#------------------------------------------------------------------------------ #$Date: 2025-05-21 03:05:01 +0100 (Wed, 21 May 2025) $ #$Revision: 299763 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023512.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_2023512 loop_ _publ_author_name 'Guseinov, Firudin I.' 'H\"okelek, Tuncer' 'Afanaseva, Ksenia A.' 'Shuvalova, Elena V.' 'Glukhov, Lev M.' 'Samigullina, Aida I.' 'Belay, Alebel N.' _publ_section_title ; Syntheses and structures of 1-[2,2-dichloro-1-hydroxy-3-(4-methylphenyl)-3-oxopropyl]urea and 1-[2,2-dichloro-3-(4-fluorophenyl)-1-hydroxy-3-oxopropyl]urea ; _journal_coeditor_code HB8127 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989025004359 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C10 H9 Cl2 F N2 O3' _chemical_formula_moiety 'C10 H9 Cl2 F N2 O3' _chemical_formula_sum 'C10 H9 Cl2 F N2 O3' _chemical_formula_weight 295.09 _chemical_name_systematic ; 1-[2,2-Dichloro-1-hydroxy-3-(4-methylphenyl)-3-oxopropyl]urea ; _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' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method ; Olex2 1.3 (compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938) ; _cell_angle_alpha 90 _cell_angle_beta 104.6220(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.61360(10) _cell_length_b 7.22140(10) _cell_length_c 10.79290(10) _cell_measurement_reflns_used 10775 _cell_measurement_temperature 99.98(10) _cell_measurement_theta_max 80.4840 _cell_measurement_theta_min 2.9270 _cell_volume 1177.51(2) _computing_cell_refinement ; CrysAlisPro 1.171.43.143a (Rigaku OD, 2024) ; _computing_data_collection 'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))' _computing_data_reduction ; CrysAlisPro 1.171.43.143a (Rigaku OD, 2024) ; _computing_molecular_graphics ; Olex2 1.3 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.3 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 99.98(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_unetI/netI 0.0240 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 16149 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.743 _diffrn_reflns_theta_min 2.925 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 5.143 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.408 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2024) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.401 _refine_diff_density_min -0.307 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 179 _refine_ls_number_reflns 2562 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0314 _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^)+(0.0418P)^2^+0.7639P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.0815 _reflns_number_gt 2494 _reflns_number_total 2562 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8127.cif _cod_data_source_block I _cod_database_code 2023512 _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 0.290 _shelx_estimated_absorpt_t_max 0.783 _shelx_hkl_file ; 0 0 1 1.08 0.46 0 0 2 3491.75 101.52 0 0 3 1.76 1.05 0 0 3 1.57 1.02 0 0 4 849.15 32.57 0 0 4 901.64 34.17 0 0 5 1.87 1.32 0 0 5 0.75 1.37 0 0 6 13.10 2.10 0 0 6 12.44 3.51 0 0 6 12.04 1.99 0 0 6 19.34 4.81 0 0 7 2.43 2.22 0 0 7 0.61 0.96 0 0 7 1.52 0.97 0 0 -7 1.08 1.14 0 0 8 0.36 0.93 0 0 8 1.45 2.17 0 0 8 1.44 