#------------------------------------------------------------------------------ #$Date: 2022-02-09 11:17:47 +0200 (Wed, 09 Feb 2022) $ #$Revision: 272870 $ #$URL: file:///home/coder/svn-repositories/cod/cif/8/10/45/8104550.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_8104550 loop_ _publ_author_name 'Cui, Mengbing' 'Zeng, Yan' 'Li, Yong' 'Chen, Heng' _publ_section_title ; The crystal structure of 6-amino-2-carboxypyridin-1-ium bromide, C6H7BrN2O2 ; _journal_issue 6 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 1145 _journal_page_last 1146 _journal_paper_doi 10.1515/ncrs-2021-0251 _journal_volume 236 _journal_year 2021 _chemical_formula_moiety 'Br, C6 H7 N2 O2' _chemical_formula_sum 'C6 H7 Br N2 O2' _chemical_formula_weight 219.05 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 127.291(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 23.7470(19) _cell_length_b 5.4355(4) _cell_length_c 15.3336(11) _cell_measurement_reflns_used 2591 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25.65 _cell_measurement_theta_min 3.34 _cell_volume 1574.6(2) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015) [1]' _computing_data_collection 'Bruker APEX-II' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015) [1]' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009) [2]' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009) [2]' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015) [3]' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018) [4]' _diffrn_ambient_temperature 150.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10308 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.386 _diffrn_reflns_theta_min 2.156 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.171 _exptl_absorpt_correction_T_max 0.0932 _exptl_absorpt_correction_T_min 0.0528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1067 before and 0.0583 after correction. The Ratio of minimum to maximum transmission is 0.5665. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.848 _exptl_crystal_description block _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.431 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.114 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 104 _refine_ls_number_reflns 1605 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0292 _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^)+(0.0284P)^2^+3.4883P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.0756 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1263 _reflns_number_total 1605 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file suppl_j_ncrs-2021-0251_suppl.