#------------------------------------------------------------------------------ #$Date: 2026-09-03 22:13:03 +0100 (Thu, 03 Sep 2026) $ #$Revision: 306853 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023552.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_2023552 loop_ _publ_author_name 'Akerele, Oluwatoyin' 'Lemmerer, Andreas' _publ_section_title ; Crystal structure and Hirshfeld surface of 5-bromosalicylic acid dimethylformamide monosolvate ; _journal_coeditor_code JP2033 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989026008984 _journal_volume 82 _journal_year 2026 _chemical_formula_iupac 'C7 H5 Br O3, C3 H7 N O' _chemical_formula_moiety 'C7 H5 Br O3, C3 H7 N O' _chemical_formula_sum 'C10 H12 Br N O4' _chemical_formula_weight 290.12 _chemical_name_common ; 5-Bromosalicylic acid dimethylformamide monosolvate ; _chemical_name_systematic ; 5-Bromo-2-hydroxybenzoic acid dimethylformamide monosolvate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2026.04.10 svn.r48fbca5a for OlexSys, GUI svn.r7537) ; _cell_angle_alpha 95.9230(10) _cell_angle_beta 99.795(2) _cell_angle_gamma 100.4610(10) _cell_formula_units_Z 4 _cell_length_a 8.5524(3) _cell_length_b 9.5175(3) _cell_length_c 14.9678(5) _cell_measurement_reflns_used 9989 _cell_measurement_temperature 173.00 _cell_measurement_theta_max 28.30 _cell_measurement_theta_min 2.47 _cell_volume 1169.27(7) _computing_cell_refinement ; SAINT V8.42 (Bruker, 2016) ; _computing_data_collection ; APEX4 (Bruker, 2021) ; _computing_data_reduction ; SAINT V8.42 (Bruker, 2016) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_structure_refinement 'SHELXL (Sheldrick, 2015b)' _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 173.00 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_unetI/netI 0.0302 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 40930 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.299 _diffrn_reflns_theta_min 2.197 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.514 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.648 _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.512 _exptl_crystal_size_mid 0.227 _exptl_crystal_size_min 0.142 _refine_diff_density_max 0.331 _refine_diff_density_min -0.457 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 297 _refine_ls_number_reflns 5813 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0237 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.2966P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.0617 _reflns_number_gt 5097 _reflns_number_total 5813 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jp2033.cif _cod_data_source_block I _cod_original_sg_symbol_H-M P-1 _cod_database_code 2023552 _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 ; -1 0 0 144.09 7.80 -1 0 0 146.49 14.60 -1 0 0 140.09 8.20 1 0 0 147.89 7.90 1 0 0 139.29 14.20 1 0 0 127.19 12.80 1 0 0 140.59 8.30 -2 0 0 265.87 28.10 -2 0 0 360.06 28.70 -2 0 0 317.77 16.40 -2 0 0 276.07 16.70 2 0 0 291.47 16.30 2 0 0 288.27 29.60 2 0 0 309.97 27.80 2 0 0 288.57 17.10 -3 0 0 145.89 29.40 -3 0 0 119.39 10.20 -3 0 0 125.09 9.60 3 0 0 114.29 26.50 3 0 0 104.29 20.30 3 0 0 122.29 9.90 3 0 0 121.79 10.70 -4 0 0 28.00 1.40 -4 0 0 25.50 1.30 4 0 0 24.90 1.30 4 0 0 26.60 1.40 4 0 0 26.90 1.40 4 0 0 25.00 1.40 -5 0 0 91.69 4.20 -5 0 0 87.59 4.10 -5 0 0 95.39 4.20 5 0 0 86.29 4.20 5 0 0 92.39 4.20 5 0 0 90.19 4.20 5 0 0 82.09 4.20 -6 0 0 6.90 0.70 -6 0 0 7.70 0.80 -6 0 0 6.30 0.60 -6 0 0 6.60 0.70 6 0 0 6.60 0.70 6 0 0 6.20 0.70 6 0 0 5.70 0.70 6 0 0 8.00 0.80 -7 0 0 18.10 1.20 -7 0 0 18.70 1.30 -7 0 0 20.20 1.30 7 0 0 15.90 1.30 7 0 0 19.60 1.30 7 0 0 19.10 1.20 -8 0 0 67.89 3.20 -8 0 0 56.49 3.10 -8 0 0 62.49 3.20 -8 0 0 58.29 3.00 8 0 0 60.89 3.20 8 0 0 59.59 3.30 8 0 0 64.89 3.20 8 0 0 58.99 3.10 -9 0 0 23.00 1.70 -9 0 0 25.60 1.80 -9 0 0 22.70 1.60 -9 0 0 20.60 1.40 9 0 0 24.90 1.80 9 0 0 22.90 1.80 9 0 0 23.40 1.60 9 0 0 23.80 1.80 -10 0 0 0.30 0.50 -10 0 0 0.10 0.70 -10 0 0 0.90 1.00 -10 0 0 0.00 0.50 10 0 0 0.70 0.60 10 0 0 1.20 0.80 10 0 0 0.20 0.80 10 0 0 -0.40 0.80 -11 0 0 -1.10 0.50 11 -1 0 0.60 0.50 11 -1 0 -0.20 0.90 11 -1 0 1.30 0.70 -11 1 0 -0.10 0.80 -11 1 0 0.30 0.70 -11 1 0 -0.10 0.50 10 -1 0 9.50 1.40 10 -1 0 7.10 1.10 10 -1 0 10.10 1.30 10 -1 0 10.50 1.20 -10 1 0 8.80 1.10 -10 1 0 10.50 1.00 -10 1 0 9.50 1.40 -10 1 0 8.60 1.10 9 -1 0 3.10 0.60 9 -1 0 3.60 0.80 9 -1 0 4.70 0.80 9 -1 0 2.50 0.70 -9 1 0 3.50 0.70 -9 1 0 4.00 0.80 -9 1 0 2.90 0.50 -9 1 0 3.40 0.60 8 -1 0 1.90 0.70 8 -1 0 2.20 0.60 8 -1 0 1.30 0.60 8 -1 0 2.50 0.60 -8 1 0 3.10 0.60 -8 1 0 2.20 0.50 -8 1 0 1.70 0.60 -8 1 0 1.30 0.60 7 -1 0 40.50 2.20 7 -1 0 37.80 2.10 7 -1 0 39.40 2.20 7 -1 0 37.30 2.20 -7 1 0 37.50 2.10 -7 1 0 41.10 2.10 -7 1 0 40.30 2.10 6 -1 0 4.50 0.50 6 -1 0 4.60 0.60 6 -1 0 4.20 0.50 6 -1 0 4.20 0.60 -6 1 0 2.70 0.50 -6 1 0 3.10 0.40 -6 1 0 6.20 0.60 5 -1 0 27.40 1.60 5 -1 0 29.40 1.60 -5 1 0 29.40 1.50 -5 1 0 29.70 1.60 4 -1 0 485.85 48.30 4 -1 0 481.95 52.59 4 -1 0 463.85 27.00 4 -1 0 454.15 28.50 -4 1 0 492.35 28.80 -4 1 0 467.75 50.89 3 -1 0 5.20 0.40 3 -1 0 4.80 0.40 3 -1 0 5.30 0.40 3 -1 0 4.40 0.40 -3 1 0 4.60 0.30 -3 1 0 4.70 0.40 -3 1 0 5.00 0.40 -3 1 0 4.60 0.40 2 -1 0 43.30 2.00 1 -1 0 29.80 1.30 1 -1 0 30.90 1.40 -1 1 0 30.20 1.40 -1 1 0 28.10 1.30 0 -1 0 0.50 0.10 0 1 0 0.40 0.10 0 1 0 0.50 0.10 -1 -1 0 0.50 0.10 -1 -1 0 0.50 0.10 -1 -1 0 0.50 0.10 -1 -1 0 0.30 0.10 1 1 0 0.40 0.10 1 1 0 0.50 0.10 1 1 0 0.40 0.10 1 1 0 0.40 0.10 -2 -1 0 774.92 51.09 -2 -1 0 803.82 54.69 -2 -1 0 754.02 36.40 2 1 0 737.33 37.60 2 1 0 641.14 52.59 2 1 0 743.03 36.80 2 1 0 743.83 52.39 -3 -1 0 18.80 1.00 -3 -1 0 18.20 1.00 3 1 0 17.60 1.00 3 1 0 18.90 1.00 3 1 0 18.50 1.00 3 1 0 19.40 1.00 -4 -1 0 587.14 31.30 -4 -1 0 560.04 57.09 -4 -1 0 472.15 50.59 4 1 0 537.25 33.20 4 1 0 617.94 105.49 4 1 0 579.74 76.19 4 1 0 544.05 40.10 -5 -1 0 