#------------------------------------------------------------------------------ #$Date: 2018-03-14 09:26:04 +0200 (Wed, 14 Mar 2018) $ #$Revision: 206945 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/90/1549065.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_1549065 loop_ _publ_author_name 'Pal, Tarun Kumar' 'Hossain, Md Dulal' 'Sheikh, Md Chanmiya' 'Miyatake, Ryuta' 'Alam, Md Ashraful' _publ_section_title ; 2,4-Dibromo-6-[(2-hydroxy-5-methylanilino)methylidene]cyclohexa-2,4-dienone ; _journal_coeditor_code IS4026 _journal_issue 3 _journal_name_full IUCrData _journal_page_first x180388 _journal_paper_doi 10.1107/S2414314618003887 _journal_volume 3 _journal_year 2018 _chemical_formula_iupac 'C14 H11 Br2 N O2' _chemical_formula_moiety 'C14 H11 Br2 N O2' _chemical_formula_sum 'C14 H11 Br2 N O2' _chemical_formula_weight 385.05 _chemical_name_systematic ; 2,4-Dibromo-6-[(2-hydroxy-5-methylanilino)methylidene]cyclohexa-2,4-dienone ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 99.502(7) _cell_angle_gamma 90.0000 _cell_formula_units_Z 8 _cell_length_a 16.7219(3) _cell_length_b 6.90389(13) _cell_length_c 23.0811(4) _cell_measurement_reflns_used 27726 _cell_measurement_temperature 173 _cell_measurement_theta_max 68.22 _cell_measurement_theta_min 3.04 _cell_volume 2628.07(10) _computing_cell_refinement ; RAPID-AUTO (Rigaku, 2001) ; _computing_data_reduction ; RAPID-AUTO (Rigaku, 2001) ; _computing_molecular_graphics ; CrystalStructure (Rigaku, 2017) ; _computing_publication_material ; CrystalStructure (Rigaku, 2017) ; _computing_structure_refinement ; SHELXL97 (Sheldrick, 2008) ; _computing_structure_solution ; SIR92 (Altomare et al., 1993) ; _diffrn_ambient_temperature 173 _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 28830 _diffrn_reflns_theta_full 67.687 _diffrn_reflns_theta_max 68.222 _diffrn_reflns_theta_min 3.038 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.813 _exptl_absorpt_correction_T_max 0.535 _exptl_absorpt_correction_T_min 0.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Higashi, 1995) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.946 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 1504.00 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.99 _refine_diff_density_min -0.61 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment mixed _refine_ls_number_parameters 361 _refine_ls_number_reflns 4799 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0293 _refine_ls_shift/su_max 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0323P)^2^+3.2500P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.0743 _reflns_number_gt 4558 _reflns_number_total 4799 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file is4026sup1.cif _cod_data_source_block I _cod_original_cell_volume 2628.06(10) _cod_database_code 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481.24 0 -4 1 5550.50 386.36 0 -4 1 5597.03 392.45 0 -4 1 5743.61 436.64 0 -4 -1 6223.52 468.97 0 -4 1 6216.00 436.86 0 -4 -1 5733.13 457.08 0 4 2 14.52 3.68 0 4 2 2.70 3.03 0 4 -2 7.46 3.18 0 4 2 10.78 2.79 0 4 -2 7.13 3.45 0 -4 2 9.96 4.39 0 -4 -2 7.29 2.73 0 -4 2 4.27 3.72 0 -4 -2 11.37 3.60 0 4 3 124.67 6.68 0 4 3 145.28 7.56 0 4 -3 134.25 8.15 0 4 3 136.40 6.89 0 4 -3 177.01 13.88 0 -4 3 131.94 6.62 0 -4 3 139.56 4.87 0 -4 3 153.08 13.93 0 -4 3 123.75 4.88 0 -4 -3 139.69 10.06 0 -4 -3 130.62 7.72 0 -4 -3 144.74 9.66 0 4 4 13.13 2.68 0 4 4 11.69 3.02 0 4 -4 17.18 3.19 0 4 4 16.63 2.58 0 4 -4 13.76 3.76 0 -4 4 15.37 2.58 0 -4 4 15.54 2.78 0 -4 4 12.57 3.75 0 -4 4 16.60 1.94 0 -4 -4 15.36 2.65 0 -4 -4 14.43 3.77 0 -4 -4 13.29 4.04 0 4 5 383.64 19.76 0 4 5 469.64 22.36 0 4 -5 439.43 18.02 0 4 5 414.00 16.27 0 4 -5 432.14 20.91 0 -4 5 470.68 17.05 0 -4 5 413.59 14.35 0 -4 5 435.56 20.92 0 -4 5 400.24 14.63 0 -4 -5 417.14 19.91 0 -4 -5 412.89 20.74 0 -4 -5 373.20 19.80 0 4 6 2.76 2.19 0 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34.37 6.49 0 -4 13 25.20 4.04 0 -4 -13 27.19 6.58 0 -4 14 65.44 10.27 0 -4 -14 61.27 8.18 0 -4 -14 52.44 8.02 0 4 -15 566.90 42.99 0 -4 15 669.93 34.31 0 -4 -15 686.83 38.33 0 4 -16 461.37 28.86 0 -4 16 513.05 27.71 0 -4 -16 537.17 30.54 0 4 -17 2.30 3.69 0 -4 17 3.32 4.09 0 -4 -17 -0.10 3.77 0 4 -18 -0.07 3.37 0 -4 18 1.02 3.63 0 -4 -18 8.09 4.06 0 -4 19 1601.47 93.69 0 -4 -19 1563.44 91.62 0 -4 20 61.20 12.78 0 -4 -20 27.61 5.66 0 -4 21 21.69 5.17 0 -4 -21 15.53 7.36 0 -4 22 5.61 3.27 0 -4 -22 3.86 3.30 0 -4 23 463.55 20.16 0 -4 -23 483.20 29.54 0 -4 24 104.22 8.28 0 -4 -24 104.30 6.51 0 -5 0 1.59 2.31 0 -5 0 -0.45 3.50 0 -5 1 38.67 4.21 0 -5 1 44.36 10.21 0 -5 -1 41.65 4.28 0 -5 -1 31.63 6.49 0 -5 2 8.37 2.95 0 -5 2 0.67 4.38 0 -5 -2 2.96 2.64 0 -5 -2 0.56 6.44 0 -5 3 2113.77 114.28 0 -5 3 2343.32 143.38 0 -5 -3 2336.88 125.65 0 -5 -3 2023.66 132.82 0 -5 4 18.47 4.12 0 -5 4 19.64 5.72 0 -5 -4 20.43 4.30 0 -5 -4 39.23 10.09 0 -5 5 269.31 12.56 0 -5 5 