#------------------------------------------------------------------------------ #$Date: 2024-03-05 21:43:51 +0100 (Tue, 05 Mar 2024) $ #$Revision: 290336 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/30/2023020.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_2023020 loop_ _publ_author_name 'Naghiyev, Farid N.' 'Khrustalev, Victor N.' 'Akkurt, Mehmet' 'Dukhnovsky, Evgeny A.' 'Bhattarai, Ajaya' 'Khalilov, Ali N.' 'Mamedov, İbrahim G' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of 4-(2-chloro-eth-yl)-5-methyl-1,2-di-hydro-pyrazol-3-one. ; _journal_coeditor_code NX2004 _journal_issue 'Pt 2' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 223 _journal_page_last 227 _journal_paper_doi 10.1107/S2056989024000835 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C6 H9 Cl N2 O' _chemical_formula_moiety 'C6 H9 Cl N2 O' _chemical_formula_sum 'C6 H9 Cl N2 O' _chemical_formula_weight 160.60 _chemical_name_systematic ; 4-(2-Chloroethyl)-5-methyl-1,2-dihydropyrazol-3-one ; _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 difmap _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 93.618(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8420(2) _cell_length_b 6.9145(2) _cell_length_c 11.1807(2) _cell_measurement_reflns_used 4592 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 77.61 _cell_measurement_theta_min 4.51 _cell_volume 759.36(3) _computing_cell_refinement ; CrysAlisPro 1.171.42.53a (Rigaku OD, 2022) ; _computing_data_collection ; CrysAlisPro 1.171.42.53a (Rigaku OD, 2022) ; _computing_data_reduction ; CrysAlisPro 1.171.42.53a (Rigaku OD, 2022) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.947 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_unetI/netI 0.0204 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6642 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.513 _diffrn_reflns_theta_min 4.502 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.917 _exptl_absorpt_correction_T_max 0.750 _exptl_absorpt_correction_T_min 0.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2022) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.405 _exptl_crystal_description prism _exptl_crystal_F_000 336 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.284 _refine_diff_density_min -0.410 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 1532 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0356 _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^)+(0.0501P)^2^+0.606P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.0972 _reflns_number_gt 1467 _reflns_number_total 1532 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file nx2004sup1.cif _cod_data_source_block I _cod_depositor_comments 'Adding full bibliography for 2023020.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2023020 _cod_database_fobs_code 2023020 _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 0.508 _shelx_estimated_absorpt_t_max 0.799 _shelx_hkl_file ; 0 0 -1 0.02 0.20 0 0 -1 -0.18 0.41 0 0 -2 235.10 7.07 0 0 -2 241.27 6.67 0 0 -3 0.42 0.56 0 0 -4 3989.89 104.48 0 0 -4 4072.33 104.48 0 0 -5 -0.06 0.69 0 0 -5 -0.07 0.83 0 0 -5 0.11 0.33 0 0 -6 47.83 1.62 0 0 -6 48.15 2.62 0 0 -6 51.46 2.75 0 0 -7 -0.22 0.98 0 0 -7 -0.10 0.82 0 0 -8 7.54 1.45 0 0 -8 5.52 0.93 0 0 -8 5.66 0.63 0 0 -8 4.49 0.58 0 0 -8 5.00 0.58 0 0 -8 4.96 0.69 