#------------------------------------------------------------------------------ #$Date: 2022-09-13 03:49:45 +0200 (Tue, 13 Sep 2022) $ #$Revision: 277788 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022669.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_2022669 loop_ _publ_author_name 'Vera, Diana Roc\'io' 'Mantilla, Juan P.' 'Palma, Alirio' 'Cobo, Justo' 'Glidewell, Christopher' _publ_section_title ; Synthesis and spectroscopic and structural characterization of three new 2-methyl-4-styrylquinolines formed using Friedl\"ander reactions between (2-aminophenyl)chalcones and acetone ; _journal_coeditor_code KY3221 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229622008634 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C18 H13 Cl2 N' _chemical_formula_moiety 'C18 H13 Cl2 N' _chemical_formula_sum 'C18 H13 Cl2 N' _chemical_formula_weight 314.19 _chemical_name_common ; (E)-4-(2,6-Dichlorostyryl)-2-methylquinoline ; _chemical_name_systematic ; (E)-4-[2-(2,6-dichlorophenyl)ethenyl]-2-methylquinoline ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 110.497(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 30.5651(15) _cell_length_b 3.8629(2) _cell_length_c 25.5357(13) _cell_measurement_reflns_used 3210 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.493 _cell_measurement_theta_min 2.573 _cell_volume 2824.1(3) _computing_cell_refinement ; SAINT (Bruker, 2017) ; _computing_data_collection ; APEX3 (Bruker, 2018) ; _computing_data_reduction ; SAINT (Bruker, 2017) ; _computing_molecular_graphics ; PLATON (Spek, 2020) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015b) and PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_unetI/netI 0.0211 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 28110 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.493 _diffrn_reflns_theta_min 2.573 _diffrn_source 'INCOATEC high brilliance microfocus sealed tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.451 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2016) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.478 _exptl_crystal_description needle _exptl_crystal_F_000 1296 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.097 _exptl_crystal_size_min 0.061 _refine_diff_density_max 0.331 _refine_diff_density_min -0.264 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 191 _refine_ls_number_reflns 3208 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0311 _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^)+(0.0342P)^2^+4.0386P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.0786 _reflns_number_gt 2930 _reflns_number_total 3208 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ky3221sup1.cif _cod_data_source_block III _cod_original_cell_volume 2824.1(2) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2022669 _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 0.915 _shelx_estimated_absorpt_t_max 0.973 _shelx_hkl_file ; 4 0 0 1419.86 59.79 4 0 0 1392.26 169.38 -4 0 0 1147.39 153.98 -4 0 0 1441.86 59.69 -6 0 0 92.39 3.90 -6 0 0 89.89 3.60 6 0 0 90.09 3.40 6 0 0 90.89 3.70 6 0 0 93.19 3.90 8 0 0 127.99 4.60 8 0 0 124.59 5.00 8 0 0 128.69 5.30 -8 0 0 118.59 5.10 -8 0 0 127.29 5.00 -10 0 0 94.29 4.70 10 0 0 102.69 5.00 10 0 0 99.19 4.50 -10 0 0 102.49 4.60 10 0 0 97.69 4.10 12 0 0 3648.73 101.59 -14 0 0 131.99 6.20 14 0 0 115.19 5.60 14 0 0 116.19 5.10 14 0 0 119.19 6.10 -14 0 0 119.39 5.60 16 0 0 55.29 3.90 -16 0 0 53.69 4.10 -16 0 0 52.09 3.80 16 0 0 55.69 3.30 16 0 0 50.29 4.10 -18 0 0 510.25 17.50 18 0 0 511.35 17.50 18 0 0 498.55 18.10 18 0 0 506.65 16.60 -18 0 0 554.24 18.30 -20 0 0 -0.10 1.20 -20 0 0 -1.30 1.30 20 0 0 0.80 1.90 20 0 0 0.20 1.20 20 0 0 1.60 1.10 22 0 0 160.98 7.30 22 0 0 165.78 8.90 -22 0 0 165.68 8.10 22 0 0 164.08 8.20 -22 0 0 163.98 8.60 -24 0 0 59.59 4.80 24 0 0 57.49 4.10 24 0 0 51.79 4.60 24 0 0 59.39 5.50 26 0 0 -1.90 3.30 -26 0 0 4.30 2.30 -26 0 0 0.50 1.40 26 0 0 1.80 1.60 26 0 0 0.90 1.60 -28 0 0 546.55 20.80 28 0 0 520.05 