105.19 4.70 -5 -1 0 98.89 4.90 -5 -1 0 95.59 4.60 -5 -1 0 105.49 4.70 5 1 0 103.79 4.70 5 1 0 96.49 4.70 5 1 0 99.09 4.70 5 1 0 97.79 4.60 -6 -1 0 28.90 1.60 -6 -1 0 27.90 1.60 -6 -1 0 29.60 1.60 -6 -1 0 26.80 1.50 6 1 0 28.70 1.60 6 1 0 27.40 1.60 6 1 0 28.80 1.70 6 1 0 26.70 1.60 -7 -1 0 122.49 5.40 -7 -1 0 112.99 5.40 -7 -1 0 103.09 5.30 7 1 0 110.69 5.50 7 1 0 118.99 5.70 7 1 0 120.39 5.40 7 1 0 110.09 5.40 -8 -1 0 1.10 0.60 -8 -1 0 0.50 0.50 -8 -1 0 0.00 0.40 -8 -1 0 0.10 0.50 8 1 0 0.50 0.60 8 1 0 1.00 0.50 8 1 0 0.50 0.60 8 1 0 0.50 0.60 -9 -1 0 0.00 0.60 -9 -1 0 1.00 0.60 -9 -1 0 0.50 0.70 -9 -1 0 0.80 0.50 9 1 0 0.50 0.60 9 1 0 0.70 0.50 9 1 0 0.20 0.70 9 1 0 1.20 0.80 -10 -1 0 0.90 0.70 -10 -1 0 -0.10 0.50 -10 -1 0 1.30 0.80 10 1 0 0.90 0.60 10 1 0 1.30 0.80 10 1 0 0.50 0.70 11 -2 0 5.20 0.90 11 -2 0 3.40 1.00 11 -2 0 3.60 0.90 11 -2 0 4.20 1.00 -11 2 0 3.00 0.60 -11 2 0 2.70 0.80 -11 2 0 4.10 1.00 -11 2 0 3.50 0.70 10 -2 0 0.80 0.80 10 -2 0 0.60 0.80 10 -2 0 0.90 0.50 10 -2 0 0.80 0.70 -10 2 0 0.40 0.60 -10 2 0 0.10 0.50 -10 2 0 0.00 0.50 -10 2 0 0.00 0.70 9 -2 0 3.40 0.80 9 -2 0 3.30 0.80 9 -2 0 3.40 0.70 9 -2 0 5.20 0.80 -9 2 0 3.70 0.70 -9 2 0 4.20 0.60 -9 2 0 3.50 0.70 -9 2 0 4.00 0.80 8 -2 0 14.60 1.10 8 -2 0 14.60 1.30 8 -2 0 16.10 1.30 -8 2 0 14.90 1.10 -8 2 0 16.20 1.30 -8 2 0 16.70 1.30 7 -2 0 0.30 0.50 7 -2 0 -0.10 0.40 7 -2 0 -0.20 0.40 -7 2 0 0.70 0.40 -7 2 0 0.20 0.40 -7 2 0 -0.60 0.40 6 -2 0 236.18 10.70 5 -2 0 73.39 3.50 5 -2 0 70.99 3.40 5 -2 0 77.29 3.50 5 -2 0 71.59 3.50 -5 2 0 74.89 3.50 -5 2 0 73.69 3.40 -5 2 0 70.59 3.40 -5 2 0 76.49 3.50 4 -2 0 0.20 0.20 4 -2 0 0.10 0.20 4 -2 0 0.10 0.20 4 -2 0 -0.20 0.20 -4 2 0 0.00 0.20 -4 2 0 0.10 0.20 -4 2 0 0.00 0.20 -4 2 0 0.30 0.20 3 -2 0 197.38 14.10 3 -2 0 167.38 28.90 -3 2 0 208.18 23.60 -3 2 0 224.58 12.90 2 -2 0 223.28 12.50 2 -2 0 205.78 22.90 2 -2 0 223.48 21.00 2 -2 0 228.58 13.50 -2 2 0 201.78 18.90 -2 2 0 237.48 13.40 -2 2 0 236.28 23.70 -2 2 0 248.58 12.40 1 -2 0 40.00 1.90 1 -2 0 38.20 1.80 -1 2 0 35.50 1.70 -1 2 0 39.50 1.90 -1 2 0 38.20 1.80 -1 2 0 35.60 1.70 0 -2 0 0.00 0.10 -1 -2 0 2.50 0.20 -1 -2 0 2.50 0.20 -1 -2 0 2.40 0.20 -1 -2 0 2.70 0.20 1 2 0 2.50 0.20 1 2 0 2.20 0.20 1 2 0 2.90 0.20 1 2 0 2.80 0.20 -2 -2 0 230.58 13.60 -2 -2 0 181.28 28.00 2 2 0 205.78 13.90 2 2 0 262.07 38.00 2 2 0 214.68 14.30 2 2 0 196.48 30.70 -3 -2 0 525.55 48.10 -3 -2 0 555.14 30.80 -3 -2 0 562.94 29.80 -3 -2 0 579.14 53.59 3 2 0 507.85 31.10 3 2 0 527.05 51.99 3 2 0 562.34 30.90 3 2 0 613.64 57.19 -4 -2 0 8.80 0.70 -4 -2 0 7.90 0.60 -4 -2 0 8.50 0.60 -4 -2 0 8.40 0.60 4 2 0 9.40 0.70 4 2 0 8.40 0.70 4 2 0 8.30 0.70 4 2 0 8.10 0.60 -5 -2 0 9.10 0.80 -5 -2 0 8.10 0.70 -5 -2 0 7.30 0.70 -5 -2 0 8.90 0.70 5 2 0 7.70 0.70 5 2 0 9.20 0.80 5 2 0 8.80 0.80 5 2 0 10.70 1.00 -6 -2 0 17.70 1.20 -6 -2 0 19.80 1.20 -6 -2 0 19.80 1.30 -6 -2 0 17.40 1.10 6 2 0 20.00 1.30 6 2 0 18.10 1.20 6 2 0 16.60 1.20 -7 -2 0 0.10 0.50 -7 -2 0 0.00 0.40 -7 -2 0 0.80 0.50 7 2 0 0.40 0.50 7 2 0 0.50 0.50 7 2 0 0.00 0.50 7 2 0 0.10 0.40 -8 -2 0 16.00 1.20 -8 -2 0 14.90 1.10 -8 -2 0 14.80 1.30 -8 -2 0 14.60 1.30 8 2 0 16.00 1.40 8 2 0 14.70 1.40 8 2 0 13.40 1.30 8 2 0 15.80 1.30 -9 -2 0 -0.40 0.50 -9 -2 0 0.60 0.70 -9 -2 0 0.50 0.40 -9 -2 0 0.20 0.60 9 2 0 0.80 0.60 9 2 0 0.90 0.60 9 2 0 0.30 0.70 9 2 0 1.30 0.80 -10 -2 0 1.60 0.50 -10 -2 0 1.50 0.60 -10 -2 0 1.70 0.80 -10 -2 0 2.70 0.90 10 2 0 1.50 0.70 10 2 0 1.10 0.60 10 2 0 2.00 0.90 11 -3 0 -0.60 0.80 11 -3 0 1.00 1.50 11 -3 0 2.00 0.80 11 -3 0 1.10 0.60 11 -3 0 0.30 0.90 -11 3 0 1.10 0.80 -11 3 0 0.80 0.80 -11 3 0 -0.50 0.60 -11 3 0 0.60 0.50 10 -3 0 1.60 1.40 10 -3 0 1.60 0.80 10 -3 0 1.40 0.60 10 -3 0 0.90 0.70 10 -3 0 2.00 0.70 -10 3 0 2.50 0.70 -10 3 0 2.50 0.80 -10 3 0 1.00 0.40 -10 3 0 2.80 0.70 9 -3 0 11.90 1.10 9 -3 0 11.10 1.10 9 -3 0 13.60 2.10 9 -3 0 16.40 1.40 9 -3 0 14.20 1.40 -9 3 0 11.00 1.00 -9 3 0 13.20 1.10 -9 3 0 13.20 1.20 -9 3 0 11.00 1.10 8 -3 0 0.90 0.50 8 -3 0 0.10 0.10 8 -3 0 1.50 0.60 8 -3 0 0.40 0.60 -8 3 0 -0.20 0.40 -8 3 0 0.30 0.60 -8 3 0 0.60 0.50 7 -3 0 83.29 4.80 7 -3 0 86.39 4.10 7 -3 0 83.49 4.10 7 -3 0 80.59 4.10 -7 3 0 91.59 4.10 -7 3 0 85.29 4.10 -7 3 0 82.69 4.00 -7 3 0 80.89 4.00 6 -3 0 125.39 5.80 6 -3 0 130.89 5.80 6 -3 0 120.99 6.30 6 -3 0 126.59 5.80 6 -3 0 118.49 5.70 -6 3 0 127.99 5.80 -6 3 0 121.59 5.70 -6 3 0 125.89 5.70 -6 3 0 126.19 5.80 5 -3 0 0.60 0.30 5 -3 0 0.50 0.30 5 -3 0 0.90 0.60 5 -3 0 0.80 0.30 5 -3 0 1.10 0.30 -5 3 0 0.50 0.30 -5 3 0 1.20 0.30 -5 3 0 0.60 0.30 -5 3 0 0.80 0.30 4 -3 0 58.79 2.80 4 -3 0 61.69 2.80 4 -3 0 58.19 2.70 4 -3 0 58.99 2.80 -4 3 0 55.69 2.70 -4 3 0 59.09 2.70 -4 3 0 61.49 2.80 -4 3 0 58.49 2.80 3 -3 0 1.80 0.20 3 -3 0 2.00 0.30 3 -3 0 1.40 0.40 3 -3 0 1.60 0.20 3 -3 0 1.10 0.20 -3 3 0 2.00 0.20 -3 3 0 1.80 0.40 -3 3 0 1.90 0.20 -3 3 0 1.40 0.20 -3 3 0 1.90 0.20 2 -3 0 464.35 24.10 2 -3 0 451.65 35.20 -2 3 0 463.25 30.10 -2 3 0 442.76 22.70 -2 3 0 514.25 40.60 -2 3 0 536.35 25.80 1 -3 0 483.95 24.10 1 -3 0 454.85 26.70 1 -3 0 454.35 20.50 1 -3 0 443.46 21.00 -1 3 0 417.86 24.10 -1 3 0 458.05 27.10 -1 3 0 437.86 20.60 0 -3 0 0.30 0.20 0 -3 0 0.20 0.10 0 -3 0 0.00 0.30 0 3 0 0.30 0.10 0 3 0 0.20 0.10 0 3 0 0.40 0.20 0 3 0 0.30 0.10 0 3 0 0.40 0.30 0 3 0 0.20 0.10 -1 -3 0 450.35 34.00 -1 -3 0 444.26 22.90 -1 -3 0 467.35 34.80 -1 -3 0 461.25 22.80 1 3 0 420.06 35.90 1 3 0 337.77 57.69 1 3 0 446.36 23.30 -2 -3 0 75.09 3.50 2 3 0 77.79 3.50 2 3 0 74.59 3.50 -3 -3 0 1.00 0.30 -3 -3 0 1.00 0.20 -3 -3 0 1.10 0.20 -3 -3 0 1.20 0.20 3 3 0 1.40 0.30 3 3 0 0.60 0.20 3 3 0 1.30 0.30 -4 -3 0 2.40 0.40 -4 -3 0 1.30 0.30 -4 -3 0 1.30 0.30 -4 -3 0 1.30 0.30 4 3 0 1.40 0.30 4 3 0 1.30 0.30 4 3 0 2.30 0.40 4 3 0 1.80 0.40 -5 -3 0 14.50 1.00 -5 -3 0 12.40 0.90 -5 -3 0 12.50 0.90 5 3 0 12.40 1.10 5 3 0 15.30 1.00 5 3 0 13.60 1.00 5 3 0 14.40 1.00 -6 -3 0 54.69 2.80 -6 -3 0 57.09 2.80 -6 -3 