#------------------------------------------------------------------------------ #$Date: 2025-05-03 21:22:12 +0200 (Sat, 03 May 2025) $ #$Revision: 299528 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/34/2023458.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_2023458 loop_ _publ_author_name 'Lerch, Timothy G.' 'Albert, Daniel R.' 'Gau, Michael' 'Rajaseelan, Edward' _publ_section_title ; Syntheses and crystal structures of 4-benzyl-1-ethyl-1,2,4-triazolium bromide and its corresponding NHC complexes of rhodium and iridium. ; _journal_coeditor_code HB8128 _journal_issue 'Pt 4' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 350 _journal_page_last 357 _journal_paper_doi 10.1107/S2056989025002671 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C11 H14 N3 +, Br -' _chemical_formula_moiety 'C11 H14 N3 +, Br -' _chemical_formula_sum 'C11 H14 Br N3' _chemical_formula_weight 268.16 _chemical_name_systematic ; 4-Benzyl-1-ethyl-1,2,4-triazolium bromide ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _cell_angle_alpha 90 _cell_angle_beta 100.400(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.6908(10) _cell_length_b 4.7431(2) _cell_length_c 12.6482(5) _cell_measurement_reflns_used 7642 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.1790 _cell_measurement_theta_min 2.0890 _cell_volume 1161.88(9) _computing_cell_refinement ; CrysAlisPro 1.171.43.142a (Rigaku OD, 2024) ; _computing_data_collection ; CrysAlisPro 1.171.43.142a (Rigaku OD, 2024) ; _computing_data_reduction ; CrysAlisPro 1.171.43.142a (Rigaku OD, 2024) ; _computing_molecular_graphics ; Olex2 1.3 (Dolomanov et al., 2009) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 10.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_unetI/netI 0.0435 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 22182 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.282 _diffrn_reflns_theta_min 2.103 _exptl_absorpt_coefficient_mu 3.510 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SCALE3 ABSPACK; Rigaku OD, 2024) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.533 _exptl_crystal_description plate _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.396 _refine_diff_density_min -0.576 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 2883 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0383 _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^)+(0.0242P)^2^+1.9068P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.0738 _reflns_number_gt 2356 _reflns_number_total 2883 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8128.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 2023458--2023461.cif.' _cod_database_code 2023458 _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_hkl_file ; 0 0 2 159.78 9.29 0 0 2 171.27 10.78 0 0 -2 165.40 11.01 0 0 -2 205.18 10.86 0 0 2 170.23 10.58 0 0 3 2.18 4.42 0 0 -3 -3.96 6.71 0 0 3 5.68 6.04 0 0 -4 3702.55 175.20 0 0 4 3848.17 175.24 0 0 -4 3970.79 178.18 0 0 4 4070.33 177.37 0 0 5 -3.17 9.00 0 0 -5 0.98 7.31 0 0 5 5.27 6.72 0 0 -5 6.57 9.92 0 0 6 3399.17 154.11 0 0 -6 3235.90 154.45 0 0 -6 3489.54 158.72 0 0 6 3323.58 157.00 0 0 -6 3415.69 157.27 0 0 -7 -3.92 13.76 0 0 7 1.78 8.80 0 0 -7 -4.83 9.52 0 0 -7 5.56 13.53 0 0 7 -1.11 12.23 0 0 -8 431.32 27.55 0 0 -8 485.44 34.40 0 0 8 497.76 27.56 0 0 8 410.24 30.93 0 0 -8 490.07 32.60 0 0 8 441.78 31.43 0 0 -9 -10.16 18.34 0 0 9 -10.56 16.09 0 0 -9 -15.01 19.60 0 0 9 9.51 12.27 0 0 -9 -22.36 13.25 0 0 9 1.43 16.91 0 0 10 924.00 54.49 0 0 -10 946.26 58.43 0 0 -10 923.98 54.79 0 0 -10 872.13 56.02 0 0 10 932.29 48.45 0 0 10 803.31 53.61 0 0 -11 -9.03 26.10 0 0 11 8.71 16.31 0 0 11 7.54 20.73 0 0 -11 -8.20 27.26 0 0 11 -15.80 22.35 0 0 -11 12.60 23.89 0 0 -12 298.70 37.13 0 0 12 238.92 33.36 0 0 12 320.68 34.92 0 0 -12 322.61 35.45 0 0 13 45.31 26.12 0 0 13 24.74 26.73 0 0 -13 63.81 29.97 0 0 14 435.60 44.45 0 0 14 398.82 42.64 0 0 -14 467.41 44.82 0 0 15 2.62 32.18 0 0 15 16.62 32.62 0 0 16 1012.33 73.81 0 0 16 1117.51 74.03 0 -1 0 -2.10 4.51 0 -1 0 1.62 4.24 0 -1 0 0.72 3.54 0 1 1 74.55 8.49 0 -1 -1 75.91 8.76 0 -1 1 84.08 5.65 0 -1 -1 72.35 