#------------------------------------------------------------------------------ #$Date: 2022-06-11 02:49:39 +0100 (Sat, 11 Jun 2022) $ #$Revision: 275968 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244110.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_2244110 loop_ _publ_author_name 'Khalilov, Ali N.' 'Khrustalev, Victor N.' 'Fortalnova, Elena A.' 'Akkurt, Mehmet' 'Y\?ild\?ir\?im, Sema \"Ozt\"urk' 'Bhattarai, Ajaya' 'Mamedov, \.Ibrahim G.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of 4-bromo-2-[3-methyl-5-(2,4,6-trimethylbenzyl)oxazolidin-2-yl]phenol ; _journal_coeditor_code TX2051 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022005928 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C20 H24 Br N O2' _chemical_formula_moiety 'C20 H24 Br N O2' _chemical_formula_sum 'C20 H24 Br N O2' _chemical_formula_weight 390.30 _chemical_name_systematic ; 4-Bromo-2-[3-methyl-5-(2,4,6-trimethylbenzyl)oxazolidin-2-yl]phenol ; _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 mixed _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 96.1425(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.1019(3) _cell_length_b 9.01359(11) _cell_length_c 10.03985(11) _cell_measurement_reflns_used 13703 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 78.56 _cell_measurement_theta_min 2.14 _cell_volume 1898.65(4) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2021) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\f and \w' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 21431 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.607 _diffrn_reflns_theta_min 2.106 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.033 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_correction_T_min 0.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2021) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.365 _exptl_crystal_description needle _exptl_crystal_F_000 808 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.584 _refine_diff_density_min -0.597 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 225 _refine_ls_number_reflns 4096 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0334 _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^)+(0.055P)^2^+1.11P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0942 _refine_ls_wR_factor_ref 0.0958 _reflns_number_gt 3783 _reflns_number_total 4096 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tx2051sup1.cif _cod_data_source_block I _cod_original_cell_volume 1898.66(4) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2244110 _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 0.444 _shelx_estimated_absorpt_t_max 0.915 _shelx_hkl_file ; 0 0 -1 0.33 1.21 0 0 -1 0.85 0.67 0 0 -2 5797.11 262.59 0 0 -2 5723.41 263.81 0 0 -3 0.69 2.95 0 0 -3 0.69 2.49 0 0 -3 0.69 1.31 0 0 -4 13.00 2.06 0 0 -4 10.69 3.81 0 0 -4 12.47 4.35 0 0 -5 2.33 3.80 0 0 -5 0.64 4.00 0 0 -5 -0.62 3.86 0 0 -6 1322.87 65.59 0 0 -6 1262.18 65.81 0 0 -7 2.72 4.30 0 0 -7 0.65 2.04 0 0 -7 -1.40 2.28 0 0 -7 -0.45 2.19 0 0 -7 2.92 4.07 0 0 -7 1.12 2.01 0 0 -8 1092.87 64.35 0 0 -8 1309.04 57.17 0 0 -8 1148.84 64.05 0 0 -8 1204.33 57.32 0 0 -8 1383.66 57.89 0 0 -8 1145.71 57.26 0 0 -8 1195.55 57.43 0 0 -8 1199.12 57.21 0 0 -8 1117.41 56.84 0 0 -8 1263.00 58.14 0 0 -9 2.73 2.40 0 0 -9 -0.53 2.57 0 0 -9 -2.57 7.22 0 0 -9 -0.92 2.02 0 0 -9 -10.14 12.20 0 0 -9 -0.83 1.90 0 0 -9 1.34 2.68 0 0 -9 2.21 4.39 0 0 -10 653.94 33.05 0 0 -10 578.09 28.64 0 0 -10 560.23 28.70 0 0 -11 -1.43 2.13 0 0 -11 -1.00 2.45 0 0 -12 47.81 3.44 0 0 -12 50.34 3.74 0 1 0 0.80 1.01 0 1 -1 786.04 36.73 0 -1 -1 799.61 36.78 0 1 -1 777.69 36.77 0 -1 -1 816.74 36.81 0 -1 -1 756.89 36.94 0 1 -2 150.01 8.78 0 1 -2 164.50 9.35 0 -1 -2 150.87 9.28 0 1 -2 163.56 9.33 0 -1 -2 164.92 9.54 0 1 -3 4.48 2.08 0 1 -3 3.79 2.93 0 -1 -3 4.85 3.04 0 1 -3 3.77 3.06 0 -1 -3 4.11 2.91 0 -1 -4 1139.09 53.64 0 1 -4 1100.68 55.20 0 -1 -4 1180.35 57.26 0 -1 -4 1232.33 57.19 0 1 -4 1237.77 57.46 0 1 -4 1205.28 57.24 0 1 -5 421.12 23.57 0 -1 -5 391.76 23.32 0 1 -5 370.13 23.52 0 1 -5 398.74 23.90 0 -1 -5 421.33 23.81 0 -1 -5 405.83 24.02 0 1 -6 44.90 6.92 0 -1 -6 42.19 6.78 0 1 -6 39.88 6.58 0 -1 -6 37.86 6.47 0 1 -7 419.64 19.59 0 -1 -7 415.09 19.55 0 1 -7 371.37 19.17 0 -1 -7 352.33 19.05 0 1 -7 367.93 19.19 0 1 -7 348.61 19.04 0 -1 -7 398.07 19.01 0 1 -7 407.98 25.25 0 -1 -7 354.20 24.38 0 -1 -7 403.54 19.76 0 -1 -7 386.51 19.31 0 1 -7 336.64 19.09 0 -1 -7 403.05 19.44 0 1 -7 362.85 19.04 0 -1 -7 345.43 24.61 0 1 -7 341.79 24.55 0 -1 -8 67.86 5.59 0 1 -8 81.64 5.86 0 -1 -8 58.22 5.15 0 1 -8 64.62 5.32 0 -1 -8 60.68 5.26 0 1 -8 62.31 4.87 0 -1 -8 60.46 8.96 0 1 -8 58.96 8.94 0 1 -8 62.96 5.17 