0 59.69 2.90 6 3 0 53.89 2.90 6 3 0 55.89 2.90 6 3 0 58.39 2.90 -7 -3 0 59.09 3.10 -7 -3 0 62.89 3.20 -7 -3 0 60.09 3.10 7 3 0 63.39 3.20 7 3 0 63.69 3.20 7 3 0 61.49 3.30 7 3 0 62.69 3.20 -8 -3 0 0.90 0.50 -8 -3 0 1.00 0.60 -8 -3 0 1.10 0.60 -8 -3 0 1.70 0.50 8 3 0 2.00 0.70 8 3 0 1.90 0.60 8 3 0 1.00 0.60 8 3 0 2.10 0.80 -9 -3 0 5.70 0.80 -9 -3 0 6.80 0.80 -9 -3 0 6.90 1.00 -9 -3 0 6.60 0.90 9 3 0 6.90 1.00 9 3 0 6.00 1.00 9 3 0 7.90 1.20 9 3 0 6.00 1.10 -10 -3 0 10.90 1.20 -10 -3 0 10.00 1.00 -10 -3 0 13.80 1.50 -10 -3 0 11.90 1.20 10 3 0 12.80 1.50 10 3 0 13.40 1.50 10 3 0 10.50 1.20 10 3 0 13.50 1.40 11 -4 0 12.30 1.50 11 -4 0 7.50 1.30 11 -4 0 6.00 2.20 11 -4 0 9.10 1.20 -11 4 0 7.70 1.10 -11 4 0 5.40 0.80 10 -4 0 5.40 1.00 10 -4 0 5.70 0.80 10 -4 0 2.90 1.70 10 -4 0 5.00 1.00 -10 4 0 4.70 0.80 -10 4 0 6.60 0.80 -10 4 0 6.80 1.20 -10 4 0 5.60 1.00 9 -4 0 0.80 0.60 9 -4 0 0.60 1.30 9 -4 0 1.00 0.70 9 -4 0 0.30 0.60 -9 4 0 1.00 0.60 -9 4 0 1.90 0.70 -9 4 0 1.50 0.60 -9 4 0 1.40 0.50 8 -4 0 44.00 2.40 8 -4 0 46.40 2.40 8 -4 0 37.90 2.30 8 -4 0 45.90 2.40 8 -4 0 42.20 3.20 -8 4 0 44.00 2.40 -8 4 0 42.10 2.30 -8 4 0 45.30 2.40 -8 4 0 40.70 2.20 7 -4 0 1.10 0.50 7 -4 0 0.70 0.50 7 -4 0 0.30 0.50 7 -4 0 0.10 0.20 7 -4 0 0.30 0.90 -7 4 0 0.60 0.80 -7 4 0 0.80 0.40 -7 4 0 0.20 0.30 -7 4 0 0.10 0.30 6 -4 0 0.20 0.30 6 -4 0 -0.40 0.60 6 -4 0 -0.10 0.30 6 -4 0 0.50 0.40 6 -4 0 -0.10 0.30 -6 4 0 0.10 0.30 -6 4 0 0.40 0.30 -6 4 0 0.60 0.30 -6 4 0 0.40 0.30 5 -4 0 44.50 2.10 5 -4 0 43.40 2.10 5 -4 0 42.30 2.10 5 -4 0 42.70 2.10 5 -4 0 41.30 2.70 -5 4 0 42.90 2.10 -5 4 0 41.90 2.10 -5 4 0 41.90 2.40 -5 4 0 42.80 2.10 -5 4 0 45.60 2.10 4 -4 0 16.80 1.00 4 -4 0 17.60 0.90 4 -4 0 16.80 0.90 4 -4 0 15.00 1.40 -4 4 0 16.70 0.90 -4 4 0 16.70 0.90 -4 4 0 17.00 1.20 -4 4 0 17.80 1.00 -4 4 0 18.10 0.90 3 -4 0 666.33 31.10 3 -4 0 639.74 44.90 3 -4 0 557.84 48.00 3 -4 0 600.34 32.10 -3 4 0 651.63 32.20 -3 4 0 684.83 49.80 -3 4 0 598.14 41.60 -3 4 0 575.84 30.10 2 -4 0 742.33 32.50 2 -4 0 657.73 32.90 2 -4 0 735.73 41.00 2 -4 0 695.03 44.10 -2 4 0 714.73 44.10 -2 4 0 712.23 33.40 -2 4 0 637.84 39.00 -2 4 0 667.33 32.30 1 -4 0 85.39 3.80 1 -4 0 82.79 4.10 -1 4 0 79.99 4.00 -1 4 0 78.69 3.80 0 4 0 102.69 4.60 0 4 0 100.69 4.60 0 4 0 104.79 5.00 -1 -4 0 3.90 0.20 -1 -4 0 3.90 0.40 -1 -4 0 3.60 0.30 -1 -4 0 3.60 0.30 1 4 0 3.90 0.30 1 4 0 4.20 0.30 1 4 0 3.10 0.30 1 4 0 3.70 0.30 1 4 0 5.80 1.00 -2 -4 0 0.00 0.10 -2 -4 0 0.00 0.20 -2 -4 0 0.10 0.20 -2 -4 0 0.00 0.10 2 4 0 0.40 0.20 2 4 0 0.00 0.20 2 4 0 0.10 0.20 2 4 0 0.30 0.20 3 4 0 142.09 6.40 3 4 0 138.79 6.40 -4 -4 0 11.60 0.80 -4 -4 0 11.00 0.70 -4 -4 0 12.20 0.80 -4 -4 0 12.40 0.80 4 4 0 11.10 0.80 4 4 0 11.90 0.80 4 4 0 11.70 0.90 4 4 0 10.20 0.90 -5 -4 0 108.79 5.00 -5 -4 0 108.99 5.00 -5 -4 0 104.29 4.90 5 4 0 110.69 5.00 5 4 0 109.39 5.00 5 4 0 105.09 5.10 5 4 0 101.39 5.00 -6 -4 0 45.40 2.50 -6 -4 0 44.80 2.30 -6 -4 0 48.80 2.40 6 4 0 44.90 2.40 6 4 0 45.50 2.40 6 4 0 44.60 2.40 -7 -4 0 5.20 0.80 -7 -4 0 4.90 0.70 -7 -4 0 6.00 0.80 7 4 0 4.50 0.80 7 4 0 5.80 0.90 7 4 0 4.70 0.80 7 4 0 6.10 0.80 -8 -4 0 5.10 0.80 -8 -4 0 5.40 0.80 -8 -4 0 5.70 0.80 -8 -4 0 5.00 0.70 8 4 0 5.50 0.90 8 4 0 5.90 1.00 8 4 0 4.60 0.80 8 4 0 4.80 0.80 -9 -4 0 0.50 0.50 -9 -4 0 0.10 0.70 -9 -4 0 -0.50 0.40 9 4 0 0.70 0.70 9 4 0 -0.30 1.20 9 4 0 0.80 0.60 11 -5 0 3.50 1.90 10 -5 0 20.80 1.80 10 -5 0 22.20 1.60 10 -5 0 23.50 1.90 10 -5 0 14.80 2.50 10 -5 0 23.40 1.80 -10 5 0 24.50 1.80 -10 5 0 24.30 1.60 9 -5 0 2.40 0.70 9 -5 0 1.50 0.70 9 -5 0 1.80 0.50 9 -5 0 2.50 1.50 9 -5 0 1.40 0.70 -9 5 0 2.00 0.70 -9 5 0 2.00 0.60 -9 5 0 1.30 0.50 8 -5 0 9.00 1.00 8 -5 0 4.90 1.40 8 -5 0 7.70 0.80 8 -5 0 8.10 0.90 8 -5 0 8.20 1.30 -8 5 0 5.10 0.80 -8 5 0 6.10 0.70 -8 5 0 8.70 0.90 -8 5 0 6.60 0.70 7 -5 0 53.79 3.50 7 -5 0 50.89 2.60 7 -5 0 48.40 2.60 7 -5 0 52.39 2.60 -7 5 0 51.19 2.50 -7 5 0 48.50 2.60 -7 5 0 46.90 2.50 -7 5 0 51.29 2.60 6 -5 0 7.50 0.70 6 -5 0 6.60 0.70 6 -5 0 4.90 1.10 6 -5 0 7.50 0.70 6 -5 0 6.30 0.60 -6 5 0 6.20 0.60 -6 5 0 7.00 0.60 -6 5 0 6.70 0.60 -6 5 0 7.90 0.70 5 -5 0 63.99 3.00 5 -5 0 66.19 3.10 5 -5 0 67.29 3.10 5 -5 0 61.79 3.00 5 -5 0 64.19 3.70 -5 5 0 66.89 3.10 -5 5 0 65.39 3.10 -5 5 0 66.89 3.10 -5 5 0 62.89 3.00 4 -5 0 144.79 7.00 4 -5 0 142.39 6.40 -4 5 0 141.49 6.40 -4 5 0 145.89 6.40 -4 5 0 144.29 6.80 -4 5 0 139.49 6.80 3 -5 0 1.20 0.60 3 -5 0 2.20 0.20 -3 5 0 2.20 0.20 -3 5 0 2.80 0.60 -3 5 0 3.40 0.60 -3 5 0 1.80 0.20 -3 5 0 2.30 0.30 -3 5 0 2.70 0.30 -2 5 0 415.56 18.60 -2 5 0 406.76 18.40 1 -5 0 76.99 3.80 1 -5 0 75.49 3.50 -1 5 0 72.69 3.20 -1 5 0 71.49 3.40 -1 5 0 64.79 3.20 -1 5 0 71.69 3.70 -1 5 0 76.59 3.20 0 -5 0 0.20 0.40 0 -5 0 0.10 0.20 0 -5 0 0.00 0.10 0 -5 0 0.20 0.10 0 5 0 0.20 0.10 0 5 0 0.00 0.10 0 5 0 0.40 0.40 0 5 0 -0.10 0.10 0 5 0 0.10 0.10 -1 -5 0 38.60 1.80 -1 -5 0 39.00 1.90 1 5 0 40.70 1.80 1 5 0 39.20 1.80 1 5 0 34.80 1.80 1 5 0 39.60 1.80 1 5 0 36.00 2.30 2 5 0 343.37 15.90 -3 -5 0 0.60 0.20 -3 -5 0 0.70 0.20 -3 -5 0 0.50 0.30 -3 -5 0 0.80 0.30 3 5 0 0.80 0.30 3 5 0 0.50 0.30 3 5 0 0.90 0.30 3 5 0 0.80 0.30 -4 -5 0 174.38 7.90 -4 -5 0 174.48 7.70 4 5 0 177.78 7.90 4 5 0 164.78 7.80 4 5 0 169.18 7.90 -5 -5 0 61.79 3.00 -5 -5 0 61.29 3.00 -5 -5 0 63.29 3.10 5 5 0 63.09 3.10 5 5 0 60.79 3.20 5 5 0 60.39 3.10 5 5 0 65.49 3.10 -6 -5 0 1.90 0.50 -6 -5 0 2.40 0.60 -6 -5 0 2.50 0.60 -6 -5 0 1.80 0.50 6 5 0 1.40 0.50 6 5 0 1.60 0.60 6 5 0 2.10 0.60 6 5 0 2.20 0.60 -7 -5 0 2.30 0.60 -7 -5 0 1.80 0.50 -7 -5 0 1.90 0.70 7 5 0 1.80 0.70 7 5 0 1.40 0.60 7 5 0 1.90 0.60 -8 -5 0 0.30 0.50 -8 -5 0 0.70 0.60 -8 -5 0 0.80 0.50 8 5 0 0.40 1.00 8 5 0 0.10 0.50 8 5 0 1.20 0.60 8 5 0 0.90 0.70 -9 -5 0 1.50 0.70 -9 -5 0 2.50 0.70 -9 -5 0 3.50 1.00 -9 -5 0 2.90 0.70 9 5 0 3.20 0.90 9 5 0 2.10 0.80 9 5 0 2.60 1.00 10 -6 0 1.00 1.70 10 -6 0 3.00 0.80 10 -6 0 2.20 0.70 10 -6 0 2.20 0.90 10 -6 0 2.20 0.70 -10 6 0 1.90 0.70 -10 6 0 3.70 0.70 -10 6 0 2.60 0.60 9 -6 0 3.10 1.50 9 -6 0 4.70 0.70 9 -6 0 6.00 0.80 9 -6 0 4.50 0.80 9 -6 0 4.30 0.80 -9 6 0 3.40 0.70 -9 6 0 5.00 0.70 -9 6 0 4.30 0.70 -9 6 0 4.70 0.80 8 -6 0 43.30 2.40 8 -6 0 42.60 2.30 8 -6 0 40.30 3.50 8 -6 0 45.30 2.50 8 -6 0 47.40 2.40 -8 6 0 46.20 2.40 -8 6 0 43.80 2.30 -8 6 0 42.80 2.30 -8 6 0 46.40 2.40 7 -6 0 1.00 0.40 7 -6 0 0.60 0.40 7 -6 0 0.60 0.40 7 -6 0 1.10 0.50 7 -6 0 0.80 1.00 -7 6 0 0.80 0.40 -7 6 0 0.70 0.40 -7 6 0 1.10 0.50 -7 6 0 0.90 0.40 6 -6 0 104.49 4.70 6 -6 0 100.59 5.60 6 -6 0 109.29 4.90 6 -6 0 104.79 4.90 6 -6 0 97.79 4.70 -6 6 0 102.89 4.80 -6 6 0 101.59 4.80 -6 6 0 101.79 4.80 -6 6 0 108.39 4.80 5 -6 0 56.99 3.90 5 -6 0 68.09 3.20 -5 6 0 71.89 3.20 -5 6 0 77.39 3.30 -5 6 0 72.99 3.30 -5 6 0 61.79 3.30 4 -6 0 0.30 0.70 4 -6 0 0.80 0.20 -4 6 0 1.20 0.30 -4 6 0 0.80 0.20 -4 6 0 1.30 0.50 -4 6 0 1.30 1.00 -4 6 0 0.70 0.30 -4 6 0 0.90 0.20 3 -6 0 19.60 1.00 3 -6 0 21.20 1.80 3 -6 0 20.50 1.00 -3 6 0 21.10 1.40 -3 6 0 20.60 1.00 -3 6 0 23.00 1.60 -3 6 0 21.60 1.00 -3 6 0 18.70 1.00 2 -6 0 74.89 4.00 -2 6 0 75.59 3.50 -2 6 0 71.29 3.20 -2 6 0 73.79 3.20 -2 6 0 63.79 3.20 -2 6 0 74.39 3.80 1 -6 0 79.79 4.20 1 -6 0 83.09 3.70 -1 6 0 80.69 3.70 -1 6 0 69.69 3.40 -1 6 0 82.59 3.40 -1 6 0 66.49 4.70 -1 6 0 74.29 3.50 0 6 0 351.96 16.20 -1 -6 0 56.59 2.60 -1 -6 0 56.79 2.70 1 6 0 57.39 2.60 1 6 0 53.49 3.20 1 6 0 51.29 2.60 1 6 0 55.69 2.60 1 6 0 59.09 2.60 -2 -6 0 207.38 9.80 2 6 0 214.48 10.00 2 6 0 214.38 11.60 2 6 0 237.48 10.10 -3 -6 0 26.80 1.30 -3 -6 0 25.00 1.20 -3 -6 0 24.70 1.30 -3 -6 0 24.90 1.40 -3 -6 0 22.20 1.40 3 6 0 23.40 1.30 3 6 0 23.00 1.40 3 6 0 23.60 1.30 3 6 0 24.80 1.40 -4 -6 0 2.90 0.50 -4 -6 0 2.20 0.40 -4 -6 0 2.20 0.30 -4 -6 0 2.90 0.40 4 6 0 3.00 0.50 4 6 0 3.00 0.60 4 6 0 2.30 0.50 4 6 0 2.60 0.50 -5 -6 0 3.60 0.50 -5 -6 0 3.10 0.50 -5 -6 0 3.60 0.50 -5 -6 0 3.80 0.60 5 6 0 4.20 0.70 5 6 0 3.50 0.60 5 6 0 3.30 0.60 5 6 0 4.70 0.80 -6 -6 0 21.30 1.50 -6 -6 0 21.70 1.50 -6 -6 0 19.10 1.50 -6 -6 0 20.70 1.30 6 6 0 22.00 1.60 6 6 0 22.00 1.60 6 6 0 23.50 1.50 6 6 0 25.30 1.60 -7 -6 0 0.90 0.50 -7 -6 0 1.30 0.50 -7 -6 0 2.20 0.60 -7 -6 0 0.70 0.60 7 6 0 2.10 0.70 7 6 0 1.70 0.60 7 6 0 1.60 0.70 7 6 0 1.90 0.70 -8 -6 0 14.60 1.30 -8 -6 0 14.60 1.20 -8 -6 0 15.40 1.40 -8 -6 0 14.30 1.10 8 6 0 11.80 1.20 8 6 0 12.20 1.30 8 6 0 12.70 1.30 8 6 0 11.30 1.20 10 -7 0 8.80 2.30 10 -7 0 14.80 1.20 10 -7 0 13.90 1.20 10 -7 0 15.40 1.50 -10 7 0 13.00 1.30 -10 7 0 11.50 1.10 -10 7 0 14.00 1.30 9 -7 0 8.30 0.90 9 -7 0 8.30 0.90 9 -7 0 7.50 2.00 9 -7 0 9.90 0.90 9 -7 0 8.60 1.00 -9 7 0 7.50 1.00 -9 7 0 7.50 1.00 -9 7 0 9.10 0.90 -9 7 0 7.70 0.80 8 -7 0 2.00 0.50 8 -7 0 0.90 1.30 8 -7 0 1.20 0.40 8 -7 0 1.30 0.40 -8 7 0 1.70 0.50 -8 7 0 1.50 0.50 -8 7 0 1.40 0.60 -8 7 0 1.50 0.50 7 -7 0 43.20 3.50 7 -7 0 43.60 2.30 7 -7 0 47.60 2.40 -7 7 0 48.20 2.40 -7 7 0 47.70 2.40 -7 7 0 43.80 2.30 -7 7 0 46.40 2.30 6 -7 0 1.60 0.40 6 -7 0 0.90 1.10 -6 7 0 0.90 0.40 -6 7 0 0.90 0.30 -6 7 0 0.60 0.40 -6 7 0 1.30 0.40 5 -7 0 2.70 0.40 5 -7 0 2.80 1.20 -5 7 0 2.50 0.40 -5 7 0 3.10 0.40 -5 7 0 3.10 0.40 -5 7 0 2.80 0.40 4 -7 0 177.68 7.60 4 -7 0 146.69 8.40 4 -7 0 172.68 7.60 -4 7 0 165.38 7.60 -4 7 0 174.08 7.60 -4 7 0 178.28 7.60 -4 7 0 175.48 7.60 -4 7 0 162.28 8.00 3 -7 0 63.99 3.80 -3 7 0 62.39 2.90 -3 7 0 60.09 2.90 -3 7 0 61.29 3.20 -3 7 0 63.39 2.90 -3 7 0 75.39 4.20 -3 7 0 63.99 2.80 2 -7 0 168.88 7.90 -2 7 0 151.48 7.00 -2 7 0 165.08 7.40 -2 7 0 144.89 8.00 -2 7 0 162.98 7.10 1 -7 0 139.19 6.90 1 -7 0 146.29 6.40 -1 7 0 131.89 6.10 -1 7 0 137.39 6.30 -1 7 0 126.99 6.00 0 -7 0 0.50 0.40 0 7 0 0.70 0.20 0 7 0 0.90 0.20 0 7 0 0.70 0.30 0 7 0 0.80 0.20 0 7 0 1.10 0.50 -1 -7 0 23.60 1.20 -1 -7 0 23.70 1.20 -1 -7 0 26.30 1.50 1 7 0 24.80 1.20 1 7 0 25.40 1.20 1 7 0 23.90 1.30 1 7 0 23.70 1.30 -2 -7 0 13.50 0.80 -2 -7 0 14.20 0.90 -2 -7 0 14.50 1.00 2 7 0 13.10 1.00 2 7 0 14.90 0.90 2 7 0 15.30 0.90 2 7 0 13.70 0.90 -3 -7 0 27.20 1.50 3 7 0 27.40 1.50 3 7 0 25.80 1.60 3 7 0 29.60 1.50 3 7 0 26.40 1.60 -4 -7 0 71.09 3.50 -4 -7 0 76.79 3.60 -4 -7 0 70.39 3.50 -4 -7 0 75.29 3.30 -4 -7 0 65.69 3.40 4 7 0 77.19 3.50 4 7 0 69.39 3.60 4 7 0 74.89 3.50 4 7 0 68.19 3.80 -5 -7 0 18.40 1.10 -5 -7 0 17.40 1.10 -5 -7 0 18.00 1.30 -5 -7 0 17.90 1.30 5 7 0 17.70 1.40 5 7 0 19.20 1.30 5 7 0 19.30 1.50 5 7 0 22.00 1.40 -6 -7 0 21.20 1.30 -6 -7 0 23.80 1.60 -6 -7 0 23.00 1.40 -6 -7 0 25.90 1.60 6 7 0 22.50 1.70 6 7 0 25.30 1.80 6 7 0 24.80 1.70 6 7 0 25.40 1.70 -7 -7 0 18.30 1.30 -7 -7 0 21.40 1.40 -7 -7 0 23.10 1.70 7 7 0 21.30 2.60 7 7 0 23.10 1.70 7 7 0 25.30 1.80 9 -8 0 -1.20 1.60 9 -8 0 0.10 0.40 -9 8 0 -0.20 0.60 -9 8 0 0.00 0.40 -9 8 0 0.50 0.60 -9 8 0 -0.10 0.40 8 -8 0 0.30 1.50 8 -8 0 1.10 0.40 8 -8 0 0.70 0.50 -8 8 0 0.30 0.40 -8 8 0 -0.30 0.50 -8 8 0 1.10 0.60 -8 8 0 0.60 0.40 7 -8 0 4.10 0.50 7 -8 0 3.20 0.60 7 -8 0 3.40 1.60 -7 8 0 4.60 0.60 -7 8 0 3.40 0.50 -7 8 0 3.70 0.60 -7 8 0 3.50 0.50 6 -8 0 16.90 2.30 -6 8 0 18.30 1.10 -6 8 0 18.80 1.20 -6 8 0 18.10 1.10 -6 8 0 17.30 1.00 5 -8 0 2.10 0.40 5 -8 0 2.00 0.30 5 -8 0 1.70 1.20 -5 8 0 1.70 0.30 -5 8 0 2.40 0.40 -5 8 0 1.80 0.40 -5 8 0 2.10 0.40 4 -8 0 9.30 1.60 -4 8 0 8.10 0.50 -4 8 0 9.20 0.60 -4 8 0 8.70 0.60 3 -8 0 91.49 5.00 -3 8 0 84.59 3.90 -3 8 0 85.19 3.80 -3 8 0 81.29 4.30 2 -8 0 49.90 3.30 -2 8 0 45.80 2.50 -2 8 0 48.00 2.20 -2 8 0 46.50 2.10 1 -8 0 0.20 0.40 1 -8 0 0.50 1.00 -1 8 0 0.20 0.40 -1 8 0 0.60 0.20 -1 8 0 0.60 0.30 0 -8 0 1.30 0.60 0 8 0 0.90 0.20 0 8 0 1.20 0.20 0 8 0 1.20 0.40 0 8 0 0.80 0.20 -1 -8 0 42.30 2.10 -1 -8 0 45.40 2.10 -1 -8 0 43.90 2.70 1 8 0 47.70 2.20 1 8 0 46.80 2.20 1 8 0 48.40 2.20 1 8 0 45.00 2.30 -2 -8 0 26.30 1.40 -2 -8 0 31.60 1.80 2 8 0 26.60 1.40 2 8 0 24.60 1.50 2 8 0 24.70 1.40 2 8 0 24.10 1.60 -3 -8 0 36.50 1.90 -3 -8 0 38.20 2.10 3 8 0 38.50 1.90 3 8 0 36.40 2.10 3 8 0 35.20 2.00 -4 -8 0 3.10 0.50 -4 -8 0 2.90 0.60 -4 -8 0 2.20 0.50 4 8 0 2.70 0.60 4 8 0 3.30 0.60 4 8 0 3.30 0.60 4 8 0 2.60 0.70 -5 -8 0 30.00 1.60 -5 -8 0 27.90 2.00 -5 -8 0 33.20 1.80 -5 -8 0 32.60 2.00 -5 -8 0 33.00 1.60 5 8 0 32.90 2.40 5 8 0 32.50 1.90 5 8 0 33.00 1.90 5 8 0 31.60 2.00 -6 -8 0 9.20 0.70 -6 -8 0 8.50 0.70 -6 -8 0 8.60 1.10 -6 -8 0 7.50 0.90 -6 -8 0 8.80 1.00 6 8 0 9.20 1.10 6 8 0 9.30 1.00 6 8 0 9.60 1.10 -7 -8 0 0.20 0.60 -7 -8 0 0.10 0.40 -7 -8 0 1.30 0.60 7 8 0 0.10 0.70 7 8 0 1.90 0.60 7 8 0 0.70 0.70 9 -9 0 1.70 0.50 9 -9 0 0.40 1.80 9 -9 0 -0.20 0.10 -9 9 0 1.40 0.60 -9 9 0 0.10 0.40 8 -9 0 5.10 0.70 8 -9 0 5.50 1.90 8 -9 0 5.30 0.60 -8 9 0 4.40 0.60 -8 9 0 3.30 0.90 -8 9 0 5.40 0.70 -8 9 0 5.50 0.80 7 -9 0 51.49 2.60 7 -9 0 58.79 4.30 7 -9 0 50.99 2.60 -7 9 0 53.79 2.60 -7 9 0 51.39 2.60 -7 9 0 57.69 2.70 -7 9 0 54.59 2.70 6 -9 0 47.20 3.60 6 -9 0 41.70 2.00 6 -9 0 41.90 2.00 -6 9 0 41.30 2.10 -6 9 0 43.00 2.10 -6 9 0 41.20 2.20 -6 9 0 43.10 2.10 5 -9 0 8.30 1.70 -5 9 0 11.40 0.70 -5 9 0 10.50 0.70 -5 9 0 10.90 0.70 -5 9 0 12.00 0.80 4 -9 0 34.40 2.90 -4 9 0 29.90 1.50 -4 9 0 29.70 1.50 3 -9 0 8.50 1.70 -3 9 0 6.80 0.50 -3 9 0 7.70 0.60 2 -9 0 37.90 2.90 -2 9 0 26.70 1.80 -2 9 0 31.40 1.50 -2 9 0 30.70 1.40 1 -9 0 46.10 2.60 1 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3.20 0.60 7 3 -10 1.00 0.50 7 3 -10 1.60 0.70 7 3 -10 1.20 0.60 7 3 -10 1.60 0.50 -7 -3 10 1.50 0.60 -7 -3 10 1.20 0.50 -7 -3 10 2.50 0.60 6 3 -10 5.90 0.90 6 3 -10 6.80 0.90 6 3 -10 4.20 0.70 6 3 -10 4.60 0.70 -6 -3 10 3.70 0.80 -6 -3 10 7.30 0.70 -6 -3 10 5.90 0.80 -6 -3 10 4.90 0.60 5 3 -10 69.19 3.40 5 3 -10 62.09 3.30 5 3 -10 65.19 3.40 -5 -3 10 67.49 3.30 -5 -3 10 65.99 3.20 -5 -3 10 68.59 3.20 4 3 -10 33.90 1.90 4 3 -10 35.80 1.90 4 3 -10 34.40 1.90 4 3 -10 32.40 1.80 4 3 -10 32.50 2.00 -4 -3 10 35.90 1.80 -4 -3 10 33.80 1.80 -4 -3 10 34.10 1.90 3 3 -10 124.69 5.90 3 3 -10 130.49 6.10 3 3 -10 133.59 6.10 3 3 -10 129.69 5.80 3 3 -10 128.09 6.00 -3 -3 10 133.09 5.90 -3 -3 10 129.39 5.90 -3 -3 10 123.39 6.00 -3 -3 10 132.29 6.00 2 3 -10 92.69 4.60 2 3 -10 100.09 4.70 2 3 -10 95.59 4.50 2 3 -10 99.19 4.60 -2 -3 10 97.99 4.50 -2 -3 10 101.99 4.60 -2 -3 10 98.49 4.50 -2 -3 10 94.79 4.70 1 3 -10 110.09 5.00 1 3 -10 111.19 5.10 1 3 -10 105.39 5.00 1 3 -10 108.69 4.90 -1 -3 10 100.99 4.90 -1 -3 10 110.99 5.00 -1 -3 10 100.79 5.10 -1 -3 10 104.69 4.90 0 3 -10 30.50 1.70 0 3 -10 30.50 1.60 0 3 -10 32.80 1.70 0 3 -10 31.10 1.80 0 -3 10 31.30 1.70 0 -3 10 30.20 1.70 0 -3 10 26.70 1.80 0 -3 10 34.00 1.50 0 -3 10 32.70 1.70 -1 3 -10 0.50 0.40 -1 3 -10 0.80 0.40 -1 3 -10 0.50 0.40 -1 3 -10 0.40 0.20 1 -3 10 0.60 0.40 1 -3 10 0.70 0.40 1 -3 10 0.90 0.30 1 -3 10 0.50 0.30 1 -3 10 -0.10 0.50 1 -3 10 0.50 0.20 -2 3 -10 8.20 0.80 -2 3 -10 7.60 0.80 -2 3 -10 7.50 0.60 -2 3 -10 8.60 0.90 -2 3 -10 7.80 0.90 2 -3 10 8.00 0.80 2 -3 10 9.30 0.80 2 -3 10 8.70 0.80 2 -3 10 8.10 0.60 2 -3 10 6.30 0.90 -3 3 -10 51.69 2.80 -3 3 -10 48.30 2.50 -3 3 -10 46.20 2.60 -3 3 -10 54.69 2.60 3 -3 10 47.30 2.80 3 -3 10 50.79 2.40 3 -3 10 49.70 2.60 3 -3 10 50.69 2.50 -4 3 -10 16.30 1.20 -4 3 -10 16.80 1.30 -4 3 -10 19.10 1.60 4 -3 10 17.40 1.10 4 -3 10 16.50 1.20 4 -3 10 16.50 1.60 4 -3 10 21.00 1.70 -5 3 -10 4.10 0.70 -5 3 -10 3.50 0.60 -5 3 -10 3.90 0.60 5 -3 10 2.80 0.60 5 -3 10 2.20 0.60 5 -3 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7 2 -10 44.00 2.50 7 2 -10 41.10 2.30 7 2 -10 39.90 2.70 7 2 -10 45.80 2.60 -7 -2 10 45.70 2.50 -7 -2 10 45.50 2.30 -7 -2 10 40.40 2.30 6 2 -10 30.10 1.70 6 2 -10 31.00 2.00 6 2 -10 28.80 1.90 6 2 -10 30.20 1.90 -6 -2 10 28.60 1.60 -6 -2 10 30.80 1.80 -6 -2 10 28.10 1.60 -6 -2 10 23.70 1.60 5 2 -10 135.39 6.60 5 2 -10 145.49 6.70 5 2 -10 137.99 6.70 5 2 -10 147.49 6.80 -5 -2 10 145.99 6.60 -5 -2 10 145.09 6.50 -5 -2 10 138.19 6.50 4 2 -10 175.28 7.90 4 2 -10 169.08 7.90 4 2 -10 177.38 8.00 4 2 -10 167.68 8.00 -4 -2 10 175.68 7.90 3 2 -10 148.29 6.80 3 2 -10 146.79 6.70 3 2 -10 147.49 6.90 3 2 -10 144.19 6.70 3 2 -10 143.59 6.70 -3 -2 10 147.89 6.70 -3 -2 10 150.28 6.80 2 2 -10 1.10 0.40 2 2 -10 1.10 0.50 2 2 -10 0.70 0.30 2 2 -10 1.20 0.40 -2 -2 10 1.30 0.40 -2 -2 10 1.00 0.50 -2 -2 10 0.80 0.30 -2 -2 10 0.80 0.30 -2 -2 10 1.00 0.40 1 2 -10 1.20 0.30 1 2 -10 2.20 0.40 1 2 -10 1.20 0.50 1 2 -10 1.60 0.50 -1 -2 10 1.60 0.30 -1 -2 10 1.30 0.40 -1 -2 10 1.70 0.40 -1 -2 10 1.60 0.40 -1 -2 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19 1.00 0.90 -1 -1 19 1.60 0.60 -1 -1 19 0.70 0.60 -1 -1 19 1.10 0.80 0 1 -19 18.90 2.10 0 1 -19 16.50 1.70 0 1 -19 11.70 1.40 0 1 -19 15.30 1.40 0 -1 19 15.50 1.60 0 -1 19 17.70 1.70 0 -1 19 16.30 1.60 0 -1 19 17.10 1.30 0 -1 19 13.40 1.40 -1 1 -19 2.00 1.20 -1 1 -19 3.60 1.00 -1 1 -19 4.50 0.80 -1 1 -19 2.90 0.90 1 -1 19 3.00 0.70 1 -1 19 2.60 0.80 1 -1 19 2.20 0.80 1 -1 19 3.10 1.10 1 -1 19 3.00 0.90 5 0 -19 0.30 0.60 5 0 -19 1.40 1.00 5 0 -19 0.40 0.60 5 0 -19 0.40 0.80 -5 0 19 0.60 0.50 -5 0 19 1.00 0.60 -5 0 19 0.50 0.90 4 0 -19 1.30 0.80 4 0 -19 2.60 0.70 4 0 -19 1.50 1.20 4 0 -19 0.50 0.80 -4 0 19 1.90 0.80 -4 0 19 2.80 0.70 -4 0 19 1.60 0.70 -4 0 19 1.20 0.90 -4 0 19 2.50 1.00 3 0 -19 7.20 1.00 3 0 -19 6.60 1.00 3 0 -19 2.70 1.10 -3 0 19 5.60 1.00 -3 0 19 6.40 1.10 -3 0 19 7.20 0.90 -3 0 19 6.90 1.10 -3 0 19 6.20 1.20 2 0 -19 2.20 0.60 2 0 -19 2.80 1.20 2 0 -19 2.00 0.80 -2 0 19 2.00 0.90 -2 0 19 1.50 0.80 -2 0 19 1.50 0.90 -2 0 19 2.30 0.70 -2 0 19 0.90 0.60 1 0 -19 0.00 1.10 1 0 -19 1.90 0.80 1 0 -19 1.90 0.60 1 0 -19 1.70 0.70 -1 0 19 2.40 0.80 -1 0 19 0.80 0.70 -1 0 19 1.00 0.90 -1 0 19 2.20 0.90 -1 0 19 1.20 0.60 0 0 -19 0.80 1.00 0 0 -19 -0.20 0.90 0 0 -19 -0.30 0.50 0 0 -19 0.90 0.70 0 0 19 0.40 0.70 0 0 19 0.10 0.80 0 0 19 0.10 0.80 0 0 19 0.00 0.50 0 0 19 -0.60 0.70 -1 0 -19 2.10 1.20 -1 0 -19 0.80 0.70 -1 0 -19 2.10 0.70 -1 0 -19 0.90 0.80 1 0 19 1.40 0.80 1 0 19 0.90 0.90 1 0 19 0.50 0.50 1 