18.60 28 0 0 546.65 21.50 28 0 0 532.15 20.30 30 0 0 74.79 9.40 -30 0 0 70.39 6.40 30 0 0 67.49 5.90 -30 0 0 56.39 5.20 30 0 0 66.99 4.90 -32 0 0 4.10 2.50 32 0 0 4.30 3.10 -32 0 0 4.40 2.60 32 0 0 2.50 2.50 34 0 0 407.76 16.20 -34 0 0 367.46 16.50 34 0 0 387.86 17.00 -34 0 0 365.46 17.10 -36 0 0 37.70 5.60 -36 0 0 50.49 6.80 36 0 0 42.00 6.60 1 -1 0 364.06 11.10 1 -1 0 367.76 11.30 -1 -1 0 345.37 10.70 -1 -1 0 355.96 10.20 -1 -1 0 344.77 11.00 1 -1 0 341.97 10.80 -1 1 0 380.76 11.00 1 1 0 348.27 11.30 1 1 0 364.96 10.80 1 1 0 367.86 11.10 -1 1 0 367.36 11.30 -3 -1 0 -0.20 0.60 -3 -1 0 -0.50 0.90 3 -1 0 0.40 0.90 3 -1 0 -0.20 1.00 -3 -1 0 0.00 0.70 -3 -1 0 0.50 0.90 -3 -1 0 0.10 0.70 3 1 0 0.10 0.60 3 1 0 1.60 1.10 3 1 0 0.00 0.60 3 1 0 0.60 0.70 -3 1 0 0.60 1.10 3 1 0 0.20 0.60 -5 -1 0 66.29 3.10 -5 -1 0 68.69 3.40 5 -1 0 63.99 2.40 5 -1 0 67.19 2.50 5 -1 0 72.19 3.70 5 1 0 68.79 2.60 5 1 0 67.09 2.90 5 1 0 64.79 3.40 5 1 0 69.29 3.10 -5 1 0 60.49 3.60 5 1 0 65.49 2.90 7 -1 0 336.87 10.50 7 -1 0 357.86 11.70 -7 -1 0 331.87 10.50 -7 -1 0 336.17 11.30 -7 -1 0 345.37 11.00 7 -1 0 337.97 10.40 7 1 0 336.97 11.30 -7 1 0 345.57 11.70 7 1 0 355.16 10.90 7 1 0 336.37 10.50 7 1 0 337.27 11.10 7 1 0 338.47 9.80 -9 -1 0 0.60 1.10 9 -1 0 -0.30 1.10 -9 -1 0 -0.60 1.30 9 -1 0 0.00 1.00 9 1 0 0.10 0.30 9 1 0 0.20 1.10 9 1 0 0.80 1.00 -9 1 0 0.60 1.30 -9 1 0 -0.60 0.60 9 1 0 -0.50 0.80 9 1 0 0.00 0.60 -9 1 0 1.50 0.70 11 -1 0 42.80 3.30 -11 -1 0 38.90 3.30 11 -1 0 50.69 3.20 -11 -1 0 42.10 3.10 11 -1 0 39.00 2.70 11 1 0 40.90 2.60 11 1 0 39.80 3.20 -11 1 0 39.60 2.30 -11 1 0 39.80 2.50 11 1 0 39.70 3.00 11 1 0 45.50 3.00 13 -1 0 22.90 2.90 13 -1 0 18.30 3.60 -13 -1 0 16.70 2.70 13 -1 0 12.90 2.00 -13 -1 0 17.70 2.50 -13 1 0 20.40 2.00 13 1 0 15.70 2.30 13 1 0 16.00 2.60 13 1 0 13.60 1.90 13 1 0 16.70 1.10 -13 1 0 12.60 1.70 -15 -1 0 83.39 4.90 15 -1 0 77.99 4.50 -15 -1 0 82.19 5.30 15 -1 0 82.99 5.00 15 -1 0 82.79 5.00 15 1 0 76.89 4.60 -15 1 0 85.19 4.20 15 1 0 84.99 4.20 15 1 0 90.79 5.30 15 1 0 82.59 3.10 -15 1 0 80.29 4.30 -17 -1 0 78.29 4.90 17 -1 0 75.59 5.10 17 -1 0 71.89 4.60 -17 -1 0 73.99 5.30 17 -1 0 71.59 4.80 17 1 0 81.29 3.20 -17 1 0 76.19 4.20 -17 1 0 70.59 4.30 17 1 0 77.59 4.30 17 1 0 73.89 5.10 17 1 0 89.79 5.00 19 -1 0 0.50 1.50 -19 -1 0 -0.60 1.30 19 -1 0 0.00 1.10 19 -1 0 0.50 1.30 -19 -1 0 0.30 1.60 -19 1 0 -1.50 1.00 -19 1 0 0.20 1.20 19 1 0 -0.50 0.90 19 1 0 0.50 0.60 19 1 0 0.50 1.10 19 1 0 -0.20 1.50 -21 -1 0 4.30 2.00 21 -1 0 7.50 2.00 -21 -1 0 3.20 2.60 21 -1 0 5.10 2.20 21 -1 0 4.40 1.90 21 1 0 6.10 1.60 -21 1 0 6.10 1.80 21 1 0 2.40 2.40 21 1 0 5.40 1.10 21 1 0 1.60 1.60 -21 1 0 2.70 1.70 -23 -1 0 1.60 2.10 23 -1 0 -0.10 1.50 23 -1 0 3.20 2.10 -23 -1 0 -0.50 1.50 23 -1 0 1.20 1.60 23 1 0 4.60 2.30 23 1 0 1.50 1.30 23 1 0 2.90 1.00 -23 1 0 4.20 1.60 -23 1 0 0.10 1.50 23 1 0 -0.40 1.50 25 -1 0 13.50 3.40 -25 -1 0 15.50 3.80 25 -1 0 15.10 3.10 -25 1 0 14.60 2.70 25 1 0 15.50 1.90 25 1 0 16.60 3.10 25 1 0 15.50 2.60 25 1 0 8.20 3.00 -25 1 0 15.60 3.00 -27 -1 0 15.50 3.40 -27 -1 0 18.40 4.10 27 -1 0 9.80 3.30 27 -1 0 13.30 3.10 27 1 0 7.90 1.50 -27 1 0 13.40 3.10 27 1 0 6.60 2.60 27 1 0 14.50 2.70 27 1 0 11.20 3.30 -27 1 0 11.40 2.60 29 -1 0 6.50 2.30 -29 -1 0 3.80 4.10 -29 -1 0 14.20 3.80 29 -1 0 5.70 2.90 29 1 0 4.20 1.10 29 1 0 1.90 2.80 29 1 0 5.80 2.40 -29 1 0 3.30 1.90 29 1 0 3.30 1.70 -29 1 0 6.70 2.50 29 1 0 7.50 2.40 -31 -1 0 52.19 6.90 -31 -1 0 56.19 5.60 31 -1 0 41.10 5.30 31 -1 0 53.49 6.50 31 1 0 45.80 5.60 -31 1 0 52.59 5.00 31 1 0 40.90 2.90 31 1 0 35.70 4.30 31 1 0 36.40 5.60 31 1 0 44.30 5.30 -31 1 0 50.39 4.60 -33 -1 0 35.50 5.40 -33 -1 0 29.40 5.50 33 -1 0 21.10 4.20 33 -1 0 27.60 5.00 33 1 0 16.00 4.00 33 1 0 23.90 4.00 33 1 0 27.50 4.00 33 1 0 22.50 4.30 -33 1 0 31.90 4.50 -33 1 0 22.90 3.70 33 1 0 22.00 2.20 35 -1 0 4.00 3.00 35 1 0 5.20 2.10 -35 1 0 -1.40 1.70 -35 1 0 2.90 2.30 35 1 0 1.90 1.30 35 1 0 4.00 2.40 0 -2 0 881.41 25.50 0 -2 0 812.42 24.00 0 -2 0 890.11 26.20 0 -2 0 869.01 