#------------------------------------------------------------------------------ #$Date: 2020-12-07 03:01:11 +0200 (Mon, 07 Dec 2020) $ #$Revision: 259635 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022296.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_2022296 loop_ _publ_author_name 'Mason, Helen E.' 'Howard, Judith A. K.' 'Sparkes, Hazel A.' _publ_section_title ; (E)-4-Bromo-2-[(phenylimino)methyl]phenol: a new polymorph and thermochromism ; _journal_coeditor_code YD3009 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1001 _journal_page_last 1004 _journal_paper_doi 10.1107/S2053229620011560 _journal_volume 76 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_iupac 'C13 H10 Br N O' _chemical_formula_moiety 'C13 H10 Br N O' _chemical_formula_sum 'C13 H10 Br N O' _chemical_formula_weight 276.13 _chemical_name_systematic ; (E)-4-Bromo-2-((phenylimino)methyl]phenol ; _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method ; Olex2 1.3 (compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032) ; _cell_angle_alpha 90 _cell_angle_beta 91.381(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 25.8944(13) _cell_length_b 6.9439(4) _cell_length_c 6.1499(4) _cell_measurement_reflns_used 3202 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.6983 _cell_measurement_theta_min 3.0312 _cell_volume 1105.48(11) _computing_cell_refinement ; CrysAlis PRO (Oxford Diffraction, 2010) ; _computing_data_collection ; CrysAlis PRO (Oxford Diffraction, 2010) ; _computing_data_reduction ; CrysAlis PRO (Oxford Diffraction, 2010) ; _computing_molecular_graphics ; OLEX (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 16.1511 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 7049 _diffrn_reflns_theta_full 26.362 _diffrn_reflns_theta_max 26.362 _diffrn_reflns_theta_min 3.037 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 3.694 _exptl_absorpt_correction_T_max 0.585 _exptl_absorpt_correction_T_min 0.190 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; [CrysAlis PRO (Oxford Diffraction, 2010), based on expressions derived by Clark & Reid (1995)] ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.659 _exptl_crystal_description block _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.950 _refine_diff_density_min -0.343 _refine_ls_abs_structure_details ; Flack x determined using 1007 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack -0.010(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 148 _refine_ls_number_reflns 2254 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0390 _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^)+(0.0670P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0958 _refine_ls_wR_factor_ref 0.0995 _reflns_number_gt 2142 _reflns_number_total 2254 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yd3009sup1.cif _cod_data_source_block 1B _cod_database_code 2022296 _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 0.223 _shelx_estimated_absorpt_t_max 0.497 _shelx_hkl_file ; -34 0 -1 172.261 392.324 8 -34 0 0 15389.1 1610.33 8 -34 0 1 1216.62 694.749 8 -34 -2 -1 3564.25 874.275 8 -34 -2 0 7315.95 1088.66 8 -34 -2 1 7949.91 1245.57 8 -34 -4 0 1894.35 766.563 8 -33 1 -2 1997.12 687.615 8 -33 -1 -2 1191.37 515.213 8 -33 1 -1 11982.4 1403.97 8 -33 -1 -1 12519.1 1430.06 8 -33 1 0 1996.74 660.317 8 -33 -1 0 2540.20 733.417 8 -33 -1 1 16034.3 1679.15 8 -33 1 1 16127.3 1631.50 8 -33 1 2 1009.24 618.227 8 -33 -1 2 804.226 574.177 8 -33 -3 -2 9020.32 1260.57 8 -33 3 -2 7900.79 1123.92 1 -33 3 -1 1367.87 497.487 1 -33 -3 -1 2052.64 692.400 8 -33 3 0 9440.83 1132.92 1 -33 3 0 9128.92 1291.92 8 -33 -3 0 9974.34 1329.08 