1.07 0 0 9 1.16 0.91 0 0 9 -0.33 1.10 0 0 9 0.57 0.96 0 0 9 1.21 1.11 0 0 9 -0.36 1.07 0 0 9 0.40 1.10 0 0 9 -0.40 1.12 0 0 9 1.81 1.11 0 0 9 1.63 2.43 0 0 9 0.40 1.19 0 0 9 0.40 1.25 0 0 9 1.56 1.37 0 0 9 0.40 1.05 0 0 9 0.40 1.28 0 0 10 56.22 5.36 0 0 10 44.49 4.92 0 0 10 44.79 4.93 0 0 10 42.49 4.82 0 0 10 42.66 4.20 0 0 10 49.33 4.87 0 0 10 46.29 5.11 0 0 10 40.17 4.43 0 0 10 42.03 4.14 0 0 10 52.51 5.32 0 0 10 46.91 5.05 0 0 10 44.15 4.80 0 0 10 49.97 4.68 0 0 11 0.35 1.18 0 0 11 -0.68 1.14 0 0 11 1.01 1.51 0 0 11 -0.29 1.01 0 0 11 -0.35 0.99 0 0 11 0.27 0.99 0 0 11 0.64 1.26 0 0 11 -1.36 1.48 0 0 11 0.25 0.83 0 0 11 1.02 1.24 0 0 12 1434.03 44.25 0 0 12 1429.42 44.17 0 0 12 1409.44 43.81 0 0 12 1388.00 44.59 0 0 12 1440.65 44.49 0 0 12 1469.99 44.56 0 0 12 1412.61 44.64 0 0 13 0.15 0.64 0 -1 0 0.15 0.47 0 -1 1 111.25 4.71 0 1 1 92.45 4.47 0 -1 -1 102.12 4.86 0 -1 1 94.86 4.61 0 1 1 98.79 4.65 0 -1 -2 407.66 13.49 0 -1 2 400.50 15.39 0 1 2 442.02 15.77 0 -1 -2 418.00 15.51 0 1 2 392.37 15.75 0 -1 2 409.80 15.82 0 -1 3 1335.02 42.23 0 -1 3 1338.07 44.14 0 1 3 1323.46 44.08 0 -1 -3 1409.21 44.56 0 1 3 1332.41 44.92 0 -1 3 1403.38 45.25 0 -1 4 1268.09 39.83 0 -1 4 1272.44 43.97 0 1 4 1206.20 43.63 0 -1 4 1257.56 44.97 0 1 4 1268.98 45.22 0 -1 -4 1265.88 43.78 0 1 5 21.22 4.11 0 -1 5 28.82 4.81 0 -1 -5 23.90 4.29 0 -1 5 19.74 2.42 0 -1 5 18.85 4.40 0 1 5 22.00 4.64 0 1 6 2942.91 86.93 0 -1 6 2973.98 86.92 0 -1 -6 2950.98 96.38 0 -1 6 2986.90 86.94 0 1 6 2885.66 86.78 0 1 6 3017.45 100.70 0 -1 6 2992.08 100.58 0 -1 6 3067.29 97.45 0 1 6 3013.08 97.11 0 1 7 26.94 3.28 0 -1 7 22.72 3.07 0 1 7 23.18 5.95 0 -1 7 28.22 6.65 0 1 7 25.82 3.19 0 -1 7 26.29 3.27 0 -1 8 69.45 5.77 0 -1 8 56.42 5.25 0 1 8 55.28 5.20 0 -1 8 59.80 5.50 0 1 8 63.90 5.52 0 -1 8 65.27 5.11 0 1 8 57.84 10.17 0 1 8 64.58 5.69 0 -1 8 61.06 5.52 0 -1 8 62.93 10.74 0 1 8 60.39 5.44 0 1 8 70.96 5.67 0 -1 8 68.31 5.85 0 -1 8 69.38 5.80 0 1 8 61.90 5.40 0 -1 8 74.23 5.89 0 1 8 65.51 5.41 0 -1 8 67.55 4.97 0 1 8 56.36 4.93 0 -1 8 62.79 5.17 0 1 8 54.89 4.54 0 1 8 62.46 5.25 0 -1 8 65.76 5.07 0 1 8 63.37 5.58 0 1 9 1137.34 39.72 0 1 9 1191.51 38.87 0 -1 9 1227.65 41.25 0 1 9 1246.85 41.09 0 -1 9 1272.72 41.35 0 1 9 1170.23 39.70 0 1 9 1191.72 38.98 0 -1 9 1225.20 40.01 0 -1 9 1206.88 39.04 0 1 9 1181.80 40.94 0 -1 9 1218.43 41.22 0 1 9 1189.67 40.81 0 1 9 1182.02 40.69 0 1 9 1224.27 41.17 0 -1 9 1194.45 41.40 0 -1 9 1280.76 41.57 0 1 9 1260.26 40.79 0 1 9 1216.61 40.93 0 -1 9 1230.72 41.03 0 1 9 1225.78 40.19 0 1 9 1209.01 40.55 0 1 9 1162.22 39.18 0 -1 9 1212.14 39.37 0 1 9 1212.04 41.09 0 1 9 1169.73 58.00 0 -1 9 1301.28 41.56 0 1 9 1249.99 41.18 0 -1 9 1180.15 58.24 0 1 10 62.33 5.33 0 -1 10 67.69 5.98 0 1 10 70.91 5.23 0 -1 10 74.50 5.61 0 -1 10 74.12 6.23 0 1 10 68.46 6.05 0 1 10 79.12 6.44 0 -1 10 73.74 6.20 0 1 10 64.51 5.77 0 -1 10 72.28 6.17 0 1 10 77.58 6.35 0 -1 10 67.99 6.12 0 -1 10 63.54 5.73 0 -1 10 73.61 6.40 0 1 10 65.25 5.83 0 1 10 73.09 5.95 0 -1 10 71.19 5.56 0 1 10 66.05 5.81 0 -1 10 86.90 5.73 0 1 10 78.42 6.35 0 1 10 67.90 5.71 0 1 10 64.38 5.26 0 -1 10 63.95 5.81 0 1 10 72.67 6.20 0 1 11 277.44 12.80 0 1 11 251.59 12.34 0 -1 11 284.00 12.22 0 -1 11 284.20 13.44 0 -1 11 262.56 12.58 0 -1 11 284.72 12.11 0 1 11 283.13 13.02 0 1 11 266.24 12.94 0 -1 11 