7.99 0 -1 -1 88.33 8.49 0 -1 -1 81.58 5.78 0 -1 1 69.98 6.90 0 -1 -2 3827.91 171.00 0 1 -2 3752.51 169.53 0 -1 2 3790.64 169.21 0 -1 -2 3708.67 171.78 0 -1 -2 3714.39 170.39 0 1 2 3654.49 171.95 0 -1 -2 3774.04 171.94 0 1 -3 8734.03 380.98 0 -1 -3 7744.35 383.65 0 1 3 8870.15 384.38 0 1 -3 6944.87 382.54 0 -1 3 8922.08 381.87 0 -1 -3 8562.18 384.39 0 1 3 8700.67 384.74 0 -1 3 8878.59 380.73 0 1 -3 8151.99 383.30 0 -1 -3 8636.42 383.28 0 1 -3 8476.96 382.03 0 -1 4 21.20 6.25 0 1 4 31.11 10.04 0 -1 4 17.09 6.14 0 1 -4 17.37 7.52 0 -1 -4 16.97 9.76 0 1 -4 20.64 6.50 0 1 4 25.40 8.98 0 1 -4 27.63 10.03 0 -1 -4 20.66 8.48 0 1 -5 564.84 30.64 0 -1 5 499.17 27.90 0 -1 5 489.15 26.83 0 1 -5 518.40 27.80 0 -1 -5 507.79 30.93 0 1 5 464.94 30.54 0 -1 -5 517.90 29.88 0 1 -5 576.73 31.20 0 -1 -5 511.52 30.12 0 1 -5 474.17 24.07 0 1 5 595.60 30.41 0 -1 -6 272.74 21.12 0 1 6 339.75 21.85 0 1 -6 254.98 14.85 0 1 -6 273.70 22.10 0 1 -6 309.63 20.02 0 -1 -6 318.84 24.07 0 1 6 294.36 23.30 0 -1 6 284.22 18.90 0 -1 -6 281.62 22.50 0 1 -6 333.18 23.48 0 -1 6 251.27 19.60 0 -1 -7 1488.69 75.02 0 1 7 1610.15 75.58 0 1 -7 1393.25 69.16 0 1 -7 1636.11 78.13 0 1 -7 1514.77 74.25 0 -1 7 1462.93 73.07 0 1 7 1487.52 77.44 0 -1 -7 1565.24 77.00 0 1 -7 1543.09 77.47 0 -1 7 1596.71 75.39 0 1 -8 607.79 34.05 0 -1 -8 648.93 40.41 0 1 8 759.17 41.54 0 1 -8 778.32 45.09 0 1 -8 749.76 40.90 0 -1 8 721.57 39.45 0 1 8 748.62 44.06 0 1 -8 698.48 43.75 0 -1 -8 724.34 43.48 0 -1 8 736.87 42.01 0 -1 -9 1178.22 67.11 0 1 9 1327.81 67.91 0 1 -9 1311.13 72.25 0 1 -9 1286.96 67.88 0 1 9 1374.46 71.71 0 -1 9 1281.40 66.77 0 -1 -9 1260.48 70.25 0 1 -9 1305.02 70.98 0 -1 9 1231.45 68.50 0 -1 10 3.14 18.59 0 1 -10 30.37 22.77 0 1 10 -7.46 21.70 0 -1 10 13.81 17.54 0 1 -10 15.17 19.79 0 -1 -10 -7.39 23.10 0 -1 -10 5.42 22.04 0 1 -10 -15.07 23.75 0 1 10 6.39 18.30 0 -1 11 36.87 21.42 0 1 -11 51.25 24.81 0 -1 11 82.50 21.30 0 1 11 95.36 27.24 0 -1 -11 73.07 25.51 0 1 -11 44.72 23.01 0 1 11 56.42 23.91 0 -1 -11 59.91 23.97 0 1 -11 45.58 25.18 0 1 11 36.13 20.95 0 -1 12 83.55 26.22 0 1 12 83.19 28.38 0 -1 12 74.54 24.16 0 1 -12 68.68 29.76 0 -1 -12 47.47 31.39 0 -1 -12 108.23 30.72 0 1 -12 77.99 25.91 0 1 12 84.89 23.89 0 1 -12 92.53 31.02 0 -1 -12 100.05 28.73 0 1 12 77.27 26.65 0 -1 -13 801.75 58.07 0 1 -13 774.14 53.38 0 1 -13 709.10 58.63 0 -1 -13 787.40 59.85 0 1 13 835.27 57.45 0 1 13 805.76 57.37 0 -1 13 746.08 51.58 0 -1 13 734.35 54.46 0 1 13 808.01 50.99 0 1 14 268.93 32.97 0 1 14 308.40 40.63 0 -1 14 246.63 34.42 0 1 14 243.74 38.14 0 1 -14 332.37 39.12 0 -1 -14 312.01 44.25 0 1 -14 330.05 44.20 0 -1 14 323.15 38.22 0 -1 -15 100.84 40.22 0 1 -15 136.68 39.81 0 1 -15 207.90 39.53 0 1 15 126.82 39.23 0 -1 15 136.25 33.43 0 -1 15 110.18 37.31 0 1 15 161.44 38.05 0 -1 16 39.06 35.76 0 1 16 17.77 38.63 0 1 16 58.96 39.26 0 1 -16 46.53 39.52 0 -1 -16 26.91 42.60 0 2 0 444.12 25.11 0 -2 0 457.97 24.13 0 -2 0 412.01 23.11 0 2 0 407.54 23.28 0 -2 0 444.14 23.45 0 2 0 432.16 26.42 0 -2 -1 3899.91 166.83 0 2 1 3589.25 167.17 0 -2 -1 3537.81 169.97 0 2 -1 3581.67 170.63 0 2 -1 3858.65 169.98 0 2 1 3736.59 170.77 0 -2 -1 3887.36 169.86 0 2 -1 3593.69 167.41 0 2 1 3301.23 169.84 0 2 -1 3705.24 167.21 0 -2 1 3533.77 169.57 0 2 -1 3892.24 167.70 0 2 -2 127.06 9.72 0 -2 -2 119.05 9.59 0 -2 -2 123.95 7.87 0 2 -2 147.51 8.88 0 2 -2 149.44 13.19 0 2 2 158.05 13.46 0 -2 -2 116.36 14.14 0 -2 -2 124.66 14.21 0 2 -2 131.89 8.85 0 2 -2 141.85 12.55 0 2 2 115.39 13.55 0 2 -2 124.28 12.16 0 2 -3 85.86 11.93 0 -2 3 101.12 8.37 0 -2 -3 108.49 14.06 0 -2 -3 87.45 14.13 0 2 -3 73.40 8.41 0 2 -3 83.13 10.32 0 -2 -3 93.42 10.51 0 2 -3 101.26 9.19 0 2 3 94.66 14.38 0 -2 -3 84.31 14.97 0 2 -3 86.38 10.50 0 2 3 103.53 14.04 0 -2 -4 81.06 11.17 0 -2 4 83.76 8.02 0 2 -4 78.02 13.19 0 -2 -4 72.28 13.91 0 2 -4 85.69 10.37 0 -2 -4 52.48 14.11 0 2 -4 48.34 8.62 0 2 -4 79.05 11.68 0 -2 -4 81.39 15.59 0 2 -4 75.38 9.20 0 2 4 77.40 15.35 0 2 -5 4486.97 206.19 0 -2 -5 4627.20 207.88 0 2 -5 4660.06 209.02 0 -2 5 4576.10 203.85 0 -2 -5 4588.10 209.45 0 2 -5 4053.56 202.34 0 2 5 4829.90 210.15 0 -2 -5 4760.70 206.98 0 2 -5 4710.89 