#------------------------------------------------------------------------------ #$Date: 2023-08-31 05:02:10 +0300 (Thu, 31 Aug 2023) $ #$Revision: 285925 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022850.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_2022850 loop_ _publ_author_name 'Akkurt, Mehmet' 'Naghiyev, Farid N.' 'Khrustalev, Victor N.' 'Asadov, Khammed A.' 'Khalilov, Ali N.' 'Bhattarai, Ajaya' 'Mamedov, \.Ibrahim G.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of (2E)-1-(4-bromophenyl)-3-(2-methylphenyl)prop-2-en-1-one ; _journal_coeditor_code TX2073 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 847 _journal_page_last 851 _journal_paper_doi 10.1107/S2056989023007387 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C16 H13 Br O' _chemical_formula_moiety 'C16 H13 Br O' _chemical_formula_sum 'C16 H13 Br O' _chemical_formula_weight 301.17 _chemical_name_systematic ; (2E)-1-(4-Bromophenyl)-3-(2-methylphenyl)prop-2-en-1-one ; _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.942 _cell_length_b 11.5915(2) _cell_length_c 28.0387(4) _cell_measurement_reflns_used 12560 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 76.868 _cell_measurement_theta_min 3.795 _cell_volume 1281.19(3) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2022) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2022) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2022) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_unetI/netI 0.0156 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 14537 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.111 _diffrn_reflns_theta_min 3.152 _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 4.231 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.251 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2022) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.561 _exptl_crystal_description needle _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.070 _refine_diff_density_max 0.511 _refine_diff_density_min -0.418 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.53(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 165 _refine_ls_number_reflns 2657 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.143 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0215 _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^)+(0.0121P)^2^+1.3924P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0524 _reflns_number_gt 2627 _reflns_number_total 2657 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tx2073sup1.cif _cod_data_source_block I _cod_database_code 2022850 _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 0.319 _shelx_estimated_absorpt_t_max 0.756 _shelx_hkl_file ; 0 0 -2 9.73 0.99 0 0 -3 0.20 0.71 0 0 -4 1747.42 31.22 0 0 -5 0.68 1.17 0 0 -6 5604.40 92.70 0 0 -7 2.11 1.55 0 0 -8 3317.01 60.02 0 0 -9 -0.21 1.76 0 0 9 0.21 1.66 0 0 10 2282.84 45.85 0 0 11 3.66 2.03 0 0 12 2849.28 57.41 0 0 13 0.98 1.95 0 0 14 672.63 22.79 0 0 15 -0.40 2.51 0 0 16 4251.68 85.75 0 0 17 0.97 2.39 0 0 -17 1.18 1.25 0 0 18 1006.31 33.67 0 0 -18 996.60 20.78 0 0 -19 8.47 1.90 0 0 19 4.02 3.37 0 0 -20 16.19 2.43 0 0 20 18.66 5.28 0 0 -21 1.17 1.74 0 0 21 -0.67 3.30 0 0 -21 1.46 2.07 0 0 -22 513.06 14.16 0 0 22 523.21 26.58 0 0 22 514.89 26.35 0 0 -22 516.12 13.76 0 0 -23 0.16 1.90 0 0 23 0.75 3.58 0 0 -23 1.17 2.26 0 0 23 3.38 3.86 0 0 -24 165.44 7.35 0 0 24 163.65 14.85 0 0 -24 187.09 8.00 0 0 -25 0.34 2.02 0 0 -25 -0.15 2.74 0 0 -26 813.45 19.60 0 0 -26 748.66 18.57 0 0 -27 0.30 2.36 0 0 -27 0.84 1.94 0 0 -28 103.08 5.82 0 0 -29 1.06 1.99 0 0 -30 166.40 6.94 0 0 -31 0.12 1.56 0 0 -32 213.55 7.18 0 -1 0 22.56 