283.96 13.17 0 -1 11 284.33 13.05 0 -1 11 298.79 13.72 0 1 11 293.20 13.16 0 1 11 291.58 12.97 0 -1 11 293.11 13.34 0 1 11 287.83 13.32 0 -1 12 136.47 7.62 0 1 12 155.10 7.95 0 -1 12 159.33 7.84 0 -1 12 143.79 7.67 0 -1 12 145.90 7.63 0 1 12 151.96 7.64 0 -1 12 144.09 7.63 0 1 12 146.84 7.63 0 -1 12 156.46 8.17 0 1 12 161.07 8.02 0 -1 12 145.14 7.77 0 -1 13 13.11 1.43 0 -2 0 772.06 27.25 0 -2 -1 207.07 9.98 0 2 1 213.62 7.42 0 -2 1 196.06 7.31 0 -2 -2 170.74 8.86 0 -2 -2 188.81 9.46 0 2 2 172.08 8.16 0 -2 2 167.56 8.01 0 -2 2 172.35 8.63 0 2 2 183.60 8.77 0 -2 -3 722.89 25.33 0 -2 -3 692.86 23.87 0 -2 3 709.27 27.39 0 -2 3 650.49 25.11 0 2 3 723.54 25.80 0 -2 3 720.92 26.61 0 2 3 663.84 26.25 0 -2 -4 281.65 13.98 0 -2 4 279.10 14.82 0 -2 4 257.98 14.24 0 2 4 287.12 14.81 0 -2 4 289.67 15.80 0 2 4 278.01 15.68 0 -2 -5 618.14 25.68 0 2 5 645.39 27.57 0 2 5 636.17 29.70 0 -2 5 631.52 29.22 0 -2 5 586.48 25.18 0 -2 6 61.00 4.52 0 2 6 61.51 4.60 0 2 6 52.39 8.06 0 2 6 59.10 4.51 0 -2 6 60.68 4.56 0 2 7 241.94 11.52 0 -2 7 224.08 19.03 0 -2 7 242.49 11.51 0 2 7 259.42 20.33 0 2 7 245.48 11.54 0 -2 7 254.37 11.64 0 -2 8 4.53 1.65 0 2 8 4.14 1.55 0 -2 8 5.86 1.69 0 2 8 6.57 1.56 0 -2 8 5.57 1.50 0 -2 8 4.30 1.61 0 -2 8 3.91 1.39 0 2 8 4.75 1.73 0 2 8 2.82 1.49 0 -2 8 6.26 2.06 0 -2 8 5.40 1.62 0 -2 8 5.30 1.76 0 -2 8 8.01 1.80 0 2 8 4.60 1.68 0 -2 8 7.31 1.95 0 2 8 2.20 1.11 0 -2 8 4.43 1.61 0 2 8 5.81 1.74 0 2 8 8.42 4.20 0 -2 8 5.67 3.35 0 2 8 5.12 1.69 0 2 8 6.34 1.83 0 -2 8 5.60 1.70 0 2 8 7.41 1.85 0 2 8 7.57 1.93 0 -2 8 3.46 1.47 0 2 8 2.94 1.21 0 -2 8 3.07 1.31 0 -2 8 6.23 2.14 0 -2 9 30.15 3.72 0 2 9 37.86 4.35 0 -2 9 41.23 4.48 0 2 9 42.29 4.48 0 -2 9 37.67 4.31 0 -2 9 46.31 4.44 0 -2 9 29.97 3.92 0 2 9 38.43 4.37 0 -2 9 42.90 4.80 0 2 9 37.26 4.05 0 -2 9 37.71 4.27 0 2 9 39.03 4.31 0 2 9 43.44 9.02 0 2 9 35.88 4.22 0 -2 9 42.67 9.03 0 -2 9 45.44 4.69 0 2 9 38.14 4.26 0 -2 9 36.75 4.26 0 2 9 36.35 4.22 0 -2 9 35.06 3.62 0 2 9 39.14 4.10 0 -2 9 38.88 4.28 0 2 9 32.55 4.05 0 -2 9 44.82 5.00 0 2 9 34.48 3.73 0 2 10 141.39 8.73 0 -2 10 135.61 8.58 0 -2 10 162.32 9.58 0 2 10 137.67 8.53 0 -2 10 140.55 8.73 0 -2 10 150.20 7.76 0 -2 10 149.80 8.41 0 -2 10 156.05 9.44 0 2 10 146.92 8.87 0 -2 10 144.47 8.77 0 -2 10 149.03 8.33 0 -2 10 159.13 8.96 0 2 10 138.34 8.43 0 2 10 146.77 8.48 0 2 10 141.50 8.59 0 2 11 115.98 7.11 0 -2 11 114.15 7.44 0 -2 11 121.01 7.27 0 -2 11 127.06 7.39 0 -2 11 126.18 6.80 0 -2 11 125.62 7.95 0 -2 11 125.59 7.17 0 2 11 111.92 6.88 0 2 11 122.87 7.29 0 -2 11 109.86 6.94 0 -2 11 119.55 7.49 0 -2 11 121.41 6.82 0 2 11 113.71 7.14 0 2 12 23.00 2.33 0 -2 12 24.96 2.85 0 -2 12 21.69 2.51 0 -2 12 24.33 2.77 0 -3 0 1.72 1.60 0 -3 -1 2202.79 70.75 0 -3 1 2059.58 71.18 0 -3 -1 2247.80 69.62 0 -3 2 109.65 9.65 0 -3 -2 105.69 8.59 0 -3 -2 110.04 8.16 0 -3 3 282.74 16.77 0 -3 -3 254.96 13.63 0 -3 -3 273.96 13.94 0 3 3 252.46 12.34 0 -3 3 253.02 12.62 0 -3 4 50.28 6.76 0 -3 -4 60.05 5.94 0 3 4 48.44 4.11 0 3 4 41.44 5.31 0 -3 4 45.09 5.48 0 3 5 290.62 12.95 0 -3 5 294.74 18.25 0 3 5 321.38 18.63 0 -3 5 286.65 17.59 0 3 6 157.71 7.89 0 3 6 169.23 14.29 0 3 6 158.19 7.88 0 -3 6 151.32 13.61 0 -3 7 298.10 12.98 0 3 7 287.90 13.07 0 -3 7 278.28 12.92 0 -3 7 314.85 13.90 0 3 7 285.39 13.02 0 -3 7 275.89 12.27 0 3 7 279.17 12.34 0 -3 7 