253.89 17.10 0 -5 -5 265.07 13.20 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113.95 -2 -2 1 2507.18 119.21 -2 -2 1 2365.64 114.94 2 -2 -1 2518.12 114.72 -2 -2 1 2346.29 103.08 -2 2 0 5228.07 327.82 2 2 0 4835.15 315.28 -2 2 0 4726.84 307.37 2 2 0 4465.71 283.59 -2 2 0 4862.53 275.71 2 2 0 5428.07 341.41 -2 2 0 5232.96 326.25 2 2 0 5062.66 303.43 2 -2 0 5247.48 340.01 2 -2 0 4780.14 285.67 2 -2 0 4855.31 301.78 2 -2 0 5230.68 326.42 -2 -2 0 5331.90 339.31 -2 -2 0 4741.98 295.61 2 -2 0 5348.62 328.64 -2 -2 0 4882.63 314.87 2 -2 0 5005.32 281.42 -2 -2 0 4845.65 289.51 -2 2 -1 2042.26 95.24 2 2 1 2160.52 112.40 2 2 1 2038.11 96.27 -2 2 -1 2041.69 92.06 2 2 1 2180.01 96.52 -2 2 -1 2113.32 91.13 2 2 1 2135.50 88.57 2 -2 1 2173.76 97.19 2 -2 1 2005.99 86.70 2 -2 1 2150.16 94.86 -2 -2 -1 2117.39 94.77 -2 -2 -1 2013.16 87.97 2 -2 1 2111.79 97.80 -2 -2 -1 1913.76 87.49 2 -2 1 2124.96 95.83 -2 -2 -1 2017.99 80.65 -2 2 -2 216.83 6.87 2 2 2 234.04 4.62 2 2 2 244.41 11.04 2 2 2 225.61 7.53 -2 2 -2 225.70 7.51 2 2 2 237.39 6.85 -2 2 -2 236.75 12.18 2 2 2 218.81 5.70 2 -2 2 233.90 6.80 2 -2 2 241.85 8.41 2 -2 2 222.78 6.33 -2 -2 -2 228.12 4.16 -2 -2 -2 226.51 8.54 -2 -2 -2 221.68 7.33 2 -2 2 232.54 7.04 -2 -2 -2 215.78 7.63 2 -2 2 221.28 7.46 -2 -2 -2 230.05 5.12 2 2 3 2717.77 137.04 2 2 3 2799.83 126.04 2 2 3 2907.00 171.80 -2 2 -3 2525.74 104.62 -2 2 -3 2775.25 139.89 2 2 3 2821.73 136.24 -2 2 -3 2629.89 131.96 2 2 3 2840.40 128.31 -2 2 -3 2700.06 109.78 -2 2 -3 2646.76 135.99 2 -2 3 2701.55 131.34 2 -2 3 2723.29 137.52 2 -2 3 2911.87 147.52 2 -2 3 2703.25 144.81 -2 -2 -3 2822.40 124.54 -2 -2 -3 2767.32 135.81 2 -2 3 2703.54 131.28 -2 -2 -3 2480.16 131.02 -2 -2 -3 2532.53 132.84 -2 -2 -3 2606.85 116.43 -2 2 -4 2169.55 96.99 2 2 4 2107.47 88.94 2 2 4 2130.07 110.04 2 2 4 2122.84 98.21 -2 2 -4 2235.36 86.66 2 2 4 2217.27 95.29 -2 2 -4 2033.82 96.97 -2 2 -4 2265.70 106.08 2 2 4 2129.75 87.33 2 -2 4 2237.45 103.30 2 -2 4 2012.27 90.85 2 -2 4 2090.04 93.08 2 -2 4 2146.78 95.81 -2 -2 -4 2149.95 103.47 2 -2 4 2309.41 109.62 -2 -2 -4 2005.05 100.81 -2 -2 -4 1876.81 87.46 -2 -2 -4 2021.26 84.74 -2 2 -5 430.94 13.24 2 2 5 442.06 13.31 -2 2 -5 400.79 13.13 -2 2 -5 447.03 15.49 2 2 5 458.30 19.46 2 2 5 446.07 15.24 2 2 5 459.92 13.39 2 2 5 439.57 10.58 -2 2 -5 431.81 10.36 2 -2 5 464.43 15.03 2 -2 5 415.52 13.30 2 -2 5 444.79 14.05 -2 -2 -5 443.71 12.85 -2 -2 -5 439.45 21.43 2 -2 5 410.18 15.95 -2 -2 -5 444.74 15.27 2 -2 5 454.55 16.67 2 -2 5 487.81 11.59 -2 -2 -5 409.01 13.13 -2 -2 -5 447.39 11.46 -2 2 -6 1.17 1.53 2 2 6 0.59 0.88 2 2 6 1.07 0.50 2 2 6 1.30 0.57 2 2 6 4.03 2.58 2 2 6 2.81 1.56 -2 2 -6 2.97 1.59 -2 2 -6 4.39 0.76 2 -2 6 1.16 0.48 2 -2 6 2.09 1.30 2 -2 6 2.74 1.81 -2 -2 -6 3.52 0.96 -2 -2 -6 4.33 2.37 -2 -2 -6 1.62 2.87 2 -2 6 6.16 2.71 2 -2 6 0.72 1.34 -2 -2 -6 5.35 1.07 -2 2 -7 4878.77 314.11 2 2 7 4562.51 297.32 -2 2 -7 4816.77 315.29 -2 2 -7 4484.80 306.13 2 2 7 4863.44 335.83 2 2 7 4503.44 301.53 2 2 7 4803.24 284.15 2 2 7 5036.72 298.85 -2 2 -7 4699.31 293.27 2 -2 7 5028.68 325.13 2 -2 7 4908.31 320.15 2 -2 7 4724.62 303.10 -2 -2 -7 4872.62 313.15 -2 -2 -7 5271.74 373.94 2 -2 7 4794.09 317.26 -2 -2 -7 5162.74 342.81 2 -2 7 4597.50 307.74 2 -2 7 4733.18 284.83 -2 -2 -7 4842.81 302.03 -2 2 -8 182.28 9.42 2 2 8 175.65 7.48 -2 2 -8 157.02 7.23 -2 2 -8 161.34 6.69 2 2 8 180.73 9.56 2 2 8 145.49 6.66 2 2 8 166.31 3.88 2 2 8 172.61 4.36 -2 2 -8 192.81 5.39 2 -2 8 174.15 6.12 2 -2 8 153.73 6.27 2 -2 8 172.93 6.67 -2 -2 -8 172.88 5.69 -2 -2 -8 200.25 9.72 2 -2 8 175.54 7.69 -2 -2 -8 176.50 8.08 2 -2 8 169.16 7.70 2 -2 8 184.26 4.88 -2 -2 -8 163.76 4.12 -2 2 -9 626.90 28.16 -2 2 -9 500.77 21.03 -2 2 -9 542.48 20.69 2 2 9 584.08 25.99 2 2 9 513.22 21.03 2 2 9 532.21 17.38 -2 2 -9 623.69 20.64 2 -2 9 625.85 19.51 2 -2 9 625.02 21.89 2 -2 9 622.70 25.72 -2 -2 -9 611.37 20.71 -2 -2 -9 607.05 26.57 2 -2 9 550.67 20.56 -2 -2 -9 570.38 23.64 2 -2 9 599.59 23.44 2 -2 9 576.07 23.45 2 2 10 604.40 34.53 2 2 10 524.67 24.39 -2 2 -10 612.93 25.03 -2 2 -10 641.01 25.19 -2 2 -10 549.31 23.58 2 -2 10 554.71 29.72 2 -2 10 624.08 25.59 2 -2 10 657.27 25.53 2 -2 10 637.24 25.22 2 -2 10 643.92 23.99 -2 -2 -10 635.74 28.83 -2 -2 -10 614.06 22.20 -2 -2 -10 580.75 25.76 2 -2 10 605.11 23.69 2 2 11 1983.61 107.96 -2 2 -11 1993.53 97.73 -2 2 -11 1921.82 99.74 2 2 11 1911.88 106.77 -2 2 -11 1919.23 103.62 2 -2 11 2032.92 103.75 2 -2 11 1929.96 95.84 2 -2 11 2049.80 110.55 2 -2 11 1844.27 99.57 -2 -2 -11 2028.96 109.93 -2 -2 -11 2024.68 103.67 -2 -2 -11 1887.66 102.35 2 -2 11 2067.71 108.69 2 2 12 106.40 8.27 -2 2 -12 106.76 8.20 -2 2 -12 103.54 7.00 2 2 12 111.07 7.65 -2 2 -12 103.25 8.41 2 -2 12 103.27 6.76 2 -2 12 99.08 6.74 2 -2 12 106.67 6.75 2 -2 12 98.34 7.54 -2 -2 -12 112.71 8.72 -2 -2 -12 111.10 5.95 -2 -2 -12 93.67 7.45 2 -2 12 105.62 6.42 -2 2 -13 100.84 12.26 2 2 13 94.56 6.70 -2 2 -13 96.86 7.11 -2 2 -13 100.37 6.30 2 -2 13 92.73 5.06 -2 -2 -13 105.24 6.30 2 -2 13 103.99 6.81 2 -2 13 105.76 7.15 -2 -2 -13 92.32 7.94 -2 -2 -13 112.99 9.41 2 2 14 496.52 21.77 -2 2 -14 492.83 25.78 2 -2 14 502.20 23.26 -2 -2 -14 531.06 27.88 2 -2 14 486.32 23.06 -2 -2 -14 451.39 32.00 2 2 15 402.15 18.79 -2 2 -15 411.11 20.70 2 -2 15 414.07 20.86 -2 -2 -15 446.17 24.55 2 -2 15 424.52 20.99 -2 -2 -15 317.51 19.11 2 2 16 191.27 15.51 -2 2 -16 204.77 12.22 2 -2 16 170.48 17.40 -2 -2 -16 225.78 22.65 2 -2 16 209.43 12.39 -2 -2 -16 155.98 12.34 2 2 17 1335.06 70.33 -2 2 -17 1368.62 74.72 2 -2 17 1358.08 73.97 -2 -2 -17 1401.60 81.42 2 -2 17 1353.72 72.84 2 2 18 125.91 13.99 -2 2 -18 126.60 13.48 2 -2 18 121.51 15.29 -2 -2 -18 148.73 12.60 2 -2 18 124.06 10.05 -2 -2 -18 110.60 10.80 2 2 19 570.56 29.69 -2 2 -19 553.65 35.71 2 -2 19 550.33 29.43 -2 -2 -19 612.40 36.27 2 -2 19 558.25 37.30 2 2 20 37.12 5.66 -2 2 -20 35.58 7.92 2 -2 20 41.20 8.70 -2 -2 -20 42.66 7.66 2 -2 20 38.85 5.94 2 2 21 943.30 48.85 2 -2 21 997.40 50.33 2 -2 21 991.40 49.82 -2 -2 -21 1136.34 66.62 2 2 22 326.97 16.50 2 -2 22 317.67 16.93 2 -2 22 336.77 16.31 -2 -2 -22 371.45 21.49 2 2 23 378.35 17.54 2 -2 23 387.37 18.65 2 -2 23 369.24 16.77 -2 -2 -23 446.90 24.24 2 2 24 19.80 5.09 2 -2 24 22.50 3.64 2 -2 24 19.33 3.13 -2 -2 -24 20.40 4.48 2 2 25 81.97 6.99 2 -2 25 92.04 8.27 2 -2 25 82.12 4.40 -2 -2 -25 103.40 10.08 2 -2 26 23.22 4.43 -2 -2 -26 27.13 5.16 -2 3 25 4.30 3.87 2 -3 -25 4.08 4.90 -2 -3 25 19.31 4.51 -2 3 24 221.13 15.83 2 -3 -24 260.30 15.64 -2 -3 24 285.60 19.41 -2 3 23 30.94 4.88 2 -3 -23 41.14 7.24 -2 -3 23 32.75 6.31 -2 3 22 544.16 26.58 2 -3 -22 641.83 37.74 -2 -3 22 470.30 24.19 -2 -3 22 643.77 32.18 -2 3 21 420.59 20.45 2 -3 -21 460.62 30.00 -2 -3 21 364.66 19.56 -2 -3 21 418.31 22.76 2 -3 -20 381.08 20.29 2 -3 -20 415.38 26.11 -2 -3 20 342.13 19.10 -2 -3 20 429.28 21.25 2 -3 -19 338.70 24.07 2 -3 -19 376.51 25.60 -2 -3 19 316.71 27.25 -2 -3 19 629.26 28.16 2 -3 -18 3.80 3.25 2 -3 -18 8.34 5.37 -2 -3 18 0.31 3.13 -2 -3 18 3.22 3.18 2 -3 -17 180.56 10.30 2 -3 -17 180.64 15.29 2 3 -16 56.44 8.15 2 -3 -16 59.64 7.93 2 -3 -16 76.59 14.28 -2 -3 16 53.65 8.58 -2 -3 16 55.90 5.66 2 3 -15 49.44 6.39 2 3 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23 26.03 5.19 -4 -3 -23 31.85 3.84 4 -3 23 24.27 3.37 4 -3 24 11.05 3.58 4 -3 24 11.85 3.50 -4 -3 -24 12.17 2.72 4 -4 -24 37.33 3.74 -4 -4 24 41.92 4.59 4 -4 -23 6.77 3.23 -4 -4 23 0.82 2.97 4 -4 -22 162.08 15.35 -4 -4 22 213.52 13.49 -4 4 21 7.10 3.28 4 -4 -21 3.18 3.54 -4 -4 21 45.38 7.21 4 -4 -20 4.24 2.97 4 -4 -20 1.11 6.00 -4 -4 20 8.37 4.17 4 -4 -19 713.36 33.42 4 -4 -19 723.49 43.50 -4 -4 19 735.96 36.92 4 -4 -18 1.21 2.67 4 -4 -18 1.47 4.29 -4 -4 18 39.30 9.36 4 -4 -17 95.22 6.71 4 -4 -17 95.58 16.62 -4 -4 17 99.39 7.89 4 -4 -16 448.68 25.79 4 -4 -16 492.48 41.95 -4 -4 16 378.91 20.00 -4 -4 16 470.63 21.61 4 -4 -15 481.78 21.67 4 -4 -15 507.12 33.36 -4 -4 15 425.97 22.36 -4 -4 15 507.29 23.69 4 4 -14 2.35 2.92 4 -4 -14 1.43 2.55 4 -4 -14 9.96 4.63 -4 -4 14 0.79 4.41 4 4 -13 53.14 5.67 4 -4 -13 57.83 4.75 4 -4 -13 49.65 8.13 -4 -4 13 59.70 6.49 4 4 -12 8.63 2.39 4 4 -12 11.84 4.22 4 4 -12 8.29 3.15 4 -4 -12 8.62 4.69 4 -4 -12 14.17 4.34 -4 -4 12 7.29 3.78 4 4 -11 4.63 3.55 4 4 -11 4.55 2.01 4 4 -11 1.81 2.65 4 -4 -11 4.97 2.36 4 -4 -11 7.13 3.51 -4 -4 11 4.96 5.84 4 4 -10 2139.06 111.82 4 4 -10 2086.90 115.16 4 -4 -10 2015.01 125.34 4 -4 -10 1977.78 102.62 -4 -4 10 2066.73 107.72 -4 -4 10 2232.21 131.98 4 4 -9 146.77 7.46 4 4 -9 130.13 8.59 4 -4 -9 142.86 17.19 4 -4 -9 129.07 6.50 -4 -4 9 148.54 6.74 -4 -4 9 142.43 10.49 -4 4 8 5.30 2.00 4 4 -8 6.92 2.96 -4 4 8 3.47 2.22 4 4 -8 4.65 2.24 4 -4 -8 4.55 2.01 4 -4 -8 5.01 1.71 4 -4 -8 2.54 4.64 -4 -4 8 7.59 2.11 -4 -4 8 3.96 3.76 -4 4 7 101.82 7.42 4 4 -7 83.71 4.51 4 4 -7 101.23 5.93 -4 4 7 92.28 5.24 4 4 -7 95.73 5.24 4 -4 -7 89.49 10.08 4 -4 -7 97.96 4.50 4 -4 -7 92.36 4.92 -4 -4 7 101.83 5.24 -4 -4 7 95.53 8.43 -4 4 6 334.96 12.80 4 4 -6 306.46 11.90 4 4 -6 374.22 18.86 -4 4 6 322.00 12.56 4 4 -6 319.78 12.37 -4 4 6 349.31 16.19 4 -4 -6 305.36 20.11 4 -4 -6 319.61 12.28 -4 -4 6 346.96 13.39 4 -4 -6 326.93 11.59 -4 -4 6 326.15 18.17 -4 -4 6 345.87 15.46 -4 4 5 157.16 6.98 4 4 -5 134.59 5.93 4 4 -5 152.74 7.98 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370.71 21.51 18 -1 -12 305.58 17.06 -18 -1 12 449.27 22.53 -18 1 11 865.23 50.19 18 1 -11 552.00 27.77 18 1 -11 715.55 31.53 18 -1 -11 551.51 26.34 -18 -1 11 833.62 49.53 -18 1 10 101.36 7.59 18 1 -10 62.29 5.59 18 1 -10 86.42 6.99 18 -1 -10 67.17 5.35 -18 -1 10 101.16 8.22 -18 1 9 108.82 7.88 18 1 -9 70.26 5.77 18 1 -9 97.68 11.16 18 -1 -9 78.89 8.22 -18 -1 9 113.00 8.32 -18 1 8 26.12 4.36 18 1 -8 23.78 4.68 18 -1 -8 20.52 3.50 18 -1 -8 14.50 3.38 -18 -1 8 27.29 4.48 -18 1 7 151.25 9.07 18 1 -7 137.56 9.62 18 -1 -7 117.80 7.90 18 -1 -7 106.00 7.19 -18 -1 7 146.67 9.02 18 1 -6 9.74 4.06 -18 1 6 