8 -33 -3 1 2385.72 808.506 8 -33 3 1 2111.42 636.400 8 -33 -3 2 1991.02 718.764 8 -32 0 -3-501.236 518.214 8 -32 0 -2 1597.68 530.504 8 -32 0 -1-242.927 324.191 8 -32 0 0 12243.7 1429.49 8 -32 0 1 1178.16 642.195 8 -32 0 2 11216.2 1480.41 8 -32 0 3-382.726 502.591 8 -32 -2 -3 3218.72 805.358 8 -32 2 -2 201.973 393.282 8 -32 -2 -2 544.515 424.000 8 -32 2 -1 5856.49 944.398 8 -32 -2 -1 6794.35 1071.28 8 -32 -2 0 4580.24 867.348 8 -32 2 0 4930.85 917.645 8 -32 2 1 8100.52 1180.12 8 -32 -2 1 8548.15 1260.17 8 -32 2 2 4421.15 966.813 8 -32 -2 2 3359.81 883.618 8 -32 -2 3 10121.9 1471.69 8 -32 -2 4 10137.9 1267.39 3 -32 -4 -2 2333.51 690.636 8 -32 4 -1 7166.48 1062.27 1 -32 -4 -1 6515.19 1024.38 8 -32 -4 0 2339.92 744.719 8 -32 -4 0 709.853 453.574 5 -32 4 0 897.663 520.497 8 -32 4 0 1249.51 520.384 1 -32 4 1 7928.97 1177.13 8 -32 -4 1 7030.74 1065.20 5 -32 4 1 6374.07 1023.30 1 -32 -4 1 8963.60 1331.54 8 -32 4 2-206.550 418.311 1 -32 -4 2-848.515 594.839 8 -31 1 -3 2022.49 652.427 8 -31 -1 -3 2687.19 788.575 8 -31 1 -2 1391.63 533.957 8 -31 -1 -2 1898.38 585.889 8 -31 -1 -1 16144.0 1536.66 8 -31 1 -1 15420.5 1534.24 8 -31 -1 0 1583.50 608.242 8 -31 1 0 1140.06 523.124 8 -31 -1 1 9583.79 1295.53 8 -31 1 1 7911.38 1169.91 8 -31 -1 2 1803.30 779.962 8 -31 1 2 2717.15 755.280 8 -31 -1 3 4214.27 848.210 8 -31 1 3 4078.23 877.647 8 -31 -3 -3-384.022 446.756 8 -31 3 -2 6472.82 1019.64 8 -31 -3 -2 6312.62 994.189 8 -31 3 -2 6445.89 1039.60 1 -31 3 -1 4397.59 801.606 1 -31 3 -1 4904.31 911.134 8 -31 -3 -1 5574.52 1001.28 8 -31 3 0 5374.52 857.695 1 -31 3 0 5850.51 958.677 8 -31 -3 0 4844.51 924.623 8 -31 3 1 1228.02 506.078 1 -31 -3 1 1888.36 728.750 8 -31 3 1 1855.81 631.869 8 -31 -3 2 7345.69 1219.64 8 -31 3 2 5661.22 892.506 1 -31 3 2 6930.12 1169.90 8 -31 -3 3 786.067 519.964 3 -31 3 3-43.4331 386.795 8 -31 -3 4 4387.79 869.143 3 -31 5 0 2035.70 594.826 8 -31 5 1 858.665 524.799 8 -31 -5 1 1076.43 530.924 5 -30 0 -4 6206.47 1164.12 8 -30 0 -3-348.135 436.437 8 -30 0 -2 19323.3 1728.28 8 -30 0 -1 473.549 385.754 8 -30 0 0 16892.5 1594.44 8 -30 0 1 485.466 505.517 8 -30 0 2 22583.7 2011.45 8 -30 0 3-385.637 595.074 8 -30 0 4 12606.2 1723.69 8 -30 -2 -4 1084.32 564.521 8 -30 2 -3 5515.91 988.044 8 -30 -2 -3 5382.10 970.505 8 -30 2 -2 7617.33 1104.96 8 -30 -2 -2 8037.21 1099.00 8 -30 2 -2 8509.61 1107.60 1 -30 2 -1 5923.22 960.661 8 -30 2 -1 6521.86 905.395 1 -30 -2 -1 7601.66 1069.20 8 -30 -2 0 6112.66 949.313 8 -30 2 0 6993.42 1029.01 8 -30 2 0 7085.56 900.663 1 -30 2 1 8098.21 990.496 1 -30 -2 1 8946.84 1259.93 8 -30 2 1 7151.50 1071.03 8 -30 2 2 6920.82 935.954 1 -30 -2 2 9343.04 1383.31 8 -30 2 2 10461.8 1385.75 8 -30 2 3 4811.13 931.668 8 -30 -2 3 3823.91 882.295 8 -30 -2 3 5364.91 877.466 3 -30 2 4 3685.49 831.405 8 -30 -2 4 3765.71 790.583 3 -30 -4 -3 6098.89 987.001 8 -30 -4 -2-341.487 439.420 5 -30 4 -2 36.5552 338.269 1 -30 -4 -2-73.0659 309.814 8 -30 4 -2-279.276 391.767 8 -30 -4 -1 6857.79 1063.31 8 -30 -4 -1 6803.17 1075.49 5 -30 4 -1 5965.39 970.770 1 -30 4 -1 6251.52 978.315 8 -30 4 0 765.109 403.837 8 -30 4 0 1091.27 553.814 1 -30 -4 0 1012.46 503.374 5 -30 -4 1 10425.2 1430.37 8 -30 4 1 8961.72 1164.74 8 -30 4 1 7884.55 1094.94 1 -30 -4 1 7053.34 1053.05 5 -30 4 2-16.0492 386.177 8 -30 -4 2-451.420 631.135 8 -30 -4 2 578.167 413.501 3 -30 4 2 435.039 411.035 1 -30 -4 3 5573.45 1219.61 8 -30 4 3 5743.59 985.284 1 -30 -4 3 7092.48 1102.40 3 -30 4 3 6100.99 1113.66 8 -29 1 -4 470.886 512.855 8 -29 -1 -4-393.803 453.564 8 -29 1 -3 4256.31 849.010 8 -29 -1 -3 3845.01 843.585 8 -29 -1 -2 2634.38 725.906 8 -29 1 -2 2314.84 654.607 8 -29 1 -1 16840.3 1565.00 8 -29 -1 -1 17404.5 1568.18 