0 0 -8 6.48 1.26 0 0 -9 0.35 0.66 0 0 -9 0.32 0.93 0 0 -9 -0.29 1.01 0 0 -9 -0.34 0.50 0 0 -9 0.12 0.49 0 0 -10 490.47 13.26 0 0 -10 478.80 13.68 0 0 -10 496.23 13.40 0 0 -10 494.22 13.33 0 0 -11 -0.03 0.50 0 0 -11 -0.31 0.69 0 0 -11 0.43 1.03 0 0 -11 -0.44 0.58 0 0 -12 306.65 8.42 0 0 -12 278.36 8.07 0 0 -13 0.64 0.80 0 -1 0 0.23 0.39 0 -1 -1 194.75 5.60 0 -1 -1 195.53 5.27 0 -1 -1 186.49 5.26 0 -1 1 202.46 5.59 0 1 -1 194.83 5.27 0 1 -1 201.18 5.29 0 -1 -1 202.29 5.55 0 -1 -2 27.35 1.22 0 1 -2 24.70 1.15 0 -1 -2 25.51 1.17 0 -1 -2 25.76 1.29 0 1 -2 26.46 1.17 0 -1 2 24.81 1.15 0 -1 -2 27.03 1.16 0 -1 -3 527.81 14.05 0 -1 -3 512.52 14.22 0 -1 3 520.44 13.95 0 1 -3 528.88 14.23 0 -1 -3 517.36 14.23 0 1 -3 538.16 14.27 0 -1 -4 0.69 0.57 0 1 -4 -0.05 0.60 0 -1 4 0.16 0.26 0 1 -4 0.15 0.69 0 -1 -4 0.99 0.73 0 1 -5 205.73 6.60 0 1 -5 206.03 5.51 0 -1 -5 202.92 6.62 0 -1 -5 203.34 6.57 0 1 -5 213.27 6.65 0 -1 -5 196.77 5.50 0 -1 -6 589.94 17.29 0 1 -6 634.07 17.47 0 -1 -6 588.67 15.88 0 -1 -6 620.60 17.48 0 1 -6 617.94 17.35 0 1 -6 612.06 15.89 0 -1 -7 1374.67 37.52 0 -1 -7 1390.44 35.77 0 -1 -7 1412.29 37.75 0 1 -7 1449.71 37.76 0 -1 -7 1333.37 35.68 0 1 -7 1398.44 37.54 0 1 -8 224.66 6.25 0 1 -8 222.39 6.19 0 1 -8 213.16 6.21 0 -1 -8 232.14 6.33 0 -1 -8 211.70 6.18 0 -1 -8 218.25 8.00 0 1 -8 213.66 6.48 0 -1 -8 216.88 6.51 0 1 -8 219.20 8.00 0 -1 -8 215.83 6.13 0 -1 -8 213.26 6.27 0 1 -8 221.78 6.18 0 -1 -8 219.69 6.19 0 -1 -9 5.18 0.76 0 -1 -9 5.53 0.85 0 1 -9 4.86 0.67 0 1 -9 4.20 1.18 0 -1 -9 4.72 1.27 0 -1 -9 5.73 0.72 0 1 -9 5.17 0.67 0 1 -9 5.36 1.03 0 -1 -9 4.35 0.60 0 1 -9 4.75 0.77 0 -1 -9 5.17 1.03 0 -1 -9 4.87 0.66 0 -1 -10 321.36 8.78 0 1 -10 306.49 8.63 0 1 -10 301.78 8.65 0 1 -10 301.14 8.96 0 -1 -10 316.05 8.65 0 1 -10 319.15 8.64 0 -1 -10 291.32 8.47 0 -1 -10 315.97 9.01 0 1 -11 347.62 9.73 0 -1 -11 362.86 10.08 0 1 -11 335.59 9.65 0 -1 -11 353.35 9.70 0 -1 -11 343.06 9.81 0 1 -11 358.97 10.06 0 1 -11 360.54 9.70 0 -1 -12 6.44 1.07 0 1 -12 6.19 1.05 0 -1 -12 5.33 0.84 0 1 -12 5.22 0.74 0 -1 -13 48.67 1.77 0 -2 0 82.77 3.17 0 -2 1 1153.89 30.73 0 -2 -1 1152.51 30.65 0 -2 -2 183.77 5.40 0 2 -2 195.61 5.43 0 -2 2 190.60 5.99 0 -2 -2 187.24 5.37 0 -2 -2 184.20 5.98 0 2 -2 200.31 5.43 0 -2 -2 199.55 6.12 0 2 -3 356.23 10.02 0 -2 -3 352.83 10.02 0 -2 -3 374.52 10.48 0 -2 3 361.77 10.30 0 -2 -3 350.00 10.56 0 -2 -3 354.46 9.98 0 2 -3 367.70 10.03 0 2 -4 17.29 1.23 0 -2 -4 19.21 1.32 0 -2 4 19.44 1.20 0 -2 -4 17.17 1.21 0 -2 -4 17.59 1.29 0 2 -4 20.06 1.36 0 2 -5 37.98 2.05 0 -2 -5 38.56 1.36 0 -2 -5 41.84 2.24 0 2 -5 37.80 2.12 0 -2 -5 39.25 2.07 0 -2 -6 320.03 8.44 0 -2 -6 309.87 9.70 0 2 -6 324.54 9.88 0 2 -6 325.08 9.79 0 -2 -6 319.03 9.90 0 -2 -6 298.53 8.34 0 2 -7 14.21 1.51 0 -2 -7 13.39 0.76 0 -2 -7 16.40 1.63 0 2 -7 16.10 0.81 0 2 -7 13.96 0.89 0 -2 -7 13.58 0.81 0 2 -7 15.47 0.94 0 -2 -7 12.03 0.84 0 2 -7 16.42 1.09 0 2 -7 15.32 0.88 0 -2 -7 15.34 1.08 0 -2 -7 13.92 0.78 0 2 -8 19.49 1.91 0 -2 -8 19.54 1.30 0 2 -8 19.03 1.29 0 -2 -8 18.02 1.02 0 2 -8 19.44 0.98 0 2 -8 20.03 1.14 0 2 -8 19.37 1.12 0 -2 -8 18.43 1.09 0 -2 -8 18.78 0.99 0 -2 -8 17.50 1.81 0 2 -8 18.62 1.06 0 2 -9 7.54 0.84 0 -2 -9 7.39 1.10 0 -2 -9 7.00 0.71 0 2 -9 8.33 0.72 0 -2 -9 7.58 0.81 0 2 -9 8.12 1.07 0 2 -9 8.76 0.85 0 2 -10 5.81 0.79 0 2 -10 7.20 0.72 0 -2 -10 5.81 0.81 0 2 -10 