1.91 2.91 18 -1 -6 7.84 3.14 -18 -1 6 5.52 2.79 18 1 -5 0.34 3.37 -18 1 5 8.74 2.77 18 -1 -5 2.67 4.26 -18 -1 5 -1.95 2.71 -18 1 4 1265.12 59.98 18 1 -4 1331.52 69.18 18 -1 -4 1144.99 62.03 18 -1 -4 1423.80 76.32 -18 -1 4 1204.57 63.93 18 1 -3 6.67 6.68 -18 1 3 3.64 3.05 18 -1 -3 8.91 3.41 -18 -1 3 9.73 2.71 18 1 -2 1199.88 59.93 -18 1 2 1092.90 56.29 18 -1 -2 1065.13 54.70 18 1 -1 182.29 11.71 18 -1 -1 173.46 14.93 18 1 0 381.07 23.50 18 -1 0 411.30 19.23 18 1 1 66.38 5.58 18 -1 1 49.27 6.46 18 -1 1 75.63 5.80 18 1 2 1.63 2.61 18 -1 2 8.12 4.19 18 1 3 38.49 4.21 18 -1 3 35.92 4.35 18 1 4 640.04 27.70 18 -1 4 699.47 29.87 18 1 5 766.73 32.67 18 -1 5 766.13 33.47 18 1 6 33.41 3.60 18 -1 6 34.98 3.79 18 1 7 99.24 5.27 18 -1 7 102.46 5.70 -18 2 14 103.71 7.02 18 2 -14 77.50 9.34 18 2 -14 82.84 5.50 18 -2 -14 77.60 5.01 -18 -2 14 95.03 6.96 -18 2 13 162.33 9.29 18 2 -13 111.76 7.77 18 2 -13 123.85 7.48 18 -2 -13 117.70 9.67 -18 -2 13 144.83 9.29 -18 2 12 166.06 9.72 18 2 -12 119.76 8.37 18 2 -12 129.12 8.16 18 -2 -12 118.48 7.62 -18 -2 12 151.81 14.57 -18 2 11 514.85 29.48 18 2 -11 379.71 19.76 18 2 -11 436.56 25.70 18 -2 -11 397.64 19.73 -18 -2 11 475.51 23.27 -18 2 10 10.88 3.75 18 2 -10 2.28 3.73 18 2 -10 10.48 3.77 18 -2 -10 17.46 3.92 -18 -2 10 10.80 3.87 -18 2 9 2544.50 146.73 18 2 -9 1933.90 128.03 18 2 -9 2259.13 135.60 18 -2 -9 1976.06 119.46 -18 -2 9 2440.08 145.16 -18 2 8 526.52 23.76 18 2 -8 393.75 20.40 18 2 -8 482.14 23.43 18 -2 -8 378.81 22.32 -18 -2 8 500.53 24.10 18 2 -7 35.17 5.04 18 2 -7 47.38 5.83 -18 2 7 49.52 4.93 -18 -2 7 40.49 5.07 -18 2 6 33.53 4.28 18 2 -6 26.30 4.43 18 2 -6 36.85 5.50 18 -2 -6 47.20 5.19 -18 -2 6 32.23 4.12 18 2 -5 102.09 7.31 18 2 -5 155.13 13.64 -18 2 5 152.84 8.28 -18 -2 5 130.62 10.93 18 2 -4 56.26 7.14 18 2 -4 67.72 5.94 -18 2 4 71.67 5.35 18 -2 -4 46.06 4.01 -18 -2 4 62.39 4.76 18 2 -3 -0.28 2.36 18 2 -3 2.31 2.95 -18 2 3 2.53 2.40 18 -2 -3 3.65 2.02 -18 -2 3 2.01 3.07 18 2 -2 89.14 9.72 18 2 -2 61.01 5.05 -18 2 2 84.17 5.48 18 -2 -2 67.61 4.93 18 -2 -2 103.39 6.92 18 2 -1 54.47 5.26 18 2 -1 39.98 5.88 -18 2 1 46.77 3.72 18 -2 -1 41.61 4.09 18 -2 -1 67.57 5.46 18 2 0 1.09 2.70 18 2 0 1.83 2.92 18 -2 0 1.09 3.42 18 -2 0 10.80 4.26 18 2 1 398.37 16.86 18 -2 1 313.05 16.05 18 -2 1 348.11 15.25 18 2 2 102.26 6.23 18 -2 2 86.16 6.18 18 -2 2 92.04 5.65 18 2 3 225.36 9.89 18 -2 3 192.49 9.52 18 -2 3 220.28 12.93 18 2 4 3.86 2.23 18 -2 4 4.24 3.53 18 -2 4 8.37 2.28 18 2 5 220.09 9.03 18 -2 5 197.77 11.30 18 -2 5 220.41 9.53 18 2 6 174.42 7.25 18 -2 6 191.10 8.17 18 3 -11 331.80 15.32 -18 3 11 399.89 17.04 18 -3 -11 320.30 15.29 -18 -3 11 350.70 16.75 -18 3 10 403.25 17.73 18 3 -10 325.17 17.22 18 3 -10 365.36 21.79 18 -3 -10 337.36 20.89 -18 -3 10 404.85 18.21 -18 3 9 191.68 13.78 18 3 -9 147.63 13.63 18 3 -9 162.60 9.14 18 -3 -9 159.39 9.62 -18 -3 9 187.73 14.09 -18 3 8 4.94 2.70 18 3 -8 0.28 2.80 18 3 -8 -1.28 4.09 18 -3 -8 5.18 2.80 -18 -3 8 3.46 2.62 -18 3 7 40.54 4.24 18 3 -7 33.04 7.17 18 3 -7 33.55 4.51 18 -3 -7 35.36 4.63 -18 -3 7 33.66 3.89 -18 3 6 466.75 18.80 18 3 -6 366.43 18.74 18 3 -6 419.63 24.03 18 -3 -6 460.55 21.90 -18 -3 6 376.64 16.52 18 3 -5 164.21 14.20 18 3 -5 179.65 9.89 -18 3 5 198.97 8.89 -18 -3 5 149.97 7.38 -18 3 4 50.75 3.79 18 3 -4 42.70 4.75 18 3 -4 53.87 4.98 18 -3 -4 50.66 5.47 -18 -3 4 25.77 2.64 18 3 -3 5.77 2.74 18 3 -3 8.08 4.55 -18 3 3 10.43 3.97 -18 3 2 164.33 7.21 18 3 -2 153.55 11.50 18 3 -2 161.74 12.23 18 -3 -2 172.37 9.70 18 3 -1 19.94 2.96 18 3 -1 23.05 3.38 -18 3 1 21.42 2.24 18 3 0 16.92 2.70 18 3 0 21.53 3.04 18 -3 0 20.51 3.58 18 3 1 16.77 2.42 18 3 1 21.59 2.80 18 -3 1 19.95 5.35 18 3 2 5.35 1.76 18 -3 2 0.50 2.31 18 3 3 0.68 1.30 18 -3 3 5.93 2.09 -19 0 13 15.25 5.17 -19 0 12 3.11 2.50 19 0 -11 63.96 4.00 -19 0 11 92.04 5.93 19 0 -10 1.10 1.97 -19 0 10 1.96 2.48 19 0 -9 1936.87 112.21 -19 0 9 2477.70 147.76 19 0 -8 1.60 4.09 -19 0 8 6.09 4.61 19 0 -7 433.37 20.42 -19 0 7 476.79 25.53 19 0 -6 -2.19 2.70 -19 0 6 2.76 3.70 19 0 -5 397.75 23.80 -19 0 5 381.36 15.61 19 0 -4 1.18 2.52 -19 0 4 1.67 1.92 19 0 -3 94.17 6.61 -19 0 3 85.53 6.64 19 0 -2 -1.02 2.42 19 0 -1 225.88 11.15 19 0 0 3.99 2.54 19 0 1 605.72 30.46 19 0 2 0.75 1.97 19 0 3 23.36 2.97 19 0 4 -1.46 1.87 19 1 -12 6.06 3.58 -19 1 12 4.37 2.74 -19 -1 12 6.70 2.65 19 1 -11 338.08 14.88 -19 1 11 401.20 21.98 -19 -1 11 371.63 20.86 19 1 -10 28.59 3.98 -19 1 10 29.42 4.16 -19 -1 10 33.17 4.09 19 1 -9 340.20 16.35 -19 1 9 380.81 16.45 -19 -1 9 379.20 16.81 19 1 -8 29.14 3.90 -19 1 8 19.83 3.70 19 -1 -8 12.67 2.19 -19 -1 8 23.09 3.64 19 1 -7 1115.52 48.85 -19 1 7 1128.80 50.66 19 -1 -7 772.46 37.85 -19 -1 7 1054.83 48.12 19 1 -6 434.50 20.13 -19 1 6 451.45 18.56 19 -1 -6 335.35 19.84 -19 -1 6 406.55 17.02 19 1 -5 9.86 3.62 -19 1 5 16.93 3.07 19 -1 -5 10.58 2.72 -19 -1 5 15.57 4.42 19 1 -4 215.08 10.79 -19 1 4 205.83 11.83 19 -1 -4 173.45 9.02 -19 -1 4 186.20 8.18 19 