1.36 0 -1 -1 88.42 3.24 0 -1 -1 88.83 2.88 0 -1 -2 1235.28 22.44 0 -1 -3 14.30 1.72 0 -1 -4 45.22 3.10 0 -1 -5 414.82 11.45 0 -1 -6 220.36 8.30 0 -1 -7 97.77 5.78 0 -1 -8 5318.47 91.95 0 1 8 5381.60 91.52 0 -1 8 5355.63 91.38 0 1 9 35.80 3.90 0 -1 9 38.23 3.97 0 -1 -9 36.47 4.13 0 1 10 2721.98 53.29 0 -1 10 2715.30 53.19 0 -1 -10 2720.75 53.91 0 1 11 256.82 11.71 0 -1 11 249.64 11.45 0 -1 -11 250.14 11.79 0 -1 12 86.62 6.98 0 1 12 88.42 7.15 0 -1 -12 75.52 6.78 0 -1 13 468.81 17.84 0 1 13 457.91 17.78 0 -1 -13 448.72 17.96 0 1 14 4665.92 89.68 0 -1 14 4675.23 89.56 0 -1 -14 4715.03 90.61 0 -1 15 902.09 28.39 0 1 15 856.67 27.99 0 -1 -15 881.09 28.70 0 -1 16 551.03 22.24 0 1 16 574.63 22.80 0 1 -17 47.15 3.27 0 -1 17 50.40 6.86 0 1 17 46.47 6.81 0 1 -18 620.63 14.81 0 -1 -18 618.63 14.78 0 1 18 671.31 26.61 0 -1 18 681.60 26.76 0 1 -19 106.92 5.28 0 -1 -19 105.29 5.27 0 1 19 113.87 11.09 0 -1 19 121.63 11.44 0 -1 -20 2331.78 42.63 0 1 -20 2319.25 42.62 0 -1 20 2427.16 62.16 0 1 20 2385.71 61.94 0 1 -21 20.18 5.04 0 -1 -21 27.71 5.94 0 -1 -21 21.14 2.89 0 1 -21 19.95 2.86 0 -1 21 20.71 5.98 0 1 21 30.34 6.34 0 1 -21 23.04 2.96 0 -1 -21 22.11 3.05 0 1 22 618.87 30.34 0 -1 22 589.03 29.37 0 1 22 695.62 31.03 0 -1 22 687.63 30.61 0 1 -22 698.42 16.99 0 -1 -22 692.38 16.96 0 1 -22 594.96 27.39 0 -1 -22 591.70 27.95 0 1 -22 648.25 16.00 0 -1 -22 646.75 16.20 0 -1 -23 35.50 3.89 0 -1 -23 44.04 7.59 0 1 -23 27.76 6.23 0 1 23 39.14 7.63 0 -1 23 22.34 6.01 0 1 -23 33.10 3.70 0 -1 -23 39.23 3.77 0 1 23 30.14 6.96 0 -1 23 30.57 7.21 0 1 -23 35.83 3.52 0 1 -23 28.09 3.54 0 -1 -23 39.62 3.60 0 1 -24 691.29 30.77 0 -1 -24 696.82 30.63 0 1 24 671.66 31.62 0 -1 24 659.70 31.53 0 -1 -24 695.59 17.28 0 1 -24 716.91 17.25 0 -1 -24 705.03 17.53 0 1 -24 706.91 17.33 0 -1 24 696.19 32.51 0 1 -24 753.77 18.37 0 -1 -24 736.47 18.21 0 1 -25 176.77 7.67 0 -1 -25 170.39 7.67 0 1 -25 184.26 8.08 0 -1 -25 182.01 8.05 0 -1 -25 181.72 7.58 0 1 -25 182.80 7.73 0 1 -26 3108.56 56.10 0 1 -26 3213.02 57.38 0 -1 -26 3191.08 57.20 0 -1 -26 3203.98 56.42 0 1 -27 45.94 4.21 0 -1 -27 56.65 4.62 0 1 -27 54.99 4.46 0 -1 -27 60.79 4.49 0 1 -28 513.54 13.80 0 1 28 499.68 13.08 0 -1 -28 517.87 14.38 0 1 -28 541.08 14.60 0 -1 -28 520.55 14.05 0 1 -29 65.37 4.57 0 -1 -29 67.53 4.61 0 1 -29 72.49 4.77 0 -1 -29 67.26 4.62 0 1 29 67.64 4.07 0 1 -30 357.47 9.71 0 -1 -30 372.63 10.83 0 -1 -30 389.86 11.23 0 1 -30 379.62 11.14 0 -1 -31 2.92 1.97 0 -1 -31 1.09 1.59 0 1 -31 2.22 1.64 0 -1 -32 824.38 17.30 0 1 -32 831.97 17.30 0 -1 -32 810.32 17.43 0 -1 -33 3.14 1.70 0 1 -33 1.72 1.63 0 -1 -33 2.36 1.31 0 -1 -34 10.46 1.79 0 1 -34 9.56 1.67 0 1 -35 8.01 1.26 0 -1 -35 8.70 1.27 0 -2 0 6547.83 107.51 0 -2 0 6788.37 106.12 0 -2 -1 5265.26 87.16 0 -2 1 5212.82 85.62 0 -2 -2 2655.97 46.79 0 -2 -2 2695.78 45.29 0 -2 -3 194.57 7.23 0 -2 -3 187.40 6.32 0 -2 -4 3307.56 57.91 0 -2 -5 33.62 3.40 0 -2 -6 2312.11 44.25 0 -2 -7 244.65 10.12 0 -2 7 252.14 9.81 0 2 7 263.92 10.16 0 -2 -8 60.96 5.25 0 2 8 61.47 5.10 0 -2 8 63.45 5.03 0 -2 -9 370.43 14.05 0 -2 9 394.20 13.87 0 2 9 373.65 13.74 0 -2 -10 1820.94 41.18 0 2 10 1894.81 40.91 0 -2 10 1881.30 40.67 0 -2 -11 913.57 26.50 0 -2 11 971.40 26.35 0 2 11 959.18 26.40 0 -2 12 5147.10 94.54 0 2 12 5115.60 94.65 0 -2 -12 5095.46 95.36 0 -2 13 113.93 8.77 0 2 13 123.09 9.15 0 -2 -13 114.79 9.02 0 -2 14 1048.74 30.82 0 2 14 1060.55 31.20 0 -2 -14 1003.97 31.06 0 2 -15 859.27 17.86 0 2 15 891.93 29.02 0 -2 15 861.42 28.49 0 -2 -15 908.75 29.67 0 2 -16 2122.70 38.25 0 2 16 2224.93 53.74 0 -2 16 2218.91 53.27 0 -2 -16 2175.23 53.87 0 2 -17 6.51 1.72 0 -2 17 2.53 2.82 0 2 17 8.82 3.63 0 -2 -17 4.26 3.12 0 2 18 