#------------------------------------------------------------------------------ #$Date: 2023-12-07 12:50:03 +0100 (Thu, 07 Dec 2023) $ #$Revision: 288138 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022868.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_2022868 loop_ _publ_author_name 'Sirenko, Valerii Y.' 'Naumova, Dina D.' 'Golenya, Irina A.' 'Shova, Sergiu' 'Gural'skiy, Il'ya A.' _publ_section_title ; Crystal structure of bis-(3-carb-oxy-1-methyl-pyrid-inium) octa-bromide. ; _journal_coeditor_code WM5697 _journal_issue 'Pt 11' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 977 _journal_page_last 981 _journal_paper_doi 10.1107/S2056989023008460 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac '2C7 H8 N O2 +, Br8 2-' _chemical_formula_moiety '2(C7 H8 N O2 +), Br8 2-' _chemical_formula_sum 'C14 H16 Br8 N2 O4' _chemical_formula_weight 915.522 _chemical_name_systematic ; Bis(3-carboxy-1-methylpyridinium) octabromide ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _cell_angle_alpha 95.746(5) _cell_angle_beta 91.156(4) _cell_angle_gamma 115.002(7) _cell_formula_units_Z 1 _cell_length_a 6.8537(5) _cell_length_b 7.0873(6) _cell_length_c 14.5145(6) _cell_measurement_reflns_used 2335 _cell_measurement_temperature 293 _cell_measurement_theta_max 23.7360 _cell_measurement_theta_min 3.1900 _cell_volume 634.23(8) _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_collection ; CrysAlisPro (Rigaku OD, 2021) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2021) ; _computing_molecular_graphics ; Olex2 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; olex2.refine (Bourhis et al., 2015) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015) ; _diffrn_ambient_temperature 293.00 _diffrn_detector_area_resol_mean 16.1593 _diffrn_measured_fraction_theta_full 0.9996 _diffrn_measured_fraction_theta_max 0.8636 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_unetI/netI 0.0665 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9457 _diffrn_reflns_theta_full 25.2417 _diffrn_reflns_theta_max 29.31 _diffrn_reflns_theta_min 2.83 _exptl_absorpt_coefficient_mu 12.666 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.45777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2021) ; _exptl_crystal_colour 