248.22 19.67 0 3 7 304.32 21.35 0 -3 7 267.12 12.18 0 3 7 276.84 12.30 0 -3 7 305.75 13.82 0 -3 7 291.19 13.17 0 -3 7 281.76 14.61 0 3 7 298.09 13.84 0 -3 8 4.94 1.95 0 3 8 1.73 1.22 0 -3 8 3.84 1.40 0 -3 8 3.78 1.60 0 -3 8 1.82 1.12 0 -3 8 3.49 1.34 0 -3 8 4.02 1.55 0 -3 8 4.89 1.78 0 -3 8 2.09 1.54 0 -3 8 4.44 1.43 0 3 8 4.74 1.54 0 -3 8 1.12 1.12 0 3 8 5.26 1.76 0 -3 8 2.41 1.19 0 3 8 4.18 1.71 0 3 9 140.77 8.73 0 -3 9 149.41 8.39 0 3 9 132.91 8.13 0 -3 9 143.59 8.99 0 -3 9 149.84 9.07 0 -3 9 136.27 8.12 0 3 9 143.99 8.32 0 -3 9 147.74 9.05 0 -3 9 149.48 9.53 0 -3 9 150.55 8.53 0 3 9 151.69 9.01 0 3 9 150.57 9.42 0 -3 9 144.65 8.14 0 3 9 158.65 8.45 0 -3 9 155.86 8.75 0 -3 10 1.65 1.16 0 3 10 0.78 0.91 0 3 10 1.71 0.93 0 -3 10 1.85 0.83 0 -3 10 2.54 1.30 0 -3 10 1.58 0.96 0 -3 10 0.74 1.10 0 3 10 2.08 1.13 0 -3 10 1.58 1.15 0 -3 11 41.99 4.01 0 -3 11 40.44 3.41 0 3 11 37.78 3.05 0 -3 11 43.99 4.17 0 -3 11 40.41 3.63 0 -3 11 39.68 3.18 0 -3 12 174.99 7.43 0 -3 12 185.86 7.80 0 -3 12 164.67 7.54 0 -3 12 170.68 7.40 0 -4 0 353.38 20.93 0 -4 1 1946.68 68.10 0 -4 -1 1787.77 65.59 0 4 2 229.60 10.65 0 -4 -2 205.33 14.82 0 -4 -3 970.18 37.50 0 4 3 958.67 32.42 0 -4 3 945.96 42.60 0 -4 -3 968.39 38.43 0 -4 4 36.30 6.83 0 -4 5 20.29 5.32 0 4 5 20.01 3.19 0 -4 6 61.30 8.88 0 -4 6 61.37 5.31 0 -4 6 57.29 4.98 0 -4 6 64.90 5.61 0 4 6 54.38 5.28 0 -4 7 16.46 3.39 0 -4 7 29.59 3.84 0 -4 7 27.13 3.60 0 4 7 23.12 3.48 0 4 7 27.74 3.88 0 -4 7 22.04 3.22 0 -4 7 19.73 3.00 0 -4 7 17.40 2.64 0 -4 8 292.06 13.88 0 -4 8 315.06 13.93 0 -4 8 307.60 14.39 0 -4 8 311.83 15.34 0 -4 8 317.23 16.33 0 4 8 337.02 15.57 0 -4 8 326.89 13.72 0 -4 9 35.24 3.43 0 -4 9 31.73 3.82 0 -4 9 42.19 4.23 0 -4 9 32.12 3.38 0 -4 9 28.89 4.18 0 -4 9 26.30 3.27 0 -4 10 733.29 23.98 0 -4 10 719.86 24.94 0 -4 10 731.60 23.92 0 -4 11 66.88 4.56 0 4 11 65.82 4.71 0 -4 11 68.04 4.16 0 -4 11 64.80 3.28 0 -4 12 68.78 3.15 0 5 0 0.31 0.73 0 -5 0 -1.14 1.21 0 5 1 248.48 12.20 0 -5 -1 238.23 19.04 0 -5 1 278.30 21.12 0 5 2 128.18 8.39 0 -5 -2 128.58 12.80 0 5 3 525.20 21.25 0 -5 -3 486.42 26.93 0 -5 3 517.41 31.27 0 -5 4 496.61 19.75 0 -5 4 486.69 30.52 0 -5 4 474.66 18.33 0 -5 4 465.83 19.13 0 5 4 441.48 19.81 0 -5 5 238.24 11.76 0 -5 5 252.02 21.09 0 -5 5 251.01 12.54 0 -5 5 235.36 13.16 0 -5 5 234.07 12.40 0 5 5 258.06 12.44 0 5 6 21.36 3.28 0 -5 6 23.46 3.24 0 -5 6 24.06 3.35 0 -5 6 26.18 3.30 0 -5 6 18.15 3.17 0 -5 6 23.91 3.51 0 5 7 1.92 1.35 0 -5 7 2.71 1.43 0 -5 7 2.30 1.46 0 -5 7 0.92 1.03 0 -5 7 4.75 1.77 0 -5 7 0.99 1.48 0 -5 8 126.44 7.49 0 5 8 124.84 8.16 0 -5 8 133.43 8.42 0 -5 8 123.68 7.84 0 -5 8 115.20 6.86 0 -5 8 97.99 8.13 0 -5 9 254.78 12.00 0 -5 9 256.77 9.84 0 -5 9 247.46 10.19 0 -5 9 263.37 11.11 0 -5 9 248.43 12.54 0 -5 10 103.47 5.29 0 -5 10 105.80 6.09 0 5 11 81.64 3.97 0 6 0 57.46 5.18 0 -6 0 61.60 5.62 0 -6 0 49.08 9.16 0 6 0 62.58 5.48 0 6 1 450.22 19.23 0 6 1 456.35 18.50 0 -6 1 469.91 18.47 0 -6 1 463.38 19.51 0 -6 -1 443.28 18.95 0 -6 1 439.86 30.12 0 -6 -1 457.09 29.47 0 -6 -2 6.23 3.23 0 6 2 1.75 1.39 0 6 2 3.54 1.50 0 -6 2 1.23 1.23 0 -6 -2 4.02 1.55 0 -6 2 1.41 1.12 0 -6 2 3.50 1.79 0 6 3 71.14 6.59 0 -6 3 54.47 10.03 0 -6 -3 72.37 5.80 0 -6 3 60.99 6.15 0 -6 3 66.69 5.83 0 6 4 224.07 13.10 0 -6 4 259.53 13.15 0 -6 4 243.62 12.43 0 -6 5 165.22 9.72 0 -6 