8 -29 1 -1 18586.6 1391.60 1 -29 1 0 3899.88 630.058 1 -29 -1 0 3519.00 739.713 8 -29 1 0 3956.21 773.814 8 -29 1 1 13527.1 1402.54 8 -29 -1 1 16072.7 1574.97 8 -29 1 2 4583.55 954.595 8 -29 -1 2 4770.28 1025.10 8 -29 1 3 8837.46 1299.45 8 -29 -1 3 8276.04 998.362 3 -29 -1 3 6144.07 1128.39 8 -29 -1 4 626.236 473.288 8 -29 -1 4 914.444 457.353 3 -29 1 4-614.444 698.714 8 -29 -3 -4 3229.71 809.626 8 -29 -3 -3 401.357 376.844 8 -29 3 -3 1399.11 603.809 8 -29 3 -2 8997.58 1158.28 8 -29 3 -2 11207.5 1297.68 1 -29 -3 -2 10564.9 1241.11 8 -29 -3 -1 646.763 429.134 8 -29 3 -1 702.274 413.569 8 -29 3 -1 578.067 414.691 1 -29 3 0 16214.7 1552.25 8 -29 -3 0 16756.8 1579.55 8 -29 -3 0 18223.1 1639.36 5 -29 3 0 16832.1 1460.23 1 -29 -3 1 1803.09 733.699 8 -29 3 1 1236.94 532.976 8 -29 -3 1 302.145 323.741 5 -29 3 1 1079.05 444.197 1 -29 -3 2 12745.3 1282.01 3 -29 3 2 13979.4 1564.66 8 -29 3 2 12280.5 1305.86 1 -29 -3 2 12242.6 1547.51 8 -29 -3 3 227.733 354.399 3 -29 3 3-167.328 484.858 8 -29 -3 4 3587.04 968.379 8 -29 3 4 3556.80 886.258 8 -29 3 4 2992.04 860.984 1 -29 -3 4 3242.67 798.082 3 -29 5 -2 4985.66 899.775 8 -29 5 -1 3713.52 821.060 1 -29 -5 -1 3051.53 836.588 5 -29 5 -1 2812.05 698.782 8 -29 5 0 8649.79 1125.31 8 -29 5 0 8320.88 1156.86 1 -29 -5 0 8719.28 1258.27 5 -29 5 1 2897.22 744.240 8 -29 5 1 3194.94 812.544 1 -29 -5 1 2479.38 745.384 3 -29 -5 1 2548.78 692.104 5 -29 -5 2 5106.72 1004.69 3 -29 5 2 5527.09 989.831 8 -29 5 2 4842.37 935.149 1 -29 5 3 1678.61 537.507 8 -28 0 -4 12157.5 1536.86 8 -28 0 -3-1206.03 617.949 8 -28 0 -2 22038.4 1799.69 8 -28 0 -1-3.98178 317.864 8 -28 0 0 19892.4 1650.73 8 -28 0 1-618.750 401.996 8 -28 0 2 18683.9 1841.71 8 -28 0 3-987.854 691.279 8 -28 0 4 11303.4 1534.70 8 -28 -2 -4 5615.32 1029.23 8 -28 2 -4 5412.29 1015.39 8 -28 2 -3 6104.98 1022.28 8 -28 -2 -3 6760.33 1073.56 8 -28 2 -2 7843.41 1091.56 8 -28 -2 -2 8399.33 1094.72 8 -28 -2 -1 12315.3 1306.09 8 -28 2 -1 11994.5 1276.51 8 -28 2 -1 13274.6 1233.44 1 -28 -2 0 8736.91 1170.26 8 -28 2 0 9120.74 987.781 1 -28 2 0 7864.58 1058.00 8 -28 -2 1 9913.39 1290.06 8 -28 2 1 7390.81 1009.61 8 -28 2 1 8213.19 995.203 1 -28 2 2 6336.17 875.244 1 -28 2 2 8270.41 1202.46 8 -28 -2 2 5769.57 823.577 3 -28 -2 2 6605.77 1140.21 8 -28 2 3 6489.59 1097.50 8 -28 -2 3 5624.07 977.782 8 -28 -2 3 6144.53 914.980 3 -28 2 3 6702.09 1035.94 1 -28 -2 4 4092.30 948.685 8 -28 2 4 5188.91 995.528 1 -28 2 4 3565.90 835.213 8 -28 -2 4 4655.94 889.079 3 -28 -2 5 4212.57 868.667 3 -28 -4 -3 10017.9 1393.04 5 -28 -4 -3 8790.32 1136.07 8 -28 4 -3 7914.55 1175.97 8 -28 -4 -2 568.328 466.937 5 -28 4 -2 114.583 310.347 8 -28 -4 -2 33.5638 358.210 8 -28 4 -2-68.0426 396.381 1 -28 4 -1 12416.3 1332.19 8 -28 -4 -1 14740.6 1600.38 5 -28 4 -1 13792.0 1405.80 1 -28 -4 -1 15932.8 1545.47 8 -28 4 0-94.2947 334.106 8 -28 -4 0-172.926 311.422 5 -28 4 0 4.60272 324.414 1 -28 4 1 8383.43 1119.93 8 -28 -4 1 8886.23 1160.85 3 -28 -4 1 7753.53 1073.75 5 -28 4 1 8972.34 1152.07 1 -28 -4 1 11354.1 1451.16 8 -28 -4 2-200.264 358.720 3 -28 4 2 222.569 346.701 1 -28 4 2 478.590 467.149 8 -28 -4 2-90.4793 477.932 8 -28 4 3 6812.88 1065.79 1 -28 4 3 6897.57 1174.99 8 -28 -4 3 6551.43 1049.86 3 -28 -4 3 8491.55 1389.58 8 -28 4 4 429.950 474.062 8 -28 4 4 516.744 634.710 1 -28 -4 4-66.1734 421.464 8 -28 -4 4-934.026 486.526 3 -28 -6 1 825.505 537.171 5 -27 -1 -5 3856.43 904.284 8 -27 -1 -4 2168.35 626.867 8 -27 1 -4 2854.41 740.604 8 -27 1 -3 18151.5 1749.19 8 -27 -1 -3 18310.4 1711.22 8 -27 -1 -2 2946.11 669.719 8 -27 1 -2 1241.85 497.138 8 -27 1 -1 19186.3 1377.47 1 -27 -1 -1 16936.0 1494.48 8 -27 1 -1 16586.2 1479.22 8 -27 -1 0 3379.61 727.826 8 -27 1 0 4023.07 775.356 8 -27 1 0 4148.20 617.980 1 -27 -1 1 10165.9 930.909 3 -27 1 1 11279.9 1065.01 1 -27 1 1 10379.1 1207.55 8 -27 -1 1 10852.5 1290.84 8 -27 -1 2 1604.97 642.244 8 -27 1 2 2508.62 726.667 8 -27 1 2 2095.47 507.770 1 -27 -1 2 2239.71 543.237 3 -27 -1 3 9482.58 1379.39 8 -27 -1 3 7696.04 965.544 3 -27 1 3 11351.0 1288.01 1 -27 1 3 8628.57 1261.14 8 -27 -1 4 830.179 566.838 8 -27 -1 4 1141.61 432.320 3 -27 1 4 603.700 433.198 8 -27 -1 5 4502.07 1019.61 8 -27 1 5 5313.09 1102.75 8 -27 -3 -5 24.0324 391.126 8 -27 -3 -4 11468.4 1438.96 8 -27 3 -4 10999.9 1383.31 8 -27 3 -3 213.366 355.198 8 -27 -3 -3 232.071 370.522 8 -27 -3 -2 11232.7 1369.43 5 -27 -3 -2 9973.64 1184.21 8 -27 3 -2 9833.92 1246.75 8 -27 -3 -1 2265.98 607.451 8 -27 3 -1 2467.56 590.405 1 -27 3 -1 1728.92 521.980 8 -27 -3 -1 2631.98 655.185 5 -27 -3 0 14622.9 1456.57 8 -27 3 0 12771.6 1246.37 1 -27 -3 0 14335.8 1402.05 5 -27 3 0 12933.1 1336.15 8 -27 -3 1 1331.10 646.015 8 -27 3 1-114.932 339.884 8 -27 -3 1 415.092 365.474 3 -27 -3 1 57.7689 326.057 5 -27 3 1 762.273 393.145 1 -27 -3 2 8680.16 1287.68 8 -27 3 2 8675.76 1192.52 8 -27 3 2 7784.07 1053.76 1 -27 -3 2 7842.43 966.670 5 -27 -3 2 7686.44 994.132 3 -27 3 3 921.184 510.039 8 -27 -3 3 643.764 386.570 3 -27 3 3 1853.72 632.461 1 -27 -3 4 5687.33 1018.56 3 -27 3 4 7206.56 1195.34 8 -27 -3 4 5687.49 1158.24 8 -27 3 4 6496.25 1172.93 1 -27 -3 5 1006.97 590.593 8 -27 3 5-873.621 645.341 1 -27 5 -3 4839.19 916.288 8 -27 5 -2 4231.93 799.864 8 -27 -5 -2 6128.06 1117.26 5 -27 5 -2 5584.64 1023.78 1 -27 5 -1 2000.29 607.404 1 -27 5 -1 1545.91 495.275 8 -27 -5 -1 1640.37 644.272 5 -27 -5 0 4904.50 952.188 5 -27 5 0 5393.05 889.856 8 -27 5 0 5125.17 901.722 1 -27 -5 1 2902.80 712.730 5 -27 5 1 2957.00 666.700 8 -27 5 1 3205.89 745.271 1 -27 5 2 2689.48 742.578 8 -27 -5 2 4168.19 840.854 5 -27 5 2 3111.41 717.373 1 -27 -5 2 2420.16 724.323 3 -27 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16538.9 1397.16 4 26 -4 1 14873.6 1581.91 4 26 -4 1 12121.4 1186.62 9 26 4 2-62.8072 408.482 4 26 -4 2-579.096 671.658 4 26 -4 3 13573.3 1614.57 4 26 4 3 12743.0 1357.18 4 26 -4 4-432.385 660.184 6 26 6 -3 597.822 582.725 7 26 6 -2 2209.79 773.062 7 26 6 -1 425.364 547.510 7 26 6 0 5393.03 1131.62 7 26 -6 0 6566.62 978.069 9 26 -6 1 696.295 397.151 9 26 -6 2 1351.74 534.573 9 27 1 -5 3544.18 901.922 4 27 -1 -5 4493.06 958.237 4 27 1 -4 1145.47 519.462 4 27 -1 -4 988.966 510.132 4 27 1 -3 6826.68 1034.74 4 27 -1 -3 7924.44 1158.10 4 27 1 -2 2258.50 632.524 4 27 -1 -2 2156.43 593.343 4 27 1 -1 8697.19 1027.15 4 27 -1 -1 8515.00 1028.91 4 27 1 0 3280.94 697.856 4 27 -1 0 3441.43 703.936 4 27 1 1 17865.5 1461.40 4 27 -1 1 14898.7 1439.85 4 27 1 2 2768.42 756.638 4 27 -1 2 1561.77 590.123 4 27 1 3 24852.4 2090.75 4 27 -1 3 23456.2 2132.16 4 27 -1 4 2733.98 816.936 6 27 1 4 4138.42 926.842 6 27 -1 4 3996.94 903.375 4 27 1 4 2718.23 761.361 4 27 1 5 5695.24 1049.59 6 27 3 -4 4830.61 947.552 4 27 -3 -4 5701.87 1007.41 4 27 3 -3 344.788 377.899 4 27 -3 -3 923.797 527.152 4 27 3 -3 358.772 427.695 7 27 3 -2 8214.81 1004.93 4 27 -3 -2 8562.53 1134.59 4 27 3 -1 599.655 424.684 4 27 -3 -1 901.696 552.586 4 27 3 0 11910.0 1156.26 4 27 -3 0 10788.6 1196.94 4 27 3 1 444.089 414.460 4 27 -3 1 336.396 482.595 4 27 3 2 10643.8 1271.00 4 27 -3 2 9236.80 1371.93 4 27 -3 3 886.362 609.419 4 27 3 3 281.003 402.902 4 27 -3 4 15914.4 1939.31 6 27 3 4 17262.8 1709.29 6 27 -5 -4 1871.48 701.879 4 27 -5 -3 2351.71 696.871 4 27 5 -3 1863.72 638.917 7 27 -5 -2 4233.47 813.599 4 27 5 -2 3655.28 943.611 7 27 5 -1 2943.06 884.432 7 27 -5 -1 1603.52 517.163 4 27 5 0 3474.21 950.180 7 27 -5 0 2207.58 