1802.47 49.40 0 -2 18 1804.78 49.08 0 2 -18 1808.75 33.12 0 -2 -18 1702.62 32.91 0 -2 19 314.18 18.56 0 2 19 287.52 18.10 0 -2 -19 290.60 9.38 0 2 -19 305.18 9.52 0 -2 -20 76.23 4.71 0 -2 -20 75.25 4.64 0 2 -20 75.36 4.69 0 2 20 67.81 9.26 0 -2 20 82.94 9.87 0 -2 -20 66.27 8.12 0 2 -20 66.85 8.03 0 2 21 229.59 17.04 0 -2 21 236.27 17.43 0 -2 -21 248.05 8.90 0 2 -21 250.00 8.58 0 2 -21 269.12 9.28 0 -2 -21 265.64 9.23 0 -2 21 273.88 18.51 0 2 21 290.02 19.13 0 2 -21 244.15 15.83 0 -2 -21 256.22 16.25 0 -2 -22 2206.10 59.39 0 2 -22 2103.37 58.39 0 -2 22 2083.53 60.73 0 2 22 2186.00 61.86 0 -2 -22 2290.42 42.14 0 2 -22 2286.96 41.57 0 2 -22 2256.79 42.62 0 -2 -22 2301.13 42.57 0 -2 22 2296.33 63.20 0 2 22 2303.43 63.78 0 2 -22 2321.19 41.28 0 -2 -22 2282.22 41.27 0 2 -23 104.72 11.61 0 -2 -23 91.52 11.21 0 2 23 89.96 11.46 0 -2 23 95.72 11.54 0 2 -23 99.57 5.59 0 -2 -23 106.00 5.93 0 2 -23 110.20 6.08 0 -2 23 110.03 12.27 0 -2 -23 107.82 5.58 0 2 -23 115.23 5.72 0 -2 -24 58.70 9.25 0 2 -24 59.90 9.26 0 -2 24 51.74 8.89 0 2 24 57.92 9.35 0 -2 -24 64.44 4.54 0 2 -24 54.50 4.37 0 2 -24 63.67 4.59 0 -2 24 70.53 10.08 0 -2 -24 58.42 4.56 0 2 -24 59.17 4.65 0 2 -25 260.05 9.22 0 2 -25 263.17 9.68 0 -2 -25 268.27 9.79 0 -2 -25 251.04 9.23 0 2 -25 255.88 9.28 0 2 26 3.90 2.06 0 -2 -26 6.18 2.39 0 2 -26 5.25 2.20 0 -2 -26 6.55 2.47 0 2 -26 4.87 2.35 0 2 -26 4.21 2.51 0 2 -27 65.10 4.66 0 2 27 62.35 4.28 0 -2 -27 64.58 4.66 0 2 -27 59.91 4.61 0 -2 -27 61.58 4.62 0 2 -27 65.82 4.70 0 2 -28 490.52 13.25 0 2 -28 516.04 13.59 0 -2 -28 505.09 13.54 0 -2 -28 491.46 13.80 0 2 -28 502.51 14.03 0 2 28 473.90 12.69 0 2 -29 11.98 2.65 0 2 -29 14.71 2.76 0 -2 -29 17.22 2.88 0 2 29 12.76 2.26 0 2 -29 8.88 2.32 0 -2 -29 14.37 2.60 0 2 -30 450.30 11.85 0 -2 -30 450.46 11.81 0 2 -30 424.45 11.45 0 2 -30 430.26 11.17 0 -2 -30 438.57 12.08 0 2 -31 215.26 6.88 0 2 -31 215.97 7.31 0 -2 -31 224.65 7.44 0 -2 -31 227.20 7.65 0 2 -32 110.11 4.37 0 -2 -32 113.81 4.83 0 2 -32 107.74 4.74 0 -2 -32 108.86 4.82 0 2 -33 101.28 4.19 0 -2 -33 108.21 4.33 0 -2 -33 106.51 4.34 0 -2 -34 417.21 9.14 0 -3 0 6.01 1.72 0 -3 0 0.17 1.37 0 -3 -1 2408.17 45.12 0 -3 -1 2437.88 42.80 0 -3 1 2391.40 42.88 0 -3 2 3512.60 58.87 0 3 2 4126.22 59.18 0 -3 2 3768.77 64.01 0 -3 -2 3741.25 63.75 0 -3 -2 3713.48 66.24 0 -3 -2 4187.01 59.35 0 3 -2 3437.81 58.86 0 -3 -3 100.08 5.94 0 -3 -3 95.14 4.99 0 -3 -4 2244.31 43.82 0 -3 -4 2260.56 41.53 0 -3 -5 1820.74 37.65 0 -3 -6 2.27 1.83 0 -3 -7 2097.88 43.55 0 3 7 2096.30 43.16 0 -3 7 2105.91 42.74 0 3 8 2460.67 49.63 0 -3 8 2446.93 49.01 0 -3 -8 2444.41 50.04 0 -3 9 719.34 20.99 0 3 9 685.32 21.09 0 -3 -9 711.57 21.69 0 3 10 1801.84 41.11 0 -3 10 1806.33 40.58 0 -3 -10 1776.05 41.51 0 3 11 435.10 17.07 0 -3 11 434.44 16.84 0 -3 -11 401.61 16.82 0 -3 12 221.76 12.16 0 3 12 218.80 12.31 0 -3 -12 223.46 12.77 0 3 13 627.47 22.79 0 -3 13 645.18 22.74 0 3 -13 611.21 13.51 0 -3 -13 620.89 23.13 0 -3 14 1053.10 31.76 0 3 14 1055.84 32.10 0 3 -14 1011.43 20.30 0 -3 -14 1011.77 32.03 0 -3 15 192.55 12.83 0 3 15 219.37 13.83 0 3 -15 200.00 6.83 0 -3 -15 214.85 13.93 0 -3 16 841.23 29.51 0 3 16 820.54 29.64 0 3 -16 813.91 17.73 0 -3 -16 824.62 30.06 0 3 17 1841.86 50.21 0 -3 17 1837.88 49.58 0 3 -17 1830.91 34.12 0 -3 -17 1834.38 50.55 0 -3 -18 51.87 7.93 0 3 18 53.35 7.91 0 -3 18 49.27 7.61 0 -3 -18 54.92 3.84 0 3 -18 47.81 3.73 0 3 -18 44.16 6.15 0 -3 -19 107.21 11.31 0 -3 19 96.43 10.24 0 -3 -19 94.28 5.15 0 3 -19 97.13 5.19 0 3 19 101.22 10.94 0 -3 19 85.01 9.93 0 -3 -19 93.42 9.20 0 3 -19 86.37 8.70 0 3 20 846.18 33.05 0 -3 20 898.53 33.63 0 -3 20 903.86 19.69 0 3 -20 887.11 19.38 0 3 -20 916.97 20.52 0 -3 -20 