5 167.27 10.06 0 -6 6 27.90 3.54 0 -6 6 19.69 2.67 0 -6 6 24.27 3.01 0 -6 6 19.46 3.03 0 -6 6 24.01 3.52 0 -6 7 124.55 6.82 0 -6 7 114.57 6.35 0 -6 7 116.75 7.36 0 6 -7 116.09 6.66 0 -6 7 116.72 8.23 0 -6 7 108.40 7.35 0 -6 8 71.50 5.08 0 -6 8 71.42 5.21 0 6 -8 67.31 4.16 0 -6 8 65.43 5.47 0 -6 8 58.72 4.06 0 -6 9 175.10 7.92 0 -6 9 187.48 7.93 0 -6 9 159.57 6.55 0 -6 10 5.88 0.91 0 6 10 8.32 1.12 0 -7 0 2.57 1.86 0 -7 0 0.39 1.25 0 7 0 1.07 1.13 0 -7 1 4.38 1.97 0 -7 -1 3.78 1.65 0 -7 1 4.43 1.81 0 7 1 3.88 1.63 0 7 -1 4.30 1.56 0 -7 2 31.42 4.21 0 -7 -2 31.06 3.73 0 7 -2 28.81 3.71 0 7 2 24.13 3.31 0 -7 2 33.76 4.42 0 -7 2 30.69 3.51 0 -7 3 43.56 4.27 0 -7 3 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1 218.45 7.64 18 2 1 209.93 7.53 -18 -2 -1 252.05 8.35 18 2 1 202.96 7.50 -18 -3 7 10.21 1.00 -18 -3 6 1.17 0.57 18 -3 -6 1.42 0.52 -18 -3 5 115.50 5.50 -18 3 5 114.84 5.46 -18 -3 4 21.64 2.15 -18 3 4 21.53 2.12 18 -3 -3 15.57 1.72 18 3 -3 14.51 1.61 -18 -3 3 16.89 1.91 -18 3 3 17.24 1.88 18 3 -2 25.44 2.27 -18 -3 2 26.20 2.38 -18 3 2 27.62 2.27 18 3 -1 91.80 4.58 -18 -3 1 83.50 4.27 -18 3 1 77.58 3.83 -18 -3 0 186.12 6.92 18 3 0 180.65 7.11 -18 4 3 46.27 2.38 -19 0 7 0.09 0.37 -19 0 7 0.38 0.42 -19 0 6 10.01 1.33 -19 0 6 9.91 1.36 19 0 -5 0.13 0.41 -19 0 5 0.77 0.69 -19 0 5 0.31 0.60 -19 0 4 1.20 0.68 -19 0 4 2.34 0.87 -19 0 4 4.10 0.98 19 0 -4 2.53 0.90 -19 0 3 0.86 0.63 19 0 -3 -0.17 0.59 -19 0 3 1.16 0.80 19 0 -3 -0.80 0.77 19 0 -3 0.31 0.62 19 0 -2 233.29 9.29 19 0 -2 241.88 9.34 -19 0 2 249.60 9.48 19 0 -1 0.28 0.51 19 0 -1 0.28 0.55 -19 0 1 0.14 0.61 19 0 -1 -0.27 0.58 -19 0 0 103.59 4.62 19 0 0 103.16 4.66 19 0 0 108.09 4.73 -19 1 7 62.31 2.86 -19 1 7 62.77 2.84 -19 -1 6 52.56 2.92 -19 1 6 49.38 2.92 -19 -1 6 49.36 2.80 -19 1 6 50.39 2.89 19 -1 -5 21.70 1.98 -19 -1 5 24.28 2.14 -19 1 5 22.41 2.11 -19 -1 5 24.49 2.08 -19 1 5 24.98 2.15 19 -1 -4 0.81 0.59 19 1 -4 2.33 0.86 19 1 -4 1.80 0.69 19 -1 -4 1.95 0.78 -19 -1 4 2.34 0.82 -19 1 4 1.51 0.71 19 -1 -4 1.24 0.76 19 1 -4 0.70 0.68 -19 -1 4 2.83 0.86 -19 1 4 1.64 0.74 19 -1 -3 0.14 0.61 19 1 -3 0.56 0.61 -19 -1 3 0.14 0.58 -19 -1 3 -0.44 0.60 -19 1 3 0.45 0.69 19 -1 -3 -0.14 0.50 19 1 -3 0.29 0.59 19 1 -3 0.16 0.55 19 -1 -3 0.93 0.61 19 1 -2 58.77 3.48 -19 -1 2 53.32 3.35 -19 1 2 57.50 3.49 19 -1 -2 55.66 3.37 19 -1 -2 53.81 3.37 19 1 -2 55.20 3.44 19 1 -2 60.82 3.71 19 -1 -2 59.04 3.56 19 -1 -1 77.75 3.89 19 1 -1 80.97 3.99 19 -1 -1 69.00 3.73 19 1 -1 66.14 3.72 -19 -1 1 82.45 3.91 -19 1 1 78.70 3.92 19 -1 -1 73.78 3.80 19 1 -1 75.83 3.89 19 -1 -1 69.21 3.75 19 -1 0 57.66 2.98 19 1 0 65.98 3.15 19 1 0 60.59 3.03 -19 -1 0 62.33 2.96 -19 1 0 62.98 3.05 19 -1 0 57.75 2.96 19 1 0 63.53 3.06 19 1 0 56.74 3.07 -19 -2 6 5.08 0.72 -19 -2 5 101.72 4.51 19 -2 -5 105.08 4.57 -19 -2 4 26.24 2.04 19 2 -4 22.83 1.58 19 -2 -4 29.57 2.17 -19 2 4 26.99 1.96 -19 -2 3 203.26 7.12 19 2 -3 198.26 6.99 19 -2 -3 179.73 6.97 -19 2 3 186.98 6.50 19 2 -3 167.82 6.21 -19 -2 2 0.31 0.45 19 2 -2 -0.07 0.31 19 2 -2 0.36 0.43 19 -2 -2 0.30 0.40 19 2 -1 38.97 2.43 -19 -2 1 36.95 2.16 0 0 0 0.00 0.00 TITL G-61_g in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 15.613590 7.221389 10.792910 90.0000 104.6224 90.0000 ZERR 4.00 0.000127 0.000067 0.000080 0.0000 0.0008 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O F Cl UNIT 36.00 36.00 8.00 12.00 4.00 8.