1 -3 139.08 11.56 -19 1 3 122.79 5.93 19 -1 -3 110.92 9.81 19 1 -2 416.51 18.41 -19 1 2 345.50 12.58 19 -1 -2 373.20 16.59 19 1 -1 3.49 2.69 19 -1 -1 3.23 2.27 19 1 0 16.95 4.70 19 -1 0 9.90 2.77 19 1 1 177.48 8.55 19 -1 1 189.22 8.69 19 1 2 196.38 8.64 19 -1 2 189.48 8.73 19 1 3 14.96 2.68 19 -1 3 16.40 2.65 19 1 4 100.61 5.30 19 -1 4 101.51 7.47 19 2 -10 8.08 2.89 -19 2 10 13.25 4.90 -19 -2 10 15.18 2.93 19 2 -9 0.21 2.21 -19 2 9 0.85 2.16 -19 -2 9 0.43 2.04 19 2 -8 114.54 6.91 -19 2 8 123.49 6.58 19 -2 -8 82.99 7.36 -19 -2 8 108.28 6.10 19 2 -7 21.92 4.74 -19 2 7 27.98 3.36 19 -2 -7 57.66 3.83 -19 -2 7 21.72 4.85 19 2 -6 96.25 6.54 -19 2 6 88.24 5.19 19 -2 -6 87.27 5.31 -19 -2 6 84.81 4.85 19 2 -5 49.99 7.70 -19 2 5 57.45 4.11 -19 -2 5 48.21 3.18 19 2 -4 1.02 2.14 -19 2 4 5.46 3.27 19 2 -3 11.69 2.73 -19 2 3 11.50 2.07 19 -2 -3 10.23 2.23 19 2 -2 5.43 3.94 19 -2 -2 5.99 1.91 19 2 -1 123.96 6.92 19 -2 -1 117.19 6.45 19 2 0 1074.93 38.61 19 -2 0 548.20 24.29 19 2 1 161.83 6.71 19 -2 1 90.99 4.12 20 0 -7 5.96 1.87 -20 0 7 1.77 1.68 20 0 -6 276.49 14.75 20 0 -5 2.46 2.04 20 0 -4 434.73 21.70 20 0 -3 -2.30 2.08 20 0 -2 12.15 3.94 ; _shelx_hkl_checksum 23657 _shelx_res_file ; TITL SH120 shelxl.res created by SHELXL-2016/6 at 13:35:40 on 01-Dec-2017 CELL 1.54187 16.72188 6.90389 23.08111 90.00000 99.50230 90.00000 ZERR 8 0.00030 0.00013 0.00042 0.00000 0.00700 0.00000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC C H BR N O UNIT 112 88 16 8 16 L.S. 5 FMAP 2 PLAN 32 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -100.0 ACTA SIZE 0.360 0.290 0.080 WGHT 0.032300 3.250000 FVAR 0.40014 BR1 3 -0.017269 0.203637 0.643041 11.00000 0.01857 0.04917 = 0.03065 -0.00265 0.00568 -0.00132 BR2 3 0.241149 0.122060 0.515543 11.00000 0.02797 0.07136 = 0.02070 0.00201 0.00913 0.00151 BR3 3 0.256139 0.096117 1.092934 11.00000 0.02106 0.06243 = 0.02539 0.00489 0.00467 0.00287 BR4 3 -0.014885 0.110475 1.207989 11.00000 0.03446 0.03847 = 0.02417 0.00366 0.01380 0.00327 O1 5 0.124855 0.239088 0.746137 11.00000 0.02201 0.04714 = 0.02154 0.00000 0.00771 0.00040 O2 5 0.212279 0.159200 0.896388 11.00000 0.02056 0.05704 = 0.02801 0.00165 0.00803 0.00307 O3 5 0.126623 0.210504 0.986057 11.00000 0.02342 0.04573 = 0.02021 0.00254 0.00647 -0.00101 O4 5 0.048124 0.357854 0.836751 11.00000 0.02307 0.04672 = 0.02911 -0.00182 0.00881 0.00259 N1 4 0.274209 0.183870 0.798447 11.00000 0.01825 0.02915 = 0.02153 0.00188 0.00246 0.00015 N2 4 -0.019804 0.298535 0.931648 11.00000 0.01828 0.02657 = 0.02424 -0.00087 0.00277 0.00042 C1 1 0.233428 0.177210 0.694023 11.00000 0.02269 0.02346 = 0.02285 0.00250 0.00500 -0.00052 C2 1 0.149040 0.207152 0.697524 11.00000 0.02304 0.02297 = 0.02370 0.00246 0.00609 -0.00206 C3 1 0.095443 0.193467 0.642108 11.00000 0.01800 0.02561 = 0.02608 0.00178 0.00455 -0.00055 C4 1 0.122403 0.169208 0.589928 11.00000 0.02529 0.02928 = 0.02192 0.00162 0.00138 0.00038 AFIX 43 H4A 2 0.084848 0.163499 0.554274 11.00000 -1.20000 AFIX 0 C5 1 0.205907 0.152717 0.589162 11.00000 0.02590 0.03321 = 0.01711 0.00256 0.00735 -0.00040 C6 1 0.260574 0.152206 0.639664 11.00000 0.01985 0.03022 = 0.02539 0.00355 0.00653 0.00016 AFIX 43 H6 2 0.316657 0.135172 0.638484 11.00000 -1.20000 AFIX 0 C7 1 0.291742 0.168017 0.745653 11.00000 0.02160 0.02542 = 0.02582 0.00100 0.00459 -0.00039 AFIX 43 H7 2 0.346874 0.149222 0.741733 11.00000 -1.20000 AFIX 0 C8 1 0.328620 0.177881 0.852050 11.00000 0.02202 0.02552 = 0.02142 0.00236 0.00285 -0.00008 C9 1 0.294177 0.166555 0.902877 11.00000 0.02338 0.02952 = 0.02460 0.00230 0.00688 0.00201 C10 1 0.345612 0.164496 0.956918 11.00000 0.03135 0.04327 = 0.02211 0.00409 0.00578 0.00350 AFIX 43 H10 2 0.323451 0.156331 0.992180 11.00000 -1.20000 AFIX 0 C11 1 0.428510 0.174242 0.959514 11.00000 0.02869 0.04051 = 0.02305 0.00316 -0.00272 -0.00017 AFIX 43 H11 2 0.462526 0.173001 0.996797 11.00000 -1.20000 AFIX 0 C12 1 0.463720 0.185846 0.909021 11.00000 0.02404 0.02925 = 0.02874 0.00172 0.00039 -0.00063 C13 1 0.412419 0.187377 0.855152 11.00000 0.02230 0.02880 = 0.02181 0.00318 0.00456 -0.00049 AFIX 43 H13 2 0.434787 0.195000 0.819967 11.00000 -1.20000 AFIX 0 C14 1 0.554296 0.199169 0.912219 11.00000 0.02362 0.04838 = 0.03603 0.00629 -0.00131 -0.00304 AFIX 137 H14A 2 0.580797 0.101170 0.939574 11.00000 -1.20000 H14B 2 0.572862 0.328325 0.926028 11.00000 -1.20000 H14C 2 0.568130 0.176676 0.873133 11.00000 -1.20000 AFIX 0 C15 1 0.011835 0.218768 1.034308 11.00000 0.02421 0.02192 = 0.02362 -0.00191 0.00547 0.00018 C16 1 0.096732 0.190390 1.032962 11.00000 0.02445 0.02231 = 0.02174 -0.00157 0.00577 -0.00340 C17 1 0.143709 0.139272 1.088834 11.00000 0.02060 0.02763 = 0.02373 0.00018 0.00335 -0.00211 C18 1 0.110883 0.119077 1.138904 11.00000 0.02739 0.02864 = 0.01924 -0.00120 0.00328 -0.00051 AFIX 43 H18 2 0.144597 0.085854 1.174796 11.00000 -1.20000 AFIX 0 C19 1 0.027466 0.147298 1.137444 11.00000 0.02753 0.02496 = 0.01924 -0.00146 0.00754 0.00001 C20 1 -0.021723 0.194730 1.086292 11.00000 0.02181 0.02671 = 0.02650 -0.00150 0.00816 0.00176 AFIX 43 H20 2 -0.078274 0.211589 1.085518 11.00000 -1.20000 AFIX 0 C21 1 -0.041895 0.269825 0.982613 11.00000 0.02334 0.02606 = 0.02424 -0.00130 0.00510 0.00149 AFIX 43 H21 2 -0.097709 0.284149 0.985166 11.00000 -1.20000 AFIX 0 C22 1 -0.071130 0.348350 0.878455 11.00000 0.02366 0.02137 = 0.02110 -0.00150 0.00249 0.00111 C23 1 -0.033937 0.373283 0.829089 11.00000 0.02382 0.02635 = 0.02667 -0.00449 0.00564 -0.00002 C24 1 -0.082204 0.414726 0.775571 11.00000 0.03440 0.03509 = 0.02166 -0.00309 0.00783 -0.00084 AFIX 43 H24 2 -0.058047 0.430591 0.741398 11.00000 -1.20000 AFIX 0 C25 1 -0.165404 0.433022 0.771809 11.00000 0.03133 0.03217 = 0.02436 -0.00119 -0.00267 0.00095 AFIX 43 H25 2 -0.197437 0.461047 0.734813 11.00000 -1.20000 AFIX 0 C26 1 -0.203326 0.411483 0.820720 11.00000 0.02509 0.02715 = 0.02682 -0.00196 0.00242 -0.00011 C27 1 -0.154692 0.369467 0.874195 11.00000 0.02388 0.02457 = 0.02411 0.00034 0.00559 0.00100 AFIX 43 H27 2 -0.178942 0.354950 0.908375 11.00000 -1.20000 AFIX 0 C28 1 -0.293885 0.430806 0.816611 11.00000 0.02553 0.04383 = 0.03755 0.00091 0.00096 0.00304 AFIX 137 H28A 2 -0.307472 0.441898 0.856187 11.00000 -1.20000 H28B 2 -0.320532 0.316250 0.797111 11.00000 -1.20000 H28C 2 -0.312521 0.546832 0.793864 11.00000 -1.20000 AFIX 0 H1 2 0.227432 0.199184 0.800094 11.00000 0.03608 H2 2 0.192721 0.164290 0.930317 11.00000 0.06145 H2A 2 0.027574 0.284120 0.930069 11.00000 0.03079 H4 2 0.063399 0.328321 0.804206 11.00000 0.04147 HKLF 4 REM SH120 REM R1 = 0.0293 for 4558 Fo > 4sig(Fo) and 0.0322 for all 4799 data REM 361 parameters refined using 0 restraints END WGHT 0.0323 3.2499 REM Instructions for potential hydrogen bonds EQIV $1 x+1/2, -y+1/2, z-1/2 HTAB C7 Br4_$1 HTAB C10 Br3 EQIV $2 x-1/2, -y+1/2, z+1/2 HTAB C21 Br2_$2 HTAB C24 Br1 HTAB C27 Br2_$2 HTAB N1 O1 HTAB O2 O3 HTAB N2 O3 HTAB O4 O1 REM Highest difference peak 0.991, deepest hole -0.611, 1-sigma level 0.084 Q1 1 0.2434 0.2411 0.5198 11.00000 0.05 0.99 Q2 1 0.0202 0.1208 1.2526 11.00000 0.05 0.58 Q3 1 -0.0435 0.0996 1.1640 11.00000 0.05 0.53 Q4 1 0.2526 0.2120 1.0925 11.00000 0.05 0.53 Q5 1 0.0124 0.2028 0.6877 11.00000 0.05 0.52 Q6 1 -0.0498 0.2037 0.5954 11.00000 0.05 0.50 Q7 1 0.2865 0.0930 1.1403 11.00000 0.05 0.46 Q8 1 -0.0557 0.2018 0.6729 11.00000 0.05 0.44 Q9 1 0.2720 0.1214 0.5601 11.00000 0.05 0.44 Q10 1 -0.0121 0.2310 1.2185 11.00000 0.05 0.44 Q11 1 0.0104 0.2446 1.2154 11.00000 0.05 0.44 Q12 1 -0.0561 0.1087 1.2359 11.00000 0.05 0.42 Q13 1 0.0208 0.2046 0.6188 11.00000 0.05 0.42 Q14 1 0.2070 0.1325 0.4697 11.00000 0.05 0.41 Q15 1 0.2008 -0.0330 0.5088 11.00000 0.05 0.40 Q16 1 0.2830 -0.0362 0.5207 11.00000 0.05 0.40 Q17 1 0.0200 0.1131 1.1820 11.00000 0.05 0.38 Q18 1 0.2955 0.0942 1.0647 11.00000 0.05 0.37 Q19 1 0.2966 -0.0557 1.1035 11.00000 0.05 0.37 Q20 1 0.2206 0.0978 1.1160 11.00000 0.05 0.37 Q21 1 -0.1802 0.3983 0.8448 11.00000 0.05 0.37 Q22 1 -0.0556 0.0527 0.6272 11.00000 0.05 0.36 Q23 1 0.2162 -0.0539 1.0881 11.00000 0.05 0.35 Q24 1 0.2298 0.0980 1.0467 11.00000 0.05 0.34 Q25 1 -0.0515 -0.0222 1.1954 11.00000 0.05 0.33 Q26 1 0.2006 0.1242 0.5451 11.00000 0.05 0.33 Q27 1 0.1202 0.1902 1.0593 11.00000 0.05 0.32 Q28 1 0.1217 0.1541 0.6721 11.00000 0.05 0.32 Q29 1 0.2249 0.0495 1.0680 11.00000 0.05 0.32 Q30 1 0.1197 0.1972 0.7206 11.00000 0.05 0.32 Q31 1 0.0192 0.0653 0.6537 11.00000 0.05 0.32 Q32 1 -0.0216 -0.0307 1.2378 11.00000 0.05 0.30 ; _shelx_res_checksum 19495 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 -1/2+X,-1/2-Y,-1/2+Z loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy Br Br1 -0.01727(2) 0.20364(5) 0.64304(2) 0.03261(10) Uani d 1 Br Br2 0.24115(2) 0.12206(6) 0.51554(2) 0.03943(11) Uani d 1 Br Br3 0.25614(2) 0.09612(5) 1.09293(2) 0.03620(10) Uani d 1 Br Br4 -0.01488(2) 0.11048(5) 1.20799(2) 0.03135(9) Uani d 1 O O1 0.12485(11) 0.2391(3) 0.74614(8) 0.0298(4) Uani d 1 O O2 0.21228(12) 0.1592(3) 0.89639(9) 0.0347(5) Uani d 1 O O3 0.12662(11) 0.2105(3) 0.98606(8) 0.0295(4) Uani d 1 O O4 0.04812(12) 0.3579(3) 0.83675(9) 0.0325(5) Uani d 1 N N1 0.27421(14) 0.1839(3) 0.79845(9) 0.0231(5) Uani d 1 N N2 -0.01980(14) 0.2985(3) 0.93165(10) 0.0231(5) Uani d 1 C C1 0.23343(16) 0.1772(4) 0.69402(11) 0.0229(5) Uani d 1 C C2 0.14904(16) 0.2072(4) 0.69752(11) 0.0230(5) Uani d 1 C C3 0.09544(15) 0.1935(4) 0.64211(11) 0.0231(5) Uani d 1 C C4 0.12240(16) 0.1692(4) 0.58993(12) 0.0258(6) Uani d 1 H H4A 0.084848 0.163499 0.554274 0.031 Uiso calc 1 C C5 0.20591(16) 0.1527(4) 0.58916(11) 0.0250(6) Uani d 1 C C6 0.26057(16) 0.1522(4) 0.63966(12) 0.0248(6) Uani d 1 H H6 0.316657 0.135172 0.638484 0.030 Uiso calc 1 C C7 0.29174(16) 0.1680(4) 0.74565(11) 0.0242(6) Uani d 1 H H7 0.346874 0.149222 0.741733 0.029 Uiso calc 1 C C8 0.32862(16) 0.1779(4) 0.85205(11) 0.0231(5) Uani d 1 C C9 