0 19 0.80 0.80 -5 1 19 6.20 1.20 4 -1 -19 0.40 0.60 4 -1 -19 -0.20 0.90 4 -1 -19 -0.40 0.60 -4 1 19 -0.40 0.80 -4 1 19 1.10 0.70 -4 1 19 0.10 0.60 3 -1 -19 3.60 0.70 3 -1 -19 2.20 0.80 3 -1 -19 3.30 1.20 -3 1 19 3.20 1.40 -3 1 19 3.80 0.70 -3 1 19 3.40 0.90 -3 1 19 2.80 1.50 2 -1 -19 0.30 0.50 2 -1 -19 -0.10 0.60 2 -1 -19 -0.50 0.90 -2 1 19 0.10 0.60 -2 1 19 -1.10 0.90 -2 1 19 -0.20 0.80 -2 1 19 -0.30 0.70 1 -1 -19 3.80 0.80 1 -1 -19 2.30 1.10 1 -1 -19 2.00 0.80 -1 1 19 2.30 0.90 -1 1 19 2.50 0.70 -1 1 19 2.70 0.90 0 -1 -19 1.10 0.90 0 -1 -19 1.20 0.80 0 -1 -19 2.80 0.70 0 -1 -19 1.90 1.10 0 1 19 1.80 0.70 0 1 19 1.10 0.70 0 1 19 1.60 0.70 0 1 19 -0.10 0.60 4 -2 -19 4.50 0.80 4 -2 -19 2.80 0.80 4 -2 -19 2.20 1.20 -4 2 19 4.60 0.80 -4 2 19 3.30 1.00 -4 2 19 4.40 1.00 -4 2 19 3.30 0.90 3 -2 -19 0.40 0.60 3 -2 -19 -0.20 0.60 3 -2 -19 0.10 0.90 -3 2 19 0.20 0.70 -3 2 19 0.70 0.70 -3 2 19 0.20 0.70 -3 2 19 -0.50 0.70 -3 2 19 0.30 0.60 2 -2 -19 1.00 1.20 2 -2 -19 0.00 0.70 2 -2 -19 0.20 0.50 -2 2 19 0.80 0.80 -2 2 19 -0.20 0.80 -2 2 19 0.00 0.50 -2 2 19 -1.00 0.70 -2 2 19 -0.10 0.60 1 -2 -19 2.90 0.70 1 -2 -19 3.70 1.20 1 -2 -19 3.50 0.90 1 -2 -19 4.50 1.20 -1 2 19 3.20 1.00 -1 2 19 2.50 0.80 -1 2 19 3.40 0.80 -1 2 19 2.90 1.00 -1 2 19 4.60 0.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 18976 _shelx_res_file ; TITL 5brsal_dmf_a.res in P-1 5brsal_dmf.res created by SHELXL-2019/3 at 13:12:26 on 12-Aug-2026 REM Old TITL 5brsal_dmf in P-1 REM SHELXT solution in P-1: R1 0.152, Rweak 0.005, Alpha 0.032 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C20 N2 O8 Br2 CELL 0.71073 8.5524 9.5175 14.9678 95.923 99.795 100.461 ZERR 4 0.0003 0.0003 0.0005 0.001 0.002 0.001 LATT 1 SFAC C H Br N O UNIT 40 48 4 4 16 L.S. 8 PLAN 2 TEMP -100.15 CONF HTAB O8 O7 HTAB O2 O1 HTAB O6 O5 HTAB O4 O3 BOND list 4 MORE -1 BOND $H fmap 2 53 HTAB acta OMIT -1 -3 1 OMIT -1 -3 3 OMIT 0 -2 2 OMIT 0 0 1 OMIT 0 2 0 OMIT 2 -4 2 REM REM REM WGHT 0.027800 0.296600 FVAR 0.26508 BR1 3 0.245570 0.909924 0.990128 11.00000 0.05939 0.02360 = 0.04263 0.00440 0.01085 0.00900 BR2 3 0.117481 -0.407500 0.658796 11.00000 0.04500 0.02475 = 0.06018 0.01047 0.01501 0.00816 O1 5 0.453138 0.204722 0.759293 11.00000 0.04558 0.02822 = 0.04009 0.00628 0.01197 0.01196 O5 5 0.335701 0.292353 0.434968 11.00000 0.05077 0.03177 = 0.03951 0.01208 0.01868 0.01482 O7 5 0.130346 0.257505 0.597878 11.00000 0.05469 0.02818 = 0.04267 0.01207 0.01894 0.01730 O8 5 0.007990 0.196290 0.738547 11.00000 0.05759 0.03320 = 0.04805 0.00898 0.02683 0.01986 AFIX 147 H8A 2 0.045021 0.249767 0.702559 11.00000 -1.50000 AFIX 0 O2 5 0.367990 0.405065 0.854733 11.00000 0.05036 0.02589 = 0.03932 0.00747 0.01865 0.01063 AFIX 147 H2 2 0.395224 0.335766 0.825995 11.00000 -1.50000 AFIX 0 O6 5 0.230867 0.091682 0.522086 11.00000 0.05085 0.03009 = 0.03445 0.01046 0.01797 0.01433 AFIX 147 H6 2 0.252385 0.158605 0.490892 11.00000 -1.50000 AFIX 0 O3 5 0.301387 0.238395 0.943626 11.00000 0.05940 0.02635 = 0.04974 0.01264 0.02155 0.01372 O4 5 0.186708 0.307121 1.086325 11.00000 0.05708 0.03554 = 0.04772 0.02174 0.02230 0.01459 AFIX 147 H4 2 0.210778 0.251409 1.045891 11.00000 -1.50000 AFIX 0 N2 4 0.342806 0.518928 0.400958 11.00000 0.03992 0.03164 = 0.03799 0.00986 0.00992 0.00995 N1 4 0.514873 -0.017076 0.754413 11.00000 0.03806 0.02954 = 0.03894 0.00436 0.00743 0.01012 C15 1 0.104888 0.024096 0.643522 11.00000 0.02700 0.02689 = 0.02968 0.00590 0.00552 0.00716 C4 1 0.312454 0.362938 0.925815 11.00000 0.03282 0.02706 = 0.03528 0.00702 0.00822 0.00576 C9 1 0.227635 0.718113 1.018307 11.00000 0.03525 0.02503 = 0.03371 0.00498 0.00518 0.00479 C6 1 0.201637 0.440687 1.062017 11.00000 0.03207 0.03172 = 0.03444 0.01246 0.00786 0.00626 C20 1 0.128849 -0.116308 0.625796 11.00000 0.02930 0.02779 = 0.03269 0.00473 0.00704 0.00564 AFIX 43 H20 2 0.176193 -0.143184 0.575298 11.00000 -1.20000 AFIX 0 C19 1 0.083322 -0.216066 0.682114 11.00000 0.03259 0.02432 = 0.03927 0.00617 0.00657 0.00560 C5 1 0.263167 0.475611 0.984224 11.00000 0.02969 0.02575 = 0.03147 0.00725 0.00608 0.00486 C1 1 0.462336 0.092043 0.793041 11.00000 0.03491 0.02867 = 0.03565 0.00221 0.00601 0.00626 AFIX 43 H1 2 0.429615 0.083668 0.850143 11.00000 -1.20000 AFIX 0 C10 1 0.276279 0.616242 0.962618 11.00000 0.03242 0.02504 = 0.03055 0.00663 0.00713 0.00259 AFIX 43 H10 2 0.318147 0.641357 0.910262 11.00000 -1.20000 AFIX 0 C16 1 0.035019 0.062466 0.718330 11.00000 0.03321 0.03124 = 0.03563 0.00525 0.00926 0.00985 C7 1 0.152433 0.545583 1.115973 11.00000 0.03798 0.04193 = 0.03224 0.00983 0.01144 0.00766 AFIX 43 H7 2 0.109281 0.521697 1.168167 11.00000 -1.20000 AFIX 0 C11 1 0.293867 0.410177 0.444268 11.00000 0.03820 0.03359 = 0.03161 0.00791 0.00944 0.01019 AFIX 43 H11 2 0.222198 0.422971 0.485064 11.00000 -1.20000 AFIX 0 C14 1 0.156238 0.134721 0.585903 11.00000 0.03334 0.02934 = 0.02980 0.00667 0.00548 0.00869 C8 1 0.165585 0.683252 1.094582 11.00000 0.03849 0.03622 = 0.03374 0.00175 0.00978 0.00904 AFIX 43 H8 2 0.132202 0.754584 1.132006 11.00000 -1.20000 AFIX 0 C17 1 -0.008115 -0.040374 0.774528 11.00000 0.04440 0.03977 = 0.03810 0.00866 0.01991 0.00977 AFIX 43 H17 2 -0.054262 -0.014639 0.825735 11.00000 -1.20000 AFIX 0 C18 1 0.015570 -0.178213 0.756432 11.00000 0.03858 0.03487 = 0.04171 0.01358 0.01234 0.00476 AFIX 43 H18 2 -0.014496 -0.247759 0.794876 11.00000 -1.20000 AFIX 0 C3 1 0.521799 -0.146503 0.797415 11.00000 0.05287 0.02791 = 0.05375 0.00630 0.00698 0.01181 AFIX 137 H3A 2 0.495315 -0.131993 0.858439 11.00000 -1.50000 H3B 2 0.631176 -0.166591 0.802887 11.00000 -1.50000 H3C 2 0.443578 -0.228194 0.759914 11.00000 -1.50000 AFIX 0 C2 1 0.563979 -0.011547 0.666745 11.00000 0.05846 0.05109 = 0.05045 0.00665 0.02201 0.02567 AFIX 137 H2A 2 0.512595 0.057446 0.634142 11.00000 -1.50000 H2B 2 0.530541 -0.107422 0.630384 11.00000 -1.50000 H2C 2 0.682051 0.019077 0.676347 11.00000 -1.50000 AFIX 0 C13 1 0.453034 0.506872 0.338090 11.00000 0.05799 0.04579 = 0.04611 0.01817 0.02306 0.01242 AFIX 137 H13A 2 0.504693 0.424583 0.348527 11.00000 -1.50000 H13B 2 0.536313 0.595507 0.348326 11.00000 -1.50000 H13C 2 0.392531 0.492385 0.274963 11.00000 -1.50000 AFIX 0 C12 1 0.289777 0.654877 0.415110 11.00000 0.05494 0.03126 = 0.06308 0.01271 0.01264 0.01532 AFIX 137 H12A 2 0.207765 0.645326 0.453748 11.00000 -1.50000 H12B 2 0.243159 0.680008 0.355874 11.00000 -1.50000 H12C 2 0.382665 0.730932 0.445248 11.00000 -1.50000 AFIX 0 HKLF 4 REM 5brsal_dmf_a.res in P-1 REM wR2 = 0.0617, GooF = S = 1.029, Restrained GooF = 1.029 for all data REM R1 = 0.0237 for 5097 Fo > 4sig(Fo) and 0.0285 for all 5813 data REM 297 parameters refined using 0 restraints END WGHT 0.0278 0.2966 REM Instructions for potential hydrogen bonds HTAB O8 O7 HTAB O2 O1 HTAB O6 O5 HTAB O4 O3 HTAB C1 O3 HTAB C11 O7 EQIV $1 -x, -y+1, -z+2 HTAB C8 O8_$1 EQIV $2 -x, -y, -z+2 HTAB C18 O4_$2 HTAB C3 Br2 EQIV $3 -x+1, -y, -z+1 HTAB C2 O5_$3 EQIV $4 -x+1, -y+1, -z+1 HTAB C13 O1_$4 REM Highest difference peak 0.331, deepest hole -0.457, 1-sigma level 0.054 Q1 1 0.2828 0.4217 0.9559 11.00000 0.05 0.33 Q2 1 0.1347 0.0770 0.6179 11.00000 0.05 0.30 ; _shelx_res_checksum 58821 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.24557(2) 0.90992(2) 0.99013(2) 0.04169(6) Uani d 1 . . Br Br2 0.11748(2) -0.40750(2) 0.65880(2) 0.04226(6) Uani d 1 . . O O1 0.45314(14) 0.20472(11) 0.75929(8) 0.0368(2) Uani d 1 . . O O5 0.33570(14) 0.29235(12) 0.43497(8) 0.0381(2) Uani d 1 . . O O7 0.13035(15) 0.25750(12) 0.59788(8) 0.0390(2) Uani d 1 . . O O8 0.00799(16) 0.19629(12) 0.73855(8) 0.0427(3) Uani d 1 . . H H8A 0.045021 0.249767 0.702559 0.064 Uiso calc 1 . . O O2 0.36799(14) 0.40506(11) 0.85473(8) 0.0367(2) Uani d 1 . . H H2 0.395224 0.335766 0.825995 0.055 Uiso calc 1 . . O O6 0.23087(14) 0.09168(11) 0.52209(7) 0.0361(2) Uani d 1 . . H H6 0.252385 0.158605 0.490892 0.054 Uiso calc 1 . . O O3 0.30139(15) 0.23840(12) 0.94363(8) 0.0427(3) Uani d 1 . . O O4 0.18671(16) 0.30712(13) 1.08632(8) 0.0435(3) Uani d 1 . . H H4 0.210778 0.251409 1.045891 0.065 Uiso calc 1 . . N N2 0.34281(16) 0.51893(14) 0.40096(9) 0.0355(3) Uani d 1 . . N N1 0.51487(16) -0.01708(14) 0.75441(9) 0.0351(3) Uani d 1 . . C C15 0.10489(16) 0.02410(15) 0.64352(9) 0.0275(3) Uani d 1 . . C C4 0.31245(17) 0.36294(15) 0.92582(10) 0.0314(3) Uani d 1 . . C C9 0.22763(18) 0.71811(15) 1.01831(10) 0.0316(3) Uani d 1 . . C C6 0.20164(18) 0.44069(16) 1.06202(10) 0.0320(3) Uani d 1 . . C C20 0.12885(16) -0.11631(15) 0.62580(10) 0.0298(3) Uani d 1 . . H H20 0.176193 -0.143184 0.575298 0.036 Uiso calc 1 . . C C19 0.08332(18) -0.21607(15) 0.68211(10) 0.0320(3) Uani d 1 . . C C5 0.26317(17) 0.47561(15) 0.98422(10) 0.0288(3) Uani d 1 . . C C1 0.46234(18) 0.09204(16) 0.79304(10) 0.0334(3) Uani d 1 . . H H1 0.429615 0.083668 0.850143 0.040 Uiso calc 1 . . C C10 0.27628(17) 0.61624(15) 0.96262(10) 0.0294(3) Uani d 1 . . H H10 0.318147 0.641357 0.910262 0.035 Uiso calc 1 . . C C16 0.03502(18) 0.06247(16) 0.71833(10) 0.0326(3) Uani d 1 . . C C7 0.15243(19) 0.54558(18) 1.11597(10) 0.0365(3) Uani d 1 . . H H7 0.109281 0.521697 1.168167 0.044 Uiso calc 1 . . C C11 0.29387(18) 0.41018(16) 0.44427(10) 0.0335(3) Uani d 1 . . H H11 0.222198 0.422971 0.485064 0.040 Uiso calc 1 . . C C14 0.15624(17) 0.13472(16) 0.58590(10) 0.0304(3) Uani d 1 . . C C8 0.16558(19) 0.68325(17) 1.09458(10) 0.0359(3) Uani d 1 . . H H8 0.132202 0.754584 1.132006 0.043 Uiso calc 1 . . C C17 -0.0081(2) -0.04037(18) 0.77453(11) 0.0389(3) Uani d 1 . . H H17 -0.054262 -0.014639 0.825735 0.047 Uiso calc 1 . . C C18 0.01557(19) -0.17821(17) 0.75643(11) 0.0376(3) Uani d 1 . . H H18 -0.014496 -0.247759 0.794876 0.045 Uiso calc 1 . . C C3 0.5218(2) -0.14650(17) 0.79741(13) 0.0447(4) Uani d 1 . . H H3A 0.495315 -0.131993 0.858439 0.067 Uiso calc 1 . . H H3B 0.631176 -0.166591 0.802887 0.067 Uiso calc 1 . . H H3C 0.443578 -0.228194 0.759914 0.067 Uiso calc 1 . . C C2 0.5640(2) -0.0115(2) 0.66674(13) 0.0501(4) Uani d 1 . . H H2A 0.512595 0.057446 0.634142 0.075 Uiso calc 1 . . H H2B 0.530541 -0.107422 0.630384 0.075 Uiso calc 1 . . H H2C 0.682051 0.019077 0.676347 0.075 Uiso calc 1 . . C C13 0.4530(2) 0.5069(2) 0.33809(12) 0.0473(4) Uani d 1 . . H H13A 0.504693 0.424583 0.348527 0.071 Uiso calc 1 . . H H13B 0.536313 0.595507 0.348326 0.071 Uiso calc 1 . . H H13C 0.392531 0.492385 0.274963 0.071 Uiso calc 1 . . C C12 0.2898(2) 0.65488(19) 0.41511(14) 0.0483(4) Uani d 1 . . H H12A 0.207765 0.645326 0.453748 0.072 Uiso calc 1 . . H H12B 0.243159 0.680008 0.355874 0.072 Uiso calc 1 . . H H12C 0.382665 0.730932 0.445248 0.072 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 0.05939(11) 0.02360(8) 0.04263(9) 0.00900(7) 0.01085(7) 0.00440(6) Br2 0.04500(10) 0.02475(8) 0.06018(11) 0.00816(6) 0.01501(7) 0.01047(7) O1 0.0456(6) 0.0282(5) 0.0401(6) 0.0120(4) 0.0120(5) 0.0063(4) O5 0.0508(6) 0.0318(6) 0.0395(6) 0.0148(5) 0.0187(5) 0.0121(4) O7 0.0547(7) 0.0282(5) 0.0427(6) 0.0173(5) 0.0189(5) 0.0121(4) O8 0.0576(7) 0.0332(6) 0.0481(7) 0.0199(5) 0.0268(6) 0.0090(5) O2 0.0504(6) 0.0259(5) 0.0393(6) 0.0106(5) 0.0187(5) 0.0075(4) O6 0.0508(6) 0.0301(6) 0.0344(5) 0.0143(5) 0.0180(5) 0.0105(4) O3 0.0594(7) 0.0264(6) 0.0497(7) 0.0137(5) 0.0215(6) 0.0126(5) O4 0.0571(7) 0.0355(6) 0.0477(7) 0.0146(5) 0.0223(6) 0.0217(5) N2 0.0399(7) 0.0316(7) 0.0380(7) 0.0100(5) 0.0099(5) 0.0099(5) N1 0.0381(7) 0.0295(6) 0.0389(7) 0.0101(5) 0.0074(5) 0.0044(5) C15 0.0270(6) 0.0269(7) 0.0297(7) 0.0072(5) 0.0055(5) 0.0059(5) C4 0.0328(7) 0.0271(7) 0.0353(7) 0.0058(5) 0.0082(6) 0.0070(5) C9 0.0353(7) 0.0250(7) 0.0337(7) 0.0048(5) 0.0052(6) 0.0050(5) C6 0.0321(7) 0.0317(7) 0.0344(7) 0.0063(5) 0.0079(6) 0.0125(6) C20 0.0293(7) 0.0278(7) 0.0327(7) 0.0056(5) 0.0070(5) 0.0047(5) C19 0.0326(7) 0.0243(7) 0.0393(8) 0.0056(5) 0.0066(6) 