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 8104550 _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_max 0.626 _shelx_estimated_absorpt_t_min 0.424 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups, All N(H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), N2(H2) 2.b X=CH2 refined with riding coordinates: N1(H1A,H1B) ; _shelx_res_file ; TITL 1.res in C2/c 1.res created by SHELXL-2018/3 at 21:14:39 on 19-Jun-2021 CELL 0.71073 23.747 5.4355 15.3336 90 127.291 90 ZERR 8 0.0019 0.0004 0.0011 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Br O N UNIT 48 56 8 16 16 L.S. 10 PLAN 10 SIZE 0.2 0.15 0.1 TEMP -123.15 CONF BOND $H MORE -1 fmap 2 acta REM REM REM WGHT 0.028400 3.488300 FVAR 0.23989 BR1 3 0.356292 0.700450 0.181864 11.00000 0.03251 0.02805 = 0.02453 -0.00136 0.01617 -0.00039 C1 1 0.354215 0.221203 0.349397 11.00000 0.02793 0.02491 = 0.02134 0.00279 0.01446 -0.00138 C2 1 0.383421 0.399768 0.441538 11.00000 0.02492 0.02541 = 0.01937 0.00164 0.01198 -0.00159 C3 1 0.450418 0.402816 0.535066 11.00000 0.02529 0.02831 = 0.02063 0.00464 0.01153 0.00203 AFIX 43 H3 2 0.483723 0.281395 0.548937 11.00000 -1.20000 AFIX 0 C4 1 0.469529 0.591815 0.611666 11.00000 0.02057 0.03465 = 0.01715 0.00073 0.00761 -0.00260 AFIX 43 H4 2 0.516490 0.598262 0.677762 11.00000 -1.20000 AFIX 0 C5 1 0.422186 0.763211 0.592475 11.00000 0.02847 0.02929 = 0.01694 -0.00078 0.01166 -0.00127 AFIX 43 H5 2 0.436086 0.890552 0.644345 11.00000 -1.20000 AFIX 0 C6 1 0.351702 0.753449 0.494958 11.00000 0.02941 0.02247 = 0.02107 0.00149 0.01500 -0.00050 H1 2 0.390931 -0.027297 0.324809 11.00000 0.04897 N1 5 0.303121 0.916865 0.471570 11.00000 0.03061 0.03043 = 0.02149 -0.00310 0.01013 0.00295 AFIX 93 H1A 2 0.260270 0.907483 0.409111 11.00000 -1.20000 H1B 2 0.313628 1.035041 0.518458 11.00000 -1.20000 AFIX 0 N2 5 0.335278 0.572158 0.422604 11.00000 0.02125 0.02387 = 0.01563 0.00185 0.00678 0.00073 AFIX 43 H2 2 0.291958 0.564967 0.361020 11.00000 -1.20000 AFIX 0 O1 4 0.401007 0.057666 0.369012 11.00000 0.03209 0.03328 = 0.02684 -0.00609 0.01377 0.00609 O2 4 0.293374 0.234466 0.267868 11.00000 0.02425 0.02833 = 0.02042 -0.00030 0.00896 -0.00198 HKLF 4 REM 1.res in C2/c REM wR2 = 0.0756, GooF = S = 1.092, Restrained GooF = 1.092 for all data REM R1 = 0.0292 for 1263 Fo > 4sig(Fo) and 0.0461 for all 1605 data REM 104 parameters refined using 0 restraints END WGHT 0.0284 3.4884 REM Highest difference peak 0.431, deepest hole -0.500, 1-sigma level 0.114 Q1 1 0.4547 0.5279 0.5609 11.00000 0.05 0.43 Q2 1 0.5000 0.5000 0.5000 10.50000 0.05 0.40 Q3 1 0.5268 0.2962 0.5066 11.00000 0.05 0.37 Q4 1 0.5003 0.5209 0.7180 11.00000 0.05 0.35 Q5 1 0.5348 0.1475 0.6981 11.00000 0.05 0.34 Q6 1 0.5071 0.5237 0.6378 11.00000 