0.29418(16) 0.1666(4) 0.90288(12) 0.0255(6) Uani d 1 C C10 0.34561(18) 0.1645(5) 0.95692(12) 0.0321(7) Uani d 1 H H10 0.323451 0.156331 0.992180 0.039 Uiso calc 1 C C11 0.42851(17) 0.1742(5) 0.95951(12) 0.0315(6) Uani d 1 H H11 0.462526 0.173001 0.996797 0.038 Uiso calc 1 C C12 0.46372(17) 0.1858(4) 0.90902(12) 0.0278(6) Uani d 1 C C13 0.41242(16) 0.1874(4) 0.85515(12) 0.0242(6) Uani d 1 H H13 0.434787 0.195000 0.819967 0.029 Uiso calc 1 C C14 0.55430(17) 0.1992(5) 0.91222(14) 0.0367(7) Uani d 1 H H14A 0.580797 0.101170 0.939574 0.044 Uiso calc 1 H H14B 0.572862 0.328325 0.926028 0.044 Uiso calc 1 H H14C 0.568130 0.176676 0.873133 0.044 Uiso calc 1 C C15 0.01183(16) 0.2188(4) 1.03431(11) 0.0231(6) Uani d 1 C C16 0.09673(16) 0.1904(4) 1.03296(11) 0.0226(5) Uani d 1 C C17 0.14371(16) 0.1393(4) 1.08883(12) 0.0240(6) Uani d 1 C C18 0.11088(17) 0.1191(4) 1.13890(12) 0.0252(6) Uani d 1 H H18 0.144597 0.085854 1.174796 0.030 Uiso calc 1 C C19 0.02747(16) 0.1473(4) 1.13744(11) 0.0235(6) Uani d 1 C C20 -0.02172(16) 0.1947(4) 1.08629(12) 0.0245(6) Uani d 1 H H20 -0.078274 0.211589 1.085518 0.029 Uiso calc 1 C C21 -0.04189(16) 0.2698(4) 0.98261(11) 0.0244(6) Uani d 1 H H21 -0.097709 0.284149 0.985166 0.029 Uiso calc 1 C C22 -0.07113(16) 0.3483(4) 0.87846(11) 0.0222(5) Uani d 1 C C23 -0.03394(16) 0.3733(4) 0.82909(12) 0.0254(6) Uani d 1 C C24 -0.08220(18) 0.4147(4) 0.77557(12) 0.0300(6) Uani d 1 H H24 -0.058047 0.430591 0.741398 0.036 Uiso calc 1 C C25 -0.16540(17) 0.4330(4) 0.77181(12) 0.0301(6) Uani d 1 H H25 -0.197437 0.461047 0.734813 0.036 Uiso calc 1 C C26 -0.20333(17) 0.4115(4) 0.82072(12) 0.0266(6) Uani d 1 C C27 -0.15469(16) 0.3695(4) 0.87419(12) 0.0240(6) Uani d 1 H H27 -0.178942 0.354950 0.908375 0.029 Uiso calc 1 C C28 -0.29388(17) 0.4308(5) 0.81661(14) 0.0361(7) Uani d 1 H H28A -0.307472 0.441898 0.856187 0.043 Uiso calc 1 H H28B -0.320532 0.316250 0.797111 0.043 Uiso calc 1 H H28C -0.312521 0.546832 0.793864 0.043 Uiso calc 1 H H1 0.227(2) 0.199(5) 0.8001(14) 0.036(10) Uiso d 1 H H2 0.193(2) 0.164(6) 0.9303(18) 0.061(12) Uiso d 1 H H2A 0.028(2) 0.284(5) 0.9301(14) 0.031(9) Uiso d 1 H H4 0.063(2) 0.328(5) 0.8042(15) 0.041(10) Uiso d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.01857(15) 0.0492(2) 0.03065(17) -0.00132(12) 0.00568(11) -0.00265(13) Br2 0.02797(17) 0.0714(3) 0.02070(16) 0.00151(15) 0.00913(12) 0.00201(14) Br3 0.02106(16) 0.0624(2) 0.02539(16) 0.00287(13) 0.00467(12) 0.00489(14) Br4 0.03446(18) 0.03847(19) 0.02417(16) 0.00327(12) 0.01380(12) 0.00366(12) O1 0.0220(10) 0.0471(12) 0.0215(9) 0.0004(9) 0.0077(7) 0.0000(9) O2 0.0206(10) 0.0570(14) 0.0280(11) 0.0031(9) 0.0080(8) 0.0017(10) O3 0.0234(10) 0.0457(12) 0.0202(9) -0.0010(9) 0.0065(7) 0.0025(9) O4 0.0231(10) 0.0467(13) 0.0291(11) 0.0026(9) 0.0088(8) -0.0018(10) N1 0.0182(12) 0.0292(13) 0.0215(12) 0.0002(10) 0.0025(9) 0.0019(9) N2 0.0183(12) 0.0266(12) 0.0242(12) 0.0004(9) 0.0028(9) -0.0009(9) C1 0.0227(13) 0.0235(14) 0.0229(13) -0.0005(11) 0.0050(10) 0.0025(11) C2 0.0230(13) 0.0230(14) 0.0237(13) -0.0021(11) 0.0061(10) 0.0025(11) C3 0.0180(13) 0.0256(14) 0.0261(14) -0.0005(10) 0.0045(10) 0.0018(11) C4 0.0253(14) 0.0293(14) 0.0219(13) 0.0004(11) 0.0014(10) 0.0016(11) C5 0.0259(14) 0.0332(15) 0.0171(12) -0.0004(12) 0.0074(10) 0.0026(11) C6 0.0199(13) 0.0302(14) 0.0254(14) 0.0002(11) 0.0065(10) 0.0036(12) C7 0.0216(13) 0.0254(14) 0.0258(14) -0.0004(11) 0.0046(10) 0.0010(11) C8 0.0220(13) 0.0255(14) 0.0214(13) -0.0001(11) 0.0028(10) 0.0024(11) C9 0.0234(14) 0.0295(14) 0.0246(14) 0.0020(11) 0.0069(11) 0.0023(11) C10 0.0314(16) 0.0433(18) 0.0221(14) 0.0035(13) 0.0058(11) 0.0041(13) C11 0.0287(15) 0.0405(17) 0.0231(14) -0.0002(13) -0.0027(11) 0.0032(12) C12 0.0240(14) 0.0293(15) 0.0287(14) -0.0006(11) 0.0004(11) 0.0017(12) C13 0.0223(14) 0.0288(14) 0.0218(13) -0.0005(11) 0.0046(10) 0.0032(11) C14 0.0236(15) 0.0484(19) 0.0360(16) -0.0030(13) -0.0013(12) 0.0063(14) C15 0.0242(13) 0.0219(13) 0.0236(13) 0.0002(11) 0.0055(10) -0.0019(11) C16 0.0244(13) 0.0223(13) 0.0217(13) -0.0034(11) 0.0058(10) -0.0016(11) C17 0.0206(13) 0.0276(14) 0.0237(13) -0.0021(11) 0.0034(10) 0.0002(11) C18 0.0274(14) 0.0286(15) 0.0192(13) -0.0005(11) 0.0033(10) -0.0012(11) C19 0.0275(14) 0.0250(14) 0.0192(13) 0.0000(11) 0.0075(10) -0.0015(11) C20 0.0218(13) 0.0267(14) 0.0265(14) 0.0018(11) 0.0082(11) -0.0015(11) C21 0.0233(13) 0.0261(14) 0.0242(13) 0.0015(11) 0.0051(10) -0.0013(11) C22 0.0237(13) 0.0214(13) 0.0211(13) 0.0011(11) 0.0025(10) -0.0015(10) C23 0.0238(14) 0.0263(14) 0.0267(14) 0.0000(11) 0.0056(11) -0.0045(11) C24 0.0344(16) 0.0351(16) 0.0217(14) -0.0008(13) 0.0078(11) -0.0031(12) C25 0.0313(15) 0.0322(16) 0.0244(14) 0.0010(12) -0.0027(11) -0.0012(12) C26 0.0251(14) 0.0272(15) 0.0268(14) -0.0001(11) 0.0024(11) -0.0020(11) C27 0.0239(14) 0.0246(14) 0.0241(13) 0.0010(11) 0.0056(10) 0.0003(11) C28 0.0255(15) 0.0438(18) 0.0375(17) 0.0030(13) 0.0010(12) 