207.45 0 2 -6 1216.59 55.48 0 -2 -6 1063.41 56.18 0 -2 6 1141.86 52.04 0 2 -6 1135.47 57.93 0 -2 -6 1161.01 58.47 0 2 6 1192.77 58.21 0 -2 -6 1121.69 55.11 0 2 -6 1207.59 56.45 0 -2 -7 58.37 17.82 0 2 7 81.26 18.76 0 2 -7 82.21 16.31 0 -2 7 56.61 13.04 0 -2 -7 57.03 19.47 0 2 -7 80.57 12.61 0 -2 7 76.40 9.97 0 2 -7 61.41 17.33 0 -2 -7 85.68 16.45 0 -2 -8 25.30 18.98 0 2 8 4.62 17.94 0 2 -8 31.95 18.41 0 -2 -8 16.56 17.28 0 2 -8 24.04 19.15 0 -2 -8 40.99 21.51 0 2 -8 24.99 13.08 0 -2 8 14.57 10.56 0 2 8 14.48 20.89 0 -2 8 33.00 15.18 0 -2 -9 199.29 25.04 0 2 -9 195.80 26.29 0 2 -9 228.26 20.92 0 2 9 136.50 25.19 0 2 -9 225.15 26.83 0 2 9 161.35 27.11 0 -2 9 173.35 17.53 0 -2 -9 265.42 30.70 0 -2 9 198.34 22.30 0 2 -10 667.86 40.10 0 -2 -10 725.84 49.44 0 -2 10 642.26 41.91 0 2 10 639.19 47.50 0 -2 10 592.16 36.91 0 2 -10 705.73 47.26 0 2 -10 611.60 45.71 0 -2 -10 601.85 44.01 0 2 10 672.36 45.73 0 2 -11 1370.23 70.23 0 2 -11 1373.05 78.11 0 2 -11 1300.67 76.77 0 -2 -11 1288.68 75.27 0 -2 11 1274.54 67.33 0 2 11 1397.22 78.78 0 2 11 1296.23 74.89 0 -2 11 1265.27 72.36 0 -2 12 51.83 24.88 0 2 12 122.11 30.10 0 2 -12 85.76 29.87 0 -2 -12 50.10 30.55 0 -2 -12 71.13 27.89 0 2 -12 122.26 25.18 0 2 12 181.70 32.41 0 -2 12 76.08 20.43 0 2 -12 97.68 30.78 0 2 12 55.73 29.56 0 -2 13 34.14 27.10 0 -2 13 -10.91 22.32 0 2 13 10.46 32.12 0 2 13 -7.85 31.51 0 2 13 19.42 30.07 0 -2 -13 19.32 35.15 0 2 -13 83.79 34.82 0 -2 14 107.10 32.50 0 2 14 157.20 38.76 0 2 14 216.73 38.69 0 2 14 161.49 35.16 0 -2 -14 209.50 41.29 0 2 -14 246.63 41.49 0 -2 15 379.41 45.19 0 2 15 417.84 49.96 0 2 -15 460.55 52.55 0 -2 -15 433.01 53.43 0 2 15 473.43 45.65 0 2 15 481.23 51.37 0 -3 0 -3.70 10.61 0 3 0 -23.66 15.09 0 -3 0 3.89 12.00 0 3 0 -1.12 14.47 0 -3 0 2.94 9.24 0 3 0 -3.34 9.88 0 3 -1 28.07 8.17 0 -3 1 15.70 10.23 0 -3 -1 13.09 9.67 0 3 1 30.49 14.24 0 3 -1 24.09 13.49 0 -3 -1 40.96 12.99 0 3 -1 23.51 6.02 0 -3 -1 29.43 5.87 0 3 1 17.18 11.90 0 3 -1 28.17 8.32 0 -3 -1 44.10 13.12 0 3 1 26.78 15.10 0 3 -1 34.43 14.49 0 3 -2 3098.62 146.79 0 -3 -2 3155.27 146.44 0 3 -2 3240.62 146.52 0 -3 -2 3173.27 145.86 0 3 2 3224.98 147.06 0 3 -2 3025.39 141.46 0 3 2 3049.93 146.91 0 3 -2 3078.31 141.72 0 3 -3 8.45 12.71 0 -3 -3 -12.80 15.31 0 3 -3 -9.06 13.12 0 -3 -3 -4.56 15.05 0 3 -3 -1.18 7.12 0 3 -3 -6.88 7.51 0 -3 -3 -0.44 7.89 0 3 -3 -3.14 7.02 0 3 3 15.88 15.18 0 3 -3 -0.63 9.86 0 3 -4 865.85 46.10 0 -3 -4 977.60 47.88 0 3 -4 989.99 47.85 0 -3 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152.50 32.64 -13 3 -8 181.20 29.66 -13 3 -8 200.62 37.06 -13 -3 -8 215.18 30.77 13 3 9 -2.92 34.87 13 -3 9 21.29 31.16 -13 3 -9 4.74 33.70 -13 -3 -9 -3.54 28.78 13 3 10 402.06 50.87 -13 3 -10 462.52 50.03 -13 4 11 320.26 51.83 -13 4 11 254.64 49.89 -13 4 11 209.70 39.09 13 4 -11 256.37 39.47 -13 4 10 287.77 46.95 13 4 -10 187.66 36.97 -13 4 10 212.56 45.15 -13 4 10 250.99 37.07 13 4 -9 249.65 33.39 -13 4 9 192.55 42.66 13 4 -9 222.47 38.67 -13 4 9 223.83 45.12 -13 -4 9 253.36 39.17 -13 4 9 220.85 34.47 13 4 -8 23.65 25.23 13 4 -8 -15.30 30.60 -13 4 8 2.92 35.31 -13 4 8 28.09 35.76 -13 -4 8 8.02 29.85 -13 4 8 17.04 24.84 13 4 -7 -9.38 22.38 13 4 -7 -13.13 29.77 -13 -4 7 18.31 28.04 -13 4 7 59.51 36.71 -13 4 7 13.28 33.75 -13 -4 7 7.68 29.59 -13 4 7 8.97 22.92 13 4 -7 -7.43 26.03 13 4 -6 45.80 29.12 -13 -4 6 -5.17 23.73 -13 4 6 60.27 33.40 13 4 -6 3.59 24.63 -13 4 6 33.93 21.28 -13 -4 6 53.99 30.52 13 4 -6 18.27 21.39 13 4 -5 533.11 51.09 -13 -4 5 630.52 46.38 -13 4 5 784.22 55.98 13 4 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45.74 -14 -1 -3 840.02 51.82 -14 1 -3 809.70 47.26 -14 -1 -3 820.57 52.45 -14 -1 -3 819.19 52.68 14 -1 3 839.29 52.89 14 1 3 719.92 49.87 -14 -1 -3 811.69 48.37 14 1 4 43.34 23.58 14 -1 4 34.29 25.74 -14 -1 -4 39.60 23.42 -14 1 -4 32.98 23.29 -14 -1 -4 -8.94 18.33 -14 1 -4 -25.42 24.47 14 -1 4 -1.80 20.96 14 1 4 -14.12 25.94 -14 1 -4 29.65 20.51 -14 -1 -4 -7.08 23.70 -14 1 -4 29.93 21.02 -14 -1 -4 7.47 24.42 -14 -1 -5 349.64 36.38 -14 1 -5 365.19 35.46 -14 1 -5 299.16 31.90 14 -1 5 343.91 34.65 14 1 5 336.78 39.33 -14 -1 -5 415.58 36.66 -14 1 -5 