(8) Uani d 1 . . C C1 0.5032(11) 0.250000 0.6066(7) 0.0138(9) Uani d 1 . . C C2 0.5755(8) 0.3312(2) 0.5256(5) 0.0145(6) Uani d 1 . . H H2 0.524333 0.385788 0.585351 0.017 Uiso calc 1 . . C C3 0.7255(8) 0.3296(2) 0.3537(5) 0.0139(6) Uani d 1 . . C C4 0.8033(11) 0.250000 0.2672(7) 0.0150(9) Uani d 1 . . H H4 0.908365 0.250000 0.150367 0.018 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 I1 0.02045(12) 0.01361(12) 0.01868(12) -0.00068(8) 0.00633(8) 0.00277(8) O1 0.0447(17) 0.0197(14) 0.0264(14) 0.0007(12) 0.0202(12) -0.0062(11) N1 0.017(2) 0.017(2) 0.0154(19) 0.000 0.0019(16) 0.000 C1 0.012(2) 0.018(2) 0.012(2) 0.000 0.0009(17) 0.000 C2 0.0142(15) 0.0134(15) 0.0157(15) 0.0008(12) 0.0009(12) -0.0009(12) C3 0.0134(14) 0.0120(15) 0.0161(15) -0.0018(12) 0.0009(12) 0.0020(12) C4 0.012(2) 0.021(2) 0.012(2) 0.000 0.0019(17) 0.000 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' I I -0.4742 1.8119 '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 . 123.9(4) ? O1 N1 C1 4_565 . 118.0(2) ? O1 N1 C1 . . 118.0(2) ? C2 C1 C2 . 4_565 123.4(4) ? C2 C1 N1 . . 118.3(2) ? C2 C1 N1 4_565 . 118.3(2) ? C1 C2 C3 . . 117.2(3) ? C1 C2 H2 . . 121.4 ? C3 C2 H2 . . 121.4 ? C4 C3 C2 . . 121.5(3) ? C4 C3 I1 . . 119.2(2) ? C2 C3 I1 . . 119.3(2) ? C3 C4 C3 4_565 . 119.1(4) ? C3 C4 H4 4_565 . 120.5 ? C3 C4 H4 . . 120.5 ? 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 I1 C3 . 2.094(3) ? O1 N1 . 1.223(3) ? N1 C1 . 1.483(6) ? C1 C2 . 1.387(4) ? C1 C2 4_565 1.387(4) ? C2 C3 . 1.388(5) ? C2 H2 . 0.9500 ? C3 C4 . 1.388(4) ? C4 H4 . 0.9500 ? 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 C2 H2 I1 3_666 0.95 3.25 4.172(3) 165.3 yes