26.30 0 -2 0 836.82 23.90 0 2 0 878.51 26.20 0 2 0 849.91 25.40 -2 -2 0 159.18 5.80 -2 -2 0 177.08 7.20 -2 -2 0 166.98 6.40 -2 -2 0 169.68 5.70 2 -2 0 176.38 7.40 2 -2 0 176.98 7.50 -2 -2 0 171.68 6.90 2 -2 0 172.38 7.00 2 2 0 168.18 6.90 -2 2 0 159.18 7.20 2 2 0 159.38 6.40 -4 -2 0 484.05 15.80 -4 -2 0 430.16 14.60 4 -2 0 481.55 15.20 -4 -2 0 474.15 14.30 4 -2 0 464.35 16.00 4 -2 0 457.55 15.20 -4 -2 0 470.35 15.00 -4 -2 0 483.55 14.70 -4 2 0 475.75 16.10 4 2 0 456.15 14.70 4 2 0 466.35 14.90 4 2 0 486.35 15.80 -6 -2 0 98.49 4.30 -6 -2 0 102.99 5.30 -6 -2 0 96.49 4.30 -6 -2 0 87.99 4.50 6 -2 0 86.09 2.90 6 -2 0 90.89 5.40 6 -2 0 97.79 4.80 -6 -2 0 93.69 4.20 6 2 0 93.69 5.10 6 2 0 86.19 4.20 6 2 0 91.69 3.10 6 2 0 97.09 3.10 -6 2 0 101.19 5.60 -8 -2 0 31.80 3.00 8 -2 0 37.80 1.90 8 -2 0 37.80 2.00 8 -2 0 37.90 3.50 -8 -2 0 40.40 2.60 8 -2 0 39.30 3.10 -8 -2 0 43.10 2.90 8 2 0 40.60 2.70 -8 2 0 33.40 3.50 8 2 0 47.50 3.60 8 2 0 41.50 2.40 8 2 0 38.50 2.40 10 -2 0 82.39 5.90 -10 -2 0 81.99 4.50 -10 -2 0 71.09 4.70 10 -2 0 83.19 3.70 -10 -2 0 78.39 3.90 10 -2 0 72.89 3.50 10 2 0 84.69 4.10 10 2 0 81.69 4.10 10 2 0 84.29 5.00 10 2 0 75.79 3.80 10 2 0 84.59 3.40 -12 -2 0 441.06 13.90 12 -2 0 406.76 13.60 -12 -2 0 373.36 14.90 -12 -2 0 448.66 14.80 12 -2 0 419.06 13.40 12 -2 0 404.66 15.60 12 2 0 452.05 14.00 12 2 0 421.76 13.80 12 2 0 420.56 15.20 12 2 0 424.46 14.20 -14 -2 0 12.60 2.70 14 -2 0 10.60 2.00 14 -2 0 8.70 1.70 14 -2 0 9.80 2.50 -14 -2 0 10.90 2.30 14 2 0 7.40 1.50 14 2 0 6.20 1.80 14 2 0 6.30 1.90 14 2 0 11.70 2.00 16 -2 0 597.64 19.30 -16 -2 0 605.04 20.50 -16 -2 0 576.64 21.10 16 -2 0 599.34 19.70 16 2 0 604.84 19.70 16 2 0 602.14 20.20 16 2 0 612.74 21.00 16 2 0 620.44 19.40 -18 -2 0 263.87 12.00 -18 -2 0 254.37 11.20 18 -2 0 272.27 10.90 18 -2 0 270.57 10.40 18 2 0 264.47 10.60 18 2 0 267.47 10.20 18 2 0 258.47 11.40 18 2 0 266.37 11.20 -20 -2 0 46.10 5.80 20 -2 0 43.70 4.30 -20 -2 0 51.29 4.60 20 -2 0 40.80 3.80 20 2 0 48.60 4.00 20 2 0 48.10 4.60 20 2 0 44.40 4.40 20 2 0 45.70 3.60 22 -2 0 77.69 5.70 -22 -2 0 66.89 6.20 22 -2 0 69.49 5.10 22 2 0 72.39 5.10 -22 2 0 69.39 2.60 22 2 0 71.79 5.60 22 2 0 71.09 4.70 22 2 0 65.79 5.60 24 -2 0 185.78 9.60 -24 -2 0 152.28 9.80 -24 -2 0 178.28 9.70 24 -2 0 191.18 9.10 24 2 0 180.38 9.00 24 2 0 184.28 8.40 -24 2 0 171.58 6.20 24 2 0 163.38 9.20 24 2 0 165.48 9.30 26 -2 0 34.30 4.40 -26 -2 0 37.40 5.90 26 -2 0 37.00 5.30 -26 2 0 36.80 2.60 26 2 0 41.80 5.60 26 2 0 41.20 5.20 26 2 0 42.40 5.00 26 2 0 39.20 4.40 -26 2 0 32.90 2.50 -28 -2 0 147.19 10.00 -28 -2 0 151.18 9.50 28 -2 0 149.69 9.50 28 -2 0 164.98 9.10 28 2 0 157.98 8.30 28 2 0 165.58 9.90 28 2 0 155.28 8.90 -28 2 0 164.08 6.60 28 2 0 157.48 9.40 -30 -2 0 132.99 9.00 30 -2 0 139.29 8.60 -30 -2 0 135.59 9.90 30 -2 0 131.59 9.00 30 2 0 137.69 9.00 30 2 0 124.59 9.00 -30 2 0 129.29 6.10 30 2 0 140.59 7.80 30 2 0 139.79 8.50 32 -2 0 -0.70 2.20 32 2 0 3.70 1.80 -32 2 0 5.40 1.60 32 2 0 -0.20 2.00 32 2 0 6.50 2.80 -32 2 0 6.20 1.80 32 2 0 8.20 3.20 34 -2 0 127.49 9.80 -34 -2 0 116.39 8.90 34 -2 0 117.69 8.70 -34 2 0 114.19 5.70 -34 2 0 128.29 6.20 34 2 0 121.59 11.10 34 2 0 116.69 7.60 -1 -3 0 36.10 2.90 -1 -3 0 40.50 3.10 1 -3 0 30.50 3.70 -1 -3 0 36.30 3.40 1 -3 0 36.10 3.00 -1 -3 0 34.80 2.30 1 -3 0 32.00 2.10 1 -3 0 36.40 3.60 -1 -3 0 44.00 3.90 -1 3 0 41.10 3.90 1 3 0 36.10 3.70 3 -3 0 180.58 8.20 3 -3 0 161.98 7.40 -3 -3 0 170.18 6.40 -3 -3 0 177.18 8.00 -3 -3 0 180.18 7.30 -3 -3 0 185.58 8.50 3 -3 0 156.08 8.20 3 -3 0 156.28 5.50 -3 -3 0 166.98 6.80 3 -3 0 154.98 5.30 3 3 0 172.88 7.30 3 3 0 177.68 7.90 -5 -3 0 123.49 5.60 5 -3 0 111.79 3.90 -5 -3 0 119.59 5.30 -5 -3 0 133.49 7.00 5 -3 0 116.99 6.30 5 -3 0 118.49 6.00 5 -3 0 116.49 3.90 -5 -3 0 112.69 5.90 -5 -3 0 103.99 5.50 5 3 0 118.19 5.70 7 -3 0 17.10 1.30 -7 -3 0 19.60 2.60 -7 -3 0 23.00 3.60 7 -3 0 16.50 1.30 -7 -3 0 19.50 2.30 -7 -3 0 17.40 2.40 -7 -3 0 20.10 2.90 7 -3 0 20.50 2.90 7 -3 0 21.20 3.00 7 3 0 14.90 2.20 9 -3 0 3.70 0.90 9 -3 0 3.50 1.70 -9 -3 0 4.40 1.50 -9 -3 0 5.80 1.90 9 -3 0 5.90 1.80 9 -3 0 6.90 1.10 -9 -3 0 3.40 1.20 9 3 0 5.80 1.60 9 3 0 1.80 1.60 11 -3 0 64.59 4.70 -11 -3 0 53.69 4.50 -11 -3 0 58.59 4.30 -11 -3 0 54.39 3.70 11 -3 0 59.99 3.10 11 -3 0 60.99 3.20 11 3 0 57.79 4.90 11 3 0 57.79 3.90 -13 -3 0 6.40 1.60 13 -3 0 5.90 2.00 13 -3 0 4.80 1.30 -13 -3 0 5.40 2.20 -13 -3 0 4.50 1.90 13 -3 0 5.50 1.50 13 3 0 3.80 1.00 13 3 0 8.10 1.80 13 3 0 3.20 1.90 15 -3 0 218.28 10.20 -15 -3 0 231.48 10.10 -15 -3 0 244.38 15.10 15 -3 0 223.88 8.50 -15 -3 0 205.68 8.70 15 -3 0 215.28 8.70 15 3 0 207.28 9.00 15 3 0 227.68 10.90 17 -3 0 22.10 4.30 17 -3 0 27.40 3.10 -17 -3 0 27.50 4.50 17 -3 0 33.40 3.70 -17 -3 0 30.70 4.20 17 3 0 29.30 4.40 17 3 0 29.40 3.50 17 3 0 27.10 2.70 17 3 0 28.10 3.10 19 -3 0 224.38 9.30 19 -3 0 227.38 9.70 -19 -3 0 214.18 11.40 19 -3 0 207.38 10.50 -19 -3 0 222.18 11.00 19 3 0 203.68 11.00 19 3 0 217.68 9.70 19 3 0 217.78 9.00 19 3 0 221.28 9.40 -21 -3 0 4.20 2.30 21 -3 0 0.90 1.40 -21 -3 0 -1.00 2.00 21 -3 0 1.00 1.50 21 3 0 0.60 1.40 21 3 0 1.30 1.70 21 3 0 2.30 1.60 21 3 0 -0.60 1.70 -23 -3 0 94.39 7.60 23 -3 0 114.49 7.10 -23 -3 0 107.99 7.50 23 3 0 98.29 6.30 23 3 0 102.19 6.20 23 3 0 109.39 8.90 23 3 0 99.49 6.50 25 -3 0 78.09 5.90 -25 -3 0 84.69 6.70 25 -3 0 88.19 6.50 25 3 0 71.89 6.60 25 3 0 94.79 6.30 25 3 0 76.59 5.60 25 3 0 81.29 5.80 -27 -3 0 9.80 3.10 -27 -3 0 11.60 3.10 27 -3 0 17.40 3.70 27 3 0 14.10 3.10 27 3 0 14.60 3.00 27 3 0 12.20 3.40 27 3 0 14.80 3.30 29 -3 0 2.00 2.10 -29 -3 0 0.50 2.00 29 -3 0 1.50 2.50 29 3 0 1.30 1.50 29 3 0 0.60 2.20 29 3 0 -0.30 2.30 0 -4 0 14.40 2.30 0 -4 0 17.60 2.60 0 -4 0 15.70 3.40 2 -4 0 2.80 1.60 -2 -4 0 1.80 1.70 2 -4 0 0.50 0.90 -2 -4 0 2.60 1.30 -2 -4 0 3.00 1.50 -2 -4 0 2.20 1.10 2 -4 0 2.70 0.90 4 -4 0 153.88 6.30 -4 -4 0 175.58 7.90 4 -4 0 176.98 9.40 -4 -4 0 158.18 7.50 4 -4 0 180.68 8.50 -4 -4 0 162.08 7.10 -4 -4 0 176.78 9.40 6 -4 0 3.70 1.80 -6 -4 0 3.90 1.50 6 -4 0 3.30 1.80 -6 -4 0 4.20 1.80 6 -4 0 4.40 0.90 -6 -4 0 4.10 1.90 -6 -4 0 2.30 1.30 6 4 0 2.10 1.50 -8 -4 0 16.30 3.00 8 -4 0 21.60 4.00 -8 -4 0 21.30 2.80 8 -4 0 18.90 1.50 -8 -4 0 18.90 2.80 8 -4 0 17.00 3.20 8 4 0 15.70 2.50 -10 -4 0 8.90 1.90 10 -4 0 11.40 1.50 -10 -4 0 6.30 2.50 10 -4 0 7.60 2.10 -10 -4 0 6.80 2.10 10 -4 0 7.80 1.30 10 -4 0 4.80 2.30 10 4 0 8.90 2.30 12 -4 0 307.07 12.70 -12 -4 0 276.67 11.10 -12 -4 0 286.37 12.80 12 -4 0 274.87 9.70 12 -4 0 282.37 12.60 -12 -4 0 292.77 12.10 12 -4 0 280.27 9.90 12 4 0 283.07 11.80 -14 -4 0 41.10 3.50 -14 -4 0 39.10 5.30 14 -4 0 39.00 3.00 14 -4 0 39.00 4.90 14 -4 0 31.00 4.30 14 -4 0 41.70 2.90 14 4 0 37.00 4.10 16 -4 0 112.89 7.30 16 -4 0 103.69 7.10 16 -4 0 99.69 5.30 16 -4 0 97.79 5.10 -16 -4 0 101.99 6.80 -16 -4 0 106.19 5.90 -16 -4 0 102.29 7.60 16 4 0 108.99 6.40 -18 -4 0 12.50 4.40 18 -4 0 3.00 3.60 18 -4 0 7.70 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12 2 -30 41.10 6.10 12 2 -30 34.60 5.60 -12 2 30 31.70 3.70 -12 2 30 39.90 6.60 10 -2 -30 30.30 7.80 -10 -2 30 27.10 5.20 -10 2 30 29.80 6.00 10 2 -30 40.50 5.80 -10 2 30 23.10 3.40 10 2 -30 33.20 5.30 -10 2 30 28.30 3.50 8 -2 -30 11.30 4.50 -8 -2 30 9.60 3.30 -8 2 30 9.30 2.40 -8 2 30 17.10 3.00 8 2 -30 10.30 3.50 -8 2 30 16.70 5.10 8 2 -30 17.70 4.10 26 0 -31 -3.20 2.60 -26 0 31 1.60 2.30 -26 0 31 0.60 1.10 -26 0 31 0.00 2.50 -26 0 31 3.50 2.70 26 0 -31 0.20 2.10 24 0 -31 1.00 1.70 -24 0 31 -2.60 1.00 24 0 -31 -0.40 2.80 -24 0 31 0.70 2.80 -24 0 31 3.00 2.40 -24 0 31 0.10 2.60 22 0 -31 3.10 1.80 22 0 -31 7.90 3.60 -22 0 31 1.10 2.10 -22 0 31 -3.00 2.40 -22 0 31 1.00 1.40 -20 0 31 2.30 2.50 20 0 -31 1.90 3.10 -20 0 31 2.10 2.10 20 0 -31 -0.20 1.60 -18 0 31 3.50 1.40 18 0 -31 2.50 1.90 -18 0 31 2.00 2.50 -18 0 31 -1.00 2.00 16 0 -31 6.00 2.20 -16 0 31 2.20 2.40 -16 0 31 0.90 1.60 16 0 -31 4.80 2.40 16 0 -31 -0.50 2.30 -16 0 31 0.30 1.10 -14 0 31 2.90 2.20 -14 0 31 0.60 1.20 -14 0 31 3.00 2.60 14 0 -31 0.70 1.60 14 0 -31 8.50 2.90 14 0 -31 -2.10 2.20 12 0 -31 -0.70 2.30 12 0 -31 -0.30 2.30 -12 0 31 -1.00 1.10 -12 0 31 4.00 2.60 -12 0 31 0.50 1.80 12 0 -31 1.00 1.50 10 0 -31 0.00 2.30 10 0 -31 3.20 2.80 -10 0 31 3.80 2.60 -10 0 31 1.30 2.00 10 0 -31 1.10 1.60 -8 0 31 2.30 2.30 8 0 -31 4.00 4.60 -8 0 31 2.20 1.60 -8 0 31 -0.90 1.60 -6 0 31 -4.30 1.70 -6 0 31 0.30 1.10 -6 0 31 3.10 2.10 4 0 -31 -2.70 2.00 -4 0 31 0.80 1.60 -4 0 31 2.60 2.50 -2 0 31 2.00 2.40 2 0 -31 1.60 2.30 0 0 -31 3.40 2.80 0 0 31 -0.70 1.40 0 0 31 1.90 2.50 -23 -1 31 145.39 8.60 -23 -1 31 149.79 8.30 23 -1 -31 152.48 8.10 23 -1 -31 169.48 11.20 -23 -1 31 144.49 9.50 23 1 -31 142.39 9.20 -23 1 31 146.59 10.90 23 1 -31 135.39 10.20 -23 1 31 156.98 9.00 -21 -1 31 72.79 5.60 21 -1 -31 72.09 8.70 21 -1 -31 63.09 4.80 -21 -1 31 50.69 4.80 -21 -1 31 71.99 6.70 -21 1 31 54.49 5.00 -21 1 31 60.49 8.00 -21 1 31 58.49 5.60 21 1 -31 50.59 7.10 21 1 -31 61.89 5.90 19 -1 -31 19.50 7.40 -19 -1 31 25.70 4.00 19 -1 -31 18.90 2.90 -19 -1 31 27.10 5.60 -19 1 31 24.30 3.80 -19 1 31 30.00 5.80 19 1 -31 25.60 5.20 -19 1 31 27.10 4.50 19 1 -31 28.30 4.50 -17 -1 31 37.30 4.70 17 -1 -31 46.10 3.80 -17 1 31 36.00 4.70 17 1 -31 33.60 6.10 15 -1 -31 19.20 4.30 -15 -1 31 16.40 3.20 15 -1 -31 19.20 2.70 15 1 -31 22.30 7.10 -15 1 31 24.00 4.30 15 1 -31 22.20 7.50 -15 1 31 19.10 4.30 15 1 -31 28.00 6.60 13 -1 -31 39.70 3.40 13 -1 -31 42.30 7.00 -13 -1 31 33.60 4.40 13 1 -31 53.19 7.80 -13 1 31 29.20 4.40 13 1 -31 42.00 6.40 13 1 -31 51.49 6.00 11 -1 -31 78.29 13.30 -11 -1 31 68.19 5.30 11 1 -31 69.29 9.30 -11 1 31 63.09 5.70 11 1 -31 72.89 6.10 11 1 -31 77.99 7.60 -11 1 31 71.39 6.20 -9 -1 31 5.70 2.20 -9 -1 31 1.20 2.40 9 -1 -31 8.30 4.90 9 1 -31 2.60 2.90 9 1 -31 5.30 3.50 9 1 -31 0.50 2.10 -9 1 31 5.60 2.40 -9 1 31 -0.40 2.40 -7 -1 31 58.89 5.00 -7 -1 31 48.60 6.30 7 -1 -31 60.19 8.10 -7 1 31 56.09 3.30 -7 1 31 47.70 5.70 -7 1 31 49.30 6.00 -5 -1 31 144.59 8.50 5 -1 -31 169.88 11.50 -5 1 31 152.98 6.20 -5 1 31 159.68 9.30 3 -1 -31 6.50 3.70 -3 -1 31 2.60 1.70 -3 -1 31 -0.40 1.90 -3 1 31 2.90 2.60 -3 1 31 7.60 3.00 -3 1 31 3.20 1.10 3 1 -31 4.00 2.80 22 0 -32 283.07 12.90 -22 0 32 258.77 13.90 -22 0 32 251.77 12.90 -22 0 32 264.67 10.90 22 0 -32 294.37 15.70 -20 0 32 6.30 2.80 20 0 -32 9.10 3.80 -20 0 32 6.90 2.90 -18 0 32 4.80 2.40 18 0 -32 5.10 3.10 -18 0 32 1.60 2.60 18 0 -32 4.60 1.90 -18 0 32 4.50 1.70 -16 0 32 89.89 7.00 -16 0 32 95.29 6.00 16 0 -32 108.09 6.80 -16 0 32 115.49 8.30 16 0 -32 99.49 9.00 -14 0 32 47.70 6.00 14 0 -32 48.00 4.80 -14 0 32 41.20 3.90 14 0 -32 53.59 7.40 12 0 -32 64.89 5.30 12 0 -32 86.99 8.10 -12 0 32 75.29 5.10 -12 0 32 69.09 6.60 -12 0 32 63.99 7.40 -10 0 32 206.68 11.40 10 0 -32 216.18 13.10 10 0 -32 203.58 10.00 -10 0 32 216.48 9.60 -10 0 32 219.28 12.20 8 0 -32 8.70 3.70 -8 0 32 4.60 1.70 -8 0 32 2.10 2.50 -8 0 32 4.80 3.30 6 0 -32 2.70 2.60 -6 0 32 7.60 1.90 4 0 -32 3.80 3.30 -4 0 32 6.60 2.80 -19 -1 32 14.90 3.80 -19 -1 32 11.10 2.50 19 -1 -32 19.10 2.90 19 -1 -32 9.00 3.30 -19 1 32 13.70 4.40 -19 1 32 13.80 3.50 -19 1 32 13.30 3.00 19 1 -32 19.00 4.20 19 1 -32 16.50 3.60 17 -1 -32 1.20 1.30 -17 -1 32 4.00 2.30 -17 -1 32 -1.00 1.30 17 -1 -32 6.10 3.00 17 1 -32 6.30 2.90 -17 1 32 0.60 1.90 -17 1 32 -2.70 2.20 17 1 -32 1.10 2.10 -15 -1 32 14.40 3.90 15 -1 -32 10.40 2.40 -15 -1 32 12.20 3.00 15 -1 -32 19.50 4.90 15 1 -32 6.90 2.90 -15 1 32 10.20 3.00 15 1 -32 17.70 4.40 -15 1 32 15.20 3.60 13 -1 -32 3.80 1.50 13 -1 -32 6.00 3.50 -13 -1 32 2.10 2.30 -13 -1 32 0.40 1.60 -13 1 32 3.10 2.40 -13 1 32 10.30 3.40 13 1 -32 7.10 3.30 13 1 -32 4.60 2.50 -11 -1 32 2.80 1.80 -11 -1 32 -0.50 1.90 11 -1 -32 0.10 2.50 11 1 -32 -1.70 2.20 -11 1 32 2.40 2.30 -11 1 32 -4.20 2.10 11 1 -32 -0.40 2.40 -9 -1 32 18.50 3.40 9 -1 -32 16.30 4.40 -9 -1 32 10.90 3.40 9 1 -32 12.30 5.00 9 1 -32 20.20 4.90 -9 1 32 24.50 4.00 7 -1 -32 12.80 4.40 -7 1 32 0.70 2.40 7 1 -32 5.40 3.60 -7 1 32 6.70 2.80 16 0 -33 2.70 2.70 16 0 -33 -1.60 1.50 -16 0 33 0.00 1.20 -16 0 33 1.80 3.00 -16 0 33 -0.10 2.00 14 0 -33 -2.70 2.30 -14 0 33 1.40 2.80 -14 0 33 0.30 1.40 14 0 -33 2.90 1.80 12 0 -33 1.40 2.80 10 0 -33 6.80 3.