635.458 4 27 -5 0 3418.92 683.499 9 27 5 1 1484.60 664.517 7 27 -5 1 3103.88 790.890 4 27 -5 1 2084.16 604.237 9 27 5 2 4332.34 1007.00 7 27 -5 2 7539.02 1281.35 4 27 -5 3 6644.15 1220.59 4 28 0 -4 8012.19 1197.08 4 28 0 -3-227.961 542.904 4 28 0 -2 17377.5 1535.67 4 28 0 -1 1111.53 503.196 4 28 0 0 19300.4 1563.14 4 28 0 1-699.492 532.118 4 28 0 2 30948.8 2223.70 4 28 0 3-706.437 585.150 4 28 0 4 15158.4 1750.11 4 28 2 -4 3546.98 835.428 4 28 -2 -4 3235.44 906.775 4 28 2 -3 4666.60 906.907 4 28 -2 -3 6199.56 1053.97 4 28 2 -2 5531.60 880.296 4 28 -2 -2 5928.79 971.837 4 28 2 -1 6231.38 874.554 4 28 -2 -1 6721.35 985.950 4 28 2 0 6950.48 912.482 4 28 -2 0 7463.57 1015.75 4 28 2 1 11427.5 1193.32 4 28 -2 1 10971.7 1275.76 4 28 2 2 12235.6 1404.41 4 28 -2 2 12518.9 1521.26 4 28 2 3 9134.09 1267.51 4 28 -2 3 9374.94 1388.81 4 28 -2 4 5159.10 1149.53 6 28 -2 4 6111.96 1196.74 4 28 2 4 6454.83 1189.37 4 28 2 4 6704.55 1211.92 6 28 2 5 638.730 479.257 6 28 4 -4-699.048 637.297 4 28 -4 -4 222.603 409.905 4 28 4 -3 7485.54 1026.84 4 28 -4 -3 6257.67 1005.14 4 28 4 -3 4952.38 1081.64 7 28 4 -2 803.949 514.561 4 28 -4 -2 1287.73 618.343 4 28 4 -2-293.479 494.778 7 28 4 -1 7117.54 916.989 4 28 -4 -1 7492.39 1044.87 4 28 4 0 239.231 302.427 4 28 -4 0-853.349 561.729 4 28 4 1 14422.1 1365.46 4 28 -4 1 15246.3 1634.54 4 28 4 2-323.482 418.507 4 28 -4 2 223.220 504.555 4 28 -4 3 10278.3 1526.64 4 28 4 3 11068.2 1334.42 4 28 -6 1 1197.02 545.749 9 28 -6 2 4485.06 933.687 9 29 1 -4 304.426 489.434 4 29 -1 -4 116.920 439.460 4 29 1 -3 6828.61 1109.30 4 29 -1 -3 7633.08 1137.39 4 29 1 -2 2510.64 719.363 4 29 -1 -2 3257.25 782.084 4 29 1 -1 15000.7 1361.11 4 29 -1 -1 15099.0 1416.38 4 29 1 0 3745.66 761.320 4 29 -1 0 2939.28 641.508 4 29 1 1 17860.0 1541.87 4 29 -1 1 18014.7 1607.59 4 29 1 2 5844.44 1056.51 4 29 -1 2 3057.47 768.852 4 29 1 3 6631.84 1139.18 4 29 -1 3 8643.62 1339.63 4 29 1 4 1269.18 622.233 6 29 -1 4 284.789 748.488 4 29 1 4 786.625 560.081 4 29 3 -4 1521.74 603.573 4 29 -3 -4 2939.54 877.933 4 29 3 -3 362.460 366.970 4 29 -3 -3 1543.82 643.341 4 29 3 -3 766.598 632.040 7 29 3 -2 13024.9 1302.95 4 29 -3 -2 14445.0 1455.74 4 29 3 -1 1133.85 468.800 4 29 -3 -1 1211.51 492.827 4 29 3 0 15755.8 1356.96 4 29 -3 0 16157.3 1491.56 4 29 3 1-30.3063 462.086 4 29 -3 1-694.188 638.217 4 29 3 2 15424.2 1598.92 4 29 -3 2 14501.6 1728.90 4 29 -3 3 1021.07 669.327 4 29 3 3 1355.61 574.985 4 29 3 4 4759.61 1000.75 6 29 -5 -3 3426.75 769.891 4 29 5 -3 1834.92 763.142 7 29 5 -2 4851.71 1124.97 7 29 -5 -2 5284.14 927.592 4 29 5 -1 1879.62 834.469 7 29 -5 -1 899.719 398.653 4 29 5 0 7550.50 1401.37 7 29 -5 0 8372.44 1224.94 4 29 -5 1 3863.97 913.462 4 29 -5 2 6625.03 1282.31 4 30 0 -4 10905.2 1410.16 4 30 0 -3 346.993 478.227 4 30 0 -2 16728.2 1548.55 4 30 0 -1 881.813 527.152 4 30 0 0 13270.3 1328.25 4 30 0 1-876.533 584.446 4 30 0 2 25656.8 2086.34 4 30 0 3-413.395 531.850 4 30 2 -4 3847.23 849.445 4 30 -2 -4 3659.37 932.226 4 30 2 -3 4860.03 934.910 4 30 -2 -3 4840.73 962.019 4 30 2 -2 7229.01 1032.06 4 30 -2 -2 8213.03 1147.80 4 30 2 -1 7192.31 994.116 4 30 -2 -1 7590.07 1089.14 4 30 2 0 4375.83 766.220 4 30 -2 0 4224.61 821.724 4 30 2 1 4588.46 790.183 4 30 -2 1 3354.64 689.423 4 30 2 2 9337.78 1269.11 4 30 -2 2 9524.51 1355.36 4 30 2 3 7821.52 1202.60 4 30 -2 3 8795.70 1395.04 4 30 2 4 2174.27 769.085 4 30 2 4 2096.86 802.737 6 30 4 -3 4738.31 865.146 4 30 -4 -3 5233.91 1031.07 4 30 4 -3 3032.37 962.919 7 30 4 -2 545.532 472.584 4 30 -4 -2 1196.71 577.209 4 30 4 -2 307.922 575.088 7 30 4 -1 6917.30 913.894 4 30 -4 -1 6615.43 1040.59 4 30 4 0 1428.75 439.545 4 30 -4 0 4.74018 560.045 4 30 4 1 