'light red' _exptl_crystal_density_diffrn 2.397 _exptl_crystal_description block _exptl_crystal_F_000 424.594 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.3755 _refine_diff_density_min -1.3169 _refine_ls_extinction_coef 0.0112(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.0231 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 13 _refine_ls_number_parameters 132 _refine_ls_number_reflns 3008 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.0229 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0473 _refine_ls_shift/su_max -0.0014 _refine_ls_shift/su_mean 0.0001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0186P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.0748 _reflns_number_gt 1848 _reflns_number_total 3008 _reflns_threshold_expression I>=2u(I) _cod_data_source_file wm5697sup1.cif _cod_data_source_block I _cod_depositor_comments 'Adding full bibliography for 2022868.cif.' _cod_database_code 2022868 _cod_database_fobs_code 2022868 _shelx_hkl_file ; 0 0 2 6.22 1.63 0 0 2 10.55 1.95 0 0 -2 8.32 1.92 0 0 -2 5.12 1.47 0 0 2 8.43 1.72 0 0 -2 6.65 1.62 0 0 -2 8.28 1.61 0 0 3 13.23 2.42 0 0 3 15.00 3.09 0 0 -3 10.06 2.18 0 0 -3 14.41 2.94 0 0 3 9.00 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8.08 -7 5 -6 5.10 6.56 -7 5 -6 15.96 11.42 7 -5 6 13.88 8.05 -7 5 -7 42.45 13.66 -7 5 -7 61.21 17.49 7 -5 7 50.79 16.33 7 -5 8 7.54 6.37 -7 5 -8 2.24 5.74 7 -5 8 6.57 9.93 -7 5 -8 -4.10 8.95 7 -5 9 16.96 9.85 -7 5 -9 0.88 6.63 7 -5 9 6.03 8.00 -7 5 -9 8.15 7.11 7 -5 10 24.29 9.37 -7 5 -10 17.57 8.53 7 -5 10 32.52 13.04 -7 5 -11 38.77 12.58 7 -4 -12 15.13 10.99 7 -4 -11 4.85 7.61 7 -4 -10 14.49 8.44 7 -4 -10 20.91 11.79 -7 4 10 23.50 9.48 7 -4 -9 -8.42 8.58 7 -4 -9 14.10 9.23 -7 4 9 2.51 5.54 -7 4 8 3.13 5.32 7 -4 -8 7.77 7.59 7 -4 -8 0.19 6.11 -7 4 7 -2.12 5.20 7 -4 -7 -13.23 7.88 -7 4 6 2.84 5.68 7 -4 -6 -6.19 9.42 7 -4 -6 3.04 5.36 -7 4 5 57.65 14.97 7 -4 -5 43.12 12.95 7 -4 -5 66.27 15.93 -7 4 4 32.83 11.23 7 -4 -4 47.52 13.62 7 -4 -4 19.05 6.34 -7 4 3 33.57 11.88 7 -4 -3 2.63 7.36 7 -4 -3 25.50 11.94 -7 4 2 -10.42 8.32 7 -4 -2 3.21 4.83 -7 4 1 -2.05 6.75 7 -4 -1 5.75 5.57 7 -4 -1 2.11 8.57 -7 4 0 14.05 