5.57 0.75 0 2 -10 5.12 1.03 0 -2 -10 5.54 0.67 0 -2 -10 6.33 1.07 0 2 -11 15.87 1.01 0 -2 -11 16.23 1.21 0 2 -11 15.38 1.02 0 2 -11 16.12 1.27 0 -2 -11 15.23 1.32 0 2 -12 0.02 0.46 0 -2 -12 0.82 0.73 0 2 -12 -0.10 0.76 0 -2 -12 0.42 0.80 0 -3 0 0.08 0.80 0 -3 -1 325.03 9.99 0 -3 1 322.45 10.01 0 -3 2 62.92 3.02 0 -3 -2 62.06 2.98 0 -3 -2 64.35 3.13 0 -3 -3 20.25 1.67 0 -3 3 19.93 1.57 0 -3 -3 16.48 1.63 0 -3 -4 0.31 0.93 0 3 -4 0.69 0.47 0 -3 -4 0.72 0.70 0 -3 4 0.83 0.62 0 3 -5 31.84 1.77 0 -3 -5 27.96 1.20 0 -3 5 27.65 1.74 0 3 -6 206.90 5.72 0 -3 -6 194.00 5.58 0 -3 -6 187.06 5.60 0 -3 -6 205.21 5.72 0 -3 -6 198.88 6.14 0 -3 -6 209.91 5.82 0 -3 -7 216.71 6.18 0 -3 -7 226.70 6.85 0 -3 -7 229.87 6.36 0 -3 -7 219.62 6.31 0 3 -7 221.63 6.40 0 3 -7 239.05 6.44 0 -3 -7 244.95 6.56 0 -3 -7 206.98 6.29 0 -3 -7 214.24 6.15 0 3 -8 10.16 0.69 0 3 -8 8.25 0.81 0 -3 -8 8.05 0.69 0 3 -8 9.55 0.97 0 -3 -8 9.28 0.81 0 -3 -8 9.87 1.05 0 -3 -8 8.55 0.66 0 -3 -8 9.60 0.69 0 -3 -8 9.62 0.97 0 3 -8 9.35 0.92 0 -3 -8 7.82 0.69 0 3 -9 303.95 8.59 0 -3 -9 301.28 8.32 0 -3 -9 296.55 8.46 0 3 -9 308.51 8.29 0 3 -9 306.08 8.43 0 -3 -9 294.57 8.58 0 3 -10 252.82 7.26 0 3 -10 252.59 7.09 0 -3 -10 244.21 7.14 0 3 -10 260.26 7.24 0 -3 -10 248.37 7.26 0 3 -11 177.79 5.20 0 3 -12 6.52 0.59 0 -4 0 1816.54 49.30 0 -4 1 1.98 0.99 0 -4 -1 2.73 1.01 0 -4 -2 142.33 5.86 0 -4 2 136.63 5.64 0 -4 -2 132.84 5.56 0 -4 -3 1.33 0.87 0 -4 -3 1.01 0.68 0 -4 3 1.58 0.83 0 -4 -3 1.89 0.90 0 -4 4 1998.03 53.33 0 -4 -4 2088.27 53.93 0 -4 -5 126.58 4.48 0 -4 -5 135.27 4.10 0 4 -6 22.81 1.20 0 -4 -6 22.42 1.59 0 -4 -6 22.26 1.09 0 -4 -6 23.79 1.23 0 4 -7 31.62 1.48 0 -4 -7 27.28 1.29 0 -4 -7 28.36 1.81 0 -4 -7 29.53 1.40 0 -4 -8 755.75 20.13 0 -4 -8 741.54 20.15 0 4 -8 789.62 20.16 0 4 -8 761.32 20.03 0 -4 -8 725.01 19.99 0 4 -8 830.11 20.27 0 -4 -8 714.04 20.06 0 4 -9 20.54 1.09 0 4 -12 12.98 0.65 0 -5 0 0.51 0.66 0 -5 0 -0.48 0.98 0 -5 0 0.57 1.02 0 -5 1 17.82 2.07 0 -5 -1 16.92 1.26 0 -5 -1 18.82 2.07 0 -5 1 19.52 1.21 0 -5 -2 149.61 6.64 0 -5 -2 142.43 4.76 0 -5 -2 139.42 6.32 0 -5 2 141.84 6.35 0 -5 -2 143.79 4.27 0 -5 -3 743.56 21.92 0 -5 3 708.11 21.33 0 -5 -3 710.38 19.42 0 -5 -3 672.40 21.45 0 -5 -4 69.27 4.32 0 -5 -4 66.93 2.96 0 -5 4 65.58 3.81 0 -5 -4 75.13 4.37 0 -5 -5 10.75 0.91 0 5 -6 206.05 5.97 0 -5 -6 210.85 6.20 0 -5 -6 202.51 6.74 0 -5 -7 618.82 16.63 0 5 -7 612.00 16.43 0 -5 -8 15.97 1.00 0 -5 8 14.61 0.92 0 5 -9 67.10 2.33 0 5 -10 12.16 0.78 0 -6 0 2.49 1.36 0 -6 0 4.31 1.36 0 -6 0 3.31 0.86 0 -6 -1 10.41 1.79 0 -6 1 11.06 1.07 0 -6 1 10.66 1.84 0 -6 1 12.27 1.90 0 -6 -1 9.08 0.77 0 -6 -1 12.35 1.20 0 -6 2 22.00 2.42 0 -6 -2 25.34 1.69 0 -6 2 25.16 2.69 0 -6 -2 25.78 1.21 0 -6 -2 20.94 2.45 0 -6 -2 26.25 2.77 0 -6 -3 172.79 7.74 0 -6 -3 181.94 5.93 0 -6 3 166.00 7.40 0 -6 -3 180.17 7.97 0 -6 -4 44.13 2.32 0 -6 -4 39.64 1.82 0 -6 -5 1.57 1.05 0 -6 -5 2.07 0.57 0 6 -6 2.45 0.53 0 -6 -6 3.08 0.58 0 -6 6 3.54 0.63 0 6 -7 27.99 1.30 0 -6 -7 28.30 1.33 0 -6 7 27.82 1.30 0 -6 -7 29.32 1.37 0 6 -8 1.32 0.50 0 -6 8 1.58 0.39 0 6 -9 18.02 0.84 0 6 -10 42.86 1.34 0 -7 0 -0.13 0.44 0 -7 0 -0.14 0.77 0 -7 0 0.13 0.43 0 -7 -1 107.46 3.84 0 -7 -1 107.46 3.52 0 -7 1 106.94 3.48 0 -7 -2 8.15 1.13 0 -7 2 9.32 0.82 0 -7 -2 8.73 0.80 0 -7 3 24.93 1.32 0 -7 -3 26.17 1.70 0 -7 -3 27.88 1.38 0 -7 4 221.26 6.51 0 -7 -4 