0.05 0.34 Q7 1 0.5448 0.3419 0.7523 11.00000 0.05 0.34 Q8 1 0.4064 -0.1016 0.2573 11.00000 0.05 0.33 Q9 1 0.4079 0.8792 0.1814 11.00000 0.05 0.33 Q10 1 0.4985 0.9885 0.6726 11.00000 0.05 0.32 ; _shelx_res_checksum 20637 _shelx_hkl_file ; 2 0 0 97.89 6.50 -4 0 0 5129.59 154.28 4 0 0 5049.49 154.18 4 0 0 5136.39 154.48 -4 0 0 5158.98 154.28 6 0 0 1683.03 57.19 -6 0 0 1659.23 56.79 6 0 0 1705.33 57.09 8 0 0 259.37 17.00 8 0 0 256.97 18.30 -8 0 0 267.57 18.00 -8 0 0 279.87 17.50 10 0 0 1086.19 44.10 -10 0 0 1073.39 43.30 -10 0 0 1103.79 43.70 -12 0 0 180.98 18.20 12 0 0 159.58 18.40 12 0 0 149.69 17.40 -12 0 0 168.58 18.70 -14 0 0 1012.30 44.80 -14 0 0 1005.90 44.70 14 0 0 1162.98 62.89 14 0 0 988.70 45.80 16 0 0 218.78 24.10 16 0 0 247.08 23.90 -16 0 0 236.08 34.80 -16 0 0 263.97 39.10 18 0 0 432.66 32.80 -18 0 0 430.86 30.10 18 0 0 417.96 32.70 -18 0 0 450.85 31.20 20 0 0 323.87 29.10 20 0 0 337.87 29.20 -20 0 0 378.66 28.00 -20 0 0 324.17 29.70 22 0 0 3.00 16.30 22 0 0 -10.10 14.00 -22 0 0 5.50 13.00 -22 0 0 35.20 24.00 1 -1 0 448.06 15.80 -1 -1 0 446.26 14.90 -1 -1 0 357.06 16.00 -1 1 0 458.25 16.00 1 1 0 429.56 14.80 1 1 0 444.26 15.00 -1 1 0 450.65 15.80 -3 -1 0 12.00 3.10 3 -1 0 15.90 5.00 3 -1 0 10.00 4.80 -3 -1 0 9.40 2.90 3 1 0 8.70 2.80 -3 1 0 20.70 5.50 -3 1 0 19.00 5.00 3 1 0 12.30 3.50 -5 -1 0 8.20 4.10 5 -1 0 9.50 6.60 5 -1 0 14.40 6.60 5 1 0 13.30 4.40 -5 1 0 19.40 6.50 5 1 0 13.90 4.40 -5 1 0 7.80 5.40 7 -1 0 808.72 33.60 7 -1 0 781.52 44.30 -7 -1 0 784.92 30.60 -7 1 0 784.52 32.60 -7 1 0 811.92 36.20 7 1 0 851.21 31.20 7 1 0 804.62 30.70 9 -1 0 250.87 19.10 -9 -1 0 238.18 15.90 -9 -1 0 245.98 16.50 9 -1 0 255.97 18.80 9 1 0 240.28 17.00 -9 1 0 254.57 18.40 -9 1 0 273.67 20.90 9 1 0 239.88 17.00 -11 -1 0 392.06 23.20 -11 -1 0 437.36 22.90 11 -1 0 378.36 25.10 11 -1 0 389.46 24.70 11 1 0 396.06 23.00 11 1 0 378.16 22.30 -11 1 0 401.76 24.50 -11 1 0 383.26 24.20 13 -1 0 24.10 11.20 -13 -1 0 49.40 12.20 -13 -1 0 38.60 10.80 13 -1 0 37.50 12.80 -13 1 0 49.00 12.10 13 1 0 33.30 10.20 13 1 0 30.50 11.20 -13 1 0 21.30 10.40 -15 -1 0 -7.90 9.50 -15 -1 0 6.40 11.20 15 -1 0 -2.50 10.90 15 -1 0 -20.70 12.00 15 1 0 6.00 10.40 15 1 0 9.70 11.30 -15 1 0 -10.20 10.20 -15 1 0 4.30 10.00 -17 -1 0 23.10 11.70 17 -1 0 1.80 12.90 -17 -1 0 0.30 11.70 17 -1 0 8.90 14.80 17 1 0 10.20 12.80 -17 1 0 18.60 14.40 -17 1 0 2.10 11.80 17 1 0 13.10 13.40 -19 -1 0 -3.60 9.40 19 -1 0 0.60 14.20 -19 -1 0 -5.40 12.50 19 -1 0 -3.20 13.90 -19 1 0 2.00 13.20 -19 1 0 -8.60 10.90 19 1 0 -5.90 13.00 19 1 0 -6.90 13.20 21 -1 0 3.10 16.60 -21 -1 0 -0.80 11.50 -21 -1 0 2.60 13.60 21 -1 0 9.30 14.90 21 1 0 12.60 15.00 21 1 0 -17.60 12.70 -21 1 0 -13.00 11.80 -21 1 0 