9.17 7 -4 0 5.10 6.06 7 -4 0 2.65 6.36 -7 4 -1 52.37 13.83 -7 4 -1 54.51 13.31 7 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9.56 -7 3 6 16.11 7.26 7 -3 -5 51.74 13.67 7 -3 -5 29.02 10.66 -7 3 5 47.46 11.03 7 -3 -4 53.04 13.09 7 -3 -4 68.54 15.66 7 -3 -4 61.26 13.87 -7 3 4 66.42 14.69 7 -3 -3 18.19 9.09 7 -3 -3 11.70 5.96 7 -3 -3 18.50 8.66 -7 3 3 19.79 9.10 7 -3 -2 -6.17 6.20 7 -3 -2 -0.38 4.36 7 -3 -2 -1.76 3.96 -7 3 2 -5.23 7.84 -7 3 1 -3.73 4.74 7 -3 -1 -10.70 9.84 7 -3 -1 9.99 7.09 -7 3 0 27.19 10.18 7 -3 0 15.23 8.37 7 -3 0 12.46 5.67 -7 3 -1 10.04 7.22 7 -3 1 14.68 7.79 7 -3 1 11.68 6.07 7 -3 2 55.72 15.25 7 -3 2 18.97 6.04 -7 3 -2 33.05 11.78 -7 3 -3 87.83 17.35 7 -3 3 97.82 19.23 -7 3 -3 75.26 15.36 -7 3 -4 24.38 12.29 7 -3 4 14.16 9.55 -7 3 -4 6.41 9.01 -7 3 -5 17.73 9.62 7 -3 5 3.86 5.97 -7 3 -5 2.48 5.43 -7 3 -6 13.87 8.52 7 -3 6 -2.23 6.13 -7 3 -6 7.18 7.41 7 -3 7 39.92 11.80 -7 3 -7 60.00 16.38 7 -3 7 47.92 14.38 -7 3 -7 62.22 13.93 7 -3 8 25.93 9.56 -7 3 -8 31.13 14.55 7 -3 8 5.69 5.16 -7 3 -8 21.43 8.68 7 -3 9 -0.15 6.04 -7 3 -9 4.35 9.56 7 -3 9 -12.01 6.86 -7 3 -9 18.13 9.19 7 -3 10 38.50 11.95 -7 3 -10 42.00 16.00 -7 3 -10 30.69 9.72 7 -3 10 44.62 14.10 -7 3 -11 -1.89 4.13 7 -2 -11 0.91 5.32 7 -2 -11 -5.90 6.70 -7 2 11 7.70 6.30 7 -2 -10 1.48 5.09 7 -2 -10 6.32 7.61 7 -2 -10 9.91 8.06 -7 2 10 10.21 6.79 7 -2 -9 7.12 7.30 7 -2 -9 6.94 8.09 7 -2 -9 -7.30 8.88 -7 2 9 -1.68 4.77 7 -2 -8 0.74 5.28 7 -2 -8 5.28 6.33 7 -2 -8 -16.47 11.17 -7 2 8 -13.22 9.22 7 -2 -7 1.49 5.10 7 -2 -7 -11.13 8.40 7 -2 -7 5.14 6.42 -7 2 7 -0.39 5.36 7 -2 -6 11.95 8.32 7 -2 -6 1.42 5.46 7 -2 -6 -5.74 7.91 -7 2 6 7.14 7.16 7 -2 -5 91.03 17.93 7 -2 -5 71.44 14.50 7 -2 -5 62.48 13.67 -7 2 5 83.79 16.24 7 -2 -4 10.25 7.90 7 -2 -4 -0.50 4.20 -7 2 4 4.89 6.71 7 -2 -3 33.57 11.41 7 -2 -3 29.00 9.15 -7 2 3 52.49 12.68 7 -2 -2 7.03 6.47 7 -2 -2 12.97 6.74 -7 2 2 12.14 8.40 7 -2 -1 15.06 7.87 7 -2 -1 3.37 4.30 -7 2 1 13.17 7.92 7 -2 0 49.99 13.49 7 -2 0 45.11 9.69 -7 2 0 50.73 12.73 7 -2 1 29.38 11.70 7 -2 1 11.53 5.06 -7 2 -1 27.17 9.89 7 -2 2 59.09 14.56 -7 2 -2 63.32 15.45 7 -2 3 128.17 21.71 -7 2 -3 82.37 15.54 7 -2 4 18.21 10.70 -7 2 -4 6.60 6.29 7 -2 5 19.39 10.24 -7 2 -5 6.80 6.39 7 -2 