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.0; aver:100.0 TEMP -173 SIZE 0.05 0.15 0.32 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 27162 _shelx_res_file ; TITL g-61_g_a.res in P2(1)/c g-61_g.res created by SHELXL-2018/3 at 16:22:58 on 18-Dec-2024 REM Old TITL G-61_g in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.084, Rweak 0.029, Alpha 0.018, Orientation as input REM Formula found by SHELXT: C11 N O3 F Cl2 CELL 1.54184 15.6136 7.2214 10.7929 90 104.622 90 ZERR 4 0.0001 0.0001 0.0001 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl F N O UNIT 40 36 8 4 8 12 EQIV $1 2-X,2-Y,1-Z EQIV $2 +X,1+Y,+Z EQIV $3 +X,2.5-Y,-0.5+Z EQIV $4 +X,1.5-Y,-0.5+Z L.S. 11 0 0 PLAN 5 SIZE 0.05 0.15 0.32 TEMP -173 CONF HTAB O4 O2_$1 HTAB N1 O4_$2 HTAB N1 O2_$3 HTAB N3 O6_$4 BOND $H list 4 MORE -1 fmap 2 53 acta REM REM REM WGHT 0.041800 0.763900 FVAR 0.71566 CL1 3 0.758125 0.640650 0.209813 11.00000 0.02614 0.02256 = 0.01572 -0.00293 0.00426 -0.00771 CL2 3 0.711083 0.907858 0.386636 11.00000 0.02389 0.01773 = 0.02451 0.00032 0.00429 0.00268 F1 4 0.459321 0.188668 0.445589 11.00000 0.02547 0.03252 = 0.03946 0.00073 0.01004 -0.00970 O2 6 0.914291 1.164678 0.499590 11.00000 0.02210 0.01987 = 0.02716 -0.00614 0.00586 -0.00360 O4 6 0.936360 0.665167 0.382190 11.00000 0.02039 0.01724 = 0.02712 -0.00571 0.00573 -0.00307 H4 2 0.984778 0.692155 0.417207 11.00000 0.03808 O6 6 0.838234 0.536276 0.551469 11.00000 0.02262 0.02290 = 0.01881 0.00106 0.00235 0.00058 N1 5 0.913210 1.274182 0.301877 11.00000 0.03586 0.01674 = 0.03209 -0.00199 0.01027 -0.00404 H1A 2 0.920571 1.389034 0.334098 11.00000 0.04034 H1B 2 0.907072 1.259291 0.220879 11.00000 0.03244 N3 5 0.885226 0.967451 0.329662 11.00000 0.02847 0.01741 = 0.01998 -0.00228 0.00459 -0.00560 H3 2 0.879642 0.957973 0.248027 11.00000 0.03465 C2 1 0.904982 1.138533 0.383318 11.00000 0.01473 0.01767 = 0.02809 -0.00383 0.00406 -0.00149 C4 1 0.879901 0.805791 0.404055 11.00000 0.02186 0.01508 = 0.02100 -0.00239 0.00428 -0.00237 AFIX 13 H4A 2 0.896975 0.839528 0.496915 11.00000 -1.20000 AFIX 0 C5 1 0.784958 0.724770 0.370278 11.00000 0.02140 0.01581 = 0.01713 -0.00175 0.00287 -0.00114 C6 1 0.774504 0.568769 0.463813 11.00000 0.02149 0.01595 = 0.01640 -0.00241 0.00568 0.00012 C7 1 0.688983 0.469052 0.450004 11.00000 0.02175 0.01646 = 0.01859 -0.00190 0.00629 -0.00079 C8 1 0.611140 0.507695 0.356082 11.00000 0.02386 0.02107 = 0.02035 0.00138 0.00451 -0.00114 AFIX 43 H8 2 0.611405 0.600113 0.293538 11.00000 -1.20000 AFIX 0 C9 1 0.533552 0.412078 0.353577 11.00000 0.02189 0.02541 = 0.02370 -0.00136 0.00425 -0.00069 AFIX 43 H9 2 0.480694 0.437166 0.289650 11.00000 -1.20000 AFIX 0 C10 1 0.535223 0.279700 0.446337 11.00000 0.02356 0.02066 = 0.02852 -0.00454 0.00930 -0.00581 C11 1 0.610518 0.236824 0.540160 11.00000 0.02972 0.02269 = 0.02687 0.00516 0.00879 -0.00319 AFIX 43 H11 2 0.609462 0.144287 0.602320 11.00000 -1.20000 AFIX 0 C12 1 0.687682 0.332116 0.541420 11.00000 0.02325 0.02101 = 0.02309 0.00280 0.00399 -0.00006 AFIX 43 H12 2 0.740343 0.304306 0.605008 11.00000 -1.20000 AFIX 0 HKLF 4 REM g-61_g_a.res in P2(1)/c REM wR2 = 0.0815, GooF = S = 1.061, Restrained GooF = 1.061 for all data REM R1 = 0.0314 for 2494 Fo > 4sig(Fo) and 