911.35 20.40 0 3 20 948.12 35.89 0 -3 20 955.66 35.53 0 -3 -20 936.55 32.34 0 3 -20 837.76 30.57 0 -3 -21 173.86 13.58 0 3 -21 178.31 13.80 0 -3 21 190.37 15.59 0 3 21 190.21 15.26 0 -3 21 197.86 7.59 0 3 -21 190.68 7.43 0 3 -21 197.38 8.00 0 -3 -21 193.56 7.91 0 3 21 232.14 17.29 0 -3 21 200.79 15.92 0 3 -21 196.54 7.25 0 -3 -21 202.85 7.38 0 -3 -22 292.56 18.85 0 3 -22 258.00 17.65 0 -3 22 237.28 18.35 0 3 22 258.59 19.04 0 3 -22 285.78 9.50 0 3 -22 315.78 10.47 0 -3 -22 302.04 10.22 0 -3 22 279.03 19.46 0 3 -22 290.91 9.31 0 -3 -22 321.57 9.65 0 3 23 189.77 7.65 0 3 -23 169.62 14.58 0 -3 -23 166.72 14.76 0 3 23 184.97 15.75 0 -3 23 163.84 14.69 0 3 -23 190.07 7.45 0 -3 -23 209.94 7.79 0 -3 23 191.88 16.25 0 3 -23 197.56 7.75 0 -3 -23 198.73 8.19 0 3 -23 197.20 8.24 0 3 -24 969.43 21.53 0 3 24 967.33 21.66 0 -3 -24 997.09 22.52 0 3 -24 1000.70 22.68 0 3 -24 988.85 21.53 0 -3 -24 991.65 21.79 0 3 -25 211.46 8.18 0 3 25 212.61 8.16 0 3 -25 226.03 8.91 0 -3 -25 215.33 8.67 0 3 -25 213.82 8.19 0 -3 -25 224.47 8.36 0 3 -26 121.56 6.06 0 3 26 127.58 6.10 0 -3 -26 123.52 6.40 0 -3 -26 118.52 6.08 0 3 -26 128.77 6.22 0 3 -27 260.72 9.00 0 3 27 252.26 8.77 0 -3 -27 260.55 9.40 0 3 -27 267.91 9.12 0 -3 -27 267.07 9.15 0 3 -28 231.49 8.23 0 3 28 233.54 8.10 0 -3 -28 229.99 8.66 0 3 -28 253.00 8.53 0 -3 -28 242.50 8.41 0 3 -29 425.97 11.45 0 3 -29 432.86 11.52 0 -3 -29 425.40 11.53 0 3 29 409.71 11.06 0 -3 -29 429.30 12.07 0 -3 -30 348.44 10.13 0 3 -30 321.65 9.41 0 3 -30 341.01 9.61 0 3 -30 332.68 9.52 0 -3 -30 346.91 9.70 0 3 -31 2.40 1.98 0 -3 -31 2.94 1.60 0 -3 -31 0.75 1.80 0 3 -32 382.28 9.25 0 -3 -32 384.52 9.81 0 -3 -32 387.85 9.46 0 -3 -33 208.86 5.83 0 3 -33 204.36 5.61 0 -4 0 2166.61 44.33 0 -4 0 2209.44 41.40 0 -4 -1 894.12 23.14 0 -4 1 887.07 23.04 0 -4 1 892.22 20.65 0 -4 -1 849.26 20.22 0 -4 2 16.37 2.75 0 -4 -2 23.31 3.02 0 -4 -2 17.63 3.16 0 -4 -3 3722.34 63.51 0 -4 -3 3790.28 59.75 0 -4 3 3792.48 60.10 0 -4 -4 109.57 7.32 0 -4 4 99.40 3.71 0 4 4 111.74 3.93 0 4 -4 104.02 3.78 0 -4 4 97.73 6.03 0 -4 -4 99.13 5.98 0 -4 -5 284.73 12.43 0 4 -5 285.66 7.96 0 -4 -5 318.46 8.39 0 4 5 291.41 8.30 0 -4 5 297.64 8.15 0 4 -6 1042.77 21.05 0 -4 -6 1082.93 28.06 0 -4 -7 827.24 24.23 0 -4 8 816.58 23.75 0 -4 -8 795.89 24.20 0 -4 9 2403.13 51.15 0 -4 -9 2385.78 52.20 0 -4 10 2880.64 59.47 0 -4 -10 2821.97 60.47 0 -4 11 210.99 11.96 0 -4 -11 213.04 12.55 0 4 12 240.39 13.68 0 -4 12 253.32 13.62 0 -4 -12 233.73 13.66 0 -4 13 609.70 23.04 0 4 13 617.59 23.60 0 4 -13 607.58 13.84 0 -4 -13 616.03 23.97 0 4 -14 8.07 1.71 0 -4 14 13.41 3.92 0 4 14 7.25 3.33 0 -4 -14 10.35 3.56 0 4 -14 6.65 2.59 0 -4 15 1327.29 38.76 0 4 15 1334.79 39.56 0 -4 -15 1269.59 33.83 0 -4 -15 1309.93 39.73 0 4 -15 1320.71 25.46 0 -4 16 1336.00 39.98 0 4 16 1254.76 39.63 0 4 -16 1194.53 33.60 0 -4 -16 1288.01 34.81 0 -4 -16 1235.29 39.75 0 -4 16 1252.60 36.50 0 4 -16 1295.60 25.51 0 4 17 147.98 12.81 0 -4 17 157.32 12.83 0 4 -17 130.64 10.12 0 -4 -17 148.08 10.68 0 4 17 157.48 11.68 0 -4 -17 148.94 12.94 0 -4 17 146.50 11.27 0 4 -17 145.59 6.34 0 4 -18 266.56 9.00 0 -4 -18 258.56 8.80 0 4 18 281.54 18.14 0 -4 18 245.97 16.74 0 4 -18 232.91 14.32 0 -4 -18 248.13 14.72 0 -4 18 252.89 15.47 0 -4 -18 274.91 17.95 0 4 18 271.29 15.78 0 4 19 1202.71 37.19 0 -4 -19 1165.01 40.52 0 -4 19 1112.96 36.16 0 4 -19 1133.74 23.93 0 -4 -19 1117.45 23.69 0 4 19 1095.02 23.06 0 4 19 1127.15 39.82 0 -4 19 1138.11 39.20 0 -4 -19 1126.52 35.70 0 4 -19 1008.04 34.09 0 4 -19 1082.48 22.56 0 -4 19 1123.27 22.89 0 -4 20 8.10 4.05 0 4 20 3.23 2.01 0 4 -20 6.16 3.53 0 -4 -20 8.86 3.83 0 -4 -20 6.14 2.14 0 4 -20 5.03 2.11 0 