4.70 14.70 23 -1 0 14.30 17.80 -23 -1 0 18.10 30.40 -23 -1 0 10.90 14.10 23 -1 0 24.70 18.60 -23 1 0 0.00 15.40 -23 1 0 32.70 16.80 23 1 0 12.60 29.60 23 1 0 -10.00 15.20 0 -2 0 1915.91 60.79 0 2 0 1902.91 60.89 0 2 0 1969.20 61.19 2 -2 0 298.37 14.50 -2 -2 0 291.87 12.80 2 -2 0 323.67 14.70 -2 -2 0 287.17 13.00 -2 2 0 287.17 14.30 -2 2 0 294.07 14.70 2 2 0 304.97 13.20 2 2 0 273.97 12.70 -4 -2 0 1152.08 38.10 4 -2 0 1179.48 41.70 4 -2 0 1163.38 41.00 -4 -2 0 1135.49 37.90 4 2 0 1157.38 38.20 -4 2 0 1156.78 41.20 -4 2 0 1182.48 41.50 4 2 0 1096.69 37.80 6 -2 0 654.13 29.00 -6 -2 0 640.14 24.50 -6 -2 0 602.04 24.00 6 -2 0 706.03 28.90 -6 2 0 647.14 28.50 6 2 0 645.24 24.50 6 2 0 663.83 24.50 -6 2 0 667.53 28.40 -8 -2 0 351.46 17.60 8 -2 0 371.16 21.50 8 -2 0 345.37 31.50 -8 -2 0 333.97 16.80 8 2 0 359.06 17.70 8 2 0 348.37 17.20 -8 2 0 293.67 20.30 -8 2 0 339.27 20.70 10 -2 0 961.00 41.80 -10 -2 0 937.81 37.00 10 -2 0 958.70 42.20 10 2 0 932.81 37.00 -10 2 0 899.31 40.40 10 2 0 1008.00 37.40 -10 2 0 915.61 41.00 -12 -2 0 46.60 10.00 12 -2 0 11.00 11.50 12 -2 0 20.10 11.30 -12 2 0 28.90 11.40 -12 2 0 14.20 10.00 12 2 0 24.60 9.60 12 2 0 18.80 9.10 14 -2 0 1229.78 55.49 14 -2 0 1154.18 52.89 14 2 0 1192.48 49.00 -14 2 0 1218.28 52.59 -14 2 0 1187.18 52.89 14 2 0 1197.68 49.60 16 -2 0 34.90 16.20 16 -2 0 53.19 16.90 -16 2 0 49.30 14.70 16 2 0 40.20 12.80 -16 2 0 92.09 17.20 16 2 0 43.80 12.90 18 -2 0 251.27 33.60 18 -2 0 345.67 30.80 -18 -2 0 289.67 26.30 18 2 0 273.27 26.30 -18 2 0 279.47 28.60 18 2 0 295.07 26.70 -18 2 0 299.47 27.70 -20 -2 0 49.30 16.40 -20 -2 0 83.79 16.20 20 -2 0 89.99 22.00 -20 2 0 102.69 19.20 -20 2 0 95.69 19.10 20 2 0 82.49 17.60 20 2 0 77.89 17.90 22 -2 0 -12.70 18.10 -22 -2 0 3.20 12.70 22 -2 0 32.10 18.50 -22 2 0 -6.50 16.40 -22 2 0 -3.20 14.10 22 2 0 -0.70 14.90 -1 -3 0 497.45 20.70 -1 -3 0 477.95 21.00 1 -3 0 477.75 21.30 -1 3 0 479.15 21.50 1 3 0 476.95 21.00 -1 3 0 490.85 21.90 1 3 0 470.95 20.50 3 -3 0 633.24 27.00 -3 -3 0 569.14 22.90 -3 -3 0 575.14 23.50 3 -3 0 555.94 24.80 -3 3 0 592.14 25.90 3 3 0 570.34 23.30 3 3 0 584.74 23.30 -3 3 0 593.34 26.00 5 -3 0 135.99 13.90 -5 -3 0 117.69 9.60 -5 -3 0 109.69 10.00 5 -3 0 114.29 13.10 -5 3 0 112.39 12.70 5 3 0 104.59 9.40 5 3 0 95.29 9.50 -5 3 0 126.89 13.80 7 -3 0 722.73 32.50 7 -3 0 724.13 34.00 -7 -3 0 740.13 28.00 -7 -3 0 727.53 28.00 -7 3 0 682.03 33.20 7 3 0 721.73 28.00 7 3 0 717.93 28.50 -7 3 0 724.43 32.70 -9 -3 0 12.10 5.90 9 -3 0 18.90 11.60 9 -3 0 11.80 9.90 -9 -3 0 20.10 6.90 9 3 0 9.30 6.80 -9 3 0 7.30 9.50 -9 3 0 23.10 10.40 9 3 0 21.70 6.70 -11 -3 0 353.56 20.00 11 -3 0 311.77 25.60 11 -3 0 343.67 25.20 -11 -3 0 325.07 18.80 -11 3 0 316.57 24.10 -11 3 0 328.87 24.10 11 3 0 310.17 19.40 11 3 0 330.37 19.10 13 -3 0 94.79 17.10 -13 -3 0 87.39 12.20 13 -3 0 67.79 17.30 -13 -3 0 77.79 12.20 -13 3 0 80.69 17.00 -13 3 0 84.49 17.00 13 3 0 80.09 12.90 -15 -3 0 36.70 11.00 15 -3 0 59.49 19.40 -15 3 0 32.40 14.20 15 3 0 49.80 11.60 15 3 0 33.30 12.00 -15 3 0 15.40 13.10 -17 -3 0 108.89 15.50 -17 -3 0 157.48 17.10 17 -3 0 89.29 20.60 17 -3 0 65.79 19.60 17 3 0 116.69 17.10 17 3 0 96.79 16.80 -17 3 0 94.49 21.40 19 -3 0 5.40 16.70 -19 -3 0 15.90 11.20 19 -3 0 -12.80 16.40 19 3 0 2.30 11.20 -19 3 0 7.60 14.90 19 3 0 22.00 13.60 -19 3 0 -10.90 12.70 21 -3 0 68.19 21.50 21 -3 0 118.99 27.00 -21 -3 0 78.09 26.90 -21 -3 0 59.99 16.30 -21 3 0 94.39 21.50 21 3 0 93.89 19.20 -21 3 0 94.29 22.30 21 3 0 87.69 18.00 0 -4 0 177.18 14.90 0 -4 0 187.48 13.90 0 4 0 181.28 14.40 0 4 0 202.58 14.80 2 -4 0 47.90 9.00 -2 -4 0 60.29 9.60 -2 -4 0 57.19 8.50 2 4 0 55.89 9.40 -2 4 0 50.79 10.20 2 4 0 82.99 10.20 -2 4 0 73.69 11.20 4 -4 0 173.48 15.50 -4 -4 0 146.79 12.00 -4 -4 0 160.38 13.30 4 -4 0 158.88 17.50 4 4 0 139.99 12.40 -4 4 0 158.28 15.80 4 4 0 134.19 12.30 -4 4 0 162.78 16.00 -6 -4 0 46.10 8.60 6 -4 0 43.20 9.80 6 -4 0 61.49 13.60 -6 -4 0 51.29 8.30 6 4 0 37.90 7.90 6 4 0 50.29 8.50 -6 4 0 39.70 11.40 -6 4 0 36.50 11.30 -8 -4 0 21.50 7.90 8 -4 0 6.50 15.50 8 -4 0 34.70 14.60 8 4 0 12.40 6.90 8 4 0 16.80 7.90 -8 4 0 30.00 10.80 -8 4 0 23.20 11.60 -10 -4 0 37.10 8.70 10 -4 0 41.20 14.70 10 -4 0 56.69 13.70 10 4 0 40.70 9.60 -10 4 0 29.60 13.20 -10 4 0 26.80 12.20 12 -4 0 -18.30 12.80 -12 -4 0 4.50 8.70 12 -4 0 6.10 12.00 12 4 0 -2.30 6.80 12 4 0 2.00 8.30 -12 4 0 9.10 12.90 -12 4 0 8.00 11.20 -14 -4 0 165.98 21.90 14 -4 0 157.88 21.80 14 -4 0 199.08 26.80 -14 -4 0 172.18 17.50 -14 4 0 171.48 22.60 14 4 0 151.08 17.90 14 4 0 203.08 16.90 -14 4 0 204.48 25.40 16 -4 0 25.10 17.60 16 -4 0 19.50 17.20 -16 -4 0 19.10 10.00 -16 -4 0 16.50 10.20 -16 4 0 14.70 15.30 -16 4 0 0.70 14.90 16 4 0 13.50 12.30 16 4 0 19.20 9.50 -18 -4 0 36.10 11.70 -18 -4 0 13.90 11.80 18 -4 0 -7.20 18.80 -18 4 0 28.50 17.80 -18 4 0 63.19 17.90 18 4 0 4.90 13.60 18 4 0 38.00 12.70 -1 -5 0 71.69 10.00 1 -5 0 40.40 11.70 -1 -5 0 53.39 11.50 1 5 0 46.80 10.40 -1 5 0 45.10 10.60 -1 5 0 45.80 11.10 1 5 0 39.60 10.50 -3 -5 0 336.37 21.40 -3 -5 0 397.16 20.50 3 -5 0 363.46 30.10 -3 5 0 392.76 25.00 3 5 0 332.27 20.10 -3 5 0 363.86 23.90 3 5 0 392.66 21.80 -5 -5 0 17.60 7.30 5 -5 0 12.70 12.00 5 5 0 10.30 7.70 5 5 0 6.20 7.50 -5 5 0 11.50 10.00 -5 5 0 11.10 9.20 7 -5 0 306.57 23.60 7 -5 0 318.87 26.30 -7 -5 0 344.67 19.80 7 5 0 280.77 18.60 -7 5 0 284.37 24.50 -7 5 0 319.87 24.90 9 -5 0 21.00 12.30 -9 -5 0 15.20 8.30 -9 5 0 4.60 10.30 9 5 