0 1 -8 64.92 5.54 0 1 -8 60.78 4.95 0 -1 -8 68.95 5.22 0 1 -8 69.21 5.20 0 -1 -8 61.74 6.18 0 1 -8 63.27 4.55 0 1 -8 84.83 10.47 0 -1 -8 69.27 9.62 0 1 -9 5.22 2.34 0 1 -9 1.49 2.91 0 -1 -9 0.77 3.01 0 1 -9 0.61 2.05 0 -1 -9 1.17 1.63 0 1 -9 2.77 2.22 0 1 -9 -0.61 1.70 0 1 -9 -0.46 2.11 0 -1 -9 8.27 15.79 0 -1 -9 0.25 2.53 0 -1 -9 3.41 3.21 0 -1 -9 2.38 2.47 0 1 -9 0.27 2.51 0 1 -9 1.09 3.99 0 -1 -9 -2.17 3.97 0 -1 -10 360.33 19.02 0 -1 -10 414.46 20.83 0 1 -10 368.36 18.98 0 1 -10 361.23 19.09 0 -1 -10 360.70 19.18 0 1 -10 400.81 19.45 0 -1 -10 374.00 19.31 0 -1 -11 103.87 6.82 0 -1 -11 116.77 7.29 0 1 -11 118.72 7.29 0 -1 -11 121.00 7.22 0 1 -11 124.11 7.19 0 -1 -12 268.84 13.00 0 1 -12 263.67 12.95 0 -1 -12 246.60 12.71 0 2 0 1513.92 70.61 0 2 -1 628.64 28.58 0 -2 -1 606.45 28.57 0 -2 -1 604.30 28.62 0 2 1 668.49 29.50 0 2 -1 597.48 28.49 0 -2 -1 589.26 28.49 0 -2 -2 1248.12 58.22 0 2 -2 1199.39 56.61 0 2 -2 1190.54 57.41 0 -2 -2 1221.48 57.40 0 -2 -2 1210.67 57.53 0 2 -2 1156.74 57.27 0 2 2 1325.29 56.99 0 2 -3 1132.24 56.47 0 2 -3 1172.74 56.65 0 -2 -3 1145.18 56.67 0 -2 -3 1185.38 56.60 0 2 3 1209.23 54.73 0 -2 -4 0.90 3.03 0 2 -4 2.92 2.98 0 2 -4 1.78 3.10 0 -2 -4 0.48 2.90 0 2 -4 0.94 3.09 0 -2 -4 -2.47 3.38 0 2 -5 1039.22 50.25 0 -2 -5 983.39 50.02 0 2 -5 998.22 50.32 0 -2 -5 912.99 50.02 0 -2 -6 627.28 35.30 0 2 -6 678.81 35.76 0 -2 -6 616.63 35.64 0 2 -6 610.14 35.70 0 -2 -7 77.80 6.19 0 2 -7 86.16 5.92 0 -2 -7 82.19 6.21 0 2 -7 77.40 5.79 0 -2 -7 70.60 5.51 0 2 -7 78.03 5.88 0 2 -7 72.01 5.54 0 -2 -7 86.20 6.74 0 -2 -7 85.68 5.48 0 2 -7 82.38 5.87 0 2 -7 79.90 5.71 0 -2 -7 91.22 6.10 0 -2 -7 88.98 5.81 0 -2 -7 64.19 9.14 0 2 -7 78.29 9.45 0 2 -7 80.60 9.82 0 -2 -7 72.33 9.48 0 -2 -8 376.53 19.68 0 2 -8 383.99 19.75 0 2 -8 375.06 19.90 0 -2 -8 401.34 19.67 0 2 -8 369.96 19.83 0 2 -8 383.47 19.64 0 2 -8 372.99 19.25 0 2 -8 403.35 19.84 0 -2 -8 397.13 20.12 0 2 -8 378.42 19.27 0 -2 -8 399.32 20.45 0 2 -8 357.63 19.53 0 2 -8 370.20 25.57 0 -2 -8 325.97 24.82 0 -2 -8 401.21 19.22 0 -2 -9 1.51 2.39 0 2 -9 3.77 2.46 0 -2 -9 0.23 2.24 0 2 -9 2.78 2.83 0 2 -9 2.43 2.45 0 -2 -9 5.12 3.17 0 2 -9 3.00 2.87 0 2 -9 -2.54 2.13 0 -2 -9 -8.45 12.60 0 2 -9 2.20 2.43 0 2 -9 -1.39 2.18 0 2 -9 3.11 3.90 0 -2 -9 -2.07 3.90 0 2 -9 0.54 1.53 0 -2 -10 115.91 7.70 0 2 -10 125.25 7.63 0 -2 -10 113.70 7.29 0 2 -10 128.50 7.98 0 -2 -10 121.71 14.85 0 -2 -10 117.75 7.99 0 2 -10 123.32 7.62 0 -2 -10 114.97 7.55 0 2 -10 122.94 7.61 0 2 -10 103.08 7.10 0 2 -11 285.60 14.48 0 -2 -11 261.81 18.80 0 2 -11 286.46 14.14 0 -2 -11 269.97 14.24 0 2 -11 279.86 14.21 0 -2 -11 268.56 14.17 0 2 -12 24.37 2.15 0 2 -12 32.03 2.46 0 2 -12 27.92 2.58 0 3 0 1.00 2.52 0 3 1 2319.15 108.02 0 3 -1 2320.71 108.60 0 3 -2 6.03 1.75 0 -3 -2 7.52 1.95 0 3 -2 4.47 1.82 0 -3 -2 8.87 2.09 0 -3 -2 5.86 3.38 0 3 2 7.75 2.32 0 -3 -3 153.40 9.27 0 3 -3 143.33 9.10 0 -3 -3 142.35 9.29 0 3 -3 139.66 9.09 0 -3 -3 144.83 10.75 0 3 -3 126.32 8.11 0 3 3 151.59 8.82 0 3 -4 118.74 9.12 0 -3 -4 120.39 9.31 0 -3 -4 115.07 10.57 0 -3 -4 120.34 9.07 0 3 -4 126.06 9.09 0 -3 -5 105.03 9.14 0 3 -5 97.80 8.74 0 -3 -5 103.01 9.30 0 3 -5 93.69 8.87 0 -3 -6 244.40 12.71 0 3 -6 229.84 12.23 0 -3 -6 214.98 12.38 0 3 -6 209.22 11.79 0 -3 -6 239.42 16.35 0 3 -6 215.29 15.86 0 3 -6 228.66 16.40 0 -3 -6 224.04 16.42 0 -3 -7 525.67 32.92 0 3 -7 530.04 26.65 0 3 -7 559.30 27.21 0 -3 -7 556.02 27.83 0 3 -7 569.83 32.61 0 -3 -7 487.77 31.73 0 -3 -7 601.90 27.03 0 -3 -7 560.91 26.87 0 3 -7 629.34 27.32 0 3 -7 558.23 26.83 0 3 -7 495.04 26.93 0 -3 -7 487.03 26.38 0 -3 -8 35.15 3.59 0 3 -8 35.45 3.64 0 3 -8 24.72 3.14 0 -3 -8 25.33 3.84 0 3 -8 25.54 3.65 0 3 -8 25.66 3.10 0 -3 -8 35.25 6.52 0 3 -8 30.13 6.16 0 3 -8 27.32 3.67 0 3 -8 25.30 3.74 0 -3 -8 29.49 3.22 0 3 -8 29.14 3.81 0 3 -8 27.43 3.81 0 3 -9 112.73 7.71 0 3 -9 125.36 7.43 0 -3 -9 97.49 7.24 0 -3 -9 99.36 13.01 0 3 -9 106.51 6.76 0 3 -9 114.68 7.17 0 -3 -9 113.12 7.19 0 3 -9 95.47 10.66 0 -3 -9 84.90 10.42 0 -3 -9 96.90 6.68 0 3 -9 123.21 7.77 0 3 -9 106.45 7.44 0 3 -10 78.60 5.40 0 -3 -10 65.04 5.34 0 3 -10 77.43 5.54 0 -3 -10 71.06 15.59 0 3 -10 72.83 5.00 0 -3 -10 60.87 4.84 0 3 -10 70.60 5.53 0 -3 -10 63.38 5.55 0 3 -10 58.30 5.02 0 -3 -11 28.67 8.34 0 3 -11 31.49 2.80 0 3 -11 30.37 3.13 0 3 -11 31.91 3.18 0 3 -12 7.83 1.35 0 3 -12 6.14 1.20 0 4 0 183.01 12.47 0 -4 -1 288.14 16.82 0 4 -1 283.51 17.57 0 4 1 281.17 17.01 0 -4 -2 6.78 3.74 0 4 2 8.71 2.81 0 4 -3 1515.36 77.70 0 -4 -3 1828.87 81.66 0 4 3 1764.93 79.06 0 4 -3 1670.07 77.34 0 -4 -3 1649.12 77.41 0 -4 -4 13.10 4.90 0 -4 -4 12.82 3.03 0 4 -4 9.74 2.63 0 -4 -5 110.68 11.67 0 4 -5 94.41 8.61 0 -4 -6 23.59 3.82 0 -4 -6 22.53 3.65 0 -4 -6 21.98 4.65 0 