6 5.21 5.16 7 -2 6 16.02 7.86 -7 2 -6 18.66 8.51 7 -2 7 2.51 5.24 7 -2 7 15.80 7.97 -7 2 -7 25.67 13.61 -7 2 -7 22.46 10.91 7 -2 8 31.63 11.09 7 -2 8 16.75 8.06 -7 2 -8 44.86 16.17 -7 2 -8 20.38 8.60 7 -2 9 1.27 5.98 -7 2 -9 3.91 8.28 7 -2 9 3.37 6.41 -7 2 -9 24.16 9.62 7 -2 10 20.73 9.00 -7 2 -10 33.43 9.96 -7 2 -11 17.46 8.16 7 -1 -11 11.35 8.36 -7 1 11 -2.94 4.57 -7 1 10 10.98 7.65 7 -1 -10 7.72 5.97 -7 1 10 11.17 6.89 7 -1 -10 7.29 7.04 7 -1 -9 10.51 8.13 -7 1 9 0.93 7.45 7 -1 -9 6.50 8.48 -7 1 9 -2.80 6.57 7 -1 -8 -2.60 5.11 -7 1 8 13.38 8.91 7 -1 -8 0.15 5.30 -7 1 8 -8.68 7.15 7 -1 -7 4.38 6.96 -7 1 7 3.87 5.63 7 -1 -6 2.38 6.17 -7 1 6 11.36 7.66 7 -1 -6 22.52 10.51 7 -1 -5 55.54 12.88 -7 1 5 69.27 14.51 7 -1 -5 82.65 16.71 7 -1 -4 -8.24 7.12 -7 1 4 -5.24 7.39 7 -1 -4 -5.06 5.42 7 -1 -3 15.48 7.90 -7 1 3 5.93 6.36 7 -1 -3 7.71 8.66 7 -1 -2 0.24 4.15 -7 1 2 -5.09 6.58 7 -1 -1 13.63 8.10 -7 1 1 0.31 4.19 7 -1 0 30.44 11.07 -7 1 0 32.18 10.12 -7 1 -1 17.34 8.35 7 -1 1 30.65 11.75 -7 1 -2 111.74 18.79 7 -1 2 124.94 20.72 -7 1 -3 16.11 6.93 7 -1 3 36.46 13.40 -7 1 -4 7.36 6.29 7 -1 4 2.15 7.04 7 -1 5 4.51 7.10 -7 1 -5 -1.79 5.28 7 -1 5 12.76 8.78 7 -1 6 12.56 7.37 -7 1 -6 3.83 6.01 7 -1 7 -3.64 5.35 7 -1 7 7.36 9.55 -7 1 -7 -6.34 7.60 7 -1 8 -0.57 4.68 7 -1 8 7.18 7.60 -7 1 -8 -4.20 5.50 7 -1 9 7.66 8.37 7 -1 9 4.49 6.18 -7 1 -9 -3.23 4.71 -7 1 -10 42.72 11.64 7 0 -12 2.05 7.06 -7 0 11 27.80 10.82 7 0 -11 -10.23 6.60 -7 0 10 -1.36 6.19 -7 0 10 1.33 5.71 7 0 -10 0.63 4.76 -7 0 9 13.84 13.56 -7 0 9 2.61 6.67 7 0 -9 -20.47 11.44 7 0 -9 14.00 8.97 -7 0 8 -3.57 6.63 -7 0 8 -0.36 4.80 -7 0 7 9.70 7.73 -7 0 7 0.31 6.64 -7 0 6 7.60 7.37 -7 0 6 0.77 5.53 -7 0 5 24.03 9.14 -7 0 5 27.77 10.37 -7 0 4 8.04 5.21 -7 0 4 4.21 5.70 -7 0 3 49.00 13.81 -7 0 2 2.29 6.00 -7 0 1 -6.28 5.37 -7 0 0 28.95 10.64 -7 0 -1 -3.86 5.68 -7 0 -2 75.84 16.44 7 0 3 11.85 7.39 -7 0 -3 27.30 10.70 7 0 4 -1.56 4.63 -7 0 -4 -9.16 7.27 7 0 5 3.76 4.50 -7 0 -5 4.81 5.83 7 0 6 7.38 7.67 -7 0 -6 -0.99 5.44 7 0 6 14.17 9.29 7 0 7 9.38 5.19 -7 0 -7 4.48 6.32 7 0 7 5.39 6.53 -7 0 -8 24.78 9.53 7 0 8 38.80 13.03 7 0 8 21.08 8.92 -7 0 -9 31.30 10.50 7 0 9 31.39 12.65 -7 0 -10 13.86 7.54 -7 -1 10 4.49 6.69 -7 -1 9 7.65 8.67 7 1 -9 