0 1.60 7.00 -9 5 0 11.40 11.70 11 -5 0 101.59 18.60 -11 -5 0 131.49 14.40 11 -5 0 109.89 20.80 -11 -5 0 119.49 12.90 -11 5 0 114.89 19.20 11 5 0 139.39 14.20 -11 5 0 92.79 17.50 11 5 0 126.09 14.30 13 -5 0 79.49 22.00 -13 -5 0 103.49 12.50 13 -5 0 72.79 17.80 -13 -5 0 85.19 12.60 13 5 0 126.39 15.60 13 5 0 112.49 13.40 -13 5 0 98.89 20.00 -13 5 0 92.39 18.20 15 -5 0 59.09 21.90 -15 -5 0 49.20 12.10 15 -5 0 39.20 19.00 -15 -5 0 32.00 10.20 15 5 0 105.49 13.60 15 5 0 61.39 13.60 -15 5 0 75.49 19.10 -15 5 0 78.19 19.10 0 -6 0 86.29 13.10 0 -6 0 54.29 14.70 0 6 0 86.99 14.20 0 6 0 77.49 13.40 2 -6 0 -16.10 7.90 -2 -6 0 -4.40 7.80 2 -6 0 -2.50 11.30 2 6 0 -10.90 7.90 2 6 0 -0.50 8.40 -2 6 0 0.80 9.80 -2 6 0 -5.70 9.40 4 -6 0 4.50 9.70 -4 -6 0 -2.40 7.50 -4 -6 0 -1.90 9.50 -4 6 0 7.80 10.80 4 6 0 8.10 9.20 4 6 0 6.10 8.30 -4 6 0 5.90 10.40 -6 -6 0 14.60 8.60 -6 -6 0 -7.70 8.60 6 -6 0 17.10 15.20 -6 6 0 -3.30 10.30 6 6 0 -8.60 7.80 -6 6 0 -13.10 11.30 -8 -6 0 18.60 8.70 8 -6 0 4.90 12.40 8 -6 0 20.30 17.00 -8 -6 0 32.70 10.00 8 6 0 6.90 9.30 -8 6 0 19.70 13.70 8 6 0 17.50 10.40 -10 -6 0 1.90 9.10 10 -6 0 -4.50 18.60 -10 -6 0 -1.00 9.40 10 -6 0 -1.30 11.60 -10 6 0 0.40 14.80 10 6 0 8.50 8.50 10 6 0 5.90 9.70 -24 0 1 -24.10 15.00 24 0 -1 -38.00 15.90 -24 0 1 -5.50 14.10 24 0 -1 6.60 18.50 22 0 -1 -5.40 13.20 -22 0 1 -2.90 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2.70 11.50 10 2 -17 1.70 12.10 -8 -2 17 58.89 17.50 8 -2 -17 71.29 11.50 8 2 -17 66.19 18.40 -8 2 17 71.09 10.60 -8 2 17 68.59 11.70 8 2 -17 68.69 17.10 -19 -3 17 30.20 16.50 19 -3 -17 14.20 13.40 19 -3 -17 25.10 9.90 -19 -3 17 -3.40 15.40 19 3 -17 10.80 11.40 -19 3 17 24.50 10.60 -17 -3 17 -5.00 13.30 -17 -3 17 10.60 14.20 17 -3 -17 18.30 8.70 17 -3 -17 6.70 11.30 -17 3 17 -18.60 10.70 17 3 -17 6.10 14.80 -15 -3 17 146.09 22.10 -15 -3 17 105.79 20.60 15 -3 -17 46.60 13.60 15 -3 -17 87.09 10.70 -15 3 17 71.09 13.60 -15 3 17 99.79 12.40 15 3 -17 80.99 16.50 13 -3 -17 1.70 6.40 -13 -3 17 2.60 15.60 -13 -3 17 -16.40 13.20 13 3 -17 4.30 13.00 -13 3 17 15.30 8.00 -13 3 17 16.50 9.60 13 3 -17 35.90 14.70 -24 0 18 -5.80 13.50 -24 0 18 5.00 18.20 24 0 -18 8.80 13.90 24 0 -18 11.40 13.40 -22 0 18 256.47 25.30 22 0 -18 271.77 25.70 -22 0 18 279.77 25.30 22 0 -18 177.48 22.40 -20 0 18 112.39 17.90 -20 0 18 85.29 16.50 20 0 -18 67.89 16.20 20 0 -18 43.70 15.00 -18 0 18 33.90 12.90 18 0 -18 39.40 14.80 18 0 -18 39.40 12.50 16 0 -18 218.78 21.70 16 0 -18 232.08 24.10 -16 0 18 236.08 22.20 -16 0 18 237.98 22.70 14 0 -18 7.90 10.50 -14 0 18 20.10 11.20 -14 0 18 20.80 11.50 -12 0 18 199.88 21.40 -10 0 18 37.40 12.40 -10 0 18 30.70 14.80 10 0 -18 23.40 13.30 10 0 -18 38.30 12.80 -23 -1 18 30.40 