384.61 35.85 14 -1 5 368.33 37.54 -14 -1 -5 319.87 30.92 -14 1 -5 287.97 32.97 -14 -1 -5 324.97 36.92 -14 -1 -6 342.84 37.85 -14 1 -6 443.96 36.18 -14 -1 -6 463.63 42.13 14 1 6 369.03 41.62 -14 1 -6 391.59 37.31 -14 -1 -6 440.16 35.52 -14 1 -6 310.92 35.84 -14 1 -6 361.42 37.16 -14 -1 -6 342.74 36.88 14 -1 6 424.19 38.99 -14 1 -7 442.87 41.26 -14 -1 -7 463.13 41.64 14 -1 7 472.00 42.54 -14 -1 -7 430.02 42.14 -14 1 -7 407.56 40.39 -14 1 -7 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19.42 33.63 22 0 5 -6.08 38.07 -22 0 -5 71.43 38.35 22 0 6 108.09 44.68 -22 0 -6 190.56 42.37 -22 -1 11 63.97 41.50 -22 1 11 115.67 45.76 -22 -1 11 120.41 38.43 22 1 -11 86.60 39.69 -22 1 11 54.53 36.65 22 -1 -11 159.37 43.27 -22 1 10 36.49 42.57 22 1 -10 -2.30 36.48 22 1 -10 -55.63 43.11 22 -1 -10 -11.36 37.08 -22 -1 10 -8.06 37.77 -22 1 10 37.52 34.54 -22 1 10 14.55 28.42 -22 -1 10 5.72 35.49 22 1 -9 70.95 38.56 22 1 -9 15.32 38.66 22 -1 -9 11.28 36.35 -22 1 9 41.13 33.22 -22 -1 9 -11.07 33.48 -22 1 9 55.46 29.15 22 1 -8 96.53 37.20 22 1 -8 101.21 39.77 22 -1 -8 129.39 39.51 -22 1 8 133.74 34.53 -22 -1 8 54.16 34.19 -22 1 8 169.40 31.28 22 1 -7 79.52 37.28 22 1 -7 125.81 38.37 22 -1 -7 124.32 38.62 -22 1 7 119.47 33.52 -22 -1 7 115.53 34.64 -22 1 7 155.83 30.84 22 1 -6 11.91 33.81 22 1 -6 18.20 34.56 22 -1 -6 -16.89 34.26 -22 1 6 22.28 27.17 22 1 -5 70.91 36.28 22 1 -5 58.80 35.86 22 -1 -5 29.91 34.77 -22 -1 4 64.31 34.47 22 1 -4 9.20 35.39 22 1 -4 25.50 33.91 22 -1 -4 12.98 32.48 22 -1 -4 24.87 30.56 22 1 -4 29.02 33.31 -22 -1 3 319.99 41.88 22 -1 -3 338.92 36.99 22 1 -3 274.00 41.10 22 -1 -3 386.06 39.96 -22 -1 2 -2.38 31.72 22 -1 -2 14.83 26.15 22 1 -2 -10.75 31.85 22 -1 -2 12.66 27.81 22 1 -2 11.42 31.11 -22 -1 1 117.49 31.72 22 -1 -1 47.16 25.57 22 1 -1 53.55 34.47 -22 -1 1 120.95 33.88 22 -1 -1 65.54 30.45 22 1 -1 34.46 30.20 -22 -1 0 21.68 29.79 22 -1 0 1.67 24.80 22 1 0 -4.28 32.14 -22 1 0 9.42 22.36 -22 -1 0 1.85 31.09 22 -1 0 28.15 28.99 22 1 0 -11.73 31.85 -22 1 -1 -48.63 34.05 -22 -1 -1 -14.83 29.27 22 -1 1 1.61 24.59 22 -1 1 70.30 32.15 22 1 1 -19.55 32.84 -22 1 -1 -21.00 24.45 22 -1 2 -7.20 31.98 22 1 2 5.15 33.35 -22 -1 -2 27.78 30.91 -22 1 -2 -54.63 36.13 22 -1 3 260.28 42.16 22 1 3 228.11 42.05 -22 -1 -3 327.12 40.25 -22 1 -3 204.77 41.11 22 -1 4 111.23 38.91 22 1 4 76.81 38.54 -22 1 -4 10.33 37.03 -22 -1 -4 84.51 33.58 22 -1 5 104.72 42.16 22 1 5 111.20 42.53 -22 1 -5 152.36 41.73 -22 -1 -5 40.66 35.84 22 -1 6 22.48 42.80 -22 -1 -6 50.33 35.32 -22 2 9 167.12 53.60 22 2 -9 193.54 46.17 22 2 -9 168.59 44.94 22 -2 -9 172.85 45.03 -22 2 9 182.15 37.50 -22 -2 9 213.80 42.80 22 2 -8 38.15 41.85 22 2 -8 -19.76 39.48 22 -2 -8 -25.35 36.77 -22 2 8 8.92 32.44 -22 -2 8 30.25 36.66 22 2 -7 43.98 41.19 22 2 -7 -32.47 38.50 22 -2 -7 55.91 37.58 -22 2 7 6.50 31.09 -22 -2 7 81.05 36.79 22 2 -6 91.82 42.09 -22 -2 6 110.37 35.80 -22 2 6 68.00 25.09 22 2 -6 157.01 41.39 22 -2 -6 35.08 36.96 22 -2 -5 317.94 42.57 22 2 -5 287.75 44.76 22 2 -5 394.13 48.49 22 -2 -4 52.79 30.37 22 2 -4 71.65 33.80 22 2 -4 73.45 40.75 -22 2 4 83.76 37.75 22 -2 -3 125.86 31.80 22 2 -3 86.17 33.63 22 2 -3 79.46 39.53 -22 2 3 144.63 39.94 22 -2 -2 14.11 28.05 22 2 -2 14.32 31.54 22 2 -2 33.46 39.17 -22 -2 2 68.64 34.05 -22 2 2 33.62 34.59 22 2 -1 -26.59 33.13 22 -2 -1 30.65 28.35 22 2 -1 76.37 37.57 -22 -2 1 80.94 32.81 -22 2 1 37.12 32.75 22 -2 0 42.52 30.14 22 2 0 52.09 32.29 22 2 0 91.76 39.17 -22 2 0 41.13 34.28 -22 -2 0 66.18 32.00 22 -2 1 195.10 36.69 22 2 1 153.90 37.48 -22 2 -1 280.44 39.42 -22 -2 -1 225.72 36.62 22 -2 2 105.64 36.02 22 2 2 137.45 38.43 -22 2 -2 56.87 36.35 -22 -2 -2 27.18 31.19 22 -2 3 36.14 35.42 22 2 3 17.64 38.18 -22 -2 -3 27.45 31.60 -22 2 -3 7.70 36.97 22 -2 4 38.68 38.10 22 2 4 -9.47 40.11 -22 -2 -4 19.56 33.79 -22 2 -4 -5.37 39.45 22 3 -7 52.47 49.14 -22 3 7 -6.32 30.96 -22 3 7 37.13 50.16 22 3 -7 45.64 41.36 22 3 -6 179.92 51.45 -22 3 6 187.77 55.26 22 3 -6 148.35 38.27 22 3 -5 20.45 35.14 22 3 -5 42.00 48.07 -22 3 4 -8.98 40.59 22 3 -4 -19.84 33.79 22 3 -4 -3.15 44.35 -22 3 3 -39.95 39.81 22 3 -3 9.86 32.41 22 3 -3 12.28 47.20 -22 3 2 