#------------------------------------------------------------------------------ #$Date: 2021-08-28 05:08:32 +0300 (Sat, 28 Aug 2021) $ #$Revision: 268277 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243907.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_2243907 loop_ _publ_author_name 'Shikhaliyev, Namiq Q.' 'Atio\(glu, Zeliha' 'Akkurt, Mehmet' 'Qacar, Ayten M.' 'Askerov, Rizvan K.' 'Bhattarai, Ajaya' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of (E)-1-[2,2-dichloro-1-(4-methylphenyl)ethenyl]-2-(4-methoxyphenyl)diazene ; _journal_coeditor_code ZN2009 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 965 _journal_page_last 970 _journal_paper_doi 10.1107/S2056989021008756 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C16 H14 Cl2 N2 O' _chemical_formula_moiety 'C16 H14 Cl2 N2 O' _chemical_formula_sum 'C16 H14 Cl2 N2 O' _chemical_formula_weight 321.19 _chemical_name_systematic (E)-1-[2,2-Dichloro-1-(4-methylphenyl)ethenyl]-2-(4-methoxyphenyl)diazene _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 99.173(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.5366(3) _cell_length_b 17.9208(8) _cell_length_c 16.2085(8) _cell_measurement_reflns_used 3046 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 23.26 _cell_measurement_theta_min 2.61 _cell_volume 1587.65(14) _computing_cell_refinement ; SAINT (Bruker, 2007) ; _computing_data_collection ; APEX2 (Bruker, 2007) ; _computing_data_reduction ; SAINT (Bruker, 2007) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2016/6 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2016/6 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_unetI/netI 0.0667 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 19301 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.349 _diffrn_reflns_theta_min 1.706 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.344 _exptl_crystal_description prism _exptl_crystal_F_000 664 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.097 _refine_diff_density_max 0.370 _refine_diff_density_min -0.316 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.11(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 288 _refine_ls_number_reflns 6444 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.010 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0594 _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^)+(0.0481P)^2^+0.5767P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1202 _refine_ls_wR_factor_ref 0.1449 _reflns_number_gt 3820 _reflns_number_total 6444 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zn2009sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2243907 _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 0.908 _shelx_estimated_absorpt_t_max 0.961 _shelx_hkl_file ; 1 0 0 0.50 0.80 1 0 0 0.70 1.00 1 0 0 -0.10 0.90 -1 0 0 1.60 1.20 -1 0 0 0.90 0.90 -1 0 0 -0.20 0.90 2 0 0 15.40 3.30 2 0 0 24.40 3.90 -2 0 0 16.10 3.70 2 0 0 18.70 3.60 2 0 0 22.20 2.90 -2 0 0 19.10 2.80 3 0 0 2.70 1.90 -3 0 0 2.50 1.80 -3 0 0 7.00 3.10 4 0 0 331.17 17.30 -4 0 0 370.86 14.70 -4 0 0 345.47 18.00 -5 0 0 0.70 2.80 -5 0 0 -0.90 1.80 5 0 0 5.40 3.90 -6 0 0 5.10 4.20 -6 0 0 9.40 3.60 6 0 0 4.40 5.20 1 -1 0 1159.78 22.30 1 -1 0 1108.49 22.70 1 -1 0 1126.09 23.50 -1 -1 0 1160.58 23.80 -1 -1 0 1144.49 21.70 -1 1 0 1104.89 23.50 1 1 0 1129.39 21.70 1 1 0 1132.79 23.60 1 1 0 1132.79 23.10 -1 1 0 1108.09 22.80 -1 1 0 1126.89 22.30 2 -1 0 194.08 9.00 -2 -1 0 183.78 7.20 -2 -1 0 192.48 9.40 2 -1 0 201.98 7.70 2 -1 0 189.88 8.70 2 1 0 185.68 7.20 -2 1 0 194.88 9.10 -2 1 0 189.58 7.70 2 1 0 166.68 8.60 2 1 0 183.48 8.90 -2 1 0 184.28 9.10 2 1 0 190.28 8.60 -3 -1 0 22.70 4.90 -3 -1 0 28.00 4.10 3 -1 0 27.80 4.20 3 -1 0 23.50 4.90 3 1 0 31.00 5.70 -3 1 0 31.80 5.90 -3 1 0 24.90 4.00 3 1 0 33.30 4.50 4 -1 0 117.69 10.20 -4 -1 0 98.19 9.80 -4 -1 0 102.39 7.60 4 1 0 107.29 9.90 -4 1 0 91.59 9.30 -4 1 0 103.99 8.00 -5 -1 0 46.70 6.70 -5 -1 0 64.39 10.70 5 -1 0 45.10 8.30 -5 1 0 55.79 7.90 -5 1 0 59.49 10.40 5 1 0 48.00 9.30 -6 -1 0 5.90 3.50 -6 -1 0 1.60 4.60 6 -1 0 7.10 5.40 -6 1 0 0.70 3.10 6 1 0 5.80 5.30 -6 1 0 13.20 5.40 0 -2 0 8.60 1.50 0 -2 0 11.80 1.80 0 -2 0 8.20 0.90 0 2 0 14.90 2.00 0 2 0 10.30 0.80 0 2 0 8.90 1.60 1 -2 0 381.36 11.20 1 -2 0 363.46 10.10 -1 -2 0 350.76 10.60 1 -2 0 362.36 9.40 -1 -2 0 357.36 9.50 -1 2 0 352.96 10.30 1 2 0 353.56 9.60 1 2 0 336.67 10.40 -1 2 0 354.46 11.00 -1 2 0 341.57 9.30 1 2 0 353.96 10.20 -2 -2 0 5.30 2.60 -2 -2 0 6.40 2.20 2 -2 0 4.90 2.10 2 -2 0 4.10 2.10 2 -2 0 2.30 1.40 -2 -2 0 4.40 1.70 2 2 0 2.40 1.80 -2 2 0 5.80 1.80 2 2 0 2.80 1.80 -2 2 0 5.00 2.30 -2 2 0 5.60 2.70 2 2 0 