15.00 23 -1 -18 37.50 13.10 -23 -1 18 60.09 14.90 23 -1 -18 20.70 15.30 23 1 -18 39.00 15.70 -23 1 18 29.60 15.20 23 1 -18 45.60 15.90 -23 1 18 20.20 14.00 -21 -1 18 -16.90 11.30 21 -1 -18 13.80 11.70 -21 -1 18 -6.60 10.80 21 -1 -18 6.50 12.90 -21 1 18 0.50 10.00 21 1 -18 -24.30 12.50 21 1 -18 26.50 13.20 -19 -1 18 20.30 13.40 19 -1 -18 21.50 12.90 -19 -1 18 23.10 11.90 19 -1 -18 -1.00 14.80 -19 1 18 6.30 10.60 -19 1 18 10.60 11.20 19 1 -18 23.10 14.80 19 1 -18 23.90 11.40 -17 -1 18 11.30 12.00 17 -1 -18 6.40 9.20 -17 -1 18 23.50 12.80 17 -1 -18 -3.40 11.80 -17 1 18 6.90 9.40 17 1 -18 19.50 12.20 -17 1 18 2.00 10.10 15 -1 -18 22.70 10.10 15 -1 -18 24.10 12.10 -15 -1 18 17.60 13.80 -15 -1 18 21.40 11.90 15 1 -18 28.70 12.70 -15 1 18 16.90 11.50 -15 1 18 20.30 10.90 13 -1 -18 14.10 9.20 -13 -1 18 8.40 11.60 13 -1 -18 15.60 11.40 -13 -1 18 11.70 13.70 -13 1 18 -4.80 14.80 13 1 -18 32.50 14.20 -13 1 18 -3.20 9.00 13 1 -18 12.30 16.10 -11 -1 18 0.90 11.20 -11 -1 18 11.00 20.90 11 -1 -18 10.10 10.20 11 -1 -18 18.90 11.30 11 1 -18 19.00 11.70 11 1 -18 -4.50 13.50 -11 1 18 5.20 9.50 20 -2 -18 99.29 15.00 -20 -2 18 110.09 22.70 20 -2 -18 112.59 23.70 -20 -2 18 103.99 18.60 20 2 -18 122.59 21.10 -20 2 18 96.99 15.00 20 2 -18 92.89 17.50 -20 2 18 48.70 14.10 18 -2 -18 51.59 15.20 -18 -2 18 78.39 17.20 -18 -2 18 82.39 18.40 18 2 -18 50.19 14.50 -18 2 18 52.99 13.50 -18 2 18 39.70 13.10 16 -2 -18 59.99 14.50 -16 -2 18 92.69 19.40 -16 -2 18 91.69 18.40 16 -2 -18 77.49 12.10 16 2 -18 77.49 18.50 16 2 -18 62.89 16.40 14 -2 -18 8.00 11.00 -14 -2 18 29.80 15.20 -14 -2 18 6.10 13.70 14 -2 -18 25.90 9.20 14 2 -18 -0.90 14.30 14 2 -18 0.30 11.20 -14 2 18 18.50 10.00 20 0 -19 9.40 12.40 -20 0 19 -9.50 11.60 -20 0 19 -6.60 10.80 18 0 -19 2.90 21.90 18 0 -19 12.70 11.20 -18 0 19 21.20 13.60 -18 0 19 13.10 11.80 16 0 -19 2.00 11.50 -16 0 19 1.40 10.20 -16 0 19 1.50 11.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 43911 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.35629(2) 0.70045(7) 0.18186(3) 0.02907(13) Uani 1 1 d . . . . . C1 C 0.35421(19) 0.2212(7) 0.3494(3) 0.0250(8) Uani 1 1 d . . . . . C2 C 0.38342(19) 0.3998(7) 0.4415(3) 0.0242(8) Uani 1 1 d . . . . . C3 C 0.45042(19) 0.4028(7) 0.5351(3) 0.0263(8) Uani 1 1 d . . . . . H3 H 0.483723 0.281395 0.548937 0.032 Uiso 1 1 calc R U . . . C4 C 0.46953(19) 0.5918(7) 0.6117(3) 0.0266(8) Uani 1 1 d . . . . . H4 H 0.516490 0.598262 0.677762 0.032 Uiso 1 1 calc R U . . . C5 C 0.4222(2) 0.7632(7) 0.5925(3) 0.0262(8) Uani 1 1 d . . . . . H5 H 0.436086 0.890552 0.644345 0.031 Uiso 1 1 calc R U . . . C6 C 0.3517(2) 0.7534(6) 0.4950(3) 0.0245(8) Uani 1 1 d . . . . . H1 H 0.391(3) -0.027(9) 0.325(4) 