0.0321 for all 2562 data REM 179 parameters refined using 0 restraints END WGHT 0.0418 0.7627 REM Highest difference peak 0.401, deepest hole -0.307, 1-sigma level 0.059 Q1 1 0.7008 0.8996 0.3049 11.00000 0.05 0.40 Q2 1 0.7793 0.5292 0.2085 11.00000 0.05 0.36 Q3 1 0.7284 0.5221 0.4528 11.00000 0.05 0.36 Q4 1 0.7566 0.8054 0.3758 11.00000 0.05 0.35 Q5 1 0.7771 0.6555 0.4148 11.00000 0.05 0.33 ; _shelx_res_checksum 14821 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 Cl Cl1 0.75812(2) 0.64065(5) 0.20981(3) 0.02166(11) Uani d 1 . . Cl Cl2 0.71108(2) 0.90786(5) 0.38664(3) 0.02237(11) Uani d 1 . . F F1 0.45932(7) 0.18867(16) 0.44559(10) 0.0321(2) Uani d 1 . . O O2 0.91429(7) 1.16468(16) 0.49959(11) 0.0231(2) Uani d 1 . . O O4 0.93636(8) 0.66517(16) 0.38219(11) 0.0216(2) Uani d 1 . . H H4 0.9848(18) 0.692(4) 0.417(2) 0.038(7) Uiso d 1 . . O O6 0.83823(7) 0.53628(16) 0.55147(10) 0.0220(2) Uani d 1 . . N N1 0.91321(10) 1.2742(2) 0.30188(16) 0.0279(3) Uani d 1 . . H H1A 0.9206(17) 1.389(4) 0.334(2) 0.040(7) Uiso d 1 . . H H1B 0.9071(15) 1.259(4) 0.221(2) 0.032(6) Uiso d 1 . . N N3 0.88523(9) 0.96745(19) 0.32966(13) 0.0222(3) Uani d 1 . . H H3 0.8796(15) 0.958(4) 0.248(2) 0.035(6) Uiso d 1 . . C C2 0.90498(10) 1.1385(2) 0.38332(16) 0.0204(3) Uani d 1 . . C C4 0.87990(10) 0.8058(2) 0.40405(14) 0.0195(3) Uani d 1 . . H H4A 0.896975 0.839528 0.496915 0.023 Uiso calc 1 . . C C5 0.78496(10) 0.7248(2) 0.37028(13) 0.0185(3) Uani d 1 . . C C6 0.77450(10) 0.5688(2) 0.46381(14) 0.0178(3) Uani d 1 . . C C7 0.68898(10) 0.4691(2) 0.45000(14) 0.0187(3) Uani d 1 . . C C8 0.61114(10) 0.5077(2) 0.35608(15) 0.0220(3) Uani d 1 . . H H8 0.611405 0.600113 0.293538 0.026 Uiso calc 1 . . C C9 0.53355(11) 0.4121(2) 0.35358(16) 0.0239(3) Uani d 1 . . H H9 0.480694 0.437166 0.289650 0.029 Uiso calc 1 . . C C10 0.53522(11) 0.2797(2) 0.44634(16) 0.0238(3) Uani d 1 . . C C11 0.61052(11) 0.2368(2) 0.54016(16) 0.0261(3) Uani d 1 . . H H11 0.609462 0.144287 0.602320 0.031 Uiso calc 1 . . C C12 0.68768(11) 0.3321(2) 0.54142(15) 0.0228(3) Uani d 1 . . H H12 0.740343 0.304306 0.605008 0.027 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 0.02614(19) 0.0226(2) 0.01572(18) -0.00771(14) 0.00426(13) -0.00293(12) Cl2 0.02389(19) 0.01773(19) 0.0245(2) 0.00268(13) 0.00429(14) 0.00032(13) F1 0.0255(5) 0.0325(6) 0.0395(6) -0.0097(4) 0.0100(4) 0.0007(5) O2 0.0221(5) 0.0199(6) 0.0272(6) -0.0036(4) 0.0059(4) -0.0061(4) O4 0.0204(5) 0.0172(5) 0.0271(6) -0.0031(4) 0.0057(4) -0.0057(4) O6 0.0226(5) 0.0229(6) 0.0188(5) 0.0006(4) 0.0023(4) 0.0011(4) N1 0.0359(8) 0.0167(7) 0.0321(8) -0.0040(6) 0.0103(6) -0.0020(6) N3 0.0285(7) 0.0174(7) 0.0200(6) -0.0056(5) 0.0046(5) -0.0023(5) C2 0.0147(6) 0.0177(7) 0.0281(8) -0.0015(5) 0.0041(6) -0.0038(6) C4 0.0219(7) 0.0151(7) 0.0210(7) -0.0024(6) 0.0043(5) -0.0024(6) C5 0.0214(7) 0.0158(7) 0.0171(6) -0.0011(6) 0.0029(5) -0.0017(5) C6 0.0215(7) 0.0160(7) 0.0164(7) 0.0001(5) 0.0057(5) -0.0024(5) C7 0.0218(7) 0.0165(7) 0.0186(7) -0.0008(6) 0.0063(5) -0.0019(5) C8 0.0239(7) 0.0211(7) 0.0204(7) -0.0011(6) 0.0045(6) 0.0014(6) C9 0.0219(7) 0.0254(8) 0.0237(7) -0.0007(6) 0.0042(6) -0.0014(6) C10 0.0236(7) 0.0207(8) 0.0285(8) -0.0058(6) 0.0093(6) -0.0045(6) C11 0.0297(8) 0.0227(8) 0.0269(8) -0.0032(7) 0.0088(6) 0.0052(6) C12 0.0233(7) 0.0210(8) 0.0231(7) -0.0001(6) 0.0040(6) 0.0028(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' N N 0.0311 0.0180 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 1 0 0.0647 0 -1 -1 0.0935 1 0 0 0.0247 -1 0 0 0.0285 0 1 0 0.0724 0 -1 0 0.0781 0 -2 1 0.0940 -1 2 2 0.0745 1 0 -2 0.1266 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 C4 O4 H4 . . 