233.76 7.02 0 -7 -5 17.41 1.02 0 -7 5 19.07 1.04 0 7 -5 18.52 0.90 0 7 -6 50.45 1.70 0 -7 -6 52.06 1.87 0 -7 6 51.73 1.83 0 -7 7 99.11 2.92 0 7 -7 98.33 2.84 0 7 -8 8.28 0.42 0 -8 0 188.69 5.32 0 -8 -1 3.10 0.44 0 -8 -2 2.80 0.41 0 -8 2 4.00 0.44 0 -8 -3 62.16 2.08 0 -8 3 64.67 2.05 0 -8 5 13.74 0.60 0 -8 -5 11.00 0.58 1 0 -13 0.78 0.57 1 0 -13 -0.61 0.77 1 0 -12 1.99 1.01 1 0 -12 1.94 0.76 1 0 -11 0.12 0.56 1 0 -11 0.04 0.72 1 0 -11 0.83 1.08 1 0 -10 320.90 8.97 1 0 -10 322.62 8.98 1 0 -10 316.89 9.07 1 0 -10 325.79 9.41 1 0 -9 0.57 0.53 1 0 -9 -0.24 0.95 1 0 -9 0.44 0.51 1 0 -9 0.15 0.94 1 0 -9 -0.13 0.69 1 0 -8 798.69 20.72 1 0 -8 784.78 20.71 1 0 -8 760.63 22.83 1 0 -8 792.50 21.07 1 0 -8 770.92 20.68 1 0 -7 -0.11 0.80 1 0 -7 -0.09 0.44 1 0 -6 -0.26 0.85 1 0 -6 0.30 0.38 1 0 -5 0.15 0.34 1 0 -5 0.69 0.78 1 0 -5 -0.13 0.80 1 0 -4 611.76 16.65 1 0 -4 597.13 16.73 1 0 -3 -0.08 0.60 1 0 -2 1299.41 35.12 -1 0 2 1370.15 34.84 -1 0 1 0.02 0.30 -1 0 0 597.01 15.75 -1 0 -1 -0.02 0.37 -1 0 -1 0.51 0.61 -1 0 -2 3126.72 87.19 -1 0 -2 3253.63 86.67 -1 0 -3 0.04 0.55 -1 0 -3 -0.37 1.21 -1 0 -3 -0.04 0.54 -1 0 -3 0.32 0.45 -1 0 -4 1417.01 35.69 -1 0 -4 1399.16 36.87 -1 0 -4 1426.47 35.76 -1 0 -5 0.49 0.79 -1 0 -5 -0.13 1.58 -1 0 -5 -0.06 0.66 -1 0 -6 1296.12 35.25 -1 0 -6 1293.60 35.06 -1 0 -7 -0.30 0.41 -1 0 -7 0.51 0.42 -1 0 -7 -0.10 0.81 -1 0 -7 -0.02 0.42 -1 0 -7 0.34 0.97 -1 0 -7 -0.10 0.68 -1 0 -8 385.49 9.97 -1 0 -8 362.18 9.85 -1 0 -8 380.01 9.88 -1 0 -8 362.12 9.84 -1 0 -8 335.38 9.86 -1 0 -8 350.84 10.13 -1 0 -8 381.90 12.23 -1 0 -8 347.23 9.75 -1 0 -9 0.22 0.91 -1 0 -9 -0.03 0.41 -1 0 -9 0.14 0.61 -1 0 -9 0.49 0.65 -1 0 -9 0.53 0.52 -1 0 -9 0.80 1.18 -1 0 -9 0.12 0.53 -1 0 -9 0.23 0.43 -1 0 -10 63.15 2.27 -1 0 -10 65.26 2.29 -1 0 -10 62.42 2.14 -1 0 -10 59.86 2.60 -1 0 -10 60.66 2.29 -1 0 -11 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-5 3 0.17 0.34 -9 -5 3 0.32 0.36 -9 -5 2 149.05 4.33 -9 -5 2 151.97 4.25 9 -5 -2 146.51 4.54 -9 -5 1 26.46 1.16 -9 -5 1 25.64 1.08 9 -5 -1 26.42 1.36 -9 -5 0 9.54 0.66 -9 -5 -1 21.16 0.98 -9 -5 -1 19.99 0.94 9 -5 1 22.50 1.20 -9 -5 -2 93.97 2.81 9 -5 2 95.32 3.06 -9 -5 -3 2.93 0.40 9 -5 3 3.14 0.52 -9 -5 -4 6.25 0.44 9 -5 4 5.63 0.48 -9 -6 2 14.41 0.58 -9 -6 2 13.17 0.54 -9 -6 1 97.25 2.70 -9 -6 0 0.69 0.20 -9 -6 0 1.09 0.23 9 -6 0 1.20 0.33 10 0 -9 -0.40 0.41 10 0 -8 1.76 0.67 10 0 -7 -0.64 0.79 10 0 -7 -0.29 0.39 10 0 -6 23.07 1.12 10 0 -6 22.09 1.60 10 0 -5 -0.96 1.05 10 0 -5 0.08 0.51 10 0 -4 242.05 6.92 10 0 -3 0.61 0.57 10 0 -2 2.72 0.65 -10 0 1 0.03 0.63 -10 0 1 0.18 0.53 10 0 -1 0.22 0.56 -10 0 0 144.27 4.27 10 0 0 146.75 4.37 -10 0 0 132.33 4.19 -10 0 -1 0.48 0.63 -10 0 -1 0.37 0.57 10 0 1 -0.06 0.53 -10 0 -2 108.25 3.32 -10 0 -2 97.56 3.22 -10 0 -3 -0.21 0.61 -10 0 -3 -0.29 0.52 -10 0 -4 43.66 1.65 -10 0 -4 38.92 1.55 -10 0 -4 41.70 1.70 -10 0 -5 0.75 0.52 -10 0 -5 0.30 0.43 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-1 -3 23.50 1.21 -10 1 -4 8.40 0.75 -10 -1 -4 9.45 0.77 -10 1 -4 7.21 0.58 -10 -1 -4 8.66 0.75 -10 -1 -4 7.44 0.75 -10 1 -4 7.76 0.74 -10 -1 -5 39.53 1.44 -10 1 -5 34.10 1.27 -10 -1 -5 37.56 1.45 -10 -1 -5 37.76 1.48 -10 1 -5 37.60 1.47 -10 1 -6 1.38 0.41 -10 -1 -6 2.09 0.44 -10 -1 -6 1.70 0.41 -10 -1 -6 1.49 0.39 -10 1 -6 1.38 0.39 -10 1 -7 42.27 1.30 -10 -1 -7 42.92 1.31 -10 -1 -7 39.49 1.30 -10 1 -7 38.95 1.30 -10 -1 -7 41.82 1.31 10 -1 7 42.01 1.40 10 -2 -7 29.86 1.31 10 -2 -6 0.12 0.73 10 2 -6 0.64 0.36 10 -2 -5 86.27 2.70 10 2 -5 86.42 2.68 10 2 -5 83.58 3.01 10 -2 -5 87.81 3.11 10 2 -4 9.33 1.13 10 -2 -4 8.56 1.20 10 -2 -4 10.49 0.75 10 2 -4 10.52 0.74 10 -2 -3 20.59 1.07 10 2 -3 21.29 1.07 -10 2 2 6.75 0.68 -10 -2 2 7.03 0.70 10 -2 -2 5.79 0.66 10 2 -2 6.67 0.68 -10 2 1 190.33 5.31 -10 -2 1 184.74 5.32 10 -2 -1 189.94 5.44 10 2 -1 192.98 5.42 10 -2 -1 175.08 5.60 -10 2 0 0.56 0.53 -10 -2 0 0.97 0.56 10 -2 0 0.67 0.46 10 2 0 0.85 0.48 10 -2 0 1.43 0.66 -10 2 -1 81.80 2.63 -10 -2 -1 83.41 2.66 10 -2 1 82.42 2.69 10 2 1 78.82 2.65 10 -2 1 86.62 3.00 -10 2 -2 22.52 1.09 -10 -2 -2 24.21 1.13 10 -2 2 23.00 1.10 10 2 2 22.03 1.08 -10 -2 -2 23.57 1.23 10 -2 2 26.39 1.40 -10 2 -3 207.90 5.69 -10 -2 -3 219.16 5.74 10 -2 3 192.26 5.68 10 2 3 208.47 5.71 -10 -2 -3 209.65 5.84 -10 -2 -3 195.63 5.77 -10 2 -3 194.00 5.74 -10 2 -4 7.98 0.61 -10 -2 -4 7.60 0.63 -10 -2 -4 7.69 0.71 -10 -2 -4 6.58 0.60 -10 2 -4 5.78 0.61 10 -2 4 7.91 0.79 -10 2 -5 8.44 0.56 -10 2 -5 7.88 0.56 -10 -2 -5 8.51 0.65 -10 2 -6 8.60 0.46 -10 -2 -6 9.90 0.60 10 -2 6 10.80 0.65 -10 -2 -7 107.72 2.96 -10 -3 4 46.07 1.45 10 -3 -4 41.76 1.72 -10 -3 3 132.98 3.90 -10 -3 3 123.95 3.65 -10 -3 2 0.52 0.46 -10 3 2 0.48 0.37 -10 -3 2 0.54 0.37 -10 -3 2 0.55 0.49 -10 -3 1 0.12 0.43 -10 3 1 0.06 0.38 -10 -3 1 0.05 0.38 -10 -3 1 0.36 0.50 10 -3 -1 0.43 0.59 -10 -3 0 32.52 1.44 -10 3 0 26.85 1.08 -10 -3 0 27.32 1.14 -10 -3 0 32.29 1.33 10 -3 0 30.58 1.52 -10 -3 -1 90.70 2.61 10 -3 1 87.14 2.85 -10 -3 -2 0.83 0.37 -10 -3 -2 1.28 0.51 -10 3 -2 0.97 0.36 -10 -3 -3 47.53 1.54 10 -3 3 50.68 1.79 -10 -3 -4 3.50 0.37 -10 -3 -4 3.46 0.48 10 -3 4 3.95 0.59 -10 -3 -5 2.31 0.39 10 -3 5 3.05 0.47 -10 -3 -6 88.46 2.46 -10 -4 4 8.05 0.46 -10 -4 3 48.28 1.65 -10 -4 3 47.33 1.52 -10 -4 2 28.49 1.18 -10 -4 2 27.68 1.05 -10 -4 1 19.97 0.97 -10 -4 1 17.72 0.82 10 -4 -1 19.90 1.11 -10 -4 0 71.35 2.24 10 -4 0 80.20 2.62 -10 -4 -1 12.31 0.66 -10 -4 -2 4.19 0.42 10 -4 2 6.47 0.68 -10 -4 -3 2.50 0.33 10 -4 3 3.28 0.53 10 -4 4 100.83 2.97 -10 -5 1 43.48 1.33 10 -5 -1 44.71 1.52 -10 -5 0 1.66 0.25 10 -5 0 1.72 0.39 -11 0 6 13.77 0.62 11 0 -6 15.43 1.00 11 0 -5 -0.31 0.77 -11 0 5 -0.04 0.33 11 0 -5 -0.02 0.35 11 0 -4 1.53 0.94 -11 0 4 1.49 0.41 11 0 -4 0.96 0.43 -11 0 3 -0.22 0.47 -11 0 3 0.12 0.39 11 0 -3 -0.60 0.44 -11 0 2 2.12 0.55 -11 0 2 1.73 0.45 11 0 -2 1.63 0.47 -11 0 1 0.79 0.53 -11 0 1 0.49 0.45 11 0 -1 -0.15 0.44 -11 0 0 423.29 10.98 11 0 0 410.51 11.03 -11 0 0 394.16 10.92 -11 0 -1 -0.47 0.52 -11 0 -1 -0.04 0.44 11 0 1 -0.25 0.42 -11 0 -2 3.64 0.58 -11 0 -2 2.82 0.48 11 0 2 3.40 0.49 -11 0 -3 0.17 0.44 -11 0 -3 -0.01 0.36 -11 0 -3 0.29 0.45 11 0 3 0.02 0.35 -11 0 -4 210.90 5.33 11 0 4 189.15 5.32 -11 0 -4 180.66 5.22 -11 0 -4 199.15 5.35 -11 0 -5 -0.10 0.30 -11 0 -5 0.02 0.28 -11 -1 7 90.09 2.38 -11 -1 7 93.20 2.39 11 1 -7 73.08 2.48 11 -1 -7 79.94 2.52 11 1 -6 169.80 5.10 11 -1 -6 192.90 5.18 11 1 -5 4.18 0.77 11 -1 -5 4.83 0.80 11 1 -5 4.13 0.44 11 -1 -5 4.60 0.46 -11 -1 5 4.33 0.46 -11 1 4 44.91 1.49 11 -1 -4 41.42 1.52 11 1 -4 41.97 1.52 -11 -1 4 42.32 1.48 11 1 -4 40.26 1.89 11 -1 -4 41.81 1.94 -11 1 3 21.20 0.94 -11 -1 3 20.28 0.95 11 -1 -3 19.89 0.98 11 1 -3 21.17 0.98 -11 -1 3 19.96 0.94 -11 1 2 2.64 0.52 -11 -1 2 