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22.92 3.27 0 12 5 58.88 4.73 0 12 6 730.56 17.43 0 12 -6 755.81 17.58 0 -12 -6 808.42 17.58 0 12 6 830.76 18.51 0 12 6 817.04 19.20 0 12 -6 785.21 17.38 0 12 -6 752.01 17.52 0 12 6 759.52 17.61 0 -12 -7 13.06 2.56 0 12 7 12.60 2.93 0 12 7 14.16 3.18 0 12 7 12.47 2.49 0 12 -7 13.18 2.73 0 12 -7 17.45 3.01 0 12 7 13.95 2.86 0 12 -7 14.28 2.64 0 12 7 15.07 2.60 0 -12 -8 0.80 1.79 0 12 8 0.15 2.39 0 12 8 -0.13 2.02 0 12 8 -1.09 2.03 0 12 -8 -1.08 1.87 0 12 8 1.07 2.00 0 12 -8 2.79 2.00 0 12 -8 1.93 1.79 0 12 8 1.57 1.80 0 12 -9 152.48 6.21 0 12 9 148.62 6.14 0 12 9 180.95 6.90 0 -12 -9 173.31 6.45 0 12 9 172.82 7.37 0 12 9 145.05 6.10 0 12 -9 167.36 6.09 0 12 9 150.04 6.21 0 12 -9 162.60 6.32 0 -12 -10 182.09 6.56 0 12 10 191.76 6.99 0 12 10 195.71 7.71 0 12 10 157.28 6.36 0 12 10 150.61 6.07 0 12 10 172.74 6.40 0 -12 -11 2.06 1.73 0 12 11 4.41 2.04 0 12 11 2.08 2.31 0 -12 -12 198.53 6.69 0 12 12 214.42 7.89 0 -12 -13 0.46 1.53 0 12 13 2.52 2.08 0 12 14 63.60 4.11 0 -12 -14 59.50 3.38 0 12 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-8 661.52 12.57 -4 6 8 669.91 13.87 -4 -6 -8 686.16 15.45 -4 -6 -7 1.97 1.20 -4 -6 -7 0.81 1.26 -4 6 7 3.96 3.00 -4 6 7 0.69 1.71 -4 -6 -7 1.90 1.24 -4 -6 -7 0.85 1.81 4 6 -7 -1.02 1.38 -4 -6 -6 20.71 2.24 -4 -6 -6 23.31 2.34 -4 -6 -6 23.99 1.89 4 6 -6 22.82 1.95 -4 6 6 25.61 2.45 -4 6 6 22.47 3.27 -4 6 5 43.17 3.05 -4 6 5 41.98 3.97 4 6 -5 43.84 2.64 -4 -6 -5 42.66 3.21 -4 -6 -5 40.33 3.11 -4 6 4 177.22 6.93 4 6 -4 177.03 5.35 -4 -6 -4 189.76 7.32 -4 6 4 180.27 6.03 -4 -6 -4 183.41 7.12 -4 6 3 42.64 3.93 -4 -6 -3 27.56 3.35 4 6 -3 29.60 2.38 -4 6 3 40.38 3.09 -4 -6 -3 25.93 3.04 -4 6 2 145.04 6.00 4 6 -2 143.15 4.84 -4 -6 -2 147.54 5.78 -4 6 2 144.95 5.27 4 6 -1 66.14 3.34 -4 6 1 72.14 3.76 -4 -6 0 125.88 5.16 -4 6 0 132.97 5.54 -4 6 0 124.38 4.82 -4 -6 1 58.03 3.45 -4 -6 1 50.67 5.48 -4 -6 1 46.38 5.35 -4 -6 2 148.21 5.32 -4 -6 2 132.89 7.40 -4 6 -2 135.34 4.85 -4 -6 3 25.97 3.24 -4 -6 3 23.19 3.09 -4 -6 4 183.24 7.33 -4 -6 4 185.77 7.40 -4 -6 5 39.26 3.15 -4 -6 5 41.48 3.25 -4 -6 5 33.33 2.92 -4 -6 6 26.94 2.52 -4 -6 6 23.14 2.35 -4 -6 6 22.14 2.60 -4 -6 7 3.30 1.38 -4 -6 7 1.56 1.67 -4 -6 7 2.73 1.32 -4 -6 8 638.81 13.46 -4 -6 8 626.32 13.47 -4 -6 8 650.31 15.85 -4 -6 9 29.89 2.79 -4 -6 9 31.38 2.14 -4 -6 9 31.36 2.15 -4 -6 9 32.31 3.41 -4 -6 10 127.90 4.76 -4 -6 10 113.34 3.68 -4 -6 10 114.39 3.74 -4 -6 10 121.45 5.82 -4 -6 11 38.43 2.59 -4 -6 11 29.34 2.81 -4 -6 12 50.51 2.72 -4 -6 14 311.95 7.62 -4 -6 15 28.30 1.79 -4 -7 -12 177.07 4.67 -4 7 12 192.22 4.65 -4 -7 -11 10.66 1.28 -4 7 11 12.26 1.37 -4 7 10 190.13 5.09 -4 7 9 6.03 1.32 -4 7 8 51.71 3.17 4 7 -8 51.22 2.35 -4 7 7 80.06 4.14 4 7 -7 79.45 3.09 -4 7 7 88.47 3.55 -4 -7 -6 527.41 11.50 -4 7 6 491.03 11.52 -4 -7 -6 499.16 10.95 4 7 -6 474.46 9.91 -4 7 6 523.01 10.65 -4 -7 -6 475.47 10.78 -4 7 5 10.63 2.70 4 7 -5 12.81 1.74 -4 -7 -5 12.85 1.76 -4 -7 -5 9.54 1.77 -4 -7 -5 8.91 1.56 -4 7 5 15.19 1.99 -4 -7 -4 163.36 5.41 -4 7 4 145.04 5.40 -4 -7 -4 153.99 5.70 4 7 -4 148.40 4.51 -4 7 4 154.73 4.83 -4 -7 -4 149.03 5.62 -4 -7 -3 27.34 2.30 -4 7 3 39.36 3.30 -4 -7 -3 30.25 2.85 -4 7 3 40.96 2.53 -4 -7 -3 29.92 2.76 4 7 -3 35.28 2.30 4 7 -2 135.62 4.39 -4 -7 -2 151.44 6.39 -4 7 2 133.61 4.50 -4 -7 -2 140.41 4.94 4 7 -1 86.58 3.95 -4 7 1 117.01 4.55 4 7 0 807.10 15.47 -4 7 0 791.75 15.29 -4 -7 0 831.26 16.03 -4 -7 1 7.18 2.42 -4 -7 1 3.72 1.45 -4 -7 1 7.90 2.39 -4 -7 2 137.74 6.32 -4 -7 2 126.55 6.15 -4 -7 3 24.50 2.68 -4 -7 3 22.65 2.64 -4 -7 4 152.73 5.84 -4 -7 4 142.67 5.73 -4 -7 5 10.88 1.79 -4 -7 5 11.27 1.71 -4 -7 6 517.19 11.45 -4 -7 6 502.66 11.43 -4 -7 7 84.99 