3.60 1.30 -3 -2 0 72.89 7.30 3 -2 0 63.69 5.20 -3 -2 0 73.59 5.50 3 2 0 69.49 6.80 -3 2 0 73.49 6.80 3 2 0 74.09 5.40 -3 2 0 71.09 7.10 -3 2 0 72.79 6.10 4 -2 0 1.00 2.80 -4 -2 0 2.60 2.30 -4 -2 0 0.80 2.90 4 2 0 1.90 3.00 -4 2 0 2.60 2.20 -4 2 0 5.60 2.90 -5 -2 0 44.30 8.90 -5 -2 0 50.39 5.80 5 -2 0 47.50 9.30 5 2 0 43.00 8.30 -5 2 0 44.80 7.00 -5 2 0 45.80 8.30 -6 -2 0 2.50 3.10 -6 -2 0 -3.90 2.90 6 -2 0 -3.10 3.20 6 -2 0 -3.70 2.80 6 2 0 3.50 3.70 -6 2 0 7.20 4.70 0 -3 0 -0.90 1.00 0 -3 0 -0.20 1.10 0 3 0 -0.10 0.50 0 3 0 -0.30 1.20 0 3 0 0.20 0.80 0 3 0 0.20 0.50 -1 -3 0 1276.97 31.20 -1 -3 0 1234.68 26.30 1 -3 0 1239.48 27.00 1 -3 0 1217.98 27.30 1 -3 0 1210.38 23.80 -1 -3 0 1247.48 25.80 1 -3 0 1247.28 26.50 -1 3 0 1221.48 23.80 1 3 0 1208.78 26.10 -1 3 0 1229.38 27.40 1 3 0 1226.48 25.90 1 3 0 1232.38 26.40 2 -3 0 18.00 3.20 2 -3 0 18.20 3.60 2 -3 0 20.40 3.50 -2 -3 0 17.30 3.10 -2 -3 0 11.70 3.10 -2 -3 0 19.70 3.80 -2 3 0 20.30 3.50 -2 3 0 20.30 3.70 2 3 0 18.40 3.60 2 3 0 22.70 3.30 2 3 0 23.80 4.60 -2 3 0 14.40 3.60 -3 -3 0 533.85 20.60 -3 -3 0 543.75 16.40 3 -3 0 539.45 17.90 -3 3 0 542.15 18.20 3 3 0 526.15 22.40 -3 3 0 521.15 20.10 3 3 0 528.75 16.70 -3 3 0 558.24 22.50 -4 -3 0 52.09 5.50 -4 -3 0 45.10 8.30 4 3 0 48.20 8.00 -4 3 0 55.99 6.30 -4 3 0 70.09 9.70 -4 3 0 65.79 9.60 5 -3 0 15.70 5.30 -5 -3 0 11.80 3.30 -5 -3 0 23.60 7.20 5 -3 0 9.30 4.30 -5 3 0 8.90 4.60 5 3 0 16.60 5.10 6 -3 0 -6.20 2.40 -6 -3 0 -0.10 2.60 6 -3 0 6.50 4.70 -6 -3 0 -0.60 3.30 -6 3 0 -3.60 2.50 6 3 0 -4.00 2.70 0 -4 0 315.17 10.90 0 -4 0 317.47 11.00 0 4 0 311.67 7.50 0 4 0 315.67 7.30 0 4 0 319.47 10.80 0 4 0 326.07 11.10 -1 -4 0 163.78 7.60 1 -4 0 171.38 5.70 -1 -4 0 175.68 7.80 -1 -4 0 173.68 7.60 1 -4 0 186.28 8.60 1 4 0 180.88 8.40 -1 4 0 174.88 8.60 -1 4 0 175.58 5.50 1 4 0 176.28 7.80 1 4 0 171.38 7.40 -1 4 0 166.18 8.00 2 -4 0 779.02 22.30 -2 -4 0 781.42 21.40 -2 -4 0 806.62 23.00 2 -4 0 765.62 21.90 -2 -4 0 785.52 20.20 2 -4 0 783.42 21.10 2 4 0 741.33 21.50 2 4 0 798.82 23.00 -2 4 0 759.32 19.90 -2 4 0 771.52 23.30 -3 -4 0 14.50 4.30 3 -4 0 24.30 4.90 -3 -4 0 29.20 4.40 -3 4 0 21.20 5.00 -3 4 0 36.20 6.90 3 4 0 24.00 4.40 -4 -4 0 38.50 5.70 4 -4 0 29.60 5.80 -4 -4 0 32.60 7.40 4 4 0 38.10 7.40 -4 4 0 33.50 6.80 -4 4 0 44.60 8.20 5 -4 0 3.60 2.80 -5 -4 0 0.70 1.80 -5 -4 0 2.40 4.20 5 -4 0 7.00 4.20 -5 4 0 4.00 2.70 5 4 0 3.20 3.30 -6 -4 0 0.80 2.50 -6 -4 0 -5.40 2.60 6 -4 0 1.40 2.80 6 -4 0 2.40 3.60 -6 4 0 -2.70 2.30 6 4 0 -1.90 3.70 0 -5 0 2.40 2.20 0 -5 0 1.80 2.80 0 5 0 0.80 0.80 0 5 0 -0.10 1.10 0 5 0 -1.00 2.50 0 5 0 6.20 2.70 -1 -5 0 160.38 8.20 1 -5 0 170.18 9.00 -1 -5 0 172.08 7.60 1 -5 0 168.78 9.00 1 -5 0 152.88 5.30 -1 -5 0 159.98 8.30 -1 5 0 165.28 8.60 1 5 0 176.78 10.60 -1 5 0 162.68 5.10 1 5 0 160.78 8.10 1 5 0 164.88 8.80 -1 5 0 160.38 8.80 -2 -5 0 106.09 7.70 -2 -5 0 117.29 7.00 2 -5 0 117.69 6.50 2 -5 0 103.69 6.80 2 -5 0 119.49 8.10 -2 -5 0 116.19 7.20 2 5 0 108.39 7.70 -2 5 0 107.49 8.20 2 5 0 101.19 6.70 -2 5 0 113.99 6.20 -3 -5 0 100.49 9.00 3 -5 0 105.49 8.40 -3 -5 0 112.89 7.30 3 5 0 93.29 6.90 -3 5 0 100.19 7.50 3 5 0 115.99 9.00 -3 5 0 109.49 9.30 4 -5 0 63.99 7.40 -4 -5 0 53.39 5.80 -4 -5 0 57.89 9.00 4 5 0 64.69 9.60 -4 5 0 71.79 7.80 -4 5 0 47.90 8.70 -5 -5 0 1.90 2.30 -5 -5 0 1.70 4.90 5 -5 0 -2.30 2.30 -5 5 0 1.90 3.30 -5 5 0 3.30 2.50 5 5 0 3.30 2.70 -6 -5 0 -4.20 2.40 6 -5 0 -3.40 3.50 -6 -5 0 -0.40 3.20 6 -5 0 -3.60 3.10 6 5 0 -6.60 3.20 -6 5 0 1.60 4.00 0 -6 0 253.97 11.40 0 -6 0 231.78 10.80 0 6 0 243.18 7.20 0 6 0 241.18 6.70 0 6 0 240.78 11.20 0 6 0 242.38 10.90 1 -6 0 612.04 20.00 1 -6 0 610.04 19.70 -1 -6 0 588.14 18.20 -1 -6 0 621.74 16.90 -1 -6 0 593.84 18.60 1 -6 0 601.24 13.10 1 6 0 610.74 18.60 1 6 0 588.64 18.70 -1 6 0 623.84 19.30 -1 6 0 608.24 19.60 -1 6 0 602.54 12.50 -2 -6 0 62.79 5.60 -2 -6 0 66.89 6.30 2 -6 0 55.89 5.00 2 -6 0 55.69 6.40 2 6 0 64.59 6.70 -2 6 0 63.89 4.60 2 6 0 56.69 5.50 -2 6 0 63.19 6.80 -3 -6 0 39.50 5.80 -3 -6 0 40.00 7.00 3 -6 0 25.50 5.50 -3 6 0 29.00 4.80 3 6 0 44.80 7.00 -3 6 0 30.00 6.60 -4 -6 0 1.50 1.90 -4 -6 0 4.90 4.30 4 -6 0 4.00 2.80 -4 6 0 -1.70 2.20 4 6 0 2.30 3.40 -4 6 0 -3.60 2.20 5 -6 0 17.00 5.00 -5 -6 0 13.70 5.70 -5 -6 0 23.20 4.80 -5 6 0 27.90 7.00 -5 6 0 23.20 7.40 5 6 0 19.80 6.00 -6 -6 0 0.20 4.30 6 -6 0 -2.80 3.60 -6 -6 0 0.00 2.20 6 -6 0 -0.90 3.20 -6 6 0 10.50 5.80 6 6 0 -7.00 3.70 0 -7 0 0.40 2.30 0 -7 0 3.20 2.20 0 7 0 1.20 1.30 0 7 0 -1.60 1.30 0 7 0 1.30 0.70 0 7 0 2.90 2.90 1 -7 0 74.09 6.90 -1 -7 0 68.69 6.30 1 -7 0 66.29 3.30 -1 -7 0 58.89 4.80 -1 -7 0 63.59 5.80 1 7 0 48.10 5.10 -1 7 0 60.29 6.40 1 7 0 64.89 6.70 1 7 0 53.99 4.30 -1 7 0 66.99 2.60 -2 -7 0 26.40 4.80 -2 -7 0 27.90 6.40 2 -7 0 29.20 3.20 2 7 0 31.20 5.70 -2 7 0 26.60 3.50 -2 7 0 20.00 5.20 3 -7 0 13.10 4.80 -3 -7 0 14.90 3.50 -3 -7 0 8.70 3.60 3 7 0 18.40 5.20 -3 7 0 13.10 5.60 -3 7 0 13.90 3.50 4 -7 0 17.50 5.60 -4 -7 0 18.30 4.40 -4 -7 0 13.80 5.30 4 7 0 23.00 6.10 -4 7 0 9.20 5.20 -4 7 0 16.10 5.20 -5 -7 0 56.49 10.90 -5 -7 0 51.49 7.70 5 -7 0 48.10 8.70 5 7 0 48.70 9.70 -5 7 0 59.79 17.40 -5 7 0 60.09 9.30 6 -7 0 4.00 3.40 -6 -7 0 2.30 3.40 6 -7 0 -1.50 1.70 -6 -7 0 0.50 2.90 6 7 0 0.50 5.10 -6 7 0 3.30 3.80 0 -8 0 833.02 25.50 0 8 0 827.42 25.50 0 8 0 810.52 18.10 0 8 0 791.92 17.10 1 -8 0 10.20 1.50 -1 -8 0 9.70 3.50 -1 -8 0 6.40 2.30 -1 8 0 8.70 1.00 1 8 0 10.10 2.20 1 8 0 12.50 4.30 2 -8 0 101.79 9.00 -2 -8 0 92.99 7.50 2 -8 0 98.99 5.60 -2 -8 0 94.59 7.70 -2 8 0 111.09 9.50 -2 8 0 104.49 5.30 -3 -8 0 3.90 3.80 3 -8 0 5.90 3.40 -3 -8 0 5.50 2.90 -3 8 0 0.90 1.70 -3 8 0 -0.70 2.40 3 8 0 10.80 4.70 -4 -8 0 29.10 5.60 4 -8 0 29.50 6.50 -4 -8 0 32.90 8.00 -4 8 0 33.20 8.00 4 8 0 31.70 7.60 -4 8 0 40.00 6.90 -5 -8 0 7.90 4.70 -5 -8 0 3.10 2.20 5 -8 0 -4.60 2.20 5 8 0 0.20 3.90 -5 8 0 3.20 3.00 -5 8 0 -2.90 3.30 -6 -8 0 0.10 2.70 6 -8 0 -5.30 3.30 -6 -8 0 17.70 7.10 -6 8 0 5.70 3.40 -6 8 0 -2.90 2.50 6 8 0 1.00 5.30 0 -9 0 -1.50 1.80 0 9 0 0.30 1.40 0 9 0 0.40 0.80 1 -9 0 30.20 6.20 -1 -9 0 25.00 4.10 -1 -9 0 33.10 6.20 1 9 0 16.60 5.40 -1 9 0 17.60 5.20 1 9 0 25.00 3.90 2 -9 0 107.59 5.80 2 -9 0 122.59 10.40 -2 -9 0 105.19 8.80 -2 -9 0 105.69 8.30 -2 9 0 114.19 5.30 -2 9 0 105.29 10.10 2 9 0 112.49 10.10 -3 -9 0 18.30 4.80 -3 -9 0 14.50 4.60 3 -9 0 12.40 3.10 3 -9 0 12.30 4.60 3 9 0 12.70 5.40 -3 9 0 18.60 3.70 -3 9 0 23.00 6.50 4 -9 0 36.10 7.80 -4 -9 0 50.59 7.30 -4 -9 0 24.90 6.70 -4 9 0 33.00 8.20 4 9 0 50.19 9.80 -4 9 0 55.09 7.90 5 -9 0 8.50 5.10 -5 -9 0 5.90 5.50 -5 -9 0 5.00 3.60 -5 9 0 4.80 3.60 5 9 0 -0.10 4.80 -5 9 0 2.70 2.60 6 -9 0 2.30 4.30 -6 -9 0 3.20 4.50 -6 -9 0 -5.80 2.90 -6 9 0 13.00 6.00 6 9 0 -9.00 3.80 -6 9 0 -5.00 3.20 0 -10 0 11.70 4.10 0 10 0 6.70 3.90 0 10 0 16.60 3.00 0 10 0 14.40 2.10 1 -10 0 305.17 16.50 -1 -10 0 311.67 12.30 -1 -10 0 309.67 15.90 1 10 0 311.27 11.90 1 10 0 309.17 16.30 -1 10 0 311.27 16.50 -2 -10 0 210.68 11.90 2 -10 0 203.68 8.00 2 -10 0 186.98 13.60 -2 -10 0 214.98 13.30 2 10 0 222.78 14.40 -2 10 0 202.98 14.40 -2 10 0 193.28 6.90 -3 -10 0 53.39 8.50 3 -10 0 42.90 8.20 -3 -10 0 58.09 9.30 3 -10 0 50.39 4.80 3 10 0 67.69 10.50 -3 10 0 49.10 4.80 -3 10 0 42.00 8.30 -4 -10 0 5.10 4.40 4 -10 0 12.20 5.00 -4 -10 0 7.20 3.70 -4 10 0 10.20 3.90 -4 10 0 8.80 4.80 4 10 0 13.00 5.00 -5 -10 0 17.20 6.90 5 -10 0 7.40 5.40 -5 -10 0 5.90 3.40 -5 10 0 6.50 5.10 5 10 0 7.60 6.60 -5 10 0 2.40 3.60 -6 -10 0 4.70 5.10 -6 -10 0 1.40 2.40 6 -10 0 1.00 3.80 -6 10 0 1.30 3.70 6 10 0 -3.80 4.10 -6 10 0 -0.30 3.90 0 -11 0 -2.60 1.40 0 11 0 -1.30 3.10 0 11 0 0.50 0.80 0 11 0 -0.90 1.40 1 -11 0 590.24 24.90 -1 -11 0 559.24 23.30 -1 -11 0 634.54 19.10 1 11 0 567.84 17.50 1 11 0 623.94 24.50 -1 11 0 578.74 24.20 -2 -11 0 8.00 4.20 -2 -11 0 16.40 5.10 2 -11 0 10.80 2.60 2 -11 0 11.30 4.50 2 11 0 9.20 5.40 -2 11 0 9.10 1.70 -2 11 0 10.70 5.00 3 -11 0 83.39 6.50 -3 -11 0 80.99 8.60 3 -11 0 99.19 11.10 -3 -11 0 84.19 9.20 -3 11 0 81.79 5.70 -3 11 0 83.19 12.50 3 11 0 92.69 12.70 -4 -11 0 1.10 2.70 -4 -11 0 3.80 4.20 4 -11 0 10.90 5.20 4 11 0 8.90 6.10 -4 11 0 8.70 5.30 -4 11 0 2.10 2.90 5 -11 0 -1.70 3.30 -5 -11 0 4.10 3.20 -5 -11 0 0.30 3.00 -5 11 0 7.40 5.20 -5 11 0 -0.10 2.40 5 11 0 -9.30 4.50 0 -12 0 133.89 11.60 0 12 0 143.59 5.80 0 12 0 136.49 7.00 0 12 0 145.99 12.50 1 -12 0 66.19 10.40 -1 -12 0 65.39 10.10 1 12 0 56.89 9.30 -1 12 0 81.19 12.10 1 12 0 64.19 6.40 1 12 0 64.69 5.30 -2 -12 0 122.89 11.10 2 -12 0 101.69 11.70 -2 -12 0 107.49 9.30 2 12 0 112.89 11.80 -2 12 0 109.59 11.70 3 -12 0 8.30 2.50 3 -12 0 9.30 4.70 -3 -12 0 3.60 4.20 -3 -12 0 11.10 4.50 -3 12 0 14.00 5.60 -3 12 0 9.70 2.60 3 12 0 7.00 5.30 -4 -12 0 -1.60 3.20 4 -12 0 -6.00 2.70 -4 -12 0 2.70 2.10 -4 12 0 -2.40 2.60 4 12 0 4.00 5.70 -4 12 0 -0.90 2.10 -5 -12 0 -3.20 2.20 -5 -12 0 -5.40 3.90 5 -12 0 3.80 5.80 -5 12 0 8.20 4.80 -5 12 0 2.40 3.20 0 -13 0 1.10 3.70 0 13 0 -0.80 2.20 0 13 0 0.40 0.90 0 13 0 0.10 3.70 -1 -13 0 7.90 4.20 1 -13 0 2.80 3.40 1 13 0 0.70 5.20 -1 13 0 -2.00 3.50 1 13 0 2.40 2.70 -2 -13 0 14.80 6.00 -2 -13 0 15.00 5.00 2 -13 0 16.90 5.50 -2 13 0 29.80 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10.90 -4 8 12 13.70 4.60 -4 8 12 10.70 6.20 -3 -8 12 7.50 4.80 3 -8 -12 1.60 4.90 -3 8 12 10.30 5.00 -3 8 12 12.20 7.60 3 8 -12 13.10 9.20 2 -8 -12 192.48 14.80 -2 -8 12 193.78 15.30 -2 8 12 186.88 14.80 -2 8 12 179.68 14.40 2 8 -12 183.48 19.40 -1 -8 12 57.99 5.30 -1 -8 12 44.20 8.50 1 -8 -12 50.59 9.10 -1 -8 12 51.29 5.30 -1 8 12 45.40 9.60 1 8 -12 65.79 13.20 -1 8 12 49.80 9.10 0 -8 -12 24.30 6.40 0 -8 -12 25.90 6.90 0 -8 12 18.80 4.70 0 -8 12 22.00 5.30 0 8 12 14.90 7.30 0 8 -12 16.40 7.70 1 -8 12 2.40 3.10 1 -8 12 -0.30 2.00 -1 -8 -12 3.10 3.30 -1 -8 -12 3.60 3.50 1 8 12 -8.10 3.70 -1 8 -12 -1.10 4.20 -2 -8 -12 8.50 3.80 2 -8 12 -1.40 2.30 2 -8 12 1.50 3.00 -2 -8 -12 -0.10 2.20 -2 -8 -12 4.30 2.80 -2 8 -12 7.90 4.80 2 8 12 2.00 6.00 -3 -8 -12 4.90 3.10 3 -8 12 4.50 3.70 3 -8 12 0.70 2.10 -3 8 -12 11.10 4.30 3 8 12 -0.30 5.80 4 -8 12 0.80 4.70 -4 -8 -12 -1.40 3.90 4 -8 12 1.20 2.30 -4 8 -12 5.20 4.10 4 8 12 -3.60 7.70 5 -9 -12 -4.10 5.10 -5 -9 12 0.20 2.20 -5 9 12 7.40 4.30 -5 9 12 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3 19 15.80 5.90 0 3 -19 6.50 4.90 0 3 19 6.30 6.30 1 -3 19 -2.30 5.40 1 -3 19 -0.30 2.90 -1 -3 -19 1.50 3.40 1 3 19 -4.90 5.70 1 3 19 -4.70 2.80 -1 3 -19 -2.20 4.70 -3 -4 19 5.30 3.10 3 -4 -19 3.30 7.50 -3 4 19 9.90 5.20 3 4 -19 -8.90 5.20 -3 4 19 -0.70 3.10 -2 -4 19 -1.50 4.60 2 -4 -19 7.30 6.90 -2 4 19 0.80 3.30 2 4 -19 2.70 7.00 -2 4 19 -1.10 3.60 -1 -4 19 4.60 4.20 -1 -4 19 3.40 4.00 1 -4 -19 9.90 6.50 1 4 -19 0.30 5.90 -1 4 19 8.00 4.50 -1 4 19 3.00 4.30 0 -4 -19 11.60 6.40 0 -4 19 3.60 4.10 0 -4 19 4.20 4.10 0 4 19 11.00 5.50 0 4 -19 -6.30 4.40 0 4 19 8.80 4.20 2 -5 -19 27.80 9.50 -2 -5 19 24.10 5.70 2 5 -19 20.10 11.10 -2 5 19 15.40 4.90 -2 5 19 11.20 5.00 -1 -5 19 0.30 3.30 -1 -5 19 -7.40 3.50 1 -5 -19 11.30 7.40 1 5 -19 3.00 6.00 -1 5 19 5.00 5.20 -1 5 19 -2.30 4.90 0 -5 -19 12.30 5.70 0 -5 19 -3.60 4.10 0 -5 19 3.10 4.00 0 5 19 1.10 3.30 0 5 -19 8.50 7.20 0 5 19 3.20 5.80 -2 -6 19 5.10 4.80 2 -6 -19 3.40 4.80 2 6 -19 6.30 8.20 -2 6 19 13.20 6.60 -2 6 19 -1.40 4.90 1 -6 -19 10.50 5.10 -1 -6 19 -4.60 3.90 -1 -6 19 -8.70 2.90 1 6 -19 2.00 6.60 -1 6 19 7.30 4.90 -1 6 19 1.00 4.90 0 -6 -19 7.70 5.70 0 -6 19 -3.10 2.70 0 -6 19 -6.80 3.30 0 6 19 3.00 3.00 0 6 19 -2.10 4.90 0 6 -19 -4.80 5.00 -2 7 19 2.50 4.50 1 -7 -19 11.00 5.10 -1 -7 19 -2.70 3.00 -1 -7 19 -7.10 3.10 1 7 -19 -5.40 5.40 -1 7 19 6.40 3.50 -1 7 19 -2.30 5.70 -2 0 20 1.60 4.50 -2 0 20 -1.40 3.00 2 0 -20 6.70 8.50 -1 0 20 0.20 3.80 -1 0 20 -0.80 3.20 1 0 -20 1.10 6.00 -2 -1 20 2.50 3.20 -2 -1 20 7.00 5.40 2 -1 -20 5.90 7.60 -2 1 20 6.10 5.20 2 1 -20 11.00 9.60 -2 1 20 6.70 4.30 -1 -1 20 -5.50 4.20 -1 -1 20 -3.60 3.40 1 -1 -20 11.00 8.40 -1 1 20 -0.40 2.70 1 1 -20 4.60 7.40 -1 1 20 2.20 4.30 -1 -2 20 5.40 5.10 1 -2 -20 23.80 10.00 -1 -2 20 14.20 5.70 1 2 -20 21.60 9.20 -1 2 20 21.00 7.10 -1 2 20 13.00 3.80 -1 -3 20 7.30 5.50 1 -3 -20 20.60 8.10 -1 -3 20 8.00 5.90 1 3 -20 26.70 12.10 -1 3 20 3.60 4.70 -1 3 20 3.40 3.60 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 30938 _shelx_res_file ; TITL AQ19-RA in P2(1) shelx.res created by SHELXL-2018/3 at 17:11:20 on 12-Jul-2021 CELL 0.71073 5.5366 17.9208 16.2085 90.000 99.173 90.000 ZERR 4.00 0.0003 0.0008 0.0008 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O CL UNIT 64 56 8 4 8 MERG 2 OMIT 2 -4 16 OMIT 2 -10 15 OMIT -4 9 13 OMIT -5 5 5 OMIT 1 -18 2 OMIT -4 -10 4 OMIT 4 -10 8 OMIT 1 7 11 TWIN EADP C19 > C24 EADP C22 > C31 FMAP 2 PLAN 5 SIZE 0.097 0.190 0.240 ACTA BOND $H CONF L.S. 13 WGHT 0.048100 0.576700 BASF 0.10756 FVAR 0.53859 MOLE 1 CL1 5 -0.254228 0.436168 0.644386 11.00000 0.09442 0.07305 = 0.07637 -0.02386 0.02894 -0.01520 CL2 5 -0.448688 0.288159 0.615493 11.00000 0.07501 0.08083 = 0.06110 -0.00028 0.02122 -0.02619 O1 4 0.697369 0.634975 0.372713 11.00000 0.07972 0.05104 = 0.08760 -0.00495 0.04189 -0.01605 N1 3 -0.013476 0.411146 0.500331 11.00000 0.05601 0.04367 = 0.06226 -0.00008 0.01336 -0.00478 N2 3 0.090442 0.403420 0.437131 11.00000 0.05619 0.04016 = 0.05081 0.00064 0.00949 0.00186 C1 1 -0.274053 0.357535 0.583149 11.00000 0.05114 0.05287 = 0.05217 -0.00301 0.00766 -0.00733 C2 1 -0.160899 0.350140 0.515945 11.00000 0.04866 0.04615 = 0.05263 0.00339 0.01104 -0.00280 C3 1 0.240736 0.464126 0.423462 11.00000 0.05801 0.03435 = 0.05033 -0.00129 0.01631 -0.00808 C4 1 0.271701 0.528814 0.471250 11.00000 0.06868 0.04977 = 0.05714 -0.01193 0.03128 -0.01480 AFIX 43 H4A 2 0.188500 0.534413 0.516384 11.00000 -1.20000 AFIX 0 C5 1 0.422980 0.584113 0.452519 11.00000 0.08431 0.04761 = 0.06025 -0.01752 0.03076 -0.01379 AFIX 43 H5A 2 0.441835 0.627135 0.484996 11.00000 -1.20000 AFIX 0 C6 1 0.550443 0.576894 0.384889 11.00000 0.05310 0.04176 = 0.05428 0.00190 0.01610 0.00383 C7 1 0.519618 0.513823 0.336744 11.00000 0.05992 0.05111 = 0.05282 -0.00521 0.02379 