265.42 45.49 22 3 -2 311.23 42.13 22 3 -2 301.21 53.40 -22 3 1 -20.70 35.58 -22 -3 1 -18.86 33.56 22 3 -1 -68.70 34.88 22 3 -1 -2.94 43.25 -22 -3 0 18.06 33.72 -22 3 0 50.04 35.06 22 3 0 45.11 36.08 22 3 0 55.81 44.96 -22 3 -1 19.81 35.33 22 3 1 -41.05 43.74 22 3 1 38.96 36.26 23 0 -10 163.30 44.42 -23 0 10 51.93 38.60 -23 0 10 87.23 36.99 23 0 -9 -27.56 38.53 -23 0 9 50.95 34.28 -23 0 9 -5.17 31.31 -23 0 8 216.39 38.48 23 0 -8 223.35 43.92 23 0 -7 -14.71 35.53 -23 0 7 -17.50 30.24 23 0 -7 79.86 38.02 23 0 -6 285.83 46.27 23 0 -6 379.20 43.71 23 0 -5 -58.80 36.71 23 0 -5 5.80 32.42 23 0 -4 53.92 32.51 23 0 -4 69.41 30.99 -23 0 4 100.94 37.21 23 0 -3 32.89 30.21 23 0 -3 5.33 28.94 -23 0 2 575.01 52.06 23 0 -2 660.00 51.51 23 0 -2 555.88 47.26 -23 0 1 26.39 32.83 -23 0 1 27.12 28.47 23 0 -1 34.67 31.25 -23 0 0 244.67 38.17 -23 0 0 239.40 34.58 23 0 0 223.16 37.68 -23 0 -1 11.60 32.26 -23 0 -1 19.85 29.77 23 0 1 26.90 31.93 -23 0 -2 -2.36 32.53 -23 0 -2 58.91 30.46 23 0 2 41.07 34.46 23 0 3 -27.33 36.86 -23 0 -3 -7.32 34.13 23 0 4 856.25 67.25 -23 0 -4 747.71 62.44 23 0 5 -81.72 43.79 -23 0 -5 21.18 39.51 -23 1 10 66.28 46.74 23 1 -10 98.53 41.37 23 -1 -10 84.49 41.46 -23 1 10 96.73 38.58 -23 1 10 21.84 30.60 -23 -1 10 119.91 39.42 23 1 -9 421.46 48.95 23 1 -9 330.55 51.52 23 -1 -9 357.15 50.93 -23 1 9 222.68 42.77 -23 -1 9 313.59 45.52 -23 1 9 360.77 40.48 23 1 -8 95.05 40.17 23 1 -8 48.79 39.67 23 -1 -8 123.63 42.02 -23 1 8 76.74 35.04 -23 -1 8 113.61 36.93 -23 1 8 135.72 33.01 23 1 -7 24.78 37.17 23 1 -7 -22.63 37.27 23 -1 -7 36.14 37.52 -23 -1 7 -14.07 33.12 -23 1 7 31.69 27.37 23 1 -6 67.22 38.15 -23 -1 6 97.22 34.26 -23 1 6 -2.13 27.96 23 1 -6 -3.17 38.39 23 -1 -6 -2.95 36.26 23 1 -5 325.24 46.19 23 1 -5 323.79 46.37 23 -1 -5 297.32 45.43 -23 -1 4 181.53 40.17 23 1 -4 130.06 39.74 23 -1 -4 122.69 36.10 23 1 -4 115.93 35.67 -23 -1 3 283.39 42.15 23 1 -3 307.55 42.68 23 -1 -3 277.43 37.51 23 1 -3 230.58 39.84 -23 -1 2 19.97 33.65 23 1 -2 13.40 32.41 23 -1 -2 -8.89 30.09 23 1 -2 -24.06 33.06 -23 -1 1 99.53 33.61 23 1 -1 48.88 34.84 23 1 -1 96.65 34.43 23 -1 -1 -24.59 31.51 -23 1 0 87.73 38.03 -23 -1 0 144.30 35.46 23 -1 0 93.51 33.29 23 1 0 137.77 34.98 -23 1 -1 251.81 42.57 -23 -1 -1 226.12 37.42 23 -1 1 264.63 40.32 23 1 1 373.89 44.62 -23 1 -2 19.97 36.56 -23 -1 -2 38.28 32.90 23 -1 2 35.18 35.52 23 1 2 123.57 38.08 -23 -1 -3 9.22 32.93 -23 1 -3 -10.34 36.72 23 -1 3 96.74 37.80 23 1 3 -8.58 36.84 -23 1 -4 5.38 38.84 -23 -1 -4 71.75 35.72 23 -1 4 14.43 38.40 23 1 4 76.59 39.88 23 2 -8 14.27 42.67 23 2 -8 24.22 39.34 23 -2 -8 77.74 40.43 -23 2 8 42.20 33.85 -23 -2 8 44.21 37.73 -23 -2 7 287.88 46.93 23 2 -7 364.02 51.62 23 2 -7 385.20 51.93 23 -2 -7 332.01 49.07 -23 -2 6 108.52 37.51 23 2 -6 55.09 42.72 23 2 -6 97.70 41.79 23 -2 -6 64.22 37.37 -23 2 5 25.58 26.02 23 -2 -5 -9.30 34.60 23 2 -5 10.69 33.55 23 2 -5 40.11 42.86 -23 2 4 39.17 39.41 23 -2 -4 28.57 31.89 23 2 -4 2.57 33.82 23 2 -4 5.60 42.00 -23 2 3 268.08 45.26 23 -2 -3 194.20 35.41 23 2 -3 241.14 39.45 23 2 -3 231.16 47.57 -23 -2 2 112.62 37.66 -23 2 2 105.75 38.35 23 -2 -2 159.50 34.50 23 2 -2 92.80 35.09 23 2 -2 165.02 43.49 -23 -2 1 409.68 43.25 -23 2 1 333.56 43.89 23 -2 -1 223.91 39.02 23 2 -1 283.83 41.59 23 2 -1 277.91 47.65 -23 2 0 17.85 35.11 -23 -2 0 -48.63 34.00 23 -2 0 -15.69 32.72 23 2 0 -7.81 32.11 23 2 0 -23.72 39.82 23 -2 1 2.35 33.21 23 2 1 -43.53 35.84 -23 2 -1 20.38 36.74 -23 -2 -1 45.00 31.89 23 -2 2 132.91 37.83 23 2 2 71.44 37.36 -23 2 -2 101.34 38.96 -23 -2 -2 97.81 34.61 23 -2 3 209.99 43.60 23 2 3 164.44 43.06 -23 -2 -3 154.19 37.82 -23 2 -3 185.46 44.47 23 3 -4 347.02 45.71 23 3 -4 393.88 59.72 -23 3 3 74.19 42.51 23 3 -3 33.59 35.33 23 3 -3 43.88 47.66 -23 3 2 36.69 38.08 23 3 -2 73.59 47.43 23 3 -2 13.02 33.83 -24 0 9 -18.85 34.64 24 0 -9 81.18 41.11 -24 0 8 157.87 37.33 24 0 -8 280.20 48.20 -24 0 7 18.30 33.61 24 0 -7 -19.44 39.26 24 0 -6 44.23 39.64 24 0 -5 -28.98 34.92 24 0 -5 -33.63 38.80 -24 0 4 198.21 43.37 24 0 -4 142.37 38.11 -24 0 3 8.27 34.28 24 0 -3 2.46 33.48 -24 0 2 10.50 35.64 24 0 -2 -29.21 34.94 -24 0 1 15.16 33.29 24 0 -1 4.87 32.39 -24 0 0 56.61 35.11 24 0 0 71.78 34.42 -24 0 -1 48.90 34.94 24 0 1 -7.70 34.99 -24 0 -2 134.05 37.72 24 0 2 134.07 38.65 -24 0 -3 -2.55 36.45 24 0 3 14.23 37.09 -24 -1 8 130.39 38.75 -24 1 8 102.45 32.84 24 1 -8 82.27 41.27 24 1 -8 85.62 43.43 24 -1 -8 127.71 43.16 -24 -1 7 137.63 38.80 -24 1 7 79.79 31.24 24 1 -7 101.47 41.44 24 1 -7 101.26 43.51 24 -1 -7 53.79 39.38 -24 -1 6 184.62 40.15 -24 1 6 84.90 33.08 24 1 -6 162.35 43.57 24 1 -6 160.42 44.68 24 -1 -6 159.48 43.46 24 1 -5 44.43 39.96 24 -1 -5 106.03 38.85 24 -1 -5 53.87 36.82 24 1 -5 43.37 38.54 24 1 -5 95.40 40.45 24 -1 -4 78.47 35.00 24 1 -4 23.53 35.58 24 1 -4 -21.80 38.56 -24 -1 3 137.92 38.69 24 -1 -3 52.16 33.18 24 1 -3 17.77 33.68 24 1 -3 51.72 37.82 -24 -1 2 180.10 38.18 24 -1 -2 110.23 35.14 24 1 -2 65.68 35.87 24 1 -2 134.49 40.06 -24 -1 1 408.31 45.38 24 -1 -1 397.17 44.41 24 1 -1 377.80 45.75 24 1 -1 339.77 46.40 -24 1 0 -28.28 39.38 -24 -1 0 -36.21 33.12 24 -1 0 45.64 34.79 24 1 0 -5.16 33.71 -24 1 -1 2.57 37.03 -24 -1 -1 26.15 33.72 24 -1 1 34.95 34.09 24 1 1 50.96 36.25 -24 1 -2 -5.24 37.83 -24 -1 -2 71.36 35.54 24 -1 2 15.74 35.15 24 1 2 -8.40 37.98 -24 1 -3 2.71 41.25 -24 -1 -3 21.86 35.04 24 -1 3 103.56 39.63 24 1 3 -8.91 41.19 -24 -2 6 60.94 40.38 24 2 -6 -20.26 43.44 24 -2 -6 32.93 37.22 24 2 -6 65.81 38.95 24 -2 -6 -2.90 39.43 24 2 -6 95.83 47.66 24 -2 -5 -36.11 36.93 24 2 -5 35.91 37.26 24 2 -5 85.32 45.79 -24 2 4 75.17 43.87 24 -2 -4 57.35 34.16 24 2 -4 167.98 38.41 24 2 -4 51.69 43.08 -24 2 3 139.64 43.35 24 -2 -3 153.03 36.33 24 2 -3 120.83 37.34 24 2 -3 145.31 45.92 -24 -2 2 -7.99 36.21 -24 2 2 -22.75 40.37 24 2 -2 -41.99 37.67 24 -2 -2 -2.24 32.37 24 2 -2 68.93 44.78 -24 -2 1 12.68 34.82 -24 2 1 21.91 37.22 24 -2 -1 54.42 34.05 24 2 -1 23.85 34.16 24 2 -1 74.08 43.94 -24 2 0 -5.37 36.78 -24 -2 0 4.87 34.05 24 -2 0 -39.94 33.92 24 2 0 16.35 35.17 24 2 0 -2.72 40.83 24 -2 1 93.57 36.91 24 2 1 101.95 39.22 -24 2 -1 131.28 40.44 -24 -2 -1 118.72 36.90 -25 0 7 -5.43 36.11 25 0 -7 10.10 40.54 25 0 -6 232.20 47.33 -25 0 6 214.52 40.37 25 0 -5 27.43 36.74 -25 0 4 15.13 40.77 25 0 -4 65.88 37.46 -25 0 3 48.95 38.01 25 0 -3 -5.15 35.25 -25 0 2 387.45 49.34 25 0 -2 467.17 48.81 -25 0 1 2.66 35.20 25 0 -1 48.58 34.86 -25 0 0 90.77 36.37 25 0 0 104.08 38.61 -25 0 -1 10.30 35.23 25 0 1 32.23 35.97 -25 0 -2 -15.68 37.04 25 0 2 -8.40 37.17 -25 -1 7 30.35 37.52 -25 1 7 13.86 32.53 25 1 -7 62.02 42.76 25 -1 -7 46.06 41.76 25 1 -6 -57.62 43.24 25 -1 -6 22.22 40.03 -25 -1 6 11.93 36.38 -25 1 6 32.53 32.14 25 1 -6 10.59 43.45 25 1 -5 190.28 45.92 25 -1 -5 183.66 42.73 25 1 -5 221.87 44.09 25 1 -4 52.12 40.46 25 -1 -4 73.81 37.69 25 1 -4 108.49 39.08 25 1 -3 9.71 39.47 25 -1 -3 117.21 37.58 25 1 -3 13.31 35.51 -25 -1 2 57.21 36.91 25 1 -2 76.76 39.22 25 -1 -2 93.55 36.27 25 1 -2 95.32 38.00 -25 -1 1 2.61 35.01 25 -1 -1 12.34 33.98 25 1 -1 2.66 37.52 -25 1 0 24.50 40.38 -25 -1 0 -10.17 35.54 25 -1 0 20.21 35.24 25 1 0 54.16 37.04 -25 -1 -1 378.69 48.08 25 -1 1 433.55 48.69 -26 0 4 319.76 50.74 26 0 -4 296.08 47.96 -26 0 3 -62.89 42.80 26 0 -3 10.80 37.29 -26 0 2 48.90 40.58 26 0 -2 -24.12 38.35 -26 0 1 -13.96 38.96 26 0 -1 -42.86 39.40 0 0 0 0.00 0.00 TITL 99726 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 19.690846 4.743103 12.648231 90.0000 100.4001 90.0000 ZERR 4.00 0.000976 0.000181 0.000502 0.0000 0.0044 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N Cl Br UNIT 44.00 56.00 12.00 8.00 4.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 70941 _shelx_res_file ; TITL 99726.res in P2(1)/c 99726.res created by SHELXL-2018/3 at 14:25:59 on 29-Jan-2025 REM Old TITL 99726 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.093, Rweak 0.005, Alpha 0.049 REM 0.370 for 304 systematic absences, Orientation as input REM Formula found by SHELXT: C12 N2 Br CELL 0.71073 19.6908 4.7431 12.6482 90 100.4 90 ZERR 4 0.001 0.0002 0.0005 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br N UNIT 44 56 4 12 EQIV $1 +X,-1+Y,+Z EQIV $2 +X,2.5-Y,-0.5+Z L.S. 4 0 0 PLAN 2 TEMP -173 CONF HTAB C1 Br1_$1 HTAB C2 Br1_$2 list 4 WPDB -2 fmap 2 53 acta MORE -1 BOND $H REM REM