2.08 0.51 -11 1 2 1.02 0.37 -11 -1 2 2.17 0.50 11 -1 -2 2.21 0.47 11 1 -2 2.40 0.46 -11 1 1 1.38 0.51 -11 -1 1 2.30 0.53 -11 1 1 1.90 0.40 -11 -1 1 1.49 0.52 11 -1 -1 2.08 0.48 11 1 -1 1.48 0.45 -11 1 0 8.92 0.70 -11 -1 0 8.79 0.71 11 -1 0 8.49 0.66 11 1 0 9.56 0.68 -11 1 0 6.46 0.52 -11 -1 0 8.10 0.70 -11 1 -1 7.37 0.65 -11 -1 -1 7.08 0.66 11 -1 1 6.32 0.59 11 1 1 5.97 0.57 -11 1 -1 5.34 0.47 -11 -1 -1 8.37 0.67 11 -1 1 8.15 0.72 -11 1 -2 3.73 0.54 -11 -1 -2 3.81 0.55 -11 -1 -2 3.14 0.52 11 -1 2 3.39 0.46 11 1 2 2.41 0.44 11 -1 2 3.41 0.58 -11 1 -3 45.99 1.49 -11 -1 -3 44.00 1.50 11 -1 3 37.81 1.45 11 1 3 40.36 1.46 -11 -1 -3 42.53 1.49 -11 -1 -3 40.66 1.51 -11 1 -3 41.54 1.51 11 -1 3 48.33 1.68 -11 1 -4 19.60 0.81 -11 -1 -4 19.09 0.82 -11 -1 -4 19.71 0.83 -11 -1 -4 17.65 0.82 -11 1 -4 19.18 0.84 -11 1 -5 8.93 0.47 -11 -1 -5 9.69 0.49 -11 -1 -5 6.92 0.44 -11 1 -5 7.60 0.46 -11 -1 -5 8.87 0.47 11 -1 5 10.50 0.60 -11 -2 6 17.18 0.68 -11 2 5 0.12 0.27 -11 -2 5 0.43 0.32 11 -2 -5 0.25 0.49 11 -2 -4 2.23 0.65 -11 2 4 2.31 0.37 -11 -2 4 2.55 0.43 -11 2 3 55.75 1.76 -11 -2 3 59.31 1.87 11 -2 -3 55.14 2.14 -11 2 2 3.64 0.45 -11 -2 2 3.02 0.46 -11 -2 2 3.07 0.53 11 2 -2 2.85 0.41 -11 2 1 5.12 0.50 -11 -2 1 5.00 0.53 11 2 -1 5.20 0.50 -11 -2 1 5.10 0.59 -11 2 0 10.97 0.66 -11 -2 0 10.84 0.69 11 2 0 10.40 0.65 -11 -2 0 11.60 0.77 -11 2 -1 253.29 6.78 -11 -2 -1 262.54 6.91 11 -2 1 261.77 7.07 -11 2 -2 39.41 1.33 -11 -2 -2 42.79 1.45 11 -2 2 44.49 1.61 -11 2 -3 0.97 0.31 -11 -2 -3 1.24 0.40 -11 2 -3 1.06 0.31 11 -2 3 1.18 0.46 -11 -2 -4 1.17 0.32 -11 2 -4 0.32 0.22 -11 -2 -5 80.00 2.25 11 -2 5 81.25 2.34 -11 -3 5 0.30 0.22 -11 -3 4 5.00 0.39 -11 -3 3 1.09 0.35 -11 -3 2 67.36 2.07 -11 -3 1 -0.16 0.35 -11 -3 0 3.16 0.43 -11 -3 -1 28.74 1.11 11 -3 1 33.02 1.28 -11 -3 -2 12.77 0.64 11 -3 2 14.29 0.79 -11 -3 -3 18.34 0.71 -12 0 4 33.46 1.07 -12 0 3 0.43 0.29 -12 0 2 0.41 0.32 -12 0 2 0.03 0.23 -12 0 1 -0.01 0.33 -12 0 1 0.10 0.25 -12 0 0 27.15 0.90 -12 0 0 18.81 0.74 -12 0 -1 -0.03 0.30 -12 0 -1 0.19 0.29 -12 0 -2 24.51 0.82 -12 0 -2 19.45 0.81 -12 -1 4 14.73 0.53 12 -1 -4 12.19 0.68 -12 1 3 17.49 0.65 -12 -1 3 17.26 0.66 -12 -1 3 16.25 0.65 12 1 -3 13.57 0.83 12 -1 -3 14.87 0.88 -12 1 2 39.85 1.24 -12 -1 2 41.52 1.26 -12 -1 2 39.56 1.25 12 1 -2 32.26 1.44 12 -1 -2 34.53 1.48 -12 1 1 39.79 1.24 -12 -1 1 37.95 1.25 -12 -1 1 37.39 1.25 -12 1 0 12.32 0.60 -12 -1 0 12.92 0.61 -12 -1 0 12.16 0.58 -12 1 -1 2.75 0.33 -12 -1 -1 2.42 0.33 -12 -1 -1 2.55 0.31 -12 -1 -1 2.09 0.31 -12 1 -1 2.17 0.31 -12 1 -2 47.84 1.33 -12 -1 -2 50.79 1.35 -12 -1 -2 45.61 1.33 -12 -1 -2 39.25 1.33 -12 1 -2 39.24 1.33 -12 -2 2 18.99 0.70 -12 -2 1 55.90 1.65 -12 -2 0 8.04 0.43 -12 -2 -1 0.75 0.22 0 0 0 0.00 0.00 TITL 22ZDA17R in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 9.841950 6.914462 11.180704 90.0000 93.6182 90.0000 ZERR 5.00 0.000207 0.000164 0.000224 0.0000 0.0018 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N Cl UNIT 30.00 30.00 10.00 5.