0.00138 AFIX 43 H7A 2 0.602750 0.508512 0.291554 11.00000 -1.20000 AFIX 0 C8 1 0.363625 0.457673 0.355569 11.00000 0.06862 0.03948 = 0.05285 -0.00441 0.01824 -0.00456 AFIX 43 H8A 2 0.341397 0.415233 0.322199 11.00000 -1.20000 AFIX 0 C9 1 0.836215 0.630341 0.307459 11.00000 0.08279 0.07215 = 0.08037 0.01473 0.04109 -0.01037 AFIX 137 H9A 2 0.958880 0.668681 0.314241 11.00000 -1.50000 H9B 2 0.730904 0.636837 0.254871 11.00000 -1.50000 H9C 2 0.913688 0.582341 0.308698 11.00000 -1.50000 AFIX 0 C10 1 -0.194835 0.283296 0.461077 11.00000 0.04491 0.03614 = 0.05095 0.00135 0.01337 -0.00378 C11 1 -0.007134 0.232544 0.459864 11.00000 0.04154 0.05449 = 0.09394 -0.00221 0.00695 0.00282 AFIX 43 H11A 2 0.141146 0.239262 0.495082 11.00000 -1.20000 AFIX 0 C12 1 -0.039022 0.171862 0.406511 11.00000 0.06082 0.04480 = 0.09828 -0.00147 0.02149 0.00858 AFIX 43 H12A 2 0.087072 0.137412 0.407601 11.00000 -1.20000 AFIX 0 C13 1 -0.253267 0.161390 0.351880 11.00000 0.07319 0.04882 = 0.06225 -0.00215 0.02741 0.00214 C14 1 -0.440770 0.210957 0.354720 11.00000 0.06244 0.06512 = 0.04562 -0.00057 0.00841 -0.00387 AFIX 43 H14A 2 -0.589706 0.203698 0.320052 11.00000 -1.20000 AFIX 0 C15 1 -0.411904 0.271468 0.408241 11.00000 0.04291 0.04667 = 0.04937 0.00496 0.00691 0.00841 AFIX 43 H15A 2 -0.540900 0.304650 0.408564 11.00000 -1.20000 AFIX 0 C16 1 -0.285372 0.094550 0.292712 11.00000 0.12264 0.06175 = 0.09143 -0.02122 0.02689 -0.00109 AFIX 137 H16A 2 -0.140574 0.064261 0.302099 11.00000 -1.50000 H16B 2 -0.312419 0.111859 0.235935 11.00000 -1.50000 H16C 2 -0.423307 0.065509 0.302905 11.00000 -1.50000 AFIX 0 MOLE 2 CL3 5 0.760396 0.700819 -0.129060 11.00000 0.12491 0.07595 = 0.06831 0.02082 0.02717 0.00504 CL4 5 0.941646 0.551161 -0.103278 11.00000 0.09052 0.08576 = 0.06473 0.00258 0.03232 0.01998 O2 4 -0.205966 0.901797 0.128926 11.00000 0.08008 0.06127 = 0.08718 0.01011 0.03202 0.01704 N3 3 0.519991 0.676224 0.014671 11.00000 0.06507 0.04828 = 0.05378 0.00461 0.01884 0.00438 N4 3 0.423802 0.670623 0.078892 11.00000 0.06550 0.04800 = 0.05217 -0.00111 0.01285 0.00024 C17 1 0.777962 0.621680 -0.068249 11.00000 0.06273 0.05652 = 0.05218 0.00088 0.01126 0.00541 C18 1 0.665283 0.614655 -0.001225 11.00000 0.05711 0.04655 = 0.04942 -0.00757 0.00503 0.00252 AFIX 66 C19 1 0.269431 0.732100 0.090662 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 C20 1 0.155433 0.729055 0.161038 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 43 H20A 2 0.186090 0.689285 0.198089 11.00000 -1.20000 AFIX 65 C21 1 -0.004384 0.785450 0.176039 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 43 H21A 2 -0.080656 0.783412 0.223126 11.00000 -1.20000 AFIX 65 C22 1 -0.050205 0.844891 0.120664 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 C23 1 0.063791 0.847937 0.050287 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 43 H23A 2 0.033133 0.887707 0.013237 11.00000 -1.20000 AFIX 65 C24 1 0.223609 0.791542 0.035285 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 43 H24A 2 0.299880 0.793580 -0.011802 11.00000 -1.20000 AFIX 0 C25 1 -0.346519 0.900663 0.194871 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 137 H25A 2 -0.457475 0.942189 0.189000 11.00000 -1.50000 H25B 2 -0.239456 0.904082 0.247500 11.00000 -1.50000 H25C 2 -0.437714 0.854952 0.192725 11.00000 -1.50000 AFIX 66 C26 1 0.695354 0.546562 0.052466 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 C27 1 0.507607 0.494553 0.048511 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 43 H27A 2 0.361256 0.502241 0.012536 11.00000 -1.20000 AFIX 65 C28 1 0.538596 0.431054 0.098324 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 43 H28A 2 0.412980 0.396257 0.095678 11.00000 -1.20000 AFIX 65 C29 1 0.757334 0.419564 0.152092 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 C30 1 0.945084 0.471572 0.156048 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 43 H30A 2 1.091434 0.463884 0.192023 11.00000 -1.20000 AFIX 65 C31 1 0.914097 0.535071 0.106235 11.00000 0.07142 0.05563 = 0.06446 0.00270 0.01904 0.00295 AFIX 43 H31A 2 1.039714 0.569868 0.108882 11.00000 -1.20000 AFIX 0 C32 1 0.792213 0.349058 0.205453 11.00000 0.12039 0.06404 = 0.07904 0.00405 0.02970 0.00489 AFIX 137 H32A 2 0.926377 0.320655 0.190966 11.00000 -1.50000 H32B 2 0.645678 0.319578 0.195512 11.00000 -1.50000 H32C 2 0.826528 0.362584 0.263450 11.00000 -1.50000 AFIX 0 HKLF 4 REM AQ19-RA in P2(1) REM wR2 = 0.1449, GooF = S = 1.010, Restrained GooF = 1.010 for all data REM R1 = 0.0594 for 3820 Fo > 4sig(Fo) and 0.1113 for all 6444 data REM 288 parameters refined using 1 restraints END WGHT 0.0479 0.5788 REM Highest difference peak 0.370, deepest