3.52 -4 -7 7 77.99 3.41 -4 -7 8 59.99 2.66 -4 -7 8 57.29 2.66 -4 -7 9 3.97 1.44 -4 -7 9 4.28 1.21 -4 -7 9 3.97 0.79 -4 -7 10 170.96 4.91 -4 -7 10 173.52 5.26 -4 -7 11 10.13 1.37 -4 -7 11 10.14 1.32 -4 -7 12 171.66 4.44 -4 -7 12 171.45 4.74 -4 -8 -8 207.21 4.94 -4 -8 -7 104.13 3.26 -4 8 7 103.95 2.95 -4 8 6 29.09 2.03 -4 8 6 31.91 1.66 -4 -8 -6 31.41 1.84 4 8 -5 21.52 1.76 -4 -8 -5 20.20 1.55 -4 -8 -4 283.23 6.88 4 8 -4 277.94 6.22 -4 8 4 286.74 6.12 -4 -8 -4 268.88 6.76 -4 -8 -4 296.56 6.60 -4 -8 -3 45.63 2.62 4 8 -3 53.31 2.53 -4 -8 -3 45.14 2.58 -4 -8 -3 46.72 2.30 -4 -8 -2 193.99 5.82 4 8 -2 188.32 4.85 -4 -8 -2 194.71 4.99 -4 -8 -2 184.24 5.71 4 8 -1 5.83 1.20 -4 8 0 13.66 1.55 4 8 0 16.24 1.48 -4 -8 1 4.99 1.28 -4 -8 1 5.74 1.33 -4 -8 2 185.13 5.92 4 8 2 204.06 5.10 -4 -8 2 195.00 5.99 -4 -8 3 47.32 2.75 -4 -8 3 50.96 2.80 -4 -8 4 277.82 7.22 -4 -8 4 292.55 7.29 -4 -8 5 19.02 1.55 4 8 5 19.13 1.66 -4 -8 5 20.59 1.61 -4 -8 6 32.72 1.81 -4 -8 6 33.49 1.81 4 8 6 34.74 1.96 4 8 7 124.53 3.68 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 35315 _shelx_res_file ; TITL T-478.res in P2(1)2(1)2(1) shelx.res created by SHELXL-2018/3 at 10:31:21 on 07-Aug-2023 CELL 1.54184 3.9420 11.5915 28.0387 90.000 90.000 90.000 ZERR 4.00 0.0000 0.0002 0.0004 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H BR O UNIT 64 52 4 4 MERG 2 OMIT -1 11 22 OMIT 1 13 1 TWIN FMAP 2 PLAN 3 SIZE 0.070 0.090 0.350 ACTA BOND BOND $H CONF LIST 4 L.S. 13 TEMP -173.00 WGHT 0.012100 1.392400 BASF 0.53322 FVAR 0.63957 C1 1 0.633780 0.673241 0.284881 11.00000 0.01359 0.01684 = 0.01644 0.00064 -0.00144 0.00048 C2 1 0.518611 0.584936 0.319755 11.00000 0.02068 0.01635 = 0.01653 -0.00006 0.00143 0.00134 AFIX 43 H2 2 0.576288 0.506108 0.315259 11.00000 -1.20000 AFIX 0 C3 1 0.333341 0.616916 0.357512 11.00000 0.01642 0.01773 = 0.01598 -0.00176 -0.00280 0.00149 AFIX 43 H3 2 0.272264 0.696111 0.359037 11.00000 -1.20000 AFIX 0 C4 1 0.213825 0.544145 0.396730 11.00000 0.01288 0.02240 = 0.01335 0.00032 -0.00302 -0.00037 C5 1 0.041910 0.594123 0.435857 11.00000 0.01369 0.03157 = 0.01453 -0.00340 -0.00306 -0.00112 C6 1 -0.061428 0.523078 0.473218 11.00000 0.01927 0.03953 = 0.01419 -0.00149 -0.00129 -0.00419 AFIX 43 H6 2 -0.174643 0.556148 0.499821 11.00000 -1.20000 AFIX 0 C7 1 -0.002547 0.405045 0.472410 11.00000 0.02490 0.03768 = 0.01530 0.00658 -0.00421 -0.01114 AFIX 43 H7 2 -0.075592 0.358302 0.498276 11.00000 -1.20000 AFIX 0 C8 1 0.162921 0.355154 0.433864 11.00000 0.02636 0.02423 = 0.02259 0.00427 -0.00788 -0.00242 AFIX 43 H8 2 0.202810 0.274348 0.433117 11.00000 -1.20000 AFIX 0 C9 1 0.269091 0.424461 0.396545 11.00000 0.02046 0.02287 = 0.01664 0.00045 -0.00160 0.00043 AFIX 43 H9 2 0.382068 0.390249 0.370170 11.00000 -1.20000 AFIX 0 C10 1 -0.031694 0.721629 0.437484 11.00000 0.01939 0.02796 = 0.02029 -0.00717 0.00094 0.00034 AFIX 137 H10A 2 -0.155611 0.739898 0.466828 11.00000 -1.50000 H10B 2 -0.169550 0.743225 0.409802 11.00000 -1.50000 H10C 2 0.182210 0.764687 0.436880 11.00000 -1.50000 AFIX 0 C11 1 0.781090 0.634076 0.238290 11.00000 0.01278 0.01714 = 0.01551 0.00231 -0.00083 0.00216 C12 1 0.741903 0.521898 0.221019 11.00000 0.01624 0.01780 = 0.01703 0.00429 0.00207 -0.00069 AFIX 43 H12 2 0.629276 0.465770 0.239962 11.00000 -1.20000 AFIX 0 C13 1 0.866416 0.491574 0.176286 11.00000 0.01997 0.01513 = 0.01901 -0.00031 0.00049 0.00046 AFIX 43 H13 2 0.839832 0.415359 0.164401 11.00000 -1.20000 AFIX 0 C14 1 1.029548 0.574957 0.149594 11.00000 0.01329 0.02531 = 0.01231 -0.00117 0.00093 0.00240 C15 1 1.076837 0.686875 0.165969 11.00000 0.01600 0.01945 = 0.01805 0.00419 -0.00072 -0.00208 AFIX 43 H15 2 1.193503 0.742210 