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87333 _shelx_res_file ; TITL FT_K in P2(1)/c CELL 1.54184 9.8420 6.9145 11.1807 90.000 93.618 90.000 ZERR 4.00 0.0002 0.0002 0.0002 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H Cl N O UNIT 24 36 4 8 4 TEMP -173.0 SIZE 0.20 0.12 0.06 L.S. 12 BOND $H ACTA CONF EQIV $1 -X,2-Y,1-Z HTAB N1 O1_$1 EQIV $2 +X,1.5-Y,-0.5+Z HTAB N2 O1_$2 WGHT 0.050100 0.606000 FVAR 0.83624 CL1 3 0.453244 0.618476 0.864965 11.00000 0.04005 0.03661 = 0.02491 -0.00157 -0.01242 0.00431 O1 5 0.067050 0.891614 0.644452 11.00000 0.03740 0.02089 = 0.01095 -0.00101 0.00065 0.00824 N1 4 0.057768 0.790518 0.446440 11.00000 0.02965 0.01804 = 0.01136 -0.00059 0.00081 0.00454 H1 2 0.013492 0.889625 0.413351 11.00000 0.03989 N2 4 0.111293 0.643670 0.382169 11.00000 0.02776 0.01943 = 0.01145 -0.00277 0.00130 0.00264 H2 2 0.095880 0.635812 0.299963 11.00000 0.03765 C3 1 0.186874 0.530207 0.457648 11.00000 0.02374 0.01791 = 0.01531 0.00082 0.00270 -0.00108 C4 1 0.183619 0.603544 0.572449 11.00000 0.02385 0.01771 = 0.01281 0.00172 0.00238 0.00080 C5 1 0.101543 0.771657 0.563111 11.00000 0.02726 0.01826 = 0.01098 0.00029 0.00228 -0.00020 C6 1 0.255988 0.355339 0.413074 11.00000 0.03332 0.02327 = 0.01983 -0.00365 0.00329 0.00573 H6A 2 0.281693 0.372394 0.331475 11.00000 0.05821 H6B 2 0.338105 0.328481 0.458440 11.00000 0.06503 H6C 2 0.205079 0.250040 0.413935 11.00000 0.06603 C7 1 0.257210 0.534154 0.685587 11.00000 0.02802 0.01919 = 0.01439 0.00156 0.00150 0.00364 H7A 2 0.193889 0.526593 0.750820 11.00000 0.02147 H7B 2 0.294845 0.406196 0.675877 11.00000 0.02900 C8 1 0.372598 0.672392 0.719414 11.00000 0.02644 0.03146 = 0.01801 0.00288 -0.00186 0.00063 H8A 2 0.339929 0.806824 0.724413 11.00000 0.03133 H8B 2 0.442663 0.665134 0.664310 11.00000 0.03675 HKLF 4 REM FT_K in P2(1)/c REM R1 = 0.0356 for 1467 Fo > 4sig(Fo) and 0.0366 for all 1532 data REM 127 parameters refined using 0 restraints END WGHT 0.0501 0.4623 REM Highest difference peak 0.284, deepest hole -0.410, 1-sigma level 0.058 Q1 1 0.2202 0.5696 0.6244 11.00000 0.05 0.28 Q2 1 0.4539 0.4431 0.8753 11.00000 0.05 0.28 Q3 1 0.1980 0.5653 0.5215 11.00000 0.05 0.27 Q4 1 0.1243 0.6566 0.5801 11.00000 0.05 0.25 Q5 1 0.3015 0.6038 0.7133 11.00000 0.05 0.25 Q6 1 0.5842 0.6219 0.9059 11.00000 0.05 0.18 Q7 1 0.2265 0.4535 0.4371 11.00000 0.05 0.18 Q8 1 0.2151 0.3122 0.3505 11.00000 0.05 0.18 Q9 1 -0.0715 0.8858 0.6169 11.00000 0.05 0.17 Q10 1 0.2929 0.2651 0.4947 11.00000 0.05 0.17 Q11 1 0.1487 0.5684 0.4184 11.00000 0.05 0.17 Q12 1 -0.0859 0.9260 0.3432 11.00000 0.05 0.17 Q13 1 0.5637 0.6683 0.8336 11.00000 0.05 0.16 Q14 1 0.3833 0.1085 0.5004 11.00000 0.05 0.16 Q15 1 0.5112 0.6919 0.7608 11.00000 0.05 0.16 Q16 1 0.4139 0.6401 0.7840 11.00000 0.05 0.16 Q17 1 0.5335 0.5938 0.6005 11.00000 0.05 0.16 Q18 1 0.0361 0.9749 0.6215 11.00000 0.05 0.15 Q19 1 0.1112 0.0990 0.4053 11.00000 0.05 0.15 Q20 1 0.3400 0.1861 0.5628 11.00000 0.05 0.15 ; _shelx_res_checksum 4990 _shelxl_version_number .2013 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 0.45324(5) 0.61848(7) 0.86496(4) 0.03447(18) Uani d 1 . . O O1 0.06705(13) 0.89161(17) 0.64445(10) 0.0231(3) Uani d 1 . . N N1 0.05777(14) 0.7905(2) 0.44644(12) 0.0197(3) Uani d 1 . . H H1 0.013(3) 0.890(4) 0.413(2) 0.040(7) Uiso d 1 . . N N2 0.11129(14) 0.6437(2) 0.38217(12) 0.0195(3) Uani d 1 . . H H2 0.096(2) 0.636(3) 0.300(2) 0.038(6) Uiso d 1 . . C C3 0.18687(16) 0.5302(2) 0.45765(14) 0.0189(3) Uani d 1 . . C C4 0.18362(16) 0.6035(2) 0.57245(14) 0.0181(3) Uani d 1 . . C C5 0.10154(16) 0.7717(2) 0.56311(13) 0.0188(3) Uani d 1 . . C C6 0.2560(2) 0.3553(3) 0.41307(16) 0.0254(4) Uani d 1 . . H H6A 0.282(3) 0.372(4) 