hole -0.316, 1-sigma level 0.044 Q1 1 0.6538 0.4249 0.1397 11.00000 0.05 0.23 Q2 1 0.9018 0.4304 0.1469 11.00000 0.05 0.21 Q3 1 0.8266 0.4694 0.1770 11.00000 0.05 0.21 Q4 1 0.5797 0.4954 0.0142 11.00000 0.05 0.19 Q5 1 1.0712 0.5931 -0.0820 11.00000 0.05 0.18 ; _shelx_res_checksum 45183 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl1 -0.2542(4) 0.43617(11) 0.64439(13) 0.0796(7) Uani d 1 . . Cl Cl2 -0.4487(3) 0.28816(11) 0.61549(11) 0.0712(6) Uani d 1 . . O O1 0.6974(9) 0.6350(3) 0.3727(3) 0.0697(14) Uani d 1 . . N N1 -0.0135(10) 0.4111(3) 0.5003(4) 0.0535(14) Uani d 1 . . N N2 0.0904(10) 0.4034(3) 0.4371(3) 0.0489(13) Uani d 1 . . C C1 -0.2741(12) 0.3575(4) 0.5831(4) 0.0521(16) Uani d 1 . . C C2 -0.1609(11) 0.3501(4) 0.5159(4) 0.0488(16) Uani d 1 . . C C3 0.2407(11) 0.4641(3) 0.4235(4) 0.0467(15) Uani d 1 . . C C4 0.2717(12) 0.5288(4) 0.4712(4) 0.0562(18) Uani d 1 . . H H4A 0.188500 0.534413 0.516384 0.067 Uiso calc 1 . . C C5 0.4230(14) 0.5841(4) 0.4525(4) 0.0620(19) Uani d 1 . . H H5A 0.441835 0.627135 0.484996 0.074 Uiso calc 1 . . C C6 0.5504(12) 0.5769(3) 0.3849(4) 0.0489(16) Uani d 1 . . C C7 0.5196(12) 0.5138(4) 0.3367(4) 0.0530(17) Uani d 1 . . H H7A 0.602750 0.508512 0.291554 0.064 Uiso calc 1 . . C C8 0.3636(12) 0.4577(4) 0.3556(4) 0.0527(17) Uani d 1 . . H H8A 0.341397 0.415233 0.322199 0.063 Uiso calc 1 . . C C9 0.8362(14) 0.6303(4) 0.3075(5) 0.075(2) Uani d 1 . . H H9A 0.958880 0.668681 0.314241 0.113 Uiso calc 1 . . H H9B 0.730904 0.636837 0.254871 0.113 Uiso calc 1 . . H H9C 0.913688 0.582341 0.308698 0.113 Uiso calc 1 . . C C10 -0.1948(11) 0.2833(3) 0.4611(4) 0.0434(14) Uani d 1 . . C C11 -0.0071(12) 0.2325(4) 0.4599(5) 0.064(2) Uani d 1 . . H H11A 0.141146 0.239262 0.495082 0.076 Uiso calc 1 . . C C12 -0.0390(14) 0.1719(4) 0.4065(5) 0.067(2) Uani d 1 . . H H12A 0.087072 0.137412 0.407601 0.080 Uiso calc 1 . . C C13 -0.2533(14) 0.1614(4) 0.3519(4) 0.0596(19) Uani d 1 . . C C14 -0.4408(13) 0.2110(4) 0.3547(4) 0.0577(18) Uani d 1 . . H H14A -0.589706 0.203698 0.320052 0.069 Uiso calc 1 . . C C15 -0.4119(11) 0.2715(3) 0.4082(4) 0.0464(15) Uani d 1 . . H H15A -0.540900 0.304650 0.408564 0.056 Uiso calc 1 . . C C16 -0.2854(17) 0.0945(5) 0.2927(5) 0.091(3) Uani d 1 . . H H16A -0.140574 0.064261 0.302099 0.136 Uiso calc 1 . . H H16B -0.312419 0.111859 0.235935 0.136 Uiso calc 1 . . H H16C -0.423307 0.065509 0.302905 0.136 Uiso calc 1 . . Cl Cl3 0.7604(5) 0.70082(12) -0.12906(13) 0.0884(8) Uani d 1 . . Cl Cl4 0.9416(4) 0.55116(12) -0.10328(12) 0.0782(7) Uani d 1 . . O O2 -0.2060(9) 0.9018(3) 0.1289(3) 0.0741(15) Uani d 1 . . N N3 0.5200(11) 0.6762(3) 0.0147(3) 0.0547(14) Uani d 1 . . N N4 0.4238(10) 0.6706(3) 0.0789(3) 0.0548(14) Uani d 1 . . C C17 0.7780(13) 0.6217(4) -0.0682(4) 0.0569(18) Uani d 1 . . C C18 0.6653(12) 0.6147(4) -0.0012(4) 0.0514(17) Uani d 1 . . C C19 0.2694(8) 0.7321(2) 0.0907(3) 0.0629(6) Uani d 1 . . C C20 0.1554(8) 0.7291(2) 0.1610(3) 0.0629(6) Uani d 1 . . H H20A 0.186090 0.689285 0.198089 0.076 Uiso calc 1 . . C C21 -0.0044(8) 0.7855(3) 0.1760(2) 0.0629(6) Uani d 1 . . H H21A -0.080656 0.783412 0.223126 0.076 Uiso calc 1 . . C C22 -0.0502(8) 0.8449(2) 0.1207(3) 0.0629(6) Uani d 1 . . C C23 0.0638(9) 0.8479(2) 0.0503(3) 0.0629(6) Uani d 1 . . H H23A 0.033133 0.887707 0.013237 0.076 Uiso calc 1 . . C C24 0.2236(8) 0.7915(2) 0.0353(2) 0.0629(6) Uani d 1 . . H H24A 0.299880 0.793580 -0.011802 0.076 Uiso calc 1 . . C C25 -0.3465(13) 0.9007(4) 0.1949(4) 0.0629(6) Uani d 1 . . H H25A -0.457475 0.942189 0.189000 0.094 Uiso calc 1 . . H H25B -0.239456 0.904082 0.247500 0.094 Uiso calc 1 . . H H25C -0.437714 0.854952 0.192725 0.094 Uiso calc 1 . . C C26 0.6954(9) 0.5466(2) 0.0525(3) 0.0629(6) Uani d 1 . . C C27 0.5076(7) 0.4946(2) 0.0485(3) 0.0629(6) Uani d 1 . . H H27A 0.361256 0.502241 0.012536 0.076 Uiso calc 1 . . C C28 0.5386(7) 0.4311(2) 0.0983(3) 0.0629(6) Uani d 1 . . H H28A 0.412980 0.396257 0.095678 0.076 Uiso calc 1 . . C C29 0.7573(8) 0.4196(2) 0.1521(3) 0.0629(6) Uani d 1 . . C C30 0.9451(7) 0.4716(3) 0.1560(3) 0.0629(6) Uani d 1 . . H H30A 1.091434 0.463884 0.192023 0.076 Uiso calc 1 . . C C31 0.9141(7) 0.5351(2) 0.1062(3) 0.0629(6) Uani d 1 . . H H31A 1.039714 0.569868 0.108882 0.076 Uiso calc 1 . . C C32 0.7922(16) 0.3491(4) 0.2055(5) 0.086(3) Uani d 1 . . H H32A 0.926377 0.320655 0.190966 0.129 Uiso calc 1 . . H H32B 0.645678 0.319578 0.195512 0.129 Uiso calc 1 . . H H32C 0.826528 0.362584 0.263450 0.129 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 0.0944(16) 0.0730(15) 0.0764(13) -0.0152(12) 0.0289(12) -0.0239(11) Cl2 0.0750(13) 0.0808(15) 0.0611(11) -0.0262(11) 0.0212(10) -0.0003(10) O1 