7.80 5.22 -7 -1 9 -8.33 7.97 -7 -1 8 18.83 10.41 7 1 -8 13.02 10.16 -7 -1 8 5.21 5.08 -7 -1 7 6.84 8.52 -7 -1 7 14.03 8.26 -7 -1 6 -2.16 5.39 -7 -1 6 -5.90 8.05 -7 -1 5 26.32 9.77 -7 -1 5 27.42 11.15 -7 -1 4 14.59 7.65 -7 -1 4 -9.71 7.07 -7 -1 3 -1.70 4.65 -7 -1 3 1.75 8.53 -7 -1 2 -2.48 5.98 -7 -1 1 -2.41 7.41 -7 -1 0 3.78 5.86 7 1 1 3.77 4.73 -7 -1 -1 2.77 6.54 7 1 2 25.72 8.25 -7 -1 -2 31.54 10.61 7 1 3 11.93 6.74 -7 -1 -3 19.31 10.47 7 1 4 13.29 7.01 -7 -1 -4 19.54 9.56 7 1 5 1.98 5.25 -7 -1 -5 7.45 6.61 7 1 6 11.52 7.38 -7 -1 -6 9.23 7.35 7 1 6 6.13 5.26 7 1 7 7.73 7.32 -7 -2 8 1.99 6.61 -7 -2 7 -0.98 5.76 -8 7 -2 24.82 10.60 -8 7 -3 8.21 9.07 -8 7 -4 1.15 7.69 -8 7 -5 -16.89 11.95 -8 6 6 35.72 13.70 -8 6 5 -7.31 8.71 8 -6 -5 12.85 9.66 -8 6 4 16.40 11.55 8 -6 -4 23.74 11.71 -8 6 3 4.05 8.54 8 -6 -3 1.71 5.52 8 -6 -3 -3.16 8.68 -8 6 2 1.32 8.96 8 -6 -2 -7.39 9.39 8 -6 -2 2.75 7.28 8 -6 -1 -0.17 7.30 -8 6 1 4.29 7.37 8 -6 -1 -3.52 7.00 8 -6 0 5.66 9.17 -8 6 0 -3.50 8.48 8 -6 0 -0.33 6.01 -8 6 0 7.34 6.95 8 -6 1 32.45 13.40 -8 6 -1 39.45 15.10 8 -6 1 62.17 16.38 -8 6 -1 31.37 11.46 8 -6 2 16.13 11.11 -8 6 -2 12.10 10.10 -8 6 -2 11.66 6.91 -8 6 -3 27.05 12.28 8 -6 3 3.22 7.49 -8 6 -3 24.21 10.82 -8 6 -4 -2.12 8.37 8 -6 4 9.83 10.32 -8 6 -4 18.41 10.33 8 -6 5 12.93 10.95 -8 6 -5 8.12 8.01 -8 6 -6 10.20 9.53 -8 5 9 -9.88 7.54 8 -5 -9 10.88 8.64 -8 5 8 11.99 8.94 8 -5 -8 4.80 8.32 -8 5 7 11.59 7.46 8 -5 -7 2.31 7.48 8 -5 -7 27.54 12.20 -8 5 6 9.67 7.35 8 -5 -6 26.55 12.94 8 -5 -6 11.64 8.96 -8 5 5 -5.49 8.06 8 -5 -5 27.37 13.50 8 -5 -5 18.99 12.65 -8 5 4 13.09 8.39 8 -5 -4 15.33 9.96 8 -5 -4 15.17 11.08 -8 5 3 -6.44 7.15 8 -5 -3 4.24 7.69 8 -5 -3 10.30 10.19 -8 5 2 24.59 13.01 8 -5 -2 18.57 10.65 8 -5 -2 7.58 7.57 -8 5 1 -8.36 8.94 8 -5 -1 11.38 9.93 8 -5 -1 3.69 9.76 -8 5 0 3.91 7.00 8 -5 0 7.14 9.71 8 -5 0 -5.16 8.45 -8 5 -1 47.18 14.58 8 -5 1 50.08 17.24 -8 5 -1 53.36 13.99 -8 5 -2 13.54 10.87 8 -5 2 8.03 9.32 -8 5 -2 19.90 10.50 -8 5 -3 8.18 10.31 8 -5 3 -13.77 10.38 -8 5 -3 -3.80 6.10 -8 5 -4 -11.58 7.91 8 -5 4 -0.48 7.40 -8 5 -4 8.99 8.43 -8 5 -5 11.29 8.12 -8 5 -5 30.31 12.54 8 -5 5 5.40 8.54 -8 5 -6 -3.68 6.83 -8 5 -6 -14.08 11.10 8 -5 6 -8.01 8.10 -8 5 -7 7.58 7.25 8 -5 7 