REM WGHT 0.024200 1.906800 FVAR 0.57989 BR1 3 0.275929 1.082234 0.655526 11.00000 0.02611 0.01224 = 0.01118 -0.00042 0.00559 -0.00239 N1 4 0.371565 0.609700 0.482705 11.00000 0.01983 0.01252 = 0.00908 0.00151 0.00358 -0.00068 N2 4 0.393682 0.791327 0.410808 11.00000 0.02291 0.02079 = 0.01309 0.00424 0.00516 -0.00315 N3 4 0.279867 0.797778 0.395258 11.00000 0.01944 0.01013 = 0.01074 -0.00021 0.00355 0.00026 C1 1 0.304033 0.617112 0.474448 11.00000 0.01978 0.00978 = 0.01136 -0.00125 0.00405 0.00084 AFIX 43 H1 2 0.277417 0.513698 0.516732 11.00000 -1.20000 AFIX 0 C2 1 0.336298 0.897990 0.358533 11.00000 0.02552 0.01612 = 0.01060 0.00184 0.00366 -0.00395 AFIX 43 H2 2 0.334033 1.030051 0.301532 11.00000 -1.20000 AFIX 0 C3 1 0.421770 0.462331 0.563674 11.00000 0.01927 0.01595 = 0.01781 0.00630 0.00316 0.00311 AFIX 23 H3A 2 0.455642 0.362518 0.528078 11.00000 -1.20000 H3B 2 0.397652 0.320393 0.600822 11.00000 -1.20000 AFIX 0 C4 1 0.459229 0.670279 0.645236 11.00000 0.02468 0.02646 = 0.01615 0.00292 0.00098 0.00263 AFIX 137 H4A 2 0.482324 0.812772 0.608167 11.00000 -1.50000 H4B 2 0.493647 0.569756 0.697392 11.00000 -1.50000 H4C 2 0.425887 0.762499 0.682781 11.00000 -1.50000 AFIX 0 C5 1 0.207752 0.895063 0.359305 11.00000 0.01806 0.01595 = 0.01549 0.00202 -0.00127 0.00101 AFIX 23 H5A 2 0.201490 0.950344 0.282680 11.00000 -1.20000 H5B 2 0.199664 1.064231 0.401177 11.00000 -1.20000 AFIX 0 C6 1 0.155105 0.674111 0.372350 11.00000 0.01689 0.01352 = 0.01303 0.00057 0.00279 0.00582 C7 1 0.139415 0.619362 0.474096 11.00000 0.02113 0.01889 = 0.01491 -0.00146 0.00378 0.00320 AFIX 43 H7 2 0.163016 0.718389 0.535103 11.00000 -1.20000 AFIX 0 C8 1 0.089418 0.420582 0.486187 11.00000 0.02367 0.02837 = 0.01679 0.00439 0.00703 0.00257 AFIX 43 H8 2 0.079519 0.382201 0.555547 11.00000 -1.20000 AFIX 0 C9 1 0.054068 0.278613 0.397461 11.00000 0.01777 0.01664 = 0.02822 0.00258 0.00544 0.00051 AFIX 43 H9 2 0.019573 0.144551 0.405767 11.00000 -1.20000 AFIX 0 C10 1 0.069101 0.332444 0.296409 11.00000 0.01794 0.01830 = 0.02116 -0.00393 0.00090 0.00204 AFIX 43 H10 2 0.044887 0.234676 0.235544 11.00000 -1.20000 AFIX 0 C11 1 0.119359 0.528493 0.283765 11.00000 0.01928 0.01874 = 0.01546 0.00157 0.00462 0.00333 AFIX 43 H11 2 0.129458 0.563655 0.214295 11.00000 -1.20000 AFIX 0 HKLF 4 REM 99726.res in P2(1)/c REM wR2 = 0.0738, GooF = S = 1.053, Restrained GooF = 1.053 for all data REM R1 = 0.0383 for 2356 Fo > 4sig(Fo) and 0.0535 for all 2883 data REM 137 parameters refined using 0 restraints END WGHT 0.0242 1.9068 REM Highest difference peak 1.396, deepest hole -0.576, 1-sigma level 0.100 Q1 1 0.3216 1.0839 0.6667 11.00000 0.05 1.40 Q2 1 0.2270 1.0845 0.6415 11.00000 0.05 1.17 ; _shelx_res_checksum 69927 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.27593(2) 1.08223(5) 0.65553(2) 0.01623(9) Uani d 1 . . N N1 0.37156(11) 0.6097(5) 0.48270(16) 0.0137(4) Uani d 1 . . N N2 0.39368(12) 0.7913(5) 0.41081(18) 0.0187(5) Uani d 1 . . N N3 0.27987(11) 0.7978(4) 0.39526(17) 0.0133(5) Uani d 1 . . C C1 0.30403(14) 0.6171(5) 0.4744(2) 0.0135(5) Uani d 1 . . H H1 0.277417 0.513698 0.516732 0.016 Uiso calc 1 . . C C2 0.33630(14) 0.8980(6) 0.3585(2) 0.0174(6) Uani d 1 . . H H2 0.334033 1.030051 0.301532 0.021 Uiso calc 1 . . C C3 0.42177(14) 0.4623(6) 0.5637(2) 0.0177(6) Uani d 1 . . H H3A 0.455642 0.362518 0.528078 0.021 Uiso calc 1 . . H H3B 0.397652 0.320393 0.600822 0.021 Uiso calc 1 . . C C4 0.45923(16) 0.6703(6) 0.6452(2) 0.0228(6) Uani d 1 . . H H4A 0.482324 0.812772 0.608167 0.034 Uiso calc 1 . . H H4B 0.493647 0.569756 0.697392 0.034 Uiso calc 1 . . H H4C 0.425887 0.762499 0.682781 0.034 Uiso calc 1 . . C C5 0.20775(14) 0.8951(6) 0.3593(2) 0.0170(6) Uani d 1 . . H H5A 0.201490 0.950344 0.282680 0.020 Uiso calc 1 . . H H5B 0.199664 1.064231 0.401177 0.020 Uiso calc 1 . . C C6 0.15510(14) 0.6741(5) 0.3724(2) 0.0145(5) Uani d 1 . . C C7 0.13942(14) 0.6194(6) 0.4741(2) 0.0182(6) Uani d 1 . . H H7 0.163016 0.718389 0.535103 0.022 Uiso calc 1 . . C C8 0.08942(15) 0.4206(7) 0.4862(2) 0.0225(6) Uani d 1 . . H H8 0.079519 0.382201 0.555547 0.027 Uiso calc 1 . . C C9 0.05407(14) 0.2786(6) 