0.080(4) 0.051(3) 0.088(4) -0.016(3) 0.042(3) -0.005(3) N1 0.056(4) 0.044(3) 0.062(3) -0.005(3) 0.013(3) 0.000(3) N2 0.056(3) 0.040(3) 0.051(3) 0.002(3) 0.009(3) 0.001(2) C1 0.051(4) 0.053(4) 0.052(4) -0.007(3) 0.008(3) -0.003(3) C2 0.049(4) 0.046(4) 0.053(4) -0.003(3) 0.011(3) 0.003(3) C3 0.058(4) 0.034(3) 0.050(4) -0.008(3) 0.016(3) -0.001(3) C4 0.069(5) 0.050(4) 0.057(4) -0.015(4) 0.031(4) -0.012(3) C5 0.084(5) 0.048(4) 0.060(4) -0.014(4) 0.031(4) -0.018(3) C6 0.053(4) 0.042(4) 0.054(4) 0.004(3) 0.016(3) 0.002(3) C7 0.060(4) 0.051(4) 0.053(4) 0.001(3) 0.024(3) -0.005(3) C8 0.069(4) 0.039(4) 0.053(4) -0.005(3) 0.018(3) -0.004(3) C9 0.083(6) 0.072(5) 0.080(5) -0.010(4) 0.041(5) 0.015(4) C10 0.045(3) 0.036(3) 0.051(3) -0.004(3) 0.013(3) 0.001(3) C11 0.042(4) 0.054(5) 0.094(6) 0.003(3) 0.007(4) -0.002(4) C12 0.061(5) 0.045(4) 0.098(6) 0.009(4) 0.021(4) -0.001(4) C13 0.073(5) 0.049(4) 0.062(4) 0.002(4) 0.027(4) -0.002(3) C14 0.062(5) 0.065(5) 0.046(4) -0.004(4) 0.008(3) -0.001(3) C15 0.043(4) 0.047(4) 0.049(3) 0.008(3) 0.007(3) 0.005(3) C16 0.123(8) 0.062(5) 0.091(6) -0.001(5) 0.027(6) -0.021(5) Cl3 0.125(2) 0.0759(16) 0.0683(13) 0.0050(13) 0.0272(13) 0.0208(11) Cl4 0.0905(17) 0.0858(16) 0.0647(12) 0.0200(12) 0.0323(11) 0.0026(11) O2 0.080(4) 0.061(3) 0.087(4) 0.017(3) 0.032(3) 0.010(3) N3 0.065(4) 0.048(4) 0.054(3) 0.004(3) 0.019(3) 0.005(3) N4 0.066(4) 0.048(3) 0.052(3) 0.000(3) 0.013(3) -0.001(3) C17 0.063(5) 0.057(4) 0.052(4) 0.005(4) 0.011(4) 0.001(3) C18 0.057(4) 0.047(4) 0.049(4) 0.003(3) 0.005(3) -0.008(3) C19 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C20 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C21 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C22 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C23 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C24 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C25 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C26 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C27 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C28 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C29 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C30 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C31 0.0714(16) 0.0556(14) 0.0645(13) 0.0030(11) 0.0190(11) 0.0027(10) C32 0.120(8) 0.064(6) 0.079(6) 0.005(5) 0.030(5) 0.004(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C6 O1 C9 . . 118.5(6) ? N2 N1 C2 . . 114.4(5) ? N1 N2 C3 . . 113.6(5) ? C2 C1 Cl2 . . 122.4(5) ? C2 C1 Cl1 . . 123.6(5) ? Cl2 C1 Cl1 . . 114.0(4) ? C1 C2 N1 . . 115.2(6) ? C1 C2 C10 . . 122.2(6) ? N1 C2 C10 . . 122.6(5) ? C8 C3 C4 . . 118.6(6) ? C8 C3 N2 . . 115.9(6) ? C4 C3 N2 . . 125.5(5) ? C5 C4 C3 . . 120.5(6) ? C5 C4 H4A . . 119.7 ? C3 C4 H4A . . 119.7 ? C4 C5 C6 . . 120.8(6) ? C4 C5 H5A . . 119.6 ? C6 C5 H5A . . 119.6 ? O1 C6 C7 . . 125.1(6) ? O1 C6 C5 . . 115.6(6) ? C7 C6 C5 . . 119.3(6) ? C6 C7 C8 . . 119.8(6) ? C6 C7 H7A . . 120.1 ? C8 C7 H7A . . 120.1 ? C3 C8 C7 . . 120.9(6) ? C3 C8 H8A . . 119.5 ? C7 C8 H8A . . 119.5 ? O1 C9 H9A . . 109.5 ? O1 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? O1 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C15 C10 C11 . . 118.2(6) ? C15 C10 C2 . . 120.7(6) ? C11 C10 C2 . . 121.0(6) ? C12 C11 C10 . . 120.3(7) ? C12 C11 H11A . . 119.9 ? C10 C11 H11A . . 119.9 ? C13 C12 C11 . . 121.4(7) ? C13 C12 H12A . . 119.3 ? C11 C12 H12A . . 119.3 ? C14 C13 C12 . . 118.0(7) ? C14 C13 C16 . . 121.0(7) ? C12 C13 C16 . . 120.9(7) ? C13 C14 C15 . . 121.1(7) ? C13 C14 H14A . . 119.5 ? C15 C14 H14A . . 119.5 ? C10 C15 C14 . . 120.9(6) ? C10 C15 H15A . . 119.6 ? C14 C15 H15A . . 119.6 ? C13 C16 H16A . . 109.5 ? C13 C16 H16B . . 109.5 ? H16A C16 H16B . . 109.5 ? C13 C16 H16C . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 109.5 ? C22 O2 C25 . . 119.8(5) ? N4 N3 C18 . . 114.9(5) ? N3 N4 C19 . . 113.2(5) ? C18 C17 Cl4 . . 122.7(6) ? C18 C17 Cl3 . . 123.4(6) ? Cl4 C17 Cl3 . . 113.9(4) ? C17 C18 N3 . . 115.2(6) ? C17 C18 C26 . . 121.7(6) ? N3 C18 C26 . . 123.1(5) ? C20 C19 C24 . . 120.0 ? C20 C19 N4 . . 116.1(4) ? C24 C19 N4 . . 123.9(4) ? C19 C20 C21 . . 120.0 ? C19 C20 H20A . . 120.0 ? C21 C20 H20A . . 120.0 ? C22 C21 C20 . . 120.0 ? C22 C21 H21A . . 120.0 ? C20 C21 H21A . . 120.0 ? O2 C22 C21 . . 124.5(4) ? O2 C22 C23 . . 115.5(4) ? C21 C22 C23 . . 120.0 ? C24 C23 C22 . . 120.0 ? C24 C23 H23A . . 120.0 ? C22 C23 H23A . . 120.0 ? C23 C24 C19 . . 120.0 ? C23 C24 H24A . . 120.0 ? C19 C24 H24A . . 120.0 ? O2 C25 H25A . . 109.5 ? O2 C25 H25B . . 109.5 ? H25A C25 H25B . . 109.5 ? O2 C25 H25C . . 109.5 ? H25A C25 H25C . . 109.5 ? H25B C25 H25C . . 