26.54 14.77 -8 5 -8 46.12 15.02 8 -5 8 24.88 12.28 8 -5 9 15.84 11.92 8 -4 -10 -6.66 7.82 -8 4 10 -7.16 6.17 8 -4 -9 -6.31 7.67 8 -4 -9 -10.90 8.75 -8 4 9 -4.25 5.41 8 -4 -8 2.93 5.16 8 -4 -8 -6.59 8.10 -8 4 8 3.87 7.44 8 -4 -7 3.96 6.97 8 -4 -7 3.56 6.66 -8 4 7 4.27 7.30 8 -4 -6 33.39 13.39 8 -4 -6 27.23 12.97 -8 4 6 16.14 9.22 8 -4 -5 15.67 10.26 8 -4 -5 7.49 7.79 -8 4 5 26.05 11.47 8 -4 -4 6.34 7.05 8 -4 -4 -8.75 10.36 -8 4 4 14.56 9.95 -8 4 3 14.17 10.75 8 -4 -3 8.24 7.16 8 -4 -3 9.92 8.51 8 -4 -3 -8.97 6.79 -8 4 2 -5.18 9.54 8 -4 -2 -8.37 8.67 8 -4 -2 -22.79 13.02 8 -4 -2 -0.57 6.00 -8 4 1 3.96 5.43 8 -4 -1 24.40 12.47 8 -4 -1 12.68 7.79 -8 4 0 0.65 5.80 8 -4 0 1.08 6.67 -8 4 -1 50.43 14.50 8 -4 1 72.17 17.84 -8 4 -2 8.25 9.60 8 -4 2 -1.32 7.52 -8 4 -3 14.41 9.86 8 -4 3 18.46 10.90 -8 4 -4 2.67 10.09 -8 4 -4 18.22 11.42 8 -4 4 -6.43 8.24 -8 4 -5 17.16 9.50 8 -4 5 11.81 8.04 -8 4 -5 26.83 10.78 -8 4 -6 16.23 11.55 8 -4 6 -18.83 11.48 -8 4 -6 -9.92 8.67 8 -4 7 -5.90 9.28 -8 4 -7 19.40 12.19 8 -4 8 22.51 11.56 -8 4 -8 19.82 9.58 8 -4 9 10.56 12.00 -8 4 -9 6.28 8.12 8 -3 -10 0.60 6.24 8 -3 -10 -2.37 9.41 -8 3 10 22.33 10.06 8 -3 -9 2.53 6.52 8 -3 -9 0.68 7.62 -8 3 9 10.21 10.76 8 -3 -8 0.44 5.06 8 -3 -8 -3.59 6.49 8 -3 -8 5.63 9.83 -8 3 8 9.68 8.12 8 -3 -7 3.23 6.33 8 -3 -7 -1.21 7.91 8 -3 -7 22.43 7.98 -8 3 7 11.70 7.74 8 -3 -6 -4.62 7.32 8 -3 -6 15.42 9.51 8 -3 -6 1.72 7.45 -8 3 6 6.26 5.63 8 -3 -5 5.38 6.31 8 -3 -5 20.55 11.81 8 -3 -5 14.25 10.53 -8 3 5 9.86 8.15 8 -3 -4 11.26 8.96 8 -3 -4 -11.12 8.13 -8 3 4 -7.69 6.45 8 -3 -3 8.66 9.06 8 -3 -3 -2.56 5.14 -8 3 3 16.76 10.77 8 -3 -2 -8.13 8.97 8 -3 -2 -2.79 4.30 -8 3 2 14.58 8.52 8 -3 -1 17.95 10.38 8 -3 -1 10.29 5.72 -8 3 1 11.26 8.54 8 -3 0 11.86 7.30 -8 3 0 28.53 12.15 8 -3 1 78.87 18.17 -8 3 -1 60.49 15.78 8 -3 2 7.83 7.80 -8 3 -2 -0.17 5.06 8 -3 3 -6.30 8.24 -8 3 -3 -9.43 9.00 8 -3 4 3.15 7.01 -8 3 -4 -10.58 8.05 8 -3 5 20.20 11.91 -8 3 -5 9.40 7.98 8 -3 6 9.07 7.77 -8 3 -6 -2.72 5.87 8 -3 7 -14.88 9.51 -8 3 -7 9.04 6.13 8 -3 8 46.65 15.19 -8 3 -8 39.53 12.92 8 -3 9 -18.62 10.95 -8 3 -9 5.35 7.94 8 -2 -10 -7.92 7.95 -8 2 10 -1.52 6.24 8 -2 -9 -15.52 8.88 -8 2 9 -3.43 6.34 8 -2 -8 -3.21 6.40 -8 2 8 1.02 4.34 8 -2 -7 11.74 8.89 