0.147111 11.00000 -1.20000 AFIX 0 C16 1 0.950018 0.715919 0.210408 11.00000 0.01723 0.01515 = 0.01936 0.00087 -0.00193 -0.00234 AFIX 43 H16 2 0.978056 0.792262 0.222085 11.00000 -1.20000 AFIX 0 BR1 3 1.194804 0.536453 0.087699 11.00000 0.02033 0.03011 = 0.01522 -0.00153 0.00375 -0.00038 O1 4 0.610950 0.775828 0.293708 11.00000 0.03029 0.01709 = 0.02516 -0.00253 0.00645 0.00097 HKLF 4 REM T-478.res in P2(1)2(1)2(1) REM wR2 = 0.0524, GooF = S = 1.143, Restrained GooF = 1.143 for all data REM R1 = 0.0215 for 2627 Fo > 4sig(Fo) and 0.0219 for all 2657 data REM 165 parameters refined using 0 restraints END WGHT 0.0121 1.3923 REM Highest difference peak 0.511, deepest hole -0.418, 1-sigma level 0.063 Q1 1 1.1918 0.6196 0.0883 11.00000 0.05 0.51 Q2 1 1.2106 0.4469 0.0883 11.00000 0.05 0.48 Q3 1 1.1966 0.5378 0.1278 11.00000 0.05 0.42 ; _shelx_res_checksum 77004 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -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 C C1 0.6338(7) 0.6732(2) 0.28488(10) 0.0156(6) Uani d 1 . . C C2 0.5186(8) 0.5849(3) 0.31975(11) 0.0179(6) Uani d 1 . . H H2 0.576288 0.506108 0.315259 0.021 Uiso calc 1 . . C C3 0.3333(8) 0.6169(3) 0.35751(10) 0.0167(6) Uani d 1 . . H H3 0.272264 0.696111 0.359037 0.020 Uiso calc 1 . . C C4 0.2138(8) 0.5441(3) 0.39673(9) 0.0162(5) Uani d 1 . . C C5 0.0419(8) 0.5941(3) 0.43586(11) 0.0199(6) Uani d 1 . . C C6 -0.0614(9) 0.5231(3) 0.47322(11) 0.0243(7) Uani d 1 . . H H6 -0.174643 0.556148 0.499821 0.029 Uiso calc 1 . . C C7 -0.0025(9) 0.4050(3) 0.47241(12) 0.0260(8) Uani d 1 . . H H7 -0.075592 0.358302 0.498276 0.031 Uiso calc 1 . . C C8 0.1629(10) 0.3552(3) 0.43386(11) 0.0244(7) Uani d 1 . . H H8 0.202810 0.274348 0.433117 0.029 Uiso calc 1 . . C C9 0.2691(8) 0.4245(3) 0.39655(10) 0.0200(6) Uani d 1 . . H H9 0.382068 0.390249 0.370170 0.024 Uiso calc 1 . . C C10 -0.0317(9) 0.7216(3) 0.43748(12) 0.0225(7) Uani d 1 . . H H10A -0.155611 0.739898 0.466828 0.034 Uiso calc 1 . . H H10B -0.169550 0.743225 0.409802 0.034 Uiso calc 1 . . H H10C 0.182210 0.764687 0.436880 0.034 Uiso calc 1 . . C C11 0.7811(8) 0.6341(2) 0.23829(10) 0.0151(5) Uani d 1 . . C C12 0.7419(7) 0.5219(2) 0.22102(9) 0.0170(6) Uani d 1 . . H H12 0.629276 0.465770 0.239962 0.020 Uiso calc 1 . . C C13 0.8664(8) 0.4916(2) 0.17629(11) 0.0180(6) Uani d 1 . . H H13 0.839832 0.415359 0.164401 0.022 Uiso calc 1 . . C C14 1.0295(8) 0.5750(3) 0.14959(10) 0.0170(6) Uani d 1 . . C C15 1.0768(8) 0.6869(3) 0.16597(11) 0.0178(6) Uani d 1 . . H H15 1.193503 0.742210 0.147111 0.021 Uiso calc 1 . . C C16 0.9500(8) 0.7159(3) 0.21041(11) 0.0172(6) Uani d 1 . . H H16 0.978056 0.792262 0.222085 0.021 Uiso calc 1 . . Br Br1 1.19480(8) 0.53645(3) 0.08770(2) 0.02188(9) Uani d 1 . . O O1 0.6109(6) 0.77583(19) 0.29371(8) 0.0242(5) 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 C1 0.0136(15) 0.0168(14) 0.0164(13) 0.0005(11) -0.0014(11) 0.0006(11) C2 0.0207(16) 0.0164(14) 0.0165(14) 0.0013(12) 0.0014(12) -0.0001(11) C3 0.0164(13) 0.0177(13) 0.0160(13) 0.0015(13) -0.0028(12) -0.0018(11) C4 0.0129(13) 0.0224(13) 0.0134(11) -0.0004(13) -0.0030(9) 0.0003(11) C5 0.0137(14) 0.0316(18) 0.0145(14) -0.0011(13) -0.0031(12) -0.0034(13) C6 0.0193(14) 0.040(2) 0.0142(13) -0.0042(16) -0.0013(11) -0.0015(14) C7 0.0249(18) 0.038(2) 0.0153(15) -0.0111(15) -0.0042(13) 0.0066(14) C8 0.0264(17) 0.0242(16) 0.0226(15) -0.0024(15) -0.0079(15) 0.0043(12) C9 0.0205(17) 0.0229(14) 0.0166(13) 0.0004(12) -0.0016(11) 0.0005(10) C10 0.0194(16) 0.0280(17) 0.0203(16) 0.0003(14) 0.0009(13) -0.0072(13) C11 0.0128(13) 0.0171(13) 0.0155(13) 0.0022(11) -0.0008(11) 0.0023(10) C12 0.0162(15) 0.0178(14) 0.0170(12) -0.0007(12) 