0.3975(2) 0.0207(6) Uani d 1 . . H H9 0.019573 0.144551 0.405767 0.025 Uiso calc 1 . . C C10 0.06910(14) 0.3324(6) 0.2964(2) 0.0195(6) Uani d 1 . . H H10 0.044887 0.234676 0.235544 0.023 Uiso calc 1 . . C C11 0.11936(14) 0.5285(6) 0.2838(2) 0.0176(6) Uani d 1 . . H H11 0.129458 0.563655 0.214295 0.021 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 0.02611(15) 0.01224(13) 0.01118(12) -0.00239(12) 0.00559(9) -0.00042(11) N1 0.0198(12) 0.0125(11) 0.0091(10) -0.0007(9) 0.0036(9) 0.0015(9) N2 0.0229(13) 0.0208(12) 0.0131(11) -0.0032(10) 0.0052(10) 0.0042(10) N3 0.0194(12) 0.0101(11) 0.0107(11) 0.0003(9) 0.0036(9) -0.0002(9) C1 0.0198(13) 0.0098(12) 0.0114(12) 0.0008(11) 0.0041(10) -0.0013(10) C2 0.0255(15) 0.0161(13) 0.0106(12) -0.0040(12) 0.0037(11) 0.0018(11) C3 0.0193(14) 0.0159(14) 0.0178(13) 0.0031(11) 0.0032(11) 0.0063(11) C4 0.0247(16) 0.0265(16) 0.0161(14) 0.0026(12) 0.0010(12) 0.0029(12) C5 0.0181(14) 0.0160(13) 0.0155(13) 0.0010(11) -0.0013(10) 0.0020(11) C6 0.0169(14) 0.0135(13) 0.0130(13) 0.0058(10) 0.0028(11) 0.0006(10) C7 0.0211(14) 0.0189(14) 0.0149(13) 0.0032(12) 0.0038(11) -0.0015(11) C8 0.0237(15) 0.0284(16) 0.0168(13) 0.0026(14) 0.0070(11) 0.0044(13) C9 0.0178(14) 0.0166(14) 0.0282(16) 0.0005(12) 0.0054(12) 0.0026(12) C10 0.0179(14) 0.0183(14) 0.0212(14) 0.0020(11) 0.0009(12) -0.0039(11) C11 0.0193(14) 0.0187(14) 0.0155(13) 0.0033(11) 0.0046(11) 0.0016(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' 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 N1 C3 . . 120.3(2) ? C1 N1 N2 . . 111.5(2) ? C1 N1 C3 . . 127.8(2) ? C2 N2 N1 . . 103.2(2) ? C1 N3 C2 . . 106.0(2) ? C1 N3 C5 . . 128.3(2) ? C2 N3 C5 . . 125.5(2) ? N1 C1 N3 . . 107.1(2) y N1 C1 H1 . . 126.4 ? N3 C1 H1 . . 126.4 ? N2 C2 N3 . . 112.1(2) ? N2 C2 H2 . . 123.9 ? N3 C2 H2 . . 123.9 ? N1 C3 H3A . . 109.6 ? N1 C3 H3B . . 109.6 ? N1 C3 C4 . . 110.4(2) ? H3A C3 H3B . . 108.1 ? C4 C3 H3A . . 109.6 ? C4 C3 H3B . . 109.6 ? C3 C4 H4A . . 109.5 ? C3 C4 H4B . . 109.5 ? C3 C4 H4C . . 109.5 ? H4A C4 H4B . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? N3 C5 H5A . . 109.0 ? N3 C5 H5B . . 109.0 ? N3 C5 C6 . . 113.0(2) ? H5A C5 H5B . . 107.8 ? C6 C5 H5A . . 109.0 ? C6 C5 H5B . . 109.0 ? C7 C6 C5 . . 120.0(2) ? C11 C6 C5 . . 121.0(2) ? C11 C6 C7 . . 118.9(3) ? C6 C7 H7 . . 119.9 ? C8 C7 C6 . . 120.3(3) ? C8 C7 H7 . . 119.9 ? C7 C8 H8 . . 119.9 ? C9 C8 C7 . . 120.2(3) ? C9 C8 H8 . . 119.9 ? C8 C9 H9 . . 120.1 ? C8 C9 C10 . . 119.9(3) ? C10 C9 H9 . . 120.1 ? C9 C10 H10 . . 119.8 ? C9 C10 C11 . . 120.3(3) ? C11 C10 H10 . . 119.8 ? C6 C11 H11 . . 119.8 ? C10 C11 C6 . . 120.4(3) ? C10 C11 H11 . . 119.8 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 N2 . 1.379(3) ? N1 C1 . 1.315(3) y N1 C3 . 1.466(3) ? N2 C2 . 1.304(4) ? N3 C1 . 1.339(3) y N3 C2 . 1.365(3) ? N3 C5 . 1.484(3) ? C1 H1 . 0.9500 ? C2 H2 . 0.9500 ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C3 C4 . 1.519(4) ? C4 H4A . 0.9800 ? C4 H4B . 0.9800 ? C4 H4C . 0.9800 ? C5 H5A . 0.9900 ? C5 H5B . 0.9900 ? C5 C6 . 1.504(4) ? C6 C7 . 1.401(4) ? C6 C11 . 1.394(4) ? C7 H7 . 0.9500 ? C7 C8 . 1.391(4) ? C8 H8 . 0.9500 ? C8 C9 . 1.384(4) ? C9 H9 . 0.9500 ? C9 C10 . 1.387(4) ? C10 H10 . 0.9500 ? C10 C11 . 1.388(4) ? 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 C1 H1 Br1 1_545 0.95 2.70 3.528(3) 146 yes C2 H2 Br1 4_585 0.95 2.71 3.603(3) 157 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 N1 N2 C2 N3 . . . . 1.3(3) ? N2 N1 C1 N3 . . . . 1.6(3) ? N2 N1 C3 C4 . . . . 67.8(3) ? N3 C5 C6 C7 . . . . 77.2(3) ? N3 C5 C6 C11 . . . . -105.3(3) ? C1 N1 N2 C2 . . . . -1.8(3) ? C1 N1 C3 C4 . . . . -104.3(3) ? C1 N3 C2 N2 . . . . -0.4(3) ? C1 N3 C5 C6 . . . . -32.3(4) ? C2 N3 C1 N1 . . . . -0.7(3) ? C2 N3 C5 C6 . . . . 153.9(2) ? C3 N1 N2 C2 . . . . -175.0(2) ? C3 N1 C1 N3 . . . . 174.2(2) ? C5 N3 C1 N1 . . . . -175.4(2) ? C5 N3 C2 N2 . . . . 174.5(2) ? C5 C6 C7 C8 . . . . 178.3(3) ? C5 C6 C11 C10 . . . . -177.6(2) ? C6 C7 C8 C9 . . . . -1.0(4) ? C7 C6 C11 C10 . . . . 0.0(4) ? C7 C8 C9 C10 . . . . 0.7(4) ? C8 C9 C10 C11 . . . . -0.1(4) ? C9 C10 C11 C6 . . . . -0.2(4) ? C11 C6 C7 C8 . . . . 0.6(4) ?