4 -6 27.27 4.88 0 -4 -6 29.21 3.71 0 4 -6 26.79 3.47 0 -4 -6 24.17 3.73 0 -4 -6 25.16 3.35 0 4 -6 21.78 3.07 0 4 -6 24.99 3.12 0 4 -7 12.50 2.89 0 -4 -7 12.55 3.91 0 -4 -7 14.02 3.34 0 -4 -7 13.85 3.19 0 4 -7 11.27 4.16 0 -4 -7 13.11 4.27 0 -4 -7 20.53 3.52 0 4 -7 14.55 2.89 0 -4 -7 11.46 2.25 0 -4 -8 12.14 4.26 0 -4 -8 13.80 4.29 0 -4 -8 8.34 3.03 0 4 -8 11.36 2.98 0 4 -8 7.74 2.22 0 -4 -8 9.56 2.34 0 4 -8 11.59 3.06 0 4 -8 10.03 2.93 0 4 -9 148.30 8.80 0 -4 -9 155.29 9.56 0 4 -9 135.37 8.38 0 4 -9 148.47 9.15 0 -4 -9 123.99 8.42 0 4 -9 148.32 8.49 0 4 -9 136.88 9.19 0 4 -9 139.52 8.11 0 4 -10 34.89 3.56 0 4 -10 36.88 3.56 0 4 -10 34.53 3.62 0 4 -10 36.83 3.94 0 -4 -10 36.92 4.09 0 4 -10 32.50 2.96 0 4 -11 305.05 15.30 0 4 -11 302.49 15.50 0 -4 -11 313.76 16.57 0 4 -11 349.37 15.54 0 5 0 -1.31 2.94 0 -5 -1 445.18 25.10 0 5 1 430.26 25.21 0 -5 -2 346.92 21.23 0 5 2 332.09 20.41 0 5 -3 176.65 11.71 0 -5 -3 200.51 14.99 0 -5 -4 276.42 16.15 0 -5 -4 284.35 15.99 0 -5 -4 323.98 16.34 0 -5 -4 324.39 15.91 0 -5 -4 286.64 21.06 0 -5 -5 232.17 12.74 0 -5 -5 217.40 12.89 0 -5 -5 229.83 18.74 0 -5 -6 220.28 13.39 0 5 -6 202.91 12.27 0 5 -6 238.27 12.24 0 -5 -6 225.71 13.14 0 5 -7 671.68 33.30 0 5 -7 744.28 33.09 0 -5 -7 647.34 34.16 0 -5 -7 676.20 34.48 0 -5 -7 696.59 34.08 0 -5 -7 648.26 34.37 0 5 -8 91.47 6.11 0 -5 -8 94.39 7.54 0 5 -8 80.29 6.58 0 -5 -8 74.80 8.47 0 5 -8 77.85 6.49 0 -5 -8 81.23 6.83 0 5 -9 123.90 7.88 0 5 -9 95.09 7.03 0 -5 -9 135.09 8.40 0 5 -9 116.90 7.09 0 -5 -9 128.05 19.03 0 5 -10 31.24 3.34 0 5 -10 22.50 2.44 0 5 -10 23.78 2.98 0 5 -11 35.81 2.60 0 -5 -11 35.42 5.52 0 5 -11 38.41 2.44 0 -6 0 449.69 26.50 0 -6 -1 76.96 8.66 0 6 -2 152.23 8.97 0 -6 -2 146.08 8.89 0 -6 -2 137.16 8.88 0 -6 2 157.71 8.59 0 6 -2 150.67 11.32 0 -6 -2 162.32 13.41 0 -6 -3 210.22 16.34 0 6 3 182.31 10.40 0 6 -3 182.65 10.75 0 -6 -3 195.86 11.09 0 -6 -4 129.76 13.14 0 6 -4 126.55 7.81 0 -6 -4 116.58 8.40 0 -6 -4 127.45 8.35 0 -6 -4 114.87 7.71 0 6 5 29.62 3.43 0 -6 -5 44.12 8.51 0 6 -5 34.43 3.54 0 -6 -5 30.88 4.12 0 -6 -5 33.52 4.52 0 -6 -6 100.65 8.05 0 -6 -6 110.54 7.90 0 -6 -6 117.39 8.35 0 -6 -7 6.00 3.23 0 -6 -7 4.41 4.72 0 -6 -7 2.86 2.93 0 6 -8 383.61 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22 -4 -5 183.96 9.62 22 -4 -5 162.46 9.09 22 -4 -5 188.61 9.55 22 -4 -4 26.08 3.01 22 -4 -4 26.43 3.26 22 4 -4 27.39 2.45 22 -4 -4 27.48 2.57 22 4 -3 170.28 9.29 22 -4 -3 177.34 9.99 22 4 -3 194.78 9.97 22 -4 -3 183.26 10.27 22 4 -2 -0.39 1.76 22 -4 -2 0.87 2.39 22 -4 -2 0.98 2.01 22 -4 -1 5.20 2.17 22 4 -1 2.03 1.66 22 4 -1 2.75 1.90 22 -4 0 2.18 2.09 22 4 0 2.21 1.67 22 4 0 3.07 1.82 22 -4 1 197.19 10.44 22 4 1 193.21 10.33 22 -4 2 5.72 1.73 22 4 2 7.31 1.76 22 -4 3 179.49 9.62 22 4 3 210.15 9.76 22 4 3 184.29 9.81 22 4 4 4.48 1.05 -22 4 -4 2.79 1.29 22 4 4 3.63 0.78 22 -5 -5 4.37 1.39 22 -5 -5 5.34 1.48 22 -5 -4 68.89 4.53 -22 5 3 99.09 5.97 22 -5 -3 113.56 6.27 22 -5 -2 4.77 1.53 22 -5 -2 5.49 2.02 22 5 -1 363.56 16.97 22 -5 -1 308.51 16.66 22 -5 -1 352.34 17.20 22 5 -1 365.88 17.18 22 5 0 9.44 1.75 22 -5 0 11.00 2.08 22 5 0 9.27 1.74 22 -5 0 6.12 1.48 22 5 1 33.14 2.55 22 -5 1 28.16 2.32 22 5 2 34.54 2.70 -22 5 -2 34.31 2.80 22 5 3 3.67 0.95 22 -6 -4 9.91 1.31 22 -6 -3 34.68 2.64 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23 -1 -7 131.66 7.01 23 1 -7 146.11 7.14 23 -1 -7 143.23 7.39 23 1 -7 128.29 7.36 23 -1 -6 159.87 8.46 23 1 -6 160.91 8.53 23 -1 -6 172.27 9.04 23 1 -6 168.80 9.06 23 -1 -5 12.55 2.55 23 -1 -5 16.50 2.81 23 1 -5 15.15 2.79 23 -1 -5 16.37 2.68 23 -1 -5 12.71 2.55 23 -1 -5 13.20 1.99 23 1 -5 11.37 2.06 23 -1 -4 232.26 12.39 23 -1 -4 243.45 12.47 23 -1 -4 233.23 12.38 23 -1 -4 233.11 12.66 23 1 -4 225.29 12.64 23 -1 -4 213.73 11.37 23 1 -4 226.64 11.61 23 1 -3 26.79 2.56 23 -1 -3 28.83 3.47 23 -1 -3 32.52 3.65 23 -1 -3 36.52 3.78 23 1 -3 30.88 3.60 23 -1 -3 25.00 3.42 23 1 -2 139.75 8.72 23 -1 -2 125.54 8.54 23 -1 -2 146.78 8.60 23 1 -2 144.55 8.24 23 -1 -2 130.98 8.35 23 -1 -2 135.18 8.37 23 1 -2 138.35 8.33 23 -1 -1 6.31 2.41 23 1 -1 4.97 2.17 23 1 -1 5.07 2.15 23 -1 -1 7.74 2.07 23 -1 0 7.09 2.56 23 -1 0 5.69 2.11 23 1 0 6.01 1.84 23 1 0 5.09 2.10 23 1 1 151.18 8.10 23 -1 1 131.02 8.09 23 1 1 129.45 7.88 23 1 1 144.10 8.36 23 1 2 93.79 5.68 23 -1 2 82.70 5.75 23 1 2 92.49 5.71 23 1 2 93.08 5.89 23 -1 3 23.85 2.53 23 1 3 24.46 2.43 23 -1 4 77.33 4.71 23 1 4 85.75 4.83 -23 1 -4 77.87 4.87 -23 -1 -4 82.73 4.92 23 1 5 2.42 0.78 -23 1 -5 0.30 0.80 -23 -1 -5 1.79 0.84 23 -2 -7 22.30 2.04 23 -2 -7 22.13 1.66 23 2 -7 24.75 1.80 23 -2 -6 81.12 4.78 23 2 -6 92.75 5.08 23 -2 -6 91.41 5.43 23 -2 -6 85.94 5.21 23 2 -6 89.61 5.27 23 -2 -5 175.93 9.42 23 -2 -5 176.01 9.22 23 2 -5 177.80 9.31 23 -2 -5 164.00 9.15 23 2 -5 178.25 9.28 23 -2 -5 154.46 8.46 23 2 -5 158.13 8.71 23 -2 -4 5.43 2.36 23 -2 -4 5.82 2.16 23 2 -4 -1.29 2.05 23 -2 -4 10.52 2.29 23 2 -4 5.58 2.10 23 -2 -4 5.30 2.37 23 2 -4 4.22 1.76 23 -2 -3 82.13 5.44 23 2 -3 81.88 5.48 23 -2 -3 72.63 5.48 23 2 -3 78.21 5.61 23 -2 -3 76.09 5.56 23 -2 -3 78.23 5.59 23 2 -3 63.80 4.47 23 2 -2 12.18 2.66 23 -2 -2 11.16 2.62 23 2 -2 12.25 2.22 23 -2 -2 17.01 2.72 23 2 -2 14.45 2.64 23 -2 -2 12.42 2.90 23 -2 -2 12.25 2.86 23 2 -1 33.38 3.68 23 -2 -1 33.20 3.66 23 2 -1 32.19 3.41 23 2 -1 33.34 3.57 23 -2 -1 37.47 3.51 23 -2 -1 35.81 3.71 23 2 0 158.89 9.11 23 -2 0 160.16 9.06 23 -2 0 158.06 9.20 23 2 1 163.12 9.18 23 2 1 175.06 9.66 23 -2 1 186.67 9.59 23 -2 1 163.78 9.54 23 -2 2 96.90 5.90 23 2 2 92.98 5.85 23 2 2 93.66 5.66 23 -2 2 85.16 5.75 23 -2 3 131.22 6.96 23 2 3 123.71 6.81 23 2 3 111.92 6.69 23 -2 4 0.92 1.28 -23 2 -4 -0.79 1.03 23 -2 5 136.86 6.60 23 2 5 129.83 6.54 23 3 -6 19.12 1.71 23 -3 -6 14.17 1.85 23 -3 -5 36.55 3.23 23 3 -5 37.53 2.77 23 -3 -5 34.30 2.95 23 -3 -5 33.99 2.74 23 -3 -4 48.07 3.78 23 -3 -4 36.86 3.25 23 -3 -4 40.03 3.25 23 3 -3 69.93 5.21 23 -3 -3 81.41 5.20 23 -3 -2 13.34 2.22 23 3 -2 14.84 2.08 23 -3 -2 10.76 2.72 23 3 -2 9.48 2.19 23 -3 -2 13.07 2.56 23 -3 -1 332.18 16.05 23 -3 -1 314.13 15.59 23 3 -1 330.80 15.92 23 3 0 13.62 2.26 23 -3 0 17.37 2.22 23 -3 0 17.91 2.68 23 -3 1 185.86 9.81 23 -3 1 187.32 10.20 23 3 1 192.60 10.27 23 -3 2 -1.14 1.63 23 3 2 1.08 1.46 23 3 2 2.05 1.37 23 -3 2 1.93 1.21 23 -3 3 3.14 0.95 23 3 3 2.16 1.09 23 3 3 1.36 1.16 23 -3 3 1.34 1.36 -23 3 -3 1.12 0.98 23 -3 4 3.41 1.00 23 -4 -5 233.86 10.59 23 4 -5 188.56 9.95 23 -4 -4 23.50 2.48 23 -4 -4 20.96 2.57 23 -4 -4 23.82 2.64 23 -4 -3 221.67 11.45 23 -4 -3 217.70 11.64 23 -4 -2 3.45 1.80 23 -4 -2 1.06 2.05 23 -4 -1 2.01 1.81 23 4 -1 2.96 1.50 23 -4 -1 1.42 2.04 23 4 0 35.07 3.09 23 -4 0 39.09 3.24 23 -4 1 136.03 7.40 23 4 2 12.50 1.67 23 -4 2 12.68 1.66 23 4 3 186.92 9.25 23 -5 -4 58.09 3.52 23 -5 -3 1.70 1.29 23 -5 -3 3.13 1.48 -23 5 2 2.05 1.10 23 -5 -2 3.60 1.52 23 -5 -2 3.29 1.02 23 -5 -1 113.14 5.97 -23 5 1 121.79 6.05 23 5 0 14.37 1.70 -23 5 0 14.90 1.88 23 -5 0 12.43 1.75 23 -5 1 120.40 6.31 23 5 2 -0.15 0.69 -23 5 -2 -0.07 0.75 24 0 -6 266.27 13.06 24 0 -6 290.77 13.68 24 0 -5 2.36 1.93 24 0 -5 -2.35 1.83 24 0 -5 1.10 1.10 24 0 -4 106.44 6.79 24 0 -4 115.17 6.55 24 0 -4 121.12 6.80 24 0 -4 99.03 5.62 24 0 -3 -0.66 1.91 24 0 -3 1.24 1.91 24 0 -3 0.57 1.97 24 0 -2 57.20 4.76 24 0 -2 66.60 4.82 24 0 -2 61.30 4.64 24 0 -1 1.80 1.89 24 0 -1 -0.18 1.87 24 0 -1 1.35 2.05 24 0 0 236.86 13.21 24 0 0 261.97 13.48 24 0 1 2.37 1.85 24 0 1 0.75 1.58 24 0 1 1.86 1.83 24 0 2 19.24 2.34 24 0 3 0.55 1.33 24 0 3 -0.67 1.19 -24 0 -4 0.18 0.89 24 0 4 0.83 0.84 24 0 4 -0.37 0.95 24 -1 -6 47.29 3.01 24 1 -6 55.50 3.21 24 -1 -6 61.51 3.68 24 1 -6 68.98 3.81 24 -1 -5 31.62 2.39 24 1 -5 40.66 2.69 24 -1 -5 41.27 3.36 24 1 -5 46.33 3.49 24 -1 -5 41.28 3.33 24 1 -5 36.60 3.27 24 -1 -5 42.06 3.33 24 -1 -4 191.87 10.86 24 -1 -4 196.57 11.13 24 1 -4 192.95 11.14 24 -1 -4 203.11 10.97 24 -1 -4 235.30 11.26 24 -1 -4 223.18 11.12 24 1 -4 205.18 10.19 24 -1 -3 13.53 2.46 24 1 -3 5.55 2.14 24 -1 -3 6.21 2.19 24 -1 -3 6.74 2.18 24 -1 -3 10.57 2.32 24 -1 -2 284.74 14.08 24 -1 -2 284.72 14.08 24 1 -2 253.59 14.15 24 -1 -2 255.49 14.15 24 -1 -2 262.93 13.99 24 1 -1 10.21 2.25 24 -1 -1 10.28 2.23 24 -1 -1 7.83 2.24 24 1 -1 9.86 2.34 24 -1 -1 9.54 2.29 24 -1 0 9.43 2.23 24 1 1 59.30 4.30 24 -1 1 58.63 4.42 24 1 1 68.97 4.70 24 1 2 86.20 5.17 24 1 2 85.12 5.26 24 -1 3 13.74 1.74 24 -1 4 117.85 5.64 -24 1 -4 101.57 5.61 -24 -1 -4 101.23 5.61 24 1 4 110.28 5.62 24 2 -6 26.81 1.88 24 -2 -6 29.97 2.25 24 -2 -6 27.94 2.01 24 -2 -6 27.94 2.16 24 -2 -5 77.76 4.70 24 -2 -5 72.92 4.44 24 2 -5 68.84 4.05 24 -2 -4 0.67 1.51 24 2 -4 0.17 1.52 24 -2 -4 1.75 1.74 24 2 -4 1.20 1.71 24 -2 -4 0.99 1.56 24 2 -4 -0.15 1.62 24 -2 -4 1.43 1.86 24 2 -4 0.56 1.14 24 -2 -3 104.63 6.97 24 2 -3 115.92 7.10 24 -2 -3 124.60 7.19 24 -2 -3 122.82 6.97 24 2 -3 121.95 7.06 24 -2 -3 121.87 7.16 24 2 -2 12.32 1.99 24 -2 -2 11.34 2.21 24 2 -2 17.86 2.44 24 -2 -2 16.21 2.71 24 -2 -2 15.86 2.57 24 -2 -2 13.90 2.44 24 2 -2 16.09 2.47 24 -2 -1 44.99 3.89 24 2 -1 46.95 3.76 24 2 -1 38.95 3.70 24 -2 -1 41.60 3.78 24 -2 -1 51.18 3.81 24 2 -1 51.24 3.85 24 -2 0 104.07 6.37 24 2 0 112.88 6.31 24 -2 0 104.43 6.15 24 2 0 99.17 6.31 24 -2 0 92.69 6.26 24 2 1 51.36 4.00 24 -2 1 55.89 4.13 24 -2 1 57.09 3.95 24 2 1 62.29 4.05 24 2 2 105.76 6.03 24 2 2 116.38 6.00 24 -2 2 103.28 5.92 24 2 2 95.54 5.80 24 -2 2 107.44 6.12 -24 2 -3 31.96 2.51 24 -2 3 38.40 2.50 24 2 3 35.80 2.59 24 -2 3 