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 78034 _shelx_res_file ; TITL 32Ccg CELL 0.71073 30.5651 3.8629 25.5357 90.000 110.497 90.000 ZERR 8.00 0.0015 0.0002 0.0013 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N CL UNIT 144 104 8 16 MERG 2 OMIT -2.00 180.0 FMAP 2 SIZE 0.061 0.097 0.200 ACTA HTAB BOND $H CONF LIST 4 L.S. 20 TEMP -173.15 OMIT 16 0 0 OMIT 3 3 9 WGHT 0.034200 4.038600 FVAR 0.22201 N1 3 0.565313 0.885158 0.489483 11.00000 0.01330 0.01274 = 0.01321 0.00093 0.00485 0.00059 C2 1 0.541980 0.730595 0.441817 11.00000 0.01253 0.01122 = 0.01429 0.00177 0.00433 0.00105 C3 1 0.563180 0.627377 0.402971 11.00000 0.01445 0.01457 = 0.01084 -0.00034 0.00278 0.00005 AFIX 43 H3 2 0.544768 0.518891 0.369013 11.00000 -1.20000 AFIX 0 C4 1 0.609908 0.681938 0.413723 11.00000 0.01522 0.01133 = 0.01067 0.00217 0.00431 0.00224 C4A 1 0.636399 0.846513 0.465447 11.00000 0.01255 0.01130 = 0.01125 0.00259 0.00350 0.00090 C5 1 0.684839 0.921763 0.481949 11.00000 0.01385 0.01444 = 0.01397 0.00267 0.00589 0.00162 AFIX 43 H5 2 0.701399 0.861203 0.457979 11.00000 -1.20000 AFIX 0 C6 1 0.707925 1.080151 0.531862 11.00000 0.01162 0.01459 = 0.01756 0.00333 0.00339 -0.00024 AFIX 43 H6 2 0.740456 1.124686 0.542600 11.00000 -1.20000 AFIX 0 C7 1 0.683728 1.178132 0.567612 11.00000 0.01694 0.01383 = 0.01201 -0.00007 0.00209 -0.00080 AFIX 43 H7 2 0.700018 1.288070 0.602258 11.00000 -1.20000 AFIX 0 C8 1 0.636774 1.114797 0.552379 11.00000 0.01743 0.01276 = 0.01158 0.00068 0.00626 0.00107 AFIX 43 H8 2 0.620635 1.185791 0.576295 11.00000 -1.20000 AFIX 0 C8A 1 0.612036 0.944916 0.501454 11.00000 0.01331 0.01007 = 0.01190 0.00253 0.00439 0.00099 C21 1 0.491051 0.655913 0.429294 11.00000 0.01346 0.01748 = 0.01783 -0.00228 0.00622 -0.00103 AFIX 137 H21A 2 0.479367 0.800813 0.453046 11.00000 -1.50000 H21B 2 0.487077 0.411284 0.436768 11.00000 -1.50000 H21C 2 0.473509 0.706958 0.389904 11.00000 -1.50000 AFIX 0 C41 1 0.632272 0.576268 0.373521 11.00000 0.01446 0.01325 = 0.01377 0.00059 0.00545 0.00178 AFIX 43 H41 2 0.662718 0.478721 0.387305 11.00000 -1.20000 AFIX 0 C42 1 0.611083 0.613401 0.318433 11.00000 0.01205 0.01515 = 0.01405 -0.00060 0.00546 0.00108 AFIX 43 H42 2 0.580839 0.714521 0.306226 11.00000 -1.20000 AFIX 0 C421 1 0.629730 0.513691 0.274378 11.00000 0.01403 0.01283 = 0.00947 0.00205 0.00354 0.00170 C422 1 0.599982 0.359826 0.224710 11.00000 0.01110 0.01497 = 0.01366 0.00209 0.00354 0.00132 CL42 4 0.542801 0.258683 0.218849 11.00000 0.01233 0.02289 = 0.01625 0.00075 0.00313 -0.00152 C423 1 0.613847 0.273829 0.180214 11.00000 0.01878 0.01380 = 0.01246 -0.00110 0.00414 0.00075 AFIX 43 H423 2 0.592518 0.169512 0.147544 11.00000 -1.20000 AFIX 0 C424 1 0.659479 0.342851 0.184228 11.00000 0.02090 0.01596 = 0.01420 0.00001 0.00891 0.00189 AFIX 43 H424 2 0.669629 0.284768 0.154170 11.00000 -1.20000 AFIX 0 C425 1 0.690230 0.496139 0.231937 11.00000 0.01404 0.01513 = 0.01615 0.00132 0.00646 0.00122 AFIX 43 H425 2 0.721392 0.544969 0.234567 11.00000 -1.20000 AFIX 0 C426 1 0.675349 0.578156 0.275894 11.00000 0.01349 0.01219 = 0.01158 0.00158 0.00225 0.00076 CL46 4 0.716482 0.775004 0.334024 11.00000 0.01376 0.02144 = 0.01317 -0.00164 0.00267 -0.00336 HKLF 4 REM 32Ccg REM R1 = 0.0311 for 2930 Fo > 4sig(Fo) and 0.0349 for all 3208 data REM 191 parameters refined using 0 restraints END WGHT 0.0342 4.0386 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+2, -z+1 HTAB C21 N1_$1 REM Highest difference peak 0.331, deepest hole -0.264, 1-sigma level 0.052 Q1 1 0.5409 0.3997 0.2479 11.00000 0.05 0.33 Q2 1 0.6223 0.5578 0.2983 11.00000 0.05 0.33 Q3 1 0.6238 0.9207 0.4835 11.00000 0.05 0.33 Q4 1 0.6058 0.3637 0.2016 11.00000 0.05 0.32 Q5 1 0.6194 0.8414 0.4326 11.00000 0.05 0.32 Q6 1 0.6116 0.4687 0.2494 11.00000 0.05 0.30 Q7 1 0.6815 0.5613 0.2509 11.00000 0.05 0.29 Q8 1 0.6543 0.5185 0.2773 11.00000 0.05 0.29 Q9 1 0.6256 0.9824 0.5293 11.00000 0.05 0.28 Q10 1 0.6951 1.1119 0.5506 11.00000 