7713.58 1079.79 4 30 -4 1 7039.93 1166.31 4 30 4 2-193.751 477.179 4 30 -4 2-423.307 561.234 4 31 1 -3 5301.65 1025.55 4 31 -1 -3 4919.29 969.038 4 31 1 -2 2422.43 722.708 4 31 -1 -2 3511.70 836.810 4 31 1 -1 10599.0 1227.66 4 31 -1 -1 11643.0 1284.08 4 31 1 0 1594.30 547.861 4 31 -1 0 1064.06 473.727 4 31 1 1 15863.9 1486.63 4 31 -1 1 15300.6 1505.96 4 31 1 2 2789.57 847.785 4 31 -1 2 3136.51 923.219 4 31 1 3 6107.05 1093.62 4 31 -1 3 3877.90 904.974 4 31 3 -3 1293.83 608.922 4 31 -3 -3 946.786 592.732 4 31 3 -3 766.571 566.446 7 31 3 -2 6680.97 982.795 4 31 -3 -2 6355.63 1058.24 4 31 3 -1 1598.01 576.340 4 31 -3 -1 1432.06 676.596 4 31 3 0 5056.35 785.250 4 31 -3 0 5796.84 926.701 4 31 3 1 4359.07 804.111 4 31 -3 1 6404.00 1082.93 4 31 3 2 7717.57 1155.83 4 31 -3 2 8142.76 1332.35 4 31 3 3-1153.19 722.950 4 31 -5 -1 352.956 397.433 4 31 -5 0 2798.17 736.713 4 31 -5 1-309.499 450.506 4 32 0 -3 121.171 469.077 4 32 0 -2 12308.2 1365.02 4 32 0 -1-166.377 373.492 4 32 0 0 9701.29 1187.27 4 32 0 1-954.222 657.132 4 32 0 2 4092.38 987.993 4 32 0 3 506.228 588.530 4 32 2 -3 10041.2 1269.76 4 32 2 -2 3097.04 785.268 4 32 -2 -2 4197.30 906.757 4 32 2 -1 5345.43 861.251 4 32 -2 -1 5677.97 989.192 4 32 2 0 3403.10 661.849 4 32 -2 0 1855.87 568.781 4 32 2 1 4333.08 794.386 4 32 -2 1 4548.69 894.220 4 32 2 2 1088.00 574.429 4 32 -2 2 1390.55 731.585 4 32 2 3 2235.93 737.089 4 32 4 -2 1145.74 525.117 4 32 4 -2 87.5474 519.000 7 32 4 -1 7301.18 990.999 4 32 -4 -1 5536.62 985.833 4 32 4 0-493.365 463.533 4 32 -4 0-838.645 757.567 4 32 4 1 9271.41 1227.91 4 32 -4 1 8089.14 1356.94 4 33 1 -2 538.700 609.682 4 33 -1 -2 674.207 567.099 4 33 1 -1 8748.77 1182.27 4 33 -1 -1 7079.37 1086.60 4 33 1 0 1795.77 569.707 4 33 -1 0 1489.25 630.434 4 33 1 1 10771.2 1301.71 4 33 -1 1 11379.7 1324.86 4 33 1 2 3040.02 847.284 4 33 -1 2 3230.15 903.504 4 33 3 -3 389.756 458.231 7 33 3 -2 950.823 561.863 4 33 3 -1 1004.59 480.036 4 33 -3 -1 919.811 539.350 4 33 3 0 6527.97 954.932 4 33 -3 0 5843.95 1000.33 4 33 3 1 1594.86 569.094 4 33 3 2 10108.5 1349.55 4 34 0 -1 505.768 516.410 4 34 0 0 16019.0 1565.20 4 34 0 1-1832.38 795.721 4 34 2 -1 5016.23 909.761 4 34 2 0 7533.31 1020.82 4 34 2 1 2976.36 778.558 4 ; _shelx_hkl_checksum 87898 _shelx_res_file ; TITL test_fac in Cc test_fac.res created by SHELXL-2018/3 at 09:54:29 on 03-Jul-2020 REM Cc (#9 in standard setting) CELL 0.71073 25.8944 6.9439 6.1499 90 91.381 90 ZERR 4 0.0013 0.0004 0.0004 0 0.005 0 LATT -7 SYMM +X,-Y,0.5+Z SFAC C H Br N O UNIT 52 40 4 4 4 L.S. 4 PLAN 5 SIZE 0.58 0.49 0.22 TEMP -123(2) HTAB O1 N1 MPLA 6 C1 C2 C3 C4 C5 C6 MPLA 6 C8 C9 C10 C11 C12 C13 MPLA 5 O1 N1 C7 C6 C1 CONF GRID BOND $H HTAB 2.0 MORE -1 fmap 2 acta 60 MERG 2 SHEL 99999 0.8 REM REM REM WGHT 0.067000 FVAR 3.17719 BR1 3 0.157290 0.683165 0.232370 11.00000 0.02122 0.03457 = 0.02762 -0.00229 -0.00355 0.00002 C5 1 0.265458 0.683406 0.321901 11.00000 0.01981 0.01720 = 0.02277 0.00189 0.00016 -0.00030 AFIX 43 H5 2 0.268030 0.635213 0.177996 11.00000 -1.20000 AFIX 0 C2 1 0.257669 0.822851 0.746158 11.00000 0.03022 0.01573 = 0.01740 0.00028 0.00128 -0.00369 AFIX 43 H2 2 0.254820 0.870832 0.890033 11.00000 -1.20000 AFIX 0 C4 1 0.217600 0.718861 0.407346 11.00000 0.02519 0.01966 = 0.01781 0.00030 -0.00011 -0.00319 C3 1 0.213098 0.789464 0.618869 11.00000 0.02460 0.01983 = 0.02397 0.00152 0.00509 0.00351 AFIX 43 H3 2 0.179986 0.814594 0.675762 11.00000 -1.20000 AFIX 0 C6 1 0.310498 0.718873 0.448666 11.00000 0.02504 0.01654 = 0.01977 -0.00022 -0.00070 0.00115 O1 5 0.348065 0.818960 0.791948 11.00000 0.02265 0.03479 = 0.02075 -0.00458 -0.00404 0.00020 H1 2 0.374988 0.788748 0.719793 11.00000 -1.20000 N1 4 0.402794 0.727628 0.460339 11.00000 0.02488 0.02006 = 0.01999 0.00114 -0.00018 0.00280 C7 1 0.360941 0.696931 0.349563 11.00000 0.02509 0.01653 = 0.02012 0.00029 0.00115 -0.00003 AFIX 43 H7 2 0.362760 0.659495 0.201366 11.00000 -1.20000 AFIX 0 C1 1 0.305904 0.786290 0.663416 11.00000 0.02653 0.01660 = 0.02104 0.00384 -0.00139 -0.00141 C8 1 0.451051 0.733252 0.359258 11.00000 0.02416 0.01383 = 0.02227 -0.00055 -0.00021 -0.00033 C10 1 0.506210 0.831858 0.068669 11.00000 0.02675 0.01927 = 0.02166 0.00028 0.00267 -0.00235 AFIX 43 H10 2 0.510473 0.889386 -0.069899 11.00000 -1.20000 AFIX 0 C9 1 0.456866 0.817134 0.154573 11.00000 0.02290 0.01750 = 0.02467 -0.00075 -0.00228 -0.00063 AFIX 43 H9 2 0.427585 0.863641 0.074706 11.00000 -1.20000 AFIX 0 C12 1 0.542729 0.679100 0.387977 11.00000 0.02006 0.02288 = 0.03131 -0.00068 -0.00446 0.00059 AFIX 43 H12 2 0.571957 0.630545 0.466579 11.00000 -1.20000 AFIX 0 C13 1 0.494017 0.666140 0.476351 11.00000 0.02643 0.01840 = 0.02104 -0.00051 -0.00744 -0.00130 AFIX 43 H13 2 0.490036 0.611519 0.616581 11.00000 -1.20000 AFIX 0 C11 1 0.548929 0.763109 0.184285 11.00000 0.02609 0.01562 = 0.03555 -0.00060 0.00418 -0.00496 AFIX 43 H11 2 0.582359 0.773163 0.124973 11.00000 -1.20000 AFIX 0 HKLF 4 REM test_fac in Cc REM wR2 = 0.0995, GooF = S = 1.053, Restrained GooF = 1.052 for all data REM R1 = 0.0390 for 2142 Fo > 4sig(Fo) and 0.0420 for all 2254 data REM 148 parameters refined using 2 restraints END WGHT 0.0670 0.0000 REM Instructions for potential hydrogen bonds HTAB O1 N1 REM Highest difference peak 0.950, deepest hole -0.343, 1-sigma level 0.081 Q1 1 0.1210 0.6963 0.2366 11.00000 0.05 0.95 Q2 1 0.1923 0.6874 0.2260 11.00000 0.05 0.88 Q3 1 0.1572 1.0523 0.7299 11.00000 0.05 0.44 Q4 1 0.2918 0.6951 0.3758 11.00000 0.05 0.33 Q5 1 0.1284 0.5716 0.3112 11.00000 0.05 0.31 ; _shelx_res_checksum 85371 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' 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 Br Br1 0.15729(2) 0.68317(7) 0.23237(2) 0.0279(2) Uani d 1 . . C C5 0.2655(3) 0.6834(8) 0.3219(12) 0.0199(13) Uani d 1 . . H H5 0.268030 0.635213 0.177996 0.024 Uiso calc 1 . . C C2 0.2577(3) 0.8229(8) 0.7462(12) 0.0211(15) Uani d 1 . . H H2 0.254820 0.870832 0.890033 0.025 Uiso calc 1 . . C C4 0.2176(3) 0.7189(9) 0.4073(11) 0.0209(13) Uani d 1 . . C C3 0.2131(3) 0.7895(8) 0.6189(12) 0.0227(13) Uani d 1 . . H H3 0.179986 0.814594 0.675762 0.027 Uiso calc 1 . . C C6 0.3105(3) 0.7189(9) 0.4487(11) 0.0205(13) Uani d 1 . . O O1 0.3481(2) 0.8190(6) 0.7919(9) 0.0261(11) Uani d 1 . . H H1 0.375(4) 0.789(12) 0.720(18) 0.031 Uiso d 1 . . N N1 0.4028(3) 0.7276(11) 0.4603(12) 0.0217(14) Uani d 1 . . C C7 0.3609(3) 0.6969(8) 0.3496(12) 0.0206(13) Uani d 1 . . H H7 0.362760 0.659495 0.201366 0.025 Uiso calc 1 . . C C1 0.3059(3) 0.7863(8) 0.6634(12) 0.0214(13) Uani d 1 . . C C8 0.4511(3) 0.7333(9) 0.3593(11) 0.0201(12) Uani d 1 . . C C10 0.5062(3) 0.8319(8) 0.0687(12) 0.0225(14) Uani d 1 . . H H10 0.510473 0.889386 -0.069899 0.027 Uiso calc 1 . . C C9 0.4569(3) 0.8171(8) 0.1546(12) 0.0217(14) Uani d 1 . . H H9 0.427585 0.863641 0.074706 0.026 Uiso calc 1 . . C C12 0.5427(3) 0.6791(9) 0.3880(13) 0.0248(15) Uani d 1 . . H H12 0.571957 0.630545 0.466579 0.030 Uiso calc 1 . . C C13 0.4940(3) 0.6661(8) 0.4764(12) 0.0221(14) Uani d 1 . . H H13 0.490036 0.611519 0.616581 0.027 Uiso calc 1 . . C C11 0.5489(3) 0.7631(11) 0.1843(13) 0.0257(15) Uani d 1 . . H H11 0.582359 0.773163 0.124973 0.031 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 Br1 0.0212(3) 0.0346(3) 0.0276(3) 0.0000(4) -0.0036(2) -0.0023(4) C5 0.020(3) 0.017(3) 0.023(4) 0.000(2) 0.000(3) 0.002(2) C2 