40.60 2.79 24 -2 4 11.55 1.17 24 3 -5 33.18 2.13 24 -3 -4 80.56 4.58 24 3 -4 90.19 4.44 24 -3 -4 68.49 4.35 24 -3 -4 101.62 5.29 24 -3 -3 44.18 3.45 24 -3 -3 40.02 2.97 24 -3 -3 37.36 2.85 24 -3 -2 20.30 2.09 24 -3 -2 22.71 2.66 24 3 -1 215.75 10.98 24 -3 -1 214.89 11.13 24 -3 -1 194.66 10.60 24 -3 -1 230.26 11.36 24 -3 0 11.85 1.59 24 -3 0 13.03 2.21 24 3 0 9.20 1.86 24 -3 1 15.65 1.61 24 -3 1 17.05 2.14 24 3 1 15.17 1.95 24 -3 2 9.43 1.50 24 3 2 10.67 1.45 24 -3 3 25.00 1.82 24 3 3 23.93 1.72 24 -4 -4 -1.90 1.10 24 -4 -4 0.40 1.22 24 -4 -3 148.04 7.89 24 -4 -3 145.50 7.67 24 -4 -2 4.23 1.49 24 -4 -2 11.26 1.98 24 -4 -1 57.16 3.73 24 -4 -1 59.49 4.00 24 -4 0 11.39 1.57 24 -4 0 10.49 1.89 24 4 0 11.70 1.58 24 -4 1 91.77 5.21 24 -4 1 108.42 5.58 24 -4 2 9.33 1.27 24 4 2 11.08 1.21 -24 4 -2 9.46 1.17 24 -5 -2 10.33 1.29 24 -5 -1 60.79 3.47 -24 5 0 2.06 0.74 25 0 -6 0.57 0.73 25 0 -5 1.30 1.31 25 0 -4 25.02 2.55 25 0 -4 24.49 2.53 25 0 -3 2.56 1.72 25 0 -3 0.17 1.45 25 0 -2 16.22 2.24 25 0 -2 15.06 2.25 25 0 -2 12.96 2.17 25 0 -1 -0.15 1.60 25 0 -1 0.85 1.50 25 0 -1 0.18 1.49 25 0 0 237.10 12.29 25 0 0 239.33 12.59 25 0 0 252.06 12.46 25 0 1 -0.12 1.28 25 0 1 1.22 1.21 25 0 1 0.13 1.41 25 0 2 123.56 6.43 25 0 2 108.48 6.35 25 0 2 130.18 6.61 25 0 3 0.39 0.90 -25 0 -3 -0.40 0.84 25 -1 -5 19.02 1.89 25 1 -5 19.21 1.95 25 -1 -4 272.91 14.40 25 -1 -4 300.18 14.49 25 1 -4 287.85 14.51 25 -1 -4 294.53 14.48 25 1 -4 308.38 14.58 25 -1 -3 8.50 1.92 25 -1 -3 8.14 1.81 25 1 -3 11.68 1.94 25 -1 -3 13.84 2.04 25 -1 -2 269.96 13.46 25 -1 -2 279.69 13.59 25 -1 -2 283.77 13.58 25 -1 -2 248.95 13.62 25 1 -2 250.51 13.65 25 -1 -1 15.57 2.24 25 1 -1 11.46 2.03 25 -1 -1 12.06 2.08 25 -1 -1 16.89 2.28 25 -1 -1 15.08 2.17 25 -1 0 52.01 4.02 25 1 0 55.05 4.11 25 -1 0 57.19 4.13 25 -1 1 33.65 2.69 25 1 1 28.19 2.65 25 -1 1 31.51 2.74 25 1 2 9.59 1.45 25 -1 2 14.06 1.61 25 1 2 11.92 1.60 25 -1 3 17.08 1.37 25 1 3 17.77 1.44 -25 -1 -3 14.02 1.34 25 -2 -4 22.33 2.12 25 -2 -4 21.60 1.98 25 -2 -4 19.14 1.90 25 -2 -3 199.22 10.26 25 -2 -3 190.79 10.05 25 2 -3 196.36 10.15 25 -2 -3 200.93 10.16 25 2 -3 204.96 10.20 25 -2 -2 57.06 3.88 25 2 -2 59.61 3.98 25 -2 -2 58.41 4.08 25 -2 -2 60.53 4.12 25 -2 -1 84.01 5.16 25 -2 -1 74.66 4.83 25 2 -1 82.44 4.98 25 2 -1 85.76 4.97 25 -2 -1 78.67 5.09 25 -2 0 150.24 7.95 25 -2 0 142.62 7.69 25 2 0 147.46 7.75 25 -2 0 141.72 7.94 25 -2 1 2.58 1.14 25 2 1 3.29 1.26 25 2 1 3.81 1.30 25 -2 1 3.32 1.43 25 -2 2 126.04 6.05 25 -2 2 150.74 6.48 25 -3 -4 34.18 2.43 25 -3 -3 0.41 1.19 25 -3 -2 56.67 3.72 25 -3 -1 173.41 8.90 25 3 -1 170.01 8.71 25 -3 0 105.72 5.79 25 3 0 108.38 5.77 25 -3 0 98.18 5.87 25 -3 1 49.19 3.31 25 -3 1 57.87 3.48 25 3 1 59.04 3.39 25 -3 2 9.04 1.10 25 -4 -2 1.62 0.92 25 -4 -2 -0.25 0.89 25 -4 -1 66.89 3.82 -25 4 0 18.81 1.53 26 0 -4 63.05 3.68 26 0 -4 61.40 3.65 26 0 -3 0.31 1.18 26 0 -3 1.58 1.29 26 0 -2 1.23 1.25 26 0 -1 -1.33 1.27 26 0 0 250.10 12.33 26 0 1 -0.09 0.97 26 -1 -4 41.11 2.57 26 1 -4 40.54 2.61 26 -1 -4 38.75 2.49 26 -1 -3 -0.09 1.12 26 -1 -3 0.09 0.99 26 1 -3 0.29 1.10 26 -1 -3 0.37 1.08 26 1 -3 -0.49 1.10 26 -1 -2 194.67 9.76 26 1 -2 197.34 9.83 26 -1 -2 188.81 9.73 26 -1 -1 38.47 2.77 26 1 -1 39.44 2.89 26 -1 -1 40.21 2.83 26 -1 0 27.98 2.15 26 1 0 27.31 2.22 26 -1 0 22.93 2.20 26 -1 1 33.68 2.26 26 1 1 33.38 2.32 26 -1 1 33.30 2.34 26 -2 -3 33.57 2.27 26 -2 -2 -0.27 0.84 26 -2 -2 2.13 1.12 26 -2 -1 29.43 2.32 26 -2 -1 31.67 2.36 26 -2 0 22.27 1.91 26 -2 0 24.67 2.00 26 -2 1 30.47 2.03 0 0 0 0.00 0.00 TITL 22SAI_R009 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 21.101877 9.013594 10.039851 90.0000 96.1425 90.0000 ZERR 4.00 0.000251 0.000113 0.000112 0.0000 0.0011 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O Br UNIT 80.00 80.00 4.00 12.00 4.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 61467 _shelx_res_file ; TITL Ai2 in P2(1)/c CELL 1.54184 21.1019 9.01359 10.03985 90.0000 96.1425 90.0000 ZERR 4.00 0.0003 0.00011 0.00011 0.0000 0.0011 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H Br N O UNIT 80 96 4 4 8 TEMP -173.0 SIZE 0.03 0.04 0.32 L.S. 12 BOND $H ACTA CONF HTAB O11 N3 WGHT 0.055000 1.110000 FVAR 0.52435 BR1 3 0.542195 0.315152 0.433755 11.00000 0.02612 0.02966 = 0.02922 0.00477 0.00584 -0.00322 O1 5 0.276327 0.251496 0.587025 11.00000 0.02691 0.03440 = 0.02960 0.01076 0.01029 0.00537 C2 1 0.329567 0.172612 0.651183 11.00000 0.02423 0.02409 = 0.02160 0.00109 0.00354 -0.00101 AFIX 13 H2 2 0.351652 0.233358 0.725551 11.00000 -1.20000 AFIX 0 N3 4 0.301192 0.039406 0.705334 11.00000 0.02580 0.02608 = 0.02012 0.00289 0.00244 -0.00149 C4 1 0.243965 0.099787 0.757793 11.00000 0.02912 0.03323 = 0.02453 0.00375 0.00759 -0.00195 