0.05 0.28 Q11 1 0.6193 0.6363 0.3922 11.00000 0.05 0.27 Q12 1 0.5537 0.6097 0.4303 11.00000 0.05 0.27 Q13 1 0.6595 0.9061 0.4723 11.00000 0.05 0.26 Q14 1 0.6605 1.0927 0.5615 11.00000 0.05 0.25 Q15 1 0.6951 0.9509 0.5117 11.00000 0.05 0.25 Q16 1 0.6390 0.2847 0.1892 11.00000 0.05 0.24 Q17 1 0.6736 0.4634 0.2062 11.00000 0.05 0.23 Q18 1 0.5182 0.6932 0.4376 11.00000 0.05 0.23 Q19 1 0.6175 0.4906 0.3429 11.00000 0.05 0.23 Q20 1 0.5884 0.9349 0.4923 11.00000 0.05 0.23 ; _shelx_res_checksum 98895 _shelxl_version_number 2.014 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 N N1 0.56531(4) 0.8852(3) 0.48948(5) 0.0130(2) Uani d 1 . . C C2 0.54198(5) 0.7306(3) 0.44182(6) 0.0128(3) Uani d 1 . . C C3 0.56318(5) 0.6274(4) 0.40297(6) 0.0137(3) Uani d 1 . . H H3 0.5448 0.5189 0.3690 0.016 Uiso calc 1 . . C C4 0.60991(5) 0.6819(4) 0.41372(5) 0.0125(3) Uani d 1 . . C C4A 0.63640(5) 0.8465(4) 0.46545(5) 0.0119(3) Uani d 1 . . C C5 0.68484(5) 0.9218(4) 0.48195(6) 0.0138(3) Uani d 1 . . H H5 0.7014 0.8612 0.4580 0.017 Uiso calc 1 . . C C6 0.70793(5) 1.0802(4) 0.53186(6) 0.0150(3) Uani d 1 . . H H6 0.7405 1.1247 0.5426 0.018 Uiso calc 1 . . C C7 0.68373(5) 1.1781(4) 0.56761(6) 0.0151(3) Uani d 1 . . H H7 0.7000 1.2881 0.6023 0.018 Uiso calc 1 . . C C8 0.63677(5) 1.1148(4) 0.55238(6) 0.0136(3) Uani d 1 . . H H8 0.6206 1.1858 0.5763 0.016 Uiso calc 1 . . C C8A 0.61204(5) 0.9449(3) 0.50145(5) 0.0118(3) Uani d 1 . . C C21 0.49105(5) 0.6559(4) 0.42929(6) 0.0161(3) Uani d 1 . . H H21A 0.4794 0.8008 0.4530 0.024 Uiso calc 1 . . H H21B 0.4871 0.4113 0.4368 0.024 Uiso calc 1 . . H H21C 0.4735 0.7070 0.3899 0.024 Uiso calc 1 . . C C41 0.63227(5) 0.5763(4) 0.37352(6) 0.0137(3) Uani d 1 . . H H41 0.6627 0.4787 0.3873 0.016 Uiso calc 1 . . C C42 0.61108(5) 0.6134(4) 0.31843(6) 0.0135(3) Uani d 1 . . H H42 0.5808 0.7145 0.3062 0.016 Uiso calc 1 . . C C421 0.62973(5) 0.5137(4) 0.27438(5) 0.0123(3) Uani d 1 . . C C422 0.59998(5) 0.3598(4) 0.22471(6) 0.0135(3) Uani d 1 . . Cl Cl42 0.54280(2) 0.25868(9) 0.21885(2) 0.01765(10) Uani d 1 . . C C423 0.61385(5) 0.2738(4) 0.18021(6) 0.0154(3) Uani d 1 . . H H423 0.5925 0.1695 0.1475 0.018 Uiso calc 1 . . C C424 0.65948(5) 0.3429(4) 0.18423(6) 0.0163(3) Uani d 1 . . H H424 0.6696 0.2848 0.1542 0.020 Uiso calc 1 . . C C425 0.69023(5) 0.4961(4) 0.23194(6) 0.0148(3) Uani d 1 . . H H425 0.7214 0.5450 0.2346 0.018 Uiso calc 1 . . C C426 0.67535(5) 0.5782(4) 0.27589(6) 0.0130(3) Uani d 1 . . Cl Cl46 0.71648(2) 0.77500(9) 0.33402(2) 0.01667(10) Uani 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 N1 0.0133(5) 0.0127(6) 0.0132(5) 0.0006(4) 0.0048(4) 0.0009(4) C2 0.0125(6) 0.0112(6) 0.0143(6) 0.0010(5) 0.0043(5) 0.0018(5) C3 0.0145(6) 0.0146(7) 0.0108(6) 0.0001(5) 0.0028(5) -0.0003(5) C4 0.0152(6) 0.0113(6) 0.0107(6) 0.0022(5) 0.0043(5) 0.0022(5) C4A 0.0126(6) 0.0113(6) 0.0113(6) 0.0009(5) 0.0035(5) 0.0026(5) C5 0.0138(6) 0.0144(7) 0.0140(6) 0.0016(5) 0.0059(5) 0.0027(5) C6 0.0116(6) 0.0146(7) 0.0176(7) -0.0002(5) 0.0034(5) 0.0033(5) C7 0.0169(7) 0.0138(7) 0.0120(6) -0.0008(5) 0.0021(5) -0.0001(5) C8 0.0174(7) 0.0128(6) 0.0116(6) 0.0011(5) 0.0063(5) 0.0007(5) C8A 0.0133(6) 0.0101(6) 0.0119(6) 0.0010(5) 0.0044(5) 0.0025(5) C21 0.0135(7) 0.0175(7) 0.0178(7) -0.0010(5) 0.0062(5) -0.0023(6) C41 0.0145(6) 0.0132(7) 0.0138(6) 0.0018(5) 0.0054(5) 0.0006(5) C42 0.0120(6) 0.0151(7) 0.0140(6) 0.0011(5) 0.0055(5) -0.0006(5) C421 0.0140(6) 0.0128(6) 0.0095(6) 0.0017(5) 0.0035(5) 0.0021(5) C422 0.0111(6) 0.0150(7) 0.0137(6) 0.0013(5) 0.0035(5) 0.0021(5) Cl42 0.01233(16) 0.0229(2) 0.01625(17) -0.00152(13) 0.00313(13) 0.00075(13) C423 0.0188(7) 0.0138(7) 0.0125(6) 0.0007(5) 0.0041(5) -0.0011(5) C424 0.0209(7) 0.0160(7) 0.0142(6) 0.0019(6) 0.0089(5) 0.0000(5) C425 0.0140(6) 0.0151(7) 0.0162(6) 0.0012(5) 0.0065(5) 0.0013(5) C426 0.0135(6) 0.0122(6) 0.0116(6) 0.0008(5) 0.0022(5) 0.0016(5) Cl46 0.01376(17) 0.02144(19) 0.01317(16) -0.00336(13) 0.00267(12) -0.00164(13) 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' 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 C2 N1 C8A . . 