0.0021(10) 0.0043(11) C13 0.0200(16) 0.0151(14) 0.0190(14) 0.0005(11) 0.0005(12) -0.0003(10) C14 0.0133(14) 0.0253(16) 0.0123(13) 0.0024(11) 0.0009(11) -0.0012(11) C15 0.0160(14) 0.0194(15) 0.0181(14) -0.0021(12) -0.0007(11) 0.0042(11) C16 0.0172(14) 0.0151(14) 0.0194(14) -0.0023(12) -0.0019(12) 0.0009(11) Br1 0.02033(14) 0.03011(16) 0.01522(13) -0.00038(13) 0.00375(12) -0.00153(13) O1 0.0303(14) 0.0171(11) 0.0252(11) 0.0010(9) 0.0064(10) -0.0025(9) 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' Br Br -0.6763 1.2805 '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 O1 C1 C2 . . 121.1(3) ? O1 C1 C11 . . 120.1(3) ? C2 C1 C11 . . 118.9(3) ? C3 C2 C1 . . 119.7(3) ? C3 C2 H2 . . 120.1 ? C1 C2 H2 . . 120.1 ? C2 C3 C4 . . 127.6(3) ? C2 C3 H3 . . 116.2 ? C4 C3 H3 . . 116.2 ? C9 C4 C5 . . 118.8(3) ? C9 C4 C3 . . 121.1(3) ? C5 C4 C3 . . 120.1(3) ? C6 C5 C4 . . 118.8(3) ? C6 C5 C10 . . 120.0(3) ? C4 C5 C10 . . 121.2(3) ? C7 C6 C5 . . 121.4(3) ? C7 C6 H6 . . 119.3 ? C5 C6 H6 . . 119.3 ? C6 C7 C8 . . 120.1(3) ? C6 C7 H7 . . 119.9 ? C8 C7 H7 . . 119.9 ? C9 C8 C7 . . 119.3(3) ? C9 C8 H8 . . 120.4 ? C7 C8 H8 . . 120.4 ? C8 C9 C4 . . 121.6(3) ? C8 C9 H9 . . 119.2 ? C4 C9 H9 . . 119.2 ? C5 C10 H10A . . 109.5 ? C5 C10 H10B . . 109.5 ? H10A C10 H10B . . 109.5 ? C5 C10 H10C . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? C12 C11 C16 . . 119.4(3) ? C12 C11 C1 . . 122.8(3) ? C16 C11 C1 . . 117.8(3) ? C13 C12 C11 . . 120.6(3) ? C13 C12 H12 . . 119.7 ? C11 C12 H12 . . 119.7 ? C14 C13 C12 . . 118.4(3) ? C14 C13 H13 . . 120.8 ? C12 C13 H13 . . 120.8 ? C13 C14 C15 . . 122.5(3) ? C13 C14 Br1 . . 119.2(2) ? C15 C14 Br1 . . 118.3(2) ? C16 C15 C14 . . 118.4(3) ? C16 C15 H15 . . 120.8 ? C14 C15 H15 . . 120.8 ? C15 C16 C11 . . 120.7(3) ? C15 C16 H16 . . 119.7 ? C11 C16 H16 . . 119.7 ? 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 C1 O1 . 1.218(4) ? C1 C2 . 1.487(4) ? C1 C11 . 1.500(4) ? C2 C3 . 1.339(4) ? C2 H2 . 0.9500 ? C3 C4 . 1.464(4) ? C3 H3 . 0.9500 ? C4 C9 . 1.404(4) ? C4 C5 . 1.414(4) ? C5 C6 . 1.393(5) ? C5 C10 . 1.507(5) ? C6 C7 . 1.388(5) ? C6 H6 . 0.9500 ? C7 C8 . 1.389(5) ? C7 H7 . 0.9500 ? C8 C9 . 1.384(4) ? C8 H8 . 0.9500 ? C9 H9 . 0.9500 ? C10 H10A . 0.9800 ? C10 H10B . 0.9800 ? C10 H10C . 0.9800 ? C11 C12 . 1.396(4) ? C11 C16 . 1.398(4) ? C12 C13 . 1.392(4) ? C12 H12 . 0.9500 ? C13 C14 . 1.381(4) ? C13 H13 . 0.9500 ? C14 C15 . 1.389(4) ? C14 Br1 . 1.907(3) ? C15 C16 . 1.384(4) ? C15 H15 . 0.9500 ? C16 H16 . 0.9500 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C3 H3 O1 . 0.95 2.45 2.791(4) 101 no C12 H12 O1 3_645 0.95 2.58 3.200(3) 124 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 O1 C1 C2 C3 . . . . 12.0(5) ? C11 C1 C2 C3 . . . . -168.2(3) ? C1 C2 C3 C4 . . . . -176.3(3) ? C2 C3 C4 C9 . . . . -4.4(5) ? C2 C3 C4 C5 . . . . 175.1(3) ? C9 C4 C5 C6 . . . . 1.1(5) ? C3 C4 C5 C6 . . . . -178.4(3) ? C9 C4 C5 C10 . . . . -178.6(3) ? C3 C4 C5 C10 . . . . 1.9(5) ? C4 C5 C6 C7 . . . . -0.8(5) ? C10 C5 C6 C7 . . . . 178.9(3) ? C5 C6 C7 C8 . . . . 0.1(6) ? C6 C7 C8 C9 . . . . 0.3(5) ? C7 C8 C9 C4 . . . . 0.1(5) ? C5 C4 C9 C8 . . . . -0.7(5) ? C3 C4 C9 C8 . . . . 178.7(3) ? O1 C1 C11 C12 . . . . -164.3(3) ? C2 C1 C11 C12 . . . . 15.9(4) ? O1 C1 C11 C16 . . . . 12.6(4) ? C2 C1 C11 C16 . . . . -167.2(3) ? C16 C11 C12 C13 . . . . -0.6(4) ? C1 C11 C12 C13 . . . . 176.2(3) ? C11 C12 C13 C14 . . . . 0.1(4) ? C12 C13 C14 C15 . . . . 0.8(5) ? C12 C13 C14 Br1 . . . . -178.8(2) ? C13 C14 C15 C16 . . . . -1.1(5) ? Br1 C14 C15 C16 . . . . 178.5(2) ? C14 C15 C16 C11 . . . . 0.6(5) ? C12 C11 C16 C15 . . . . 0.3(5) ? C1 C11 C16 C15 . . . . -176.7(3) ? _cod_database_fobs_code 2022850