AFIX 23 H4A 2 0.254811 0.151788 0.844078 11.00000 -1.20000 H4B 2 0.212357 0.020992 0.769563 11.00000 -1.20000 AFIX 0 C5 1 0.219704 0.207535 0.646726 11.00000 0.02697 0.03152 = 0.02487 0.00212 0.00683 -0.00027 AFIX 13 H5 2 0.190100 0.154127 0.578468 11.00000 -1.20000 AFIX 0 C6 1 0.374828 0.136692 0.549071 11.00000 0.02542 0.02501 = 0.01735 0.00213 0.00178 0.00177 C7 1 0.428049 0.225055 0.539913 11.00000 0.02687 0.02307 = 0.02012 0.00149 0.00071 0.00055 AFIX 43 H7 2 0.436444 0.306586 0.599141 11.00000 -1.20000 AFIX 0 C8 1 0.469038 0.194158 0.444042 11.00000 0.02230 0.02503 = 0.02119 0.00397 0.00140 -0.00016 C9 1 0.457799 0.075311 0.356760 11.00000 0.02574 0.02728 = 0.01827 0.00136 0.00179 0.00482 AFIX 43 H9 2 0.486461 0.054093 0.292474 11.00000 -1.20000 AFIX 0 C10 1 0.404392 -0.011796 0.364516 11.00000 0.02961 0.02661 = 0.01972 -0.00249 0.00051 0.00392 AFIX 43 H10 2 0.396092 -0.092469 0.304280 11.00000 -1.20000 AFIX 0 C11 1 0.362523 0.017547 0.459950 11.00000 0.02603 0.02379 = 0.02086 0.00395 0.00015 -0.00146 O11 5 0.311229 -0.072050 0.464933 11.00000 0.02966 0.03165 = 0.02491 -0.00432 0.00397 -0.00749 H11 2 0.298037 -0.053095 0.536191 11.00000 0.05030 C12 1 0.344574 -0.036453 0.806901 11.00000 0.03471 0.02905 = 0.02389 0.00432 -0.00093 0.00270 AFIX 137 H12A 2 0.382251 -0.070675 0.766541 11.00000 -1.50000 H12B 2 0.322788 -0.121783 0.841833 11.00000 -1.50000 H12C 2 0.357707 0.032346 0.880279 11.00000 -1.50000 AFIX 0 C13 1 0.185947 0.342938 0.696530 11.00000 0.03122 0.03216 = 0.02598 0.00182 0.00929 0.00046 AFIX 23 H13A 2 0.150209 0.309258 0.745340 11.00000 -1.20000 H13B 2 0.216175 0.398160 0.760558 11.00000 -1.20000 AFIX 0 C14 1 0.160294 0.446635 0.585063 11.00000 0.02822 0.03351 = 0.02641 0.00043 0.01090 0.00764 C15 1 0.193834 0.576055 0.557419 11.00000 0.03688 0.03188 = 0.02305 -0.00071 0.01019 0.00557 C16 1 0.167921 0.672254 0.456317 11.00000 0.04206 0.03762 = 0.03140 0.00622 0.01673 0.00919 AFIX 43 H16 2 0.190385 0.760281 0.438917 11.00000 -1.20000 AFIX 0 C17 1 0.110550 0.642564 0.381183 11.00000 0.03639 0.05871 = 0.03606 0.01691 0.01424 0.01589 C18 1 0.078582 0.513480 0.407916 11.00000 0.02524 0.06677 = 0.04354 0.01109 0.00319 0.00947 AFIX 43 H18 2 0.039284 0.491507 0.356414 11.00000 -1.20000 AFIX 0 C19 1 0.102361 0.414511 0.508361 11.00000 0.02404 0.04708 = 0.03925 0.00408 0.00724 0.00594 C20 1 0.257094 0.614052 0.633546 11.00000 0.05146 0.03585 = 0.03061 -0.00006 0.00389 -0.00864 AFIX 137 H20A 2 0.251188 0.634384 0.727310 11.00000 -1.50000 H20B 2 0.274798 0.702065 0.593763 11.00000 -1.50000 H20C 2 0.286486 0.530448 0.629137 11.00000 -1.50000 AFIX 0 C21 1 0.083615 0.749247 0.273245 11.00000 0.04459 0.09422 = 0.05745 0.04219 0.01193 0.02110 AFIX 137 H21A 2 0.077581 0.846817 0.313066 11.00000 -1.50000 H21B 2 0.042533 0.711949 0.231818 11.00000 -1.50000 H21C 2 0.113291 0.758057 0.204955 11.00000 -1.50000 AFIX 0 C22 1 0.064449 0.276545 0.531512 11.00000 0.02653 0.06089 = 0.06886 0.00953 0.00157 -0.00464 AFIX 137 H22A 2 0.085947 0.189735 0.498458 11.00000 -1.50000 H22B 2 0.021665 0.285305 0.483521 11.00000 -1.50000 H22C 2 0.061131 0.265056 0.627583 11.00000 -1.50000 AFIX 0 HKLF 4 REM Ai2 in P2(1)/c REM R1 = 0.0334 for 3783 Fo > 4sig(Fo) and 0.0357 for all 4096 data REM 225 parameters refined using 0 restraints END WGHT 0.0550 0.9070 REM Highest difference peak 0.584, deepest hole -0.597, 1-sigma level 0.073 Q1 1 0.5538 0.3096 0.3330 11.00000 0.05 0.58 Q2 1 0.5303 0.3196 0.5368 11.00000 0.05 0.43 Q3 1 0.5413 0.4406 0.4407 11.00000 0.05 0.43 Q4 1 0.4689 0.1429 0.4010 11.00000 0.05 0.40 Q5 1 0.5258 0.4077 0.5005 11.00000 0.05 0.38 Q6 1 0.5342 0.1975 0.4684 11.00000 0.05 0.37 Q7 1 0.5563 0.1912 0.4149 11.00000 0.05 0.34 Q8 1 0.3594 0.1440 0.5946 11.00000 0.05 0.31 Q9 1 0.5237 0.2201 0.4947 11.00000 0.05 0.28 Q10 1 0.0413 0.8024 0.2891 11.00000 0.05 0.28 Q11 1 0.3802 0.0074 0.4102 11.00000 0.05 0.28 Q12 1 0.4563 0.1993 0.4961 11.00000 0.05 0.27 Q13 1 0.2798 0.2972 0.6558 11.00000 0.05 0.27 Q14 1 0.1786 0.6173 0.5111 11.00000 0.05 0.26 Q15 1 0.0789 0.6820 0.1881 11.00000 0.05 0.25 Q16 1 0.0997 0.5507 0.3628 11.00000 0.05 0.25 Q17 1 0.0845 0.1639 0.5661 11.00000 0.05 0.24 Q18 1 0.1958 0.2838 0.6668 11.00000 0.05 0.24 Q19 1 0.1797 0.3824 0.6397 11.00000 0.05 0.24 Q20 1 0.1820 0.4835 0.5609 11.00000 0.05 0.22 ; _shelx_res_checksum 27419 _shelxl_version_number .2013 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 0.54220(2) 0.31515(2) 0.43375(2) 0.02813(9) Uani d 1 . . O O1 0.27633(7) 0.25150(17) 0.58702(14) 0.0298(3) Uani d 1 . . C C2 0.32957(9) 0.1726(2) 0.65118(19) 0.0232(4) Uani d 1 . . H H2 0.3517 0.2334 0.7256 0.028 Uiso calc 1 . . N N3 0.30119(8) 0.03941(18) 0.70533(15) 0.0240(3) Uani d 