0.030(4) 0.016(3) 0.017(4) -0.004(3) 0.001(3) 0.000(2) C4 0.025(3) 0.020(3) 0.018(3) -0.003(2) 0.000(2) 0.000(2) C3 0.025(3) 0.020(3) 0.024(3) 0.004(2) 0.005(3) 0.002(2) C6 0.025(3) 0.017(3) 0.020(3) 0.001(2) -0.001(2) 0.000(2) O1 0.023(3) 0.035(3) 0.021(3) 0.0002(19) -0.004(2) -0.0046(19) N1 0.025(3) 0.020(3) 0.020(3) 0.003(2) 0.000(2) 0.001(2) C7 0.025(4) 0.017(3) 0.020(3) 0.000(2) 0.001(3) 0.000(2) C1 0.027(4) 0.017(3) 0.021(3) -0.001(2) -0.001(3) 0.004(2) C8 0.024(3) 0.014(3) 0.022(3) 0.000(2) 0.000(2) -0.001(2) C10 0.027(4) 0.019(3) 0.022(3) -0.002(2) 0.003(3) 0.000(2) C9 0.023(3) 0.017(3) 0.025(4) -0.001(2) -0.002(3) -0.001(2) C12 0.020(4) 0.023(3) 0.031(4) 0.001(2) -0.004(3) -0.001(2) C13 0.026(4) 0.018(3) 0.021(4) -0.001(2) -0.007(3) -0.001(2) C11 0.026(4) 0.016(4) 0.036(4) -0.005(3) 0.004(3) -0.001(3) 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' Br Br -0.2901 2.4595 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 3 7 -6 0.3239 -15 7 5 0.2211 15 -7 -5 0.2211 -9 10 -1 0.3028 1 0 0 0.0777 -1 0 0 0.0777 -3 -7 6 0.2449 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C4 C5 H5 . . 120.1 ? C4 C5 C6 . . 119.8(6) ? C6 C5 H5 . . 120.1 ? C3 C2 H2 . . 119.9 ? C1 C2 H2 . . 119.9 ? C1 C2 C3 . . 120.3(7) ? C5 C4 Br1 . . 119.8(5) ? C5 C4 C3 . . 120.9(6) ? C3 C4 Br1 . . 119.3(5) ? C2 C3 H3 . . 120.2 ? C4 C3 C2 . . 119.5(6) ? C4 C3 H3 . . 120.2 ? C5 C6 C7 . . 119.1(6) ? C5 C6 C1 . . 119.3(6) ? C1 C6 C7 . . 121.4(6) ? C1 O1 H1 . . 108(7) ? C7 N1 C8 . . 121.1(7) ? C6 C7 H7 . . 119.6 ? N1 C7 C6 . . 120.8(7) ? N1 C7 H7 . . 119.6 ? C2 C1 C6 . . 120.2(7) ? O1 C1 C2 . . 118.5(7) ? O1 C1 C6 . . 121.2(6) ? C9 C8 N1 . . 121.6(7) ? C13 C8 N1 . . 118.0(7) ? C13 C8 C9 . . 120.2(6) ? C9 C10 H10 . . 119.8 ? C11 C10 H10 . . 119.8 ? C11 C10 C9 . . 120.4(7) ? C8 C9 H9 . . 120.3 ? C10 C9 C8 . . 119.3(7) ? C10 C9 H9 . . 120.3 ? C13 C12 H12 . . 119.9 ? C13 C12 C11 . . 120.3(7) ? C11 C12 H12 . . 119.9 ? C8 C13 H13 . . 120.0 ? C12 C13 C8 . . 119.9(7) ? C12 C13 H13 . . 120.0 ? C10 C11 C12 . . 119.8(7) ? C10 C11 H11 . . 120.1 ? C12 C11 H11 . . 120.1 ? 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 Br1 C4 . 1.891(7) ? C5 H5 . 0.9500 ? C5 C4 . 1.380(10) ? C5 C6 . 1.409(10) ? C2 H2 . 0.9500 ? C2 C3 . 1.398(11) ? C2 C1 . 1.383(11) ? C4 C3 . 1.398(9) ? C3 H3 . 0.9500 ? C6 C7 . 1.463(9) ? C6 C1 . 1.409(10) ? O1 H1 . 0.86(11) ? O1 C1 . 1.351(9) ? N1 C7 . 1.284(10) ? N1 C8 . 1.410(10) ? C7 H7 . 0.9500 ? C8 C9 . 1.398(10) ? C8 C13 . 1.391(10) ? C10 H10 . 0.9500 ? C10 C9 . 1.398(10) ? C10 C11 . 1.385(11) ? C9 H9 . 0.9500 ? C12 H12 . 0.9500 ? C12 C13 . 1.388(11) ? C12 C11 . 1.395(11) ? C13 H13 . 0.9500 ? C11 H11 . 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 O1 H1 N1 . 0.86(11) 1.82(11) 2.590(10) 148(10) 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 Br1 C4 C3 C2 . . . . -177.7(5) ? C5 C4 C3 C2 . . . . -0.6(9) ? C5 C6 C7 N1 . . . . -179.8(6) ? C5 C6 C1 C2 . . . . -2.0(9) ? C5 C6 C1 O1 . . . . 178.8(5) ? C4 C5 C6 C7 . . . . -174.6(6) ? C4 C5 C6 C1 . . . . 1.4(9) ? C3 C2 C1 C6 . . . . 1.3(9) ? C3 C2 C1 O1 . . . . -179.5(5) ? C6 C5 C4 Br1 . . . . 176.9(4) ? C6 C5 C4 C3 . . . . -0.1(9) ? N1 C8 C9 C10 . . . . 175.2(6) ? N1 C8 C13 C12 . . . . -176.3(6) ? C7 C6 C1 C2 . . . . 173.9(5) ? C7 C6 C1 O1 . . . . -5.2(9) ? C7 N1 C8 C9 . . . . 38.4(11) ? C7 N1 C8 C13 . . . . -146.6(7) ? C1 C2 C3 C4 . . . . 0.0(9) ? C1 C6 C7 N1 . . . . 4.2(10) ? C8 N1 C7 C6 . . . . -171.0(6) ? C9 C8 C13 C12 . . . . -1.2(9) ? C9 C10 C11 C12 . . . . -0.2(10) ? C13 C8 C9 C10 . . . . 0.3(9) ? C13 C12 C11 C10 . . . . -0.7(10) ? C11 C10 C9 C8 . . . . 0.4(9) ? C11 C12 C13 C8 . . . . 1.5(10) ? _cod_database_fobs_code 2022296