0.331(3) 0.058(8) Uiso d 1 . . H H6B 0.338(3) 0.328(5) 0.458(3) 0.065(9) Uiso d 1 . . H H6C 0.205(3) 0.250(5) 0.414(3) 0.066(9) Uiso d 1 . . C C7 0.25721(17) 0.5342(2) 0.68559(14) 0.0205(3) Uani d 1 . . H H7A 0.194(2) 0.527(3) 0.7508(18) 0.021(5) Uiso d 1 . . H H7B 0.295(2) 0.406(3) 0.676(2) 0.029(5) Uiso d 1 . . C C8 0.37260(18) 0.6724(3) 0.71941(16) 0.0254(4) Uani d 1 . . H H8A 0.340(2) 0.807(4) 0.724(2) 0.031(6) Uiso d 1 . . H H8B 0.443(2) 0.665(4) 0.664(2) 0.037(6) Uiso d 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 0.0401(3) 0.0366(3) 0.0249(3) 0.00431(18) -0.01242(19) -0.00157(17) O1 0.0374(7) 0.0209(6) 0.0110(5) 0.0082(5) 0.0007(5) -0.0010(4) N1 0.0297(7) 0.0180(7) 0.0114(6) 0.0045(5) 0.0008(5) -0.0006(5) N2 0.0278(7) 0.0194(7) 0.0115(7) 0.0026(5) 0.0013(5) -0.0028(5) C3 0.0237(7) 0.0179(7) 0.0153(7) -0.0011(6) 0.0027(6) 0.0008(6) C4 0.0238(7) 0.0177(7) 0.0128(7) 0.0008(6) 0.0024(6) 0.0017(6) C5 0.0273(8) 0.0183(7) 0.0110(7) -0.0002(6) 0.0023(6) 0.0003(6) C6 0.0333(9) 0.0233(8) 0.0198(9) 0.0057(7) 0.0033(7) -0.0036(7) C7 0.0280(8) 0.0192(8) 0.0144(8) 0.0036(6) 0.0015(6) 0.0016(6) C8 0.0264(8) 0.0315(9) 0.0180(8) 0.0006(7) -0.0019(6) 0.0029(7) 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' 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_ _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 C5 N1 N2 . . 108.95(13) ? C5 N1 H1 . . 126.8(17) ? N2 N1 H1 . . 123.6(17) ? C3 N2 N1 . . 108.66(13) ? C3 N2 H2 . . 129.9(15) ? N1 N2 H2 . . 121.4(15) ? N2 C3 C4 . . 108.96(14) ? N2 C3 C6 . . 120.74(15) ? C4 C3 C6 . . 130.29(15) ? C3 C4 C5 . . 106.22(14) ? C3 C4 C7 . . 128.97(15) ? C5 C4 C7 . . 124.69(14) ? O1 C5 N1 . . 122.31(15) ? O1 C5 C4 . . 130.49(14) ? N1 C5 C4 . . 107.19(13) ? C3 C6 H6A . . 111.6(17) ? C3 C6 H6B . . 111.9(19) ? H6A C6 H6B . . 105(2) ? C3 C6 H6C . . 113(2) ? H6A C6 H6C . . 107(3) ? H6B C6 H6C . . 107(3) ? C4 C7 C8 . . 108.91(14) ? C4 C7 H7A . . 110.2(12) ? C8 C7 H7A . . 110.3(12) ? C4 C7 H7B . . 111.5(13) ? C8 C7 H7B . . 108.6(13) ? H7A C7 H7B . . 107.3(18) ? C7 C8 Cl1 . . 112.04(12) ? C7 C8 H8A . . 111.5(13) ? Cl1 C8 H8A . . 105.7(13) ? C7 C8 H8B . . 111.5(15) ? Cl1 C8 H8B . . 106.1(15) ? H8A C8 H8B . . 109.7(19) ? 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 C8 . 1.8040(18) ? O1 C5 . 1.2920(19) ? N1 C5 . 1.354(2) ? N1 N2 . 1.3685(19) ? N1 H1 . 0.88(3) ? N2 C3 . 1.342(2) ? N2 H2 . 0.92(3) ? C3 C4 . 1.382(2) ? C3 C6 . 1.489(2) ? C4 C5 . 1.416(2) ? C4 C7 . 1.496(2) ? C6 H6A . 0.97(3) ? C6 H6B . 0.95(3) ? C6 H6C . 0.88(3) ? C7 C8 . 1.514(2) ? C7 H7A . 0.99(2) ? C7 H7B . 0.97(2) ? C8 H8A . 0.99(2) ? C8 H8B . 0.95(2) ? 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 N1 H1 O1 3_576 0.88(3) 1.81(3) 2.6861(18) 174(2) N2 H2 O1 4_575 0.92(3) 1.75(3) 2.6772(17) 177(2) 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 C5 N1 N2 C3 . . . . 0.98(18) ? N1 N2 C3 C4 . . . . -0.30(18) ? N1 N2 C3 C6 . . . . 178.79(15) ? N2 C3 C4 C5 . . . . -0.45(18) ? C6 C3 C4 C5 . . . . -179.43(17) ? N2 C3 C4 C7 . . . . -176.56(16) ? C6 C3 C4 C7 . . . . 4.5(3) ? N2 N1 C5 O1 . . . . 179.70(15) ? N2 N1 C5 C4 . . . . -1.24(18) ? C3 C4 C5 O1 . . . . 179.99(17) ? C7 C4 C5 O1 . . . . -3.7(3) ? C3 C4 C5 N1 . . . . 1.04(18) ? C7 C4 C5 N1 . . . . 177.36(15) ? C3 C4 C7 C8 . . . . 105.67(19) ? C5 C4 C7 C8 . . . . -69.8(2) ? C4 C7 C8 Cl1 . . . . 172.38(11) ?