1 . . C C4 0.24396(10) 0.0998(2) 0.7578(2) 0.0286(4) Uani d 1 . . H H4A 0.2548 0.1518 0.8441 0.034 Uiso calc 1 . . H H4B 0.2124 0.0210 0.7696 0.034 Uiso calc 1 . . C C5 0.21970(10) 0.2075(2) 0.6467(2) 0.0275(4) Uani d 1 . . H H5 0.1901 0.1541 0.5785 0.033 Uiso calc 1 . . C C6 0.37483(9) 0.1367(2) 0.54907(18) 0.0226(4) Uani d 1 . . C C7 0.42805(9) 0.2251(2) 0.53991(18) 0.0235(4) Uani d 1 . . H H7 0.4364 0.3066 0.5991 0.028 Uiso calc 1 . . C C8 0.46904(9) 0.1942(2) 0.44404(19) 0.0229(4) Uani d 1 . . C C9 0.45780(9) 0.0753(2) 0.35676(18) 0.0238(4) Uani d 1 . . H H9 0.4865 0.0541 0.2925 0.029 Uiso calc 1 . . C C10 0.40439(10) -0.0118(2) 0.36452(18) 0.0255(4) Uani d 1 . . H H10 0.3961 -0.0925 0.3043 0.031 Uiso calc 1 . . C C11 0.36252(9) 0.0175(2) 0.45995(18) 0.0237(4) Uani d 1 . . O O11 0.31123(7) -0.07205(17) 0.46493(15) 0.0287(3) Uani d 1 . . H H11 0.2980(17) -0.053(4) 0.536(4) 0.050(9) Uiso d 1 . . C C12 0.34457(10) -0.0365(2) 0.8069(2) 0.0295(4) Uani d 1 . . H H12A 0.3823 -0.0707 0.7665 0.044 Uiso calc 1 . . H H12B 0.3228 -0.1218 0.8418 0.044 Uiso calc 1 . . H H12C 0.3577 0.0323 0.8803 0.044 Uiso calc 1 . . C C13 0.18595(10) 0.3429(2) 0.6965(2) 0.0293(4) Uani d 1 . . H H13A 0.1502 0.3093 0.7453 0.035 Uiso calc 1 . . H H13B 0.2162 0.3982 0.7606 0.035 Uiso calc 1 . . C C14 0.16029(10) 0.4466(2) 0.5851(2) 0.0288(4) Uani d 1 . . C C15 0.19383(11) 0.5761(2) 0.5574(2) 0.0301(4) Uani d 1 . . C C16 0.16792(12) 0.6723(3) 0.4563(2) 0.0361(5) Uani d 1 . . H H16 0.1904 0.7603 0.4389 0.043 Uiso calc 1 . . C C17 0.11055(12) 0.6426(3) 0.3812(3) 0.0430(6) Uani d 1 . . C C18 0.07858(11) 0.5135(4) 0.4079(3) 0.0452(6) Uani d 1 . . H H18 0.0393 0.4915 0.3564 0.054 Uiso calc 1 . . C C19 0.10236(10) 0.4145(3) 0.5084(2) 0.0365(5) Uani d 1 . . C C20 0.25709(13) 0.6141(3) 0.6335(2) 0.0393(5) Uani d 1 . . H H20A 0.2512 0.6344 0.7273 0.059 Uiso calc 1 . . H H20B 0.2748 0.7021 0.5938 0.059 Uiso calc 1 . . H H20C 0.2865 0.5304 0.6291 0.059 Uiso calc 1 . . C C21 0.08362(15) 0.7492(5) 0.2732(3) 0.0650(10) Uani d 1 . . H H21A 0.0776 0.8468 0.3131 0.097 Uiso calc 1 . . H H21B 0.0425 0.7119 0.2318 0.097 Uiso calc 1 . . H H21C 0.1133 0.7581 0.2050 0.097 Uiso calc 1 . . C C22 0.06445(12) 0.2765(4) 0.5315(3) 0.0523(7) Uani d 1 . . H H22A 0.0859 0.1897 0.4985 0.079 Uiso calc 1 . . H H22B 0.0217 0.2853 0.4835 0.079 Uiso calc 1 . . H H22C 0.0611 0.2651 0.6276 0.079 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 0.02612(13) 0.02966(14) 0.02922(14) -0.00322(7) 0.00584(9) 0.00477(7) O1 0.0269(7) 0.0344(8) 0.0296(7) 0.0054(6) 0.0103(6) 0.0108(6) C2 0.0242(9) 0.0241(9) 0.0216(8) -0.0010(7) 0.0035(7) 0.0011(7) N3 0.0258(8) 0.0261(8) 0.0201(7) -0.0015(6) 0.0024(6) 0.0029(6) C4 0.0291(9) 0.0332(10) 0.0245(9) -0.0019(8) 0.0076(7) 0.0037(8) C5 0.0270(10) 0.0315(10) 0.0249(9) -0.0003(8) 0.0068(7) 0.0021(8) C6 0.0254(9) 0.0250(9) 0.0173(8) 0.0018(7) 0.0018(6) 0.0021(7) C7 0.0269(9) 0.0231(8) 0.0201(8) 0.0005(7) 0.0007(7) 0.0015(7) C8 0.0223(9) 0.0250(9) 0.0212(9) -0.0002(7) 0.0014(7) 0.0040(7) C9 0.0257(9) 0.0273(9) 0.0183(8) 0.0048(7) 0.0018(6) 0.0014(7) C10 0.0296(9) 0.0266(9) 0.0197(8) 0.0039(8) 0.0005(7) -0.0025(7) C11 0.0260(9) 0.0238(9) 0.0209(8) -0.0015(7) 0.0002(7) 0.0039(7) O11 0.0297(7) 0.0317(8) 0.0249(7) -0.0075(6) 0.0040(6) -0.0043(6) C12 0.0347(10) 0.0290(10) 0.0239(9) 0.0027(8) -0.0009(8) 0.0043(8) C13 0.0312(10) 0.0322(10) 0.0260(10) 0.0005(8) 0.0093(8) 0.0018(8) C14 0.0282(9) 0.0335(10) 0.0264(9) 0.0076(8) 0.0109(7) 0.0004(8) C15 0.0369(11) 0.0319(10) 0.0231(9) 0.0056(8) 0.0102(8) -0.0007(8) C16 0.0421(13) 0.0376(12) 0.0314(11) 0.0092(9) 0.0167(10) 0.0062(9) C17 0.0364(12) 0.0587(15) 0.0361(12) 0.0159(11) 0.0142(10) 0.0169(11) C18 0.0252(10) 0.0668(17) 0.0435(13) 0.0095(11) 0.0032(9) 0.0111(12) C19 0.0240(9) 0.0471(13) 0.0392(11) 0.0059(9) 0.0072(8) 0.0041(10) C20 0.0515(14) 0.0358(12) 0.0306(11) -0.0086(10) 0.0039(10) -0.0001(9) C21 0.0446(15) 0.094(3) 0.0574(17) 0.0211(17) 0.0119(13) 0.0422(19) C22 0.0265(11) 0.0609(17) 0.0689(18) -0.0046(12) 0.0016(11) 0.0095(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 O1 C5 . . 108.79(14) ? O1 C2 N3 . . 104.01(15) ? O1 C2 C6 . . 109.02(15) ? N3 C2 C6 . . 112.83(16) ? O1 C2 H2 . . 110.3 ? N3 C2 H2 . . 110.3 ? C6 C2 H2 . . 110.3 ? C12 N3 C2 . . 112.92(16) ? C12 N3 C4 . . 113.51(15) ? C2 N3 C4 . . 102.26(15) ? N3 C4 C5 . . 101.41(15) ? N3 C4 H4A . . 111.5 ? C5 C4 H4A . . 111.5 ? N3 C4 H4B . . 111.5 ? C5 C4 H4B . . 111.5 ? H4A C4 H4B . . 109.3 ? O1 C5 C13 . . 110.61(17) ? O1 C5 C4 . . 104.45(16) ? C13 C5 C4 . . 113.71(17) ? O1 C5 H5 . . 109.3 ? C13 C5 H5 . . 109.3 ? C4 C5 H5 . . 109.3 ? C7 C6 C11 . . 119.50(17) ? C7 C6 C2 . . 119.82(17) ? C11 C6 C2 . . 120.64(17) ? C6 C7 C8 . . 