109.5 ? C27 C26 C31 . . 120.0 ? C27 C26 C18 . . 120.5(4) ? C31 C26 C18 . . 119.5(4) ? C28 C27 C26 . . 120.0 ? C28 C27 H27A . . 120.0 ? C26 C27 H27A . . 120.0 ? C27 C28 C29 . . 120.0 ? C27 C28 H28A . . 120.0 ? C29 C28 H28A . . 120.0 ? C30 C29 C28 . . 120.0 ? C30 C29 C32 . . 120.2(5) ? C28 C29 C32 . . 119.8(5) ? C29 C30 C31 . . 120.0 ? C29 C30 H30A . . 120.0 ? C31 C30 H30A . . 120.0 ? C30 C31 C26 . . 120.0 ? C30 C31 H31A . . 120.0 ? C26 C31 H31A . . 120.0 ? C29 C32 H32A . . 109.5 ? C29 C32 H32B . . 109.5 ? H32A C32 H32B . . 109.5 ? C29 C32 H32C . . 109.5 ? H32A C32 H32C . . 109.5 ? H32B C32 H32C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C1 . 1.717(7) ? Cl2 C1 . 1.708(7) ? O1 C6 . 1.355(7) ? O1 C9 . 1.406(8) ? N1 N2 . 1.260(7) ? N1 C2 . 1.411(8) ? N2 C3 . 1.408(7) ? C1 C2 . 1.347(9) ? C2 C10 . 1.486(8) ? C3 C8 . 1.388(8) ? C3 C4 . 1.390(8) ? C4 C5 . 1.363(9) ? C4 H4A . 0.9300 ? C5 C6 . 1.401(9) ? C5 H5A . 0.9300 ? C6 C7 . 1.369(8) ? C7 C8 . 1.391(8) ? C7 H7A . 0.9300 ? C8 H8A . 0.9300 ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? C10 C15 . 1.376(8) ? C10 C11 . 1.384(8) ? C11 C12 . 1.383(9) ? C11 H11A . 0.9300 ? C12 C13 . 1.375(10) ? C12 H12A . 0.9300 ? C13 C14 . 1.373(9) ? C13 C16 . 1.527(10) ? C14 C15 . 1.382(8) ? C14 H14A . 0.9300 ? C15 H15A . 0.9300 ? C16 H16A . 0.9600 ? C16 H16B . 0.9600 ? C16 H16C . 0.9600 ? Cl3 C17 . 1.721(7) ? Cl4 C17 . 1.704(7) ? O2 C22 . 1.356(5) ? O2 C25 . 1.419(8) ? N3 N4 . 1.247(7) ? N3 C18 . 1.413(8) ? N4 C19 . 1.426(6) ? C17 C18 . 1.342(9) ? C18 C26 . 1.493(7) ? C19 C20 . 1.3900 ? C19 C24 . 1.3900 ? C20 C21 . 1.3900 ? C20 H20A . 0.9300 ? C21 C22 . 1.3900 ? C21 H21A . 0.9300 ? C22 C23 . 1.3900 ? C23 C24 . 1.3900 ? C23 H23A . 0.9300 ? C24 H24A . 0.9300 ? C25 H25A . 0.9600 ? C25 H25B . 0.9600 ? C25 H25C . 0.9600 ? C26 C27 . 1.3900 ? C26 C31 . 1.3900 ? C27 C28 . 1.3900 ? C27 H27A . 0.9300 ? C28 C29 . 1.3900 ? C28 H28A . 0.9300 ? C29 C30 . 1.3900 ? C29 C32 . 1.526(8) ? C30 C31 . 1.3900 ? C30 H30A . 0.9300 ? C31 H31A . 0.9300 ? C32 H32A . 0.9600 ? C32 H32B . 0.9600 ? C32 H32C . 0.9600 ? 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 C5 H5A Cg2 2_556 0.93 2.84 3.645(8) 146 yes C23 H23A Cg4 2_655 0.93 3.00 3.775(5) 142 yes C25 H25C Cg3 1_455 0.96 2.93 3.717(7) 140 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 C2 N1 N2 C3 . . . . -178.8(5) ? Cl2 C1 C2 N1 . . . . -176.8(5) ? Cl1 C1 C2 N1 . . . . 2.5(9) ? Cl2 C1 C2 C10 . . . . 4.8(9) ? Cl1 C1 C2 C10 . . . . -175.9(5) ? N2 N1 C2 C1 . . . . -179.8(6) ? N2 N1 C2 C10 . . . . -1.4(9) ? N1 N2 C3 C8 . . . . 178.7(6) ? N1 N2 C3 C4 . . . . -2.2(9) ? C8 C3 C4 C5 . . . . -1.1(11) ? N2 C3 C4 C5 . . . . 179.7(7) ? C3 C4 C5 C6 . . . . -0.1(11) ? C9 O1 C6 C7 . . . . -2.0(10) ? C9 O1 C6 C5 . . . . 178.1(6) ? C4 C5 C6 O1 . . . . -179.3(7) ? C4 C5 C6 C7 . . . . 0.8(11) ? O1 C6 C7 C8 . . . . 179.9(6) ? C5 C6 C7 C8 . . . . -0.3(10) ? C4 C3 C8 C7 . . . . 1.6(10) ? N2 C3 C8 C7 . . . . -179.2(6) ? C6 C7 C8 C3 . . . . -0.9(10) ? C1 C2 C10 C15 . . . . 71.9(8) ? N1 C2 C10 C15 . . . . -106.4(7) ? C1 C2 C10 C11 . . . . -110.1(7) ? N1 C2 C10 C11 . . . . 71.6(8) ? C15 C10 C11 C12 . . . . 0.2(10) ? C2 C10 C11 C12 . . . . -177.9(6) ? C10 C11 C12 C13 . . . . 1.9(11) ? C11 C12 C13 C14 . . . . -3.4(11) ? C11 C12 C13 C16 . . . . 179.4(7) ? C12 C13 C14 C15 . . . . 2.8(10) ? C16 C13 C14 C15 . . . . 180.0(6) ? C11 C10 C15 C14 . . . . -0.7(9) ? C2 C10 C15 C14 . . . . 177.4(5) ? C13 C14 C15 C10 . . . . -0.8(10) ? C18 N3 N4 C19 . . . . -177.2(5) ? Cl4 C17 C18 N3 . . . . -174.6(5) ? Cl3 C17 C18 N3 . . . . 2.6(9) ? Cl4 C17 C18 C26 . . . . 6.0(10) ? Cl3 C17 C18 C26 . . . . -176.8(5) ? N4 N3 C18 C17 . . . . -177.2(6) ? N4 N3 C18 C26 . . . . 2.2(9) ? N3 N4 C19 C20 . . . . 179.7(4) ? N3 N4 C19 C24 . . . . 1.8(7) ? C24 C19 C20 C21 . . . . 0.0 ? N4 C19 C20 C21 . . . . -178.0(5) ? C19 C20 C21 C22 . . . . 0.0 ? C25 O2 C22 C21 . . . . -4.0(8) ? C25 O2 C22 C23 . . . . 174.8(5) ? C20 C21 C22 O2 . . . . 178.8(5) ? C20 C21 C22 C23 . . . . 0.0 ? O2 C22 C23 C24 . . . . -178.9(5) ? C21 C22 C23 C24 . . . . 0.0 ? C22 C23 C24 C19 . . . . 0.0 ? C20 C19 C24 C23 . . . . 0.0 ? N4 C19 C24 C23 . . . . 177.8(5) ? C17 C18 C26 C27 . . . . -105.8(6) ? N3 C18 C26 C27 . . . . 74.8(7) ? C17 C18 C26 C31 . . . . 73.7(7) ? N3 C18 C26 C31 . . . . -105.7(6) ? C31 C26 C27 C28 . . . . 0.0 ? C18 C26 C27 C28 . . . . 179.5(5) ? C26 C27 C28 C29 . . . . 0.0 ? C27 C28 C29 C30 . . . . 0.0 ? C27 C28 C29 C32 . . . . -178.9(5) ? C28 C29 C30 C31 . . . . 0.0 ? C32 C29 C30 C31 . . . . 178.9(5) ? C29 C30 C31 C26 . . . . 0.0 ? C27 C26 C31 C30 . . . . 0.0 ? C18 C26 C31 C30 . . . . -179.5(5) ? _cod_database_fobs_code 2243907