117.80(12) ? N1 C2 C3 . . 122.74(13) ? N1 C2 C21 . . 117.92(12) ? C3 C2 C21 . . 119.32(12) ? C4 C3 C2 . . 120.99(13) ? C4 C3 H3 . . 119.5 ? C2 C3 H3 . . 119.5 ? C3 C4 C4A . . 117.69(12) ? C3 C4 C41 . . 121.40(13) ? C4A C4 C41 . . 120.91(12) ? C5 C4A C8A . . 118.73(12) ? C5 C4A C4 . . 123.91(12) ? C8A C4A C4 . . 117.34(12) ? C6 C5 C4A . . 120.84(13) ? C6 C5 H5 . . 119.6 ? C4A C5 H5 . . 119.6 ? C5 C6 C7 . . 120.43(13) ? C5 C6 H6 . . 119.8 ? C7 C6 H6 . . 119.8 ? C8 C7 C6 . . 120.11(13) ? C8 C7 H7 . . 119.9 ? C6 C7 H7 . . 119.9 ? C7 C8 C8A . . 120.84(13) ? C7 C8 H8 . . 119.6 ? C8A C8 H8 . . 119.6 ? N1 C8A C8 . . 117.54(12) ? N1 C8A C4A . . 123.43(12) ? C8 C8A C4A . . 119.04(12) ? C2 C21 H21A . . 109.5 ? C2 C21 H21B . . 109.5 ? H21A C21 H21B . . 109.5 ? C2 C21 H21C . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 109.5 ? C42 C41 C4 . . 122.10(13) ? C42 C41 H41 . . 119.0 ? C4 C41 H41 . . 119.0 ? C41 C42 C421 . . 126.85(13) ? C41 C42 H42 . . 116.6 ? C421 C42 H42 . . 116.6 ? C426 C421 C422 . . 114.95(12) ? C426 C421 C42 . . 125.20(12) ? C422 C421 C42 . . 119.73(12) ? C423 C422 C421 . . 123.63(13) ? C423 C422 Cl42 . . 117.44(11) ? C421 C422 Cl42 . . 118.90(10) ? C422 C423 C424 . . 118.79(13) ? C422 C423 H423 . . 120.6 ? C424 C423 H423 . . 120.6 ? C425 C424 C423 . . 120.14(13) ? C425 C424 H424 . . 119.9 ? C423 C424 H424 . . 119.9 ? C424 C425 C426 . . 119.72(13) ? C424 C425 H425 . . 120.1 ? C426 C425 H425 . . 120.1 ? C425 C426 C421 . . 122.76(13) ? C425 C426 Cl46 . . 116.38(10) ? C421 C426 Cl46 . . 120.85(10) ? 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 N1 C2 . 1.3186(18) ? N1 C8A . 1.3713(17) ? C2 C3 . 1.4188(19) ? C2 C21 . 1.5034(18) ? C3 C4 . 1.3730(19) ? C3 H3 . 0.9500 ? C4 C4A . 1.4336(19) ? C4 C41 . 1.4762(18) ? C4A C5 . 1.4203(18) ? C4A C8A . 1.4227(18) ? C5 C6 . 1.366(2) ? C5 H5 . 0.9500 ? C6 C7 . 1.4130(19) ? C6 H6 . 0.9500 ? C7 C8 . 1.3711(19) ? C7 H7 . 0.9500 ? C8 C8A . 1.4159(19) ? C8 H8 . 0.9500 ? C21 H21A . 0.9800 ? C21 H21B . 0.9800 ? C21 H21C . 0.9800 ? C41 C42 . 1.3345(19) ? C41 H41 . 0.9500 ? C42 C421 . 1.4791(18) ? C42 H42 . 0.9500 ? C421 C426 . 1.4035(18) ? C421 C422 . 1.4075(18) ? C422 C423 . 1.3850(19) ? C422 Cl42 . 1.7454(14) ? C423 C424 . 1.388(2) ? C423 H423 . 0.9500 ? C424 C425 . 1.384(2) ? C424 H424 . 0.9500 ? C425 C426 . 1.3874(19) ? C425 H425 . 0.9500 ? C426 Cl46 . 1.7479(14) ? 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 C8A N1 C2 C3 . . . . -0.4(2) ? C8A N1 C2 C21 . . . . 178.35(12) ? N1 C2 C3 C4 . . . . 0.6(2) ? C21 C2 C3 C4 . . . . -178.06(13) ? C2 C3 C4 C4A . . . . 0.0(2) ? C2 C3 C4 C41 . . . . -179.85(13) ? C3 C4 C4A C5 . . . . -179.50(13) ? C41 C4 C4A C5 . . . . 0.3(2) ? C3 C4 C4A C8A . . . . -0.78(19) ? C41 C4 C4A C8A . . . . 179.06(12) ? C8A C4A C5 C6 . . . . 1.1(2) ? C4 C4A C5 C6 . . . . 179.83(13) ? C4A C5 C6 C7 . . . . -1.2(2) ? C5 C6 C7 C8 . . . . 0.0(2) ? C6 C7 C8 C8A . . . . 1.3(2) ? C2 N1 C8A C8 . . . . 179.24(12) ? C2 N1 C8A C4A . . . . -0.5(2) ? C7 C8 C8A N1 . . . . 178.89(13) ? C7 C8 C8A C4A . . . . -1.3(2) ? C5 C4A C8A N1 . . . . 179.88(12) ? C4 C4A C8A N1 . . . . 1.1(2) ? C5 C4A C8A C8 . . . . 0.12(19) ? C4 C4A C8A C8 . . . . -178.67(12) ? C3 C4 C41 C42 . . . . 39.5(2) ? C4A C4 C41 C42 . . . . -140.35(15) ? C4 C41 C42 C421 . . . . -179.23(13) ? C41 C42 C421 C426 . . . . -44.5(2) ? C41 C42 C421 C422 . . . . 139.58(15) ? C426 C421 C422 C423 . . . . 0.4(2) ? C42 C421 C422 C423 . . . . 176.74(13) ? C426 C421 C422 Cl42 . . . . 178.52(10) ? C42 C421 C422 Cl42 . . . . -5.14(18) ? C421 C422 C423 C424 . . . . -0.2(2) ? Cl42 C422 C423 C424 . . . . -178.36(11) ? C422 C423 C424 C425 . . . . -0.2(2) ? C423 C424 C425 C426 . . . . 0.5(2) ? C424 C425 C426 C421 . . . . -0.3(2) ? C424 C425 C426 Cl46 . . . . -179.35(11) ? C422 C421 C426 C425 . . . . -0.2(2) ? C42 C421 C426 C425 . . . . -176.27(13) ? C422 C421 C426 Cl46 . . . . 178.89(10) ? C42 C421 C426 Cl46 . . . . 2.8(2) ? _cod_database_fobs_code 2022669