119.94(18) ? C6 C7 H7 . . 120.0 ? C8 C7 H7 . . 120.0 ? C9 C8 C7 . . 121.00(18) ? C9 C8 Br1 . . 119.54(14) ? C7 C8 Br1 . . 119.46(15) ? C10 C9 C8 . . 119.20(17) ? C10 C9 H9 . . 120.4 ? C8 C9 H9 . . 120.4 ? C9 C10 C11 . . 120.70(18) ? C9 C10 H10 . . 119.7 ? C11 C10 H10 . . 119.7 ? O11 C11 C10 . . 118.61(18) ? O11 C11 C6 . . 121.74(17) ? C10 C11 C6 . . 119.65(18) ? C11 O11 H11 . . 105(2) ? N3 C12 H12A . . 109.5 ? N3 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? N3 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? C14 C13 C5 . . 113.25(17) ? C14 C13 H13A . . 108.9 ? C5 C13 H13A . . 108.9 ? C14 C13 H13B . . 108.9 ? C5 C13 H13B . . 108.9 ? H13A C13 H13B . . 107.7 ? C19 C14 C15 . . 119.3(2) ? C19 C14 C13 . . 120.0(2) ? C15 C14 C13 . . 120.7(2) ? C16 C15 C14 . . 119.4(2) ? C16 C15 C20 . . 118.9(2) ? C14 C15 C20 . . 121.7(2) ? C17 C16 C15 . . 121.8(2) ? C17 C16 H16 . . 119.1 ? C15 C16 H16 . . 119.1 ? C16 C17 C18 . . 118.2(2) ? C16 C17 C21 . . 120.5(3) ? C18 C17 C21 . . 121.3(3) ? C17 C18 C19 . . 122.1(2) ? C17 C18 H18 . . 119.0 ? C19 C18 H18 . . 119.0 ? C18 C19 C14 . . 119.2(2) ? C18 C19 C22 . . 118.8(2) ? C14 C19 C22 . . 122.0(2) ? C15 C20 H20A . . 109.5 ? C15 C20 H20B . . 109.5 ? H20A C20 H20B . . 109.5 ? C15 C20 H20C . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? C17 C21 H21A . . 109.5 ? C17 C21 H21B . . 109.5 ? H21A C21 H21B . . 109.5 ? C17 C21 H21C . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 109.5 ? C19 C22 H22A . . 109.5 ? C19 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C19 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C8 . 1.9019(19) ? O1 C2 . 1.424(2) ? O1 C5 . 1.448(2) ? C2 N3 . 1.472(2) ? C2 C6 . 1.509(3) ? C2 H2 . 1.0000 ? N3 C12 . 1.465(2) ? N3 C4 . 1.472(3) ? C4 C5 . 1.525(3) ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? C5 C13 . 1.524(3) ? C5 H5 . 1.0000 ? C6 C7 . 1.388(3) ? C6 C11 . 1.404(3) ? C7 C8 . 1.389(3) ? C7 H7 . 0.9500 ? C8 C9 . 1.388(3) ? C9 C10 . 1.383(3) ? C9 H9 . 0.9500 ? C10 C11 . 1.396(3) ? C10 H10 . 0.9500 ? C11 O11 . 1.356(2) ? O11 H11 . 0.81(4) ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 0.9800 ? C13 C14 . 1.513(3) ? C13 H13A . 0.9900 ? C13 H13B . 0.9900 ? C14 C19 . 1.404(3) ? C14 C15 . 1.407(3) ? C15 C16 . 1.401(3) ? C15 C20 . 1.505(3) ? C16 C17 . 1.382(4) ? C16 H16 . 0.9500 ? C17 C18 . 1.385(4) ? C17 C21 . 1.513(4) ? C18 C19 . 1.399(4) ? C18 H18 . 0.9500 ? C19 C22 . 1.510(4) ? C20 H20A . 0.9800 ? C20 H20B . 0.9800 ? C20 H20C . 0.9800 ? C21 H21A . 0.9800 ? C21 H21B . 0.9800 ? C21 H21C . 0.9800 ? C22 H22A . 0.9800 ? C22 H22B . 0.9800 ? C22 H22C . 0.9800 ? 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 O11 H11 N3 . 0.81(4) 1.89(4) 2.644(2) 155(3) yes C4 H4A O1 4_566 0.99 2.58 3.564(2) 171 yes C20 H20B O11 1_565 0.98 2.57 3.548(3) 173 yes C20 H20C O1 . 0.98 2.55 3.332(3) 136 yes C2 H2 Cg2 4_566 1.00 2.91 3.908(2) 176 yes C4 H4B Cg3 4_566 0.99 2.88 3.622(2) 132 yes C21 H21C Cg3 4_575 0.98 2.93 3.723(4) 138 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 C5 O1 C2 N3 . . . . 23.8(2) ? C5 O1 C2 C6 . . . . 144.39(16) ? O1 C2 N3 C12 . . . . -163.70(15) ? C6 C2 N3 C12 . . . . 78.3(2) ? O1 C2 N3 C4 . . . . -41.36(18) ? C6 C2 N3 C4 . . . . -159.35(16) ? C12 N3 C4 C5 . . . . 163.78(17) ? C2 N3 C4 C5 . . . . 41.84(18) ? C2 O1 C5 C13 . . . . 125.28(18) ? C2 O1 C5 C4 . . . . 2.6(2) ? N3 C4 C5 O1 . . . . -27.6(2) ? N3 C4 C5 C13 . . . . -148.32(17) ? O1 C2 C6 C7 . . . . 98.9(2) ? N3 C2 C6 C7 . . . . -146.13(17) ? O1 C2 C6 C11 . . . . -79.0(2) ? N3 C2 C6 C11 . . . . 36.0(2) ? C11 C6 C7 C8 . . . . -0.7(3) ? C2 C6 C7 C8 . . . . -178.59(17) ? C6 C7 C8 C9 . . . . -0.2(3) ? C6 C7 C8 Br1 . . . . -179.44(14) ? C7 C8 C9 C10 . . . . 1.0(3) ? Br1 C8 C9 C10 . . . . -179.76(14) ? C8 C9 C10 C11 . . . . -0.9(3) ? C9 C10 C11 O11 . . . . -179.15(17) ? C9 C10 C11 C6 . . . . -0.1(3) ? C7 C6 C11 O11 . . . . 179.93(17) ? C2 C6 C11 O11 . . . . -2.2(3) ? C7 C6 C11 C10 . . . . 0.9(3) ? C2 C6 C11 C10 . . . . 178.71(17) ? O1 C5 C13 C14 . . . . 64.6(2) ? C4 C5 C13 C14 . . . . -178.21(18) ? C5 C13 C14 C19 . . . . 80.4(2) ? C5 C13 C14 C15 . . . . -99.8(2) ? C19 C14 C15 C16 . . . . 1.7(3) ? C13 C14 C15 C16 . . . . -178.05(18) ? C19 C14 C15 C20 . . . . -178.2(2) ? C13 C14 C15 C20 . . . . 2.1(3) ? C14 C15 C16 C17 . . . . -1.0(3) ? C20 C15 C16 C17 . . . . 178.9(2) ? C15 C16 C17 C18 . . . . -0.1(4) ? C15 C16 C17 C21 . . . . 179.6(2) ? C16 C17 C18 C19 . . . . 0.5(4) ? C21 C17 C18 C19 . . . . -179.2(3) ? C17 C18 C19 C14 . . . . 0.2(4) ? C17 C18 C19 C22 . . . . 179.8(3) ? C15 C14 C19 C18 . . . . -1.3(3) ? C13 C14 C19 C18 . . . . 178.4(2) ? C15 C14 C19 C22 . . . . 179.1(2) ? C13 C14 C19 C22 . . . . -1.1(3) ? _cod_database_fobs_code 2244110