0.0062(6) C5 0.0297(7) 0.0258(7) 0.0315(7) 0.0049(5) 0.0061(5) 0.0072(5) C1 0.0349(7) 0.0287(7) 0.0356(7) 0.0063(6) 0.0060(6) 0.0022(6) C10 0.0324(7) 0.0250(7) 0.0306(7) 0.0026(5) 0.0071(5) 0.0066(5) C16 0.0332(7) 0.0312(7) 0.0356(7) 0.0098(6) 0.0093(6) 0.0052(6) C7 0.0380(8) 0.0419(9) 0.0322(7) 0.0077(6) 0.0114(6) 0.0098(6) C11 0.0382(8) 0.0336(8) 0.0316(7) 0.0102(6) 0.0094(6) 0.0079(6) C14 0.0333(7) 0.0293(7) 0.0298(7) 0.0087(5) 0.0055(5) 0.0067(5) C8 0.0385(8) 0.0362(8) 0.0337(7) 0.0090(6) 0.0098(6) 0.0018(6) C17 0.0444(9) 0.0398(9) 0.0381(8) 0.0098(7) 0.0199(7) 0.0087(6) C18 0.0386(8) 0.0349(8) 0.0417(8) 0.0048(6) 0.0123(6) 0.0136(6) C3 0.0529(10) 0.0279(8) 0.0538(10) 0.0118(7) 0.0070(8) 0.0063(7) C2 0.0585(11) 0.0511(11) 0.0504(10) 0.0257(9) 0.0220(9) 0.0067(8) C13 0.0580(11) 0.0458(10) 0.0461(9) 0.0124(8) 0.0231(8) 0.0182(8) C12 0.0549(10) 0.0313(9) 0.0631(11) 0.0153(7) 0.0126(9) 0.0127(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 C16 O8 H8A . . 109.5 ? C4 O2 H2 . . 109.5 ? C14 O6 H6 . . 109.5 ? C6 O4 H4 . . 109.5 ? C11 N2 C13 . . 120.83(13) ? C11 N2 C12 . . 121.35(14) ? C13 N2 C12 . . 117.82(14) ? C1 N1 C3 . . 121.27(14) ? C1 N1 C2 . . 120.51(14) ? C2 N1 C3 . . 118.21(14) ? C20 C15 C16 . . 119.67(13) ? C20 C15 C14 . . 120.93(13) ? C16 C15 C14 . . 119.38(13) ? O2 C4 C5 . . 115.34(12) ? O3 C4 O2 . . 122.88(14) ? O3 C4 C5 . . 121.78(13) ? C10 C9 Br1 . . 119.67(11) ? C10 C9 C8 . . 121.19(14) ? C8 C9 Br1 . . 119.14(11) ? O4 C6 C5 . . 122.19(14) ? O4 C6 C7 . . 118.17(13) ? C7 C6 C5 . . 119.64(14) ? C15 C20 H20 . . 120.2 ? C19 C20 C15 . . 119.56(13) ? C19 C20 H20 . . 120.2 ? C20 C19 Br2 . . 119.71(11) ? C20 C19 C18 . . 120.90(14) ? C18 C19 Br2 . . 119.38(11) ? C6 C5 C4 . . 119.55(13) ? C10 C5 C4 . . 120.86(13) ? C10 C5 C6 . . 119.59(13) ? O1 C1 N1 . . 124.04(15) ? O1 C1 H1 . . 118.0 ? N1 C1 H1 . . 118.0 ? C9 C10 C5 . . 119.18(13) ? C9 C10 H10 . . 120.4 ? C5 C10 H10 . . 120.4 ? O8 C16 C15 . . 122.35(14) ? O8 C16 C17 . . 118.25(13) ? C17 C16 C15 . . 119.40(14) ? C6 C7 H7 . . 119.7 ? C8 C7 C6 . . 120.56(14) ? C8 C7 H7 . . 119.7 ? O5 C11 N2 . . 123.98(14) ? O5 C11 H11 . . 118.0 ? N2 C11 H11 . . 118.0 ? O7 C14 O6 . . 123.02(13) ? O7 C14 C15 . . 122.06(13) ? O6 C14 C15 . . 114.92(12) ? C9 C8 H8 . . 120.1 ? C7 C8 C9 . . 119.82(14) ? C7 C8 H8 . . 120.1 ? C16 C17 H17 . . 119.7 ? C18 C17 C16 . . 120.50(14) ? C18 C17 H17 . . 119.7 ? C19 C18 H18 . . 120.0 ? C17 C18 C19 . . 119.96(14) ? C17 C18 H18 . . 120.0 ? N1 C3 H3A . . 109.5 ? N1 C3 H3B . . 109.5 ? N1 C3 H3C . . 109.5 ? H3A C3 H3B . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? N1 C2 H2A . . 109.5 ? N1 C2 H2B . . 109.5 ? N1 C2 H2C . . 109.5 ? H2A C2 H2B . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? N2 C13 H13A . . 109.5 ? N2 C13 H13B . . 109.5 ? N2 C13 H13C . . 109.5 ? H13A C13 H13B . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? N2 C12 H12A . . 109.5 ? N2 C12 H12B . . 109.5 ? N2 C12 H12C . . 109.5 ? H12A C12 H12B . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 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 C9 . 1.9009(14) ? Br2 C19 . 1.9036(14) ? O1 C1 . 1.2411(18) ? O5 C11 . 1.2391(18) ? O7 C14 . 1.2292(18) ? O8 H8A . 0.8400 ? O8 C16 . 1.3485(18) ? O2 H2 . 0.8400 ? O2 C4 . 1.3073(18) ? O6 H6 . 0.8400 ? O6 C14 . 1.3074(17) ? O3 C4 . 1.2321(18) ? O4 H4 . 0.8400 ? O4 C6 . 1.3480(18) ? N2 C11 . 1.3192(19) ? N2 C13 . 1.451(2) ? N2 C12 . 1.454(2) ? N1 C1 . 1.3224(19) ? N1 C3 . 1.453(2) ? N1 C2 . 1.447(2) ? C15 C20 . 1.394(2) ? C15 C16 . 1.402(2) ? C15 C14 . 1.4811(19) ? C4 C5 . 1.479(2) ? C9 C10 . 1.380(2) ? C9 C8 . 1.384(2) ? C6 C5 . 1.4029(19) ? C6 C7 . 1.388(2) ? C20 H20 . 0.9500 ? C20 C19 . 1.381(2) ? C19 C18 . 1.384(2) ? C5 C10 . 1.3985(19) ? C1 H1 . 0.9500 ? C10 H10 . 0.9500 ? C16 C17 . 1.395(2) ? C7 H7 . 0.9500 ? C7 C8 . 1.370(2) ? C11 H11 . 0.9500 ? C8 H8 . 0.9500 ? C17 H17 . 0.9500 ? C17 C18 . 1.370(2) ? C18 H18 . 0.9500 ? C3 H3A . 0.9800 ? C3 H3B . 0.9800 ? C3 H3C . 0.9800 ? C2 H2A . 0.9800 ? C2 H2B . 0.9800 ? C2 H2C . 0.9800 ? C13 H13A . 0.9800 ? C13 H13B . 0.9800 ? C13 H13C . 0.9800 ? C12 H12A . 0.9800 ? C12 H12B . 0.9800 ? C12 H12C . 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 O8 H8A O7 . 0.84 1.84 2.5786(16) 145.8 yes O2 H2 O1 . 0.84 1.71 2.5500(15) 174.5 yes O6 H6 O5 . 0.84 1.71 2.5381(15) 168.5 yes O4 H4 O3 . 0.84 1.83 2.5708(17) 145.8 yes C1 H1 O3 . 0.95 2.45 3.165(2) 132 yes C2 H2B O5 2_656 0.98 2.47 3.261(2) 137 yes C8 H8 O8 2_567 0.95 2.49 3.323(2) 146 yes C11 H11 O7 . 0.95 2.55 3.2248(19) 128 yes C18 H18 O4 2_557 0.95 2.54 3.354(2) 144 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Br1 C9 C10 C5 . . . . 179.73(11) ? Br1 C9 C8 C7 . . . . -179.77(12) ? Br2 C19 C18 C17 . . . . 179.33(13) ? O8 C16 C17 C18 . . . . 179.43(15) ? O2 C4 C5 C6 . . . . 179.84(13) ? O2 C4 C5 C10 . . . . 0.2(2) ? O3 C4 C5 C6 . . . . -0.2(2) ? O3 C4 C5 C10 . . . . -179.81(14) ? O4 C6 C5 C4 . . . . 0.6(2) ? O4 C6 C5 C10 . . . . -179.80(14) ? O4 C6 C7 C8 . . . . 179.72(14) ? C15 C20 C19 Br2 . . . . -179.47(11) ? C15 C20 C19 C18 . . . . -0.6(2) ? C15 C16 C17 C18 . . . . -0.8(2) ? C4 C5 C10 C9 . . . . 179.40(14) ? C6 C5 C10 C9 . . . . -0.2(2) ? C6 C7 C8 C9 . . . . 0.3(2) ? C20 C15 C16 O8 . . . . -179.60(14) ? C20 C15 C16 C17 . . . . 0.6(2) ? C20 C15 C14 O7 . . . . 176.93(14) ? C20 C15 C14 O6 . . . . -3.2(2) ? C20 C19 C18 C17 . . . . 0.4(2) ? C5 C6 C7 C8 . . . . -0.9(2) ? C10 C9 C8 C7 . . . . 0.3(2) ? C16 C15 C20 C19 . . . . 0.1(2) ? C16 C15 C14 O7 . . . . -4.7(2) ? C16 C15 C14 O6 . . . . 175.13(13) ? C16 C17 C18 C19 . . . . 0.2(3) ? C7 C6 C5 C4 . . . . -178.79(14) ? C7 C6 C5 C10 . . . . 0.9(2) ? C14 C15 C20 C19 . . . . 178.40(13) ? C14 C15 C16 O8 . . . . 2.0(2) ? C14 C15 C16 C17 . . . . -177.75(14) ? C8 C9 C10 C5 . . . . -0.3(2) ? C3 N1 C1 O1 . . . . -179.67(15) ? C2 N1 C1 O1 . . . . -1.0(2) ? C13 N2 C11 O5 . . . . -0.4(2) ? C12 N2 C11 O5 . . . . -179.75(16) ?