108.1(19) ? H1A N1 H1B . . 119(2) ? C2 N1 H1A . . 116.4(17) ? C2 N1 H1B . . 124.6(17) ? C2 N3 H3 . . 117.2(17) ? C2 N3 C4 . . 122.60(14) ? C4 N3 H3 . . 120.1(17) ? O2 C2 N1 . . 122.99(15) n O2 C2 N3 . . 121.50(15) n N1 C2 N3 . . 115.50(15) ? O4 C4 N3 . . 111.59(13) n O4 C4 H4A . . 109.0 ? O4 C4 C5 . . 106.95(12) ? N3 C4 H4A . . 109.0 ? N3 C4 C5 . . 111.33(13) n C5 C4 H4A . . 109.0 ? Cl1 C5 Cl2 . . 110.35(8) n C4 C5 Cl1 . . 109.49(10) ? C4 C5 Cl2 . . 107.43(10) ? C6 C5 Cl1 . . 110.36(10) ? C6 C5 Cl2 . . 107.22(10) ? C6 C5 C4 . . 111.93(12) n O6 C6 C5 . . 116.71(13) ? O6 C6 C7 . . 121.55(14) ? C7 C6 C5 . . 121.69(13) ? C8 C7 C6 . . 124.60(14) ? C8 C7 C12 . . 119.10(14) ? C12 C7 C6 . . 116.26(14) ? C7 C8 H8 . . 119.7 ? C9 C8 C7 . . 120.56(15) ? C9 C8 H8 . . 119.7 ? C8 C9 H9 . . 120.9 ? C10 C9 C8 . . 118.28(15) ? C10 C9 H9 . . 120.9 ? F1 C10 C9 . . 118.43(15) ? F1 C10 C11 . . 118.56(15) ? C11 C10 C9 . . 123.01(15) ? C10 C11 H11 . . 120.9 ? C10 C11 C12 . . 118.29(15) ? C12 C11 H11 . . 120.9 ? C7 C12 H12 . . 119.6 ? C11 C12 C7 . . 120.75(15) ? C11 C12 H12 . . 119.6 ? 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 C5 . 1.7826(14) ? Cl2 C5 . 1.7923(16) ? F1 C10 . 1.3534(18) ? O2 C2 . 1.241(2) ? O4 H4 . 0.78(3) ? O4 C4 . 1.4032(19) ? O6 C6 . 1.2103(19) ? N1 H1A . 0.90(3) ? N1 H1B . 0.86(2) ? N1 C2 . 1.344(2) ? N3 H3 . 0.87(2) ? N3 C2 . 1.366(2) ? N3 C4 . 1.431(2) ? C4 H4A . 1.0000 ? C4 C5 . 1.549(2) ? C5 C6 . 1.549(2) ? C6 C7 . 1.491(2) ? C7 C8 . 1.400(2) ? C7 C12 . 1.401(2) ? C8 H8 . 0.9500 ? C8 C9 . 1.389(2) ? C9 H9 . 0.9500 ? C9 C10 . 1.380(2) ? C10 C11 . 1.379(2) ? C11 H11 . 0.9500 ? C11 C12 . 1.385(2) ? C12 H12 . 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 N1 H1A O4 1_565 0.90(3) 2.06(3) 2.9488(19) 172(2) yes N1 H1B O2 4_585 0.86(2) 2.48(2) 3.297(2) 158(2) yes N3 H3 O6 4_575 0.87(2) 2.06(2) 2.9055(18) 167(2) yes O4 H4 O2 3_776 0.78(3) 1.91(3) 2.6596(16) 161(3) 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 Cl1 C5 C6 O6 . . . . 125.15(13) ? Cl1 C5 C6 C7 . . . . -57.44(16) ? Cl2 C5 C6 O6 . . . . -114.62(13) ? Cl2 C5 C6 C7 . . . . 62.78(15) ? F1 C10 C11 C12 . . . . -179.17(15) ? O4 C4 C5 Cl1 . . . . -56.04(14) ? O4 C4 C5 Cl2 . . . . -175.90(10) ? O4 C4 C5 C6 . . . . 66.65(15) ? O6 C6 C7 C8 . . . . 175.69(15) ? O6 C6 C7 C12 . . . . -2.1(2) ? N3 C4 C5 Cl1 . . . . 66.10(14) ? N3 C4 C5 Cl2 . . . . -53.75(14) ? N3 C4 C5 C6 . . . . -171.20(12) ? C2 N3 C4 O4 . . . . -124.46(15) ? C2 N3 C4 C5 . . . . 116.12(15) ? C4 N3 C2 O2 . . . . -4.3(2) ? C4 N3 C2 N1 . . . . 175.81(14) ? C4 C5 C6 O6 . . . . 2.95(19) ? C4 C5 C6 C7 . . . . -179.65(13) ? C5 C6 C7 C8 . . . . -1.6(2) ? C5 C6 C7 C12 . . . . -179.34(13) ? C6 C7 C8 C9 . . . . -177.53(15) ? C6 C7 C12 C11 . . . . 177.33(15) ? C7 C8 C9 C10 . . . . 0.5(2) ? C8 C7 C12 C11 . . . . -0.5(2) ? C8 C9 C10 F1 . . . . 178.80(15) ? C8 C9 C10 C11 . . . . -0.8(3) ? C9 C10 C11 C12 . . . . 0.4(3) ? C10 C11 C12 C7 . . . . 0.3(3) ? C12 C7 C8 C9 . . . . 0.2(2) ?