0.049(17) Uiso 1 1 d . . . . . N1 N 0.30312(17) 0.9169(6) 0.4716(2) 0.0311(7) Uani 1 1 d . . . . . H1A H 0.260270 0.907483 0.409111 0.037 Uiso 1 1 calc R U . . . H1B H 0.313628 1.035041 0.518458 0.037 Uiso 1 1 calc R U . . . N2 N 0.33528(15) 0.5722(5) 0.4226(2) 0.0231(7) Uani 1 1 d . . . . . H2 H 0.291958 0.564967 0.361020 0.028 Uiso 1 1 calc R U . . . O1 O 0.40101(15) 0.0577(5) 0.3690(2) 0.0333(7) Uani 1 1 d . . . . . O2 O 0.29337(13) 0.2345(5) 0.26787(19) 0.0273(6) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0325(2) 0.0281(2) 0.0245(2) -0.00136(18) 0.01617(16) -0.00039(19) C1 0.028(2) 0.0249(19) 0.0213(18) 0.0028(15) 0.0145(16) -0.0014(16) C2 0.0249(19) 0.0254(19) 0.0194(17) 0.0016(15) 0.0120(16) -0.0016(16) C3 0.025(2) 0.028(2) 0.0206(17) 0.0046(16) 0.0115(16) 0.0020(16) C4 0.0206(19) 0.035(2) 0.0171(17) 0.0007(16) 0.0076(15) -0.0026(16) C5 0.0285(19) 0.029(2) 0.0169(17) -0.0008(15) 0.0117(15) -0.0013(16) C6 0.029(2) 0.022(2) 0.0211(17) 0.0015(14) 0.0150(16) -0.0005(15) N1 0.0306(18) 0.0304(18) 0.0215(16) -0.0031(14) 0.0101(15) 0.0029(15) N2 0.0213(16) 0.0239(16) 0.0156(14) 0.0018(12) 0.0068(13) 0.0007(13) O1 0.0321(16) 0.0333(17) 0.0268(15) -0.0061(13) 0.0138(13) 0.0061(13) O2 0.0243(14) 0.0283(16) 0.0204(13) -0.0003(11) 0.0090(11) -0.0020(11) 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' O O 0.0106 0.0060 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 C1 C2 112.4(3) . . O2 C1 C2 121.2(3) . . O2 C1 O1 126.4(4) . . C3 C2 C1 125.8(4) . . C3 C2 N2 120.9(3) . . N2 C2 C1 113.3(3) . . C2 C3 H3 121.0 . . C2 C3 C4 118.1(4) . . C4 C3 H3 121.0 . . C3 C4 H4 119.5 . . C5 C4 C3 121.0(3) . . C5 C4 H4 119.5 . . C4 C5 H5 120.0 . . C4 C5 C6 120.0(3) . . C6 C5 H5 120.0 . . N1 C6 C5 122.7(3) . . N1 C6 N2 119.8(3) . . N2 C6 C5 117.5(3) . . C6 N1 H1A 120.0 . . C6 N1 H1B 120.0 . . H1A N1 H1B 120.0 . . C2 N2 H2 118.8 . . C6 N2 C2 122.5(3) . . C6 N2 H2 118.8 . . C1 O1 H1 117(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C2 1.494(5) . C1 O1 1.308(5) . C1 O2 1.211(4) . C2 C3 1.350(5) . C2 N2 1.366(5) . C3 H3 0.9500 . C3 C4 1.412(5) . C4 H4 0.9500 . C4 C5 1.348(5) . C5 H5 0.9500 . C5 C6 1.417(5) . C6 N1 1.322(5) . C6 N2 1.353(4) . N1 H1A 0.8800 . N1 H1B 0.8800 . N2 H2 0.8800 . O1 H1 0.73(4) . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C1 C2 C3 C4 177.6(3) . . . . C1 C2 N2 C6 -178.6(3) . . . . C2 C3 C4 C5 0.5(5) . . . . C3 C2 N2 C6 0.3(5) . . . . C3 C4 C5 C6 0.9(6) . . . . C4 C5 C6 N1 -179.7(3) . . . . C4 C5 C6 N2 -1.7(5) . . . . C5 C6 N2 C2 1.1(5) . . . . N1 C6 N2 C2 179.2(3) . . . . N2 C2 C3 C4 -1.1(5) . . . . O1 C1 C2 C3 1.3(5) . . . . O1 C1 C2 N2 -180.0(3) . . . . O2 C1 C2 C3 -179.2(4) . . . . O2 C1 C2 N2 -0.4(5) . . . .