0.0009(14) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; Br Br -0.6763 1.2805 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0492 0.0322 ; International Tables for Crystallography (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 C9 O2 H2 114(3) C23 O4 H4 110(2) C7 N1 C8 127.3(2) C7 N1 H1 115(2) C8 N1 H1 117(2) C21 N2 C22 126.6(2) C21 N2 H2A 117(2) C22 N2 H2A 117(2) C7 C1 C6 117.8(2) C7 C1 C2 120.4(2) C6 C1 C2 121.9(2) O1 C2 C3 123.6(2) O1 C2 C1 122.0(2) C3 C2 C1 114.4(2) C4 C3 C2 123.0(2) C4 C3 Br1 119.4(2) C2 C3 Br1 117.62(19) C3 C4 C5 119.7(2) C3 C4 H4A 120.2 C5 C4 H4A 120.2 C6 C5 C4 121.3(2) C6 C5 Br2 120.2(2) C4 C5 Br2 118.44(19) C5 C6 C1 119.5(2) C5 C6 H6 120.2 C1 C6 H6 120.2 N1 C7 C1 123.7(3) N1 C7 H7 118.2 C1 C7 H7 118.2 C9 C8 C13 120.8(2) C9 C8 N1 116.4(2) C13 C8 N1 122.8(2) O2 C9 C8 117.4(2) O2 C9 C10 124.2(2) C8 C9 C10 118.4(3) C11 C10 C9 120.4(3) C11 C10 H10 119.8 C9 C10 H10 119.8 C10 C11 C12 121.8(3) C10 C11 H11 119.1 C12 C11 H11 119.1 C13 C12 C11 117.8(3) C13 C12 C14 120.7(3) C11 C12 C14 121.5(3) C12 C13 C8 120.9(2) C12 C13 H13 119.6 C8 C13 H13 119.6 C12 C14 H14A 109.5 C12 C14 H14B 109.5 H14A C14 H14B 109.5 C12 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C21 C15 C20 117.3(2) C21 C15 C16 120.5(2) C20 C15 C16 122.2(2) O3 C16 C15 122.1(2) O3 C16 C17 123.8(2) C15 C16 C17 114.1(2) C18 C17 C16 123.2(2) C18 C17 Br3 118.5(2) C16 C17 Br3 118.35(19) C17 C18 C19 120.1(2) C17 C18 H18 119.9 C19 C18 H18 119.9 C20 C19 C18 120.6(2) C20 C19 Br4 121.2(2) C18 C19 Br4 118.12(19) C19 C20 C15 119.7(3) C19 C20 H20 120.2 C15 C20 H20 120.2 N2 C21 C15 124.3(3) N2 C21 H21 117.9 C15 C21 H21 117.9 C27 C22 C23 120.4(2) C27 C22 N2 122.9(2) C23 C22 N2 116.7(2) O4 C23 C24 123.9(3) O4 C23 C22 117.4(2) C24 C23 C22 118.6(3) C25 C24 C23 120.3(3) C25 C24 H24 119.8 C23 C24 H24 119.8 C24 C25 C26 121.8(3) C24 C25 H25 119.1 C26 C25 H25 119.1 C25 C26 C27 117.6(3) C25 C26 C28 121.8(2) C27 C26 C28 120.5(3) C26 C27 C22 121.1(3) C26 C27 H27 119.4 C22 C27 H27 119.4 C26 C28 H28A 109.5 C26 C28 H28B 109.5 H28A C28 H28B 109.5 C26 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C3 1.890(3) Br2 C5 1.900(3) Br3 C17 1.890(3) Br4 C19 1.897(3) O1 C2 1.273(3) O2 C9 1.354(3) O2 H2 0.90(4) O3 C16 1.273(3) O4 C23 1.358(3) O4 H4 0.86(3) N1 C7 1.304(3) N1 C8 1.410(3) N1 H1 0.80(3) N2 C21 1.305(3) N2 C22 1.419(3) N2 H2A 0.81(3) C1 C7 1.411(4) C1 C6 1.414(4) C1 C2 1.442(4) C2 C3 1.439(4) C3 C4 1.364(4) C4 C5 1.404(4) C4 H4A 0.9500 C5 C6 1.357(4) C6 H6 0.9500 C7 H7 0.9500 C8 C9 1.392(4) C8 C13 1.393(4) C9 C10 1.393(4) C10 C11 1.379(4) C10 H10 0.9500 C11 C12 1.392(4) C11 H11 0.9500 C12 C13 1.389(4) C12 C14 1.507(4) C13 H13 0.9500 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 C21 1.415(4) C15 C20 1.416(4) C15 C16 1.438(4) C16 C17 1.439(4) C17 C18 1.366(4) C18 C19 1.403(4) C18 H18 0.9500 C19 C20 1.363(4) C20 H20 0.9500 C21 H21 0.9500 C22 C27 1.392(4) C22 C23 1.396(4) C23 C24 1.389(4) C24 C25 1.385(4) C24 H24 0.9500 C25 C26 1.391(4) C25 H25 0.9500 C26 C27 1.392(4) C26 C28 1.507(4) C27 H27 0.9500 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O2 H2 O3 0.90(4) 1.86(4) 2.728(3) 163(4) yes O4 H4 O1 0.86(4) 1.92(4) 2.753(3) 164(3) yes N1 H1 O1 0.80(4) 1.97(3) 2.616(3) 139(3) yes N2 H2A O3 0.81(3) 1.99(3) 2.632(3) 136(3) 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 C7 C1 C2 O1 4.8(4) C6 C1 C2 O1 -176.5(3) C7 C1 C2 C3 -173.9(3) C6 C1 C2 C3 4.8(4) O1 C2 C3 C4 176.5(3) C1 C2 C3 C4 -4.8(4) O1 C2 C3 Br1 -5.1(4) C1 C2 C3 Br1 173.57(19) C2 C3 C4 C5 1.3(4) Br1 C3 C4 C5 -177.1(2) C3 C4 C5 C6 2.8(4) C3 C4 C5 Br2 -179.3(2) C4 C5 C6 C1 -2.8(4) Br2 C5 C6 C1 179.3(2) C7 C1 C6 C5 177.5(3) C2 C1 C6 C5 -1.2(4) C8 N1 C7 C1 -179.5(3) C6 C1 C7 N1 -178.2(3) C2 C1 C7 N1 0.5(4) C7 N1 C8 C9 -169.9(3) C7 N1 C8 C13 11.6(4) C13 C8 C9 O2 179.5(3) N1 C8 C9 O2 1.0(4) C13 C8 C9 C10 -0.1(4) N1 C8 C9 C10 -178.6(3) O2 C9 C10 C11 -179.4(3) C8 C9 C10 C11 0.2(5) C9 C10 C11 C12 -0.2(5) C10 C11 C12 C13 0.0(5) C10 C11 C12 C14 179.2(3) C11 C12 C13 C8 0.1(4) C14 C12 C13 C8 -179.1(3) C9 C8 C13 C12 0.0(4) N1 C8 C13 C12 178.4(3) C21 C15 C16 O3 0.3(4) C20 C15 C16 O3 179.4(3) C21 C15 C16 C17 179.9(2) C20 C15 C16 C17 -1.0(4) O3 C16 C17 C18 179.7(3) C15 C16 C17 C18 0.1(4) O3 C16 C17 Br3 -0.8(4) C15 C16 C17 Br3 179.56(19) C16 C17 C18 C19 0.4(4) Br3 C17 C18 C19 -179.1(2) C17 C18 C19 C20 0.1(4) C17 C18 C19 Br4 178.4(2) C18 C19 C20 C15 -1.0(4) Br4 C19 C20 C15 -179.2(2) C21 C15 C20 C19 -179.4(3) C16 C15 C20 C19 1.5(4) C22 N2 C21 C15 179.5(3) C20 C15 C21 N2 179.4(3) C16 C15 C21 N2 -1.5(4) C21 N2 C22 C27 -1.3(4) C21 N2 C22 C23 179.6(3) C27 C22 C23 O4 177.6(2) N2 C22 C23 O4 -3.3(4) C27 C22 C23 C24 -1.6(4) N2 C22 C23 C24 177.5(2) O4 C23 C24 C25 -178.3(3) C22 C23 C24 C25 0.8(4) C23 C24 C25 C26 0.2(5) C24 C25 C26 C27 -0.3(4) C24 C25 C26 C28 -179.8(3) C25 C26 C27 C22 -0.5(4) C28 C26 C27 C22 179.0(3) C23 C22 C27 C26 1.4(4) N2 C22 C27 C26 -177.6(3) _cod_database_fobs_code 1549065