8 -2 -7 17.25 11.40 -8 2 7 22.93 10.10 8 -2 -6 -2.25 6.58 8 -2 -6 14.91 9.97 -8 2 6 5.87 6.68 8 -2 -5 27.70 12.22 8 -2 -5 12.32 8.10 -8 2 5 15.05 9.85 8 -2 -4 10.48 8.54 8 -2 -4 -1.48 5.32 -8 2 4 -1.21 7.99 8 -2 -3 9.05 7.26 8 -2 -3 5.35 5.34 -8 2 3 3.60 6.05 8 -2 -2 5.45 7.68 8 -2 -2 12.23 7.08 -8 2 2 -0.99 6.54 8 -2 -1 19.78 10.85 8 -2 -1 -0.13 4.47 -8 2 1 5.83 7.56 8 -2 0 23.62 11.66 -8 2 0 26.23 11.49 8 -2 1 53.84 15.32 -8 2 -1 19.20 10.51 8 -2 2 21.46 11.08 -8 2 -2 -6.92 6.59 8 -2 3 2.93 5.81 -8 2 -3 -1.85 7.39 8 -2 4 1.34 7.92 -8 2 -4 3.32 6.05 8 -2 5 24.74 11.20 8 -2 5 24.29 11.55 -8 2 -5 51.06 14.15 8 -2 6 8.99 7.63 -8 2 -6 1.40 7.19 8 -2 7 -17.28 10.22 -8 2 -7 4.68 8.10 8 -2 8 12.02 8.37 -8 1 7 2.77 7.84 8 -1 -7 22.63 11.64 -8 1 7 10.87 8.67 8 -1 -6 0.18 6.93 -8 1 6 -0.32 6.82 8 -1 -6 10.62 8.10 -8 1 5 31.92 13.12 8 -1 -5 13.52 9.27 -8 1 4 19.34 11.92 8 -1 -4 -1.35 6.01 -8 1 3 -2.82 6.20 8 -1 -3 19.76 10.63 -8 1 2 3.79 6.67 8 -1 -2 17.79 10.41 -8 1 1 1.70 6.88 8 -1 -1 16.89 9.64 -8 1 0 43.49 14.93 8 -1 0 21.92 10.98 -8 1 -1 19.29 9.60 8 -1 1 11.63 10.53 -8 1 -2 22.41 12.12 8 -1 2 24.82 11.67 -8 1 -3 -6.29 8.24 8 -1 3 10.02 8.88 8 -1 4 16.26 11.73 8 -1 4 16.95 9.56 8 -1 5 -0.04 5.07 -8 0 7 9.29 7.26 -8 0 6 -1.60 7.08 -8 0 5 2.00 5.35 -8 0 4 -2.47 5.42 8 0 2 3.84 5.06 8 0 3 -0.88 4.94 8 0 4 11.38 7.20 9 -5 -4 2.99 6.16 9 -4 -5 18.12 10.94 9 -4 -4 0.20 6.13 9 -3 -5 -6.60 7.22 9 -3 -4 -3.98 6.11 0 0 0 0.00 0.00 TITL shI_5164_IgFr_auto in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 6.853741 7.087260 14.514541 95.7462 91.1555 115.0016 ZERR 3.00 0.000455 0.000586 0.000566 0.0047 0.0042 0.0072 LATT 1 SFAC C H N O Br Pb UNIT 18.00 24.00 3.00 6.00 6.00 3.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 46070 _shelx_res_file ; TITL shi_5164_igfr_auto_a.res in P-1 shi_5164_igfr_auto.res created by SHELXL-2018/3 at 15:55:24 on 14-Jun-2023 REM Old TITL shI_5164_IgFr_auto in P-1 REM SHELXT solution in P-1: R1 0.187, Rweak 0.025, Alpha 0.050 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C7 N2 O Br4 CELL 0.71073 6.8537 7.0873 14.5145 95.746 91.156 115.002 ZERR 1 0.0005 0.0006 0.0006 0.005 0.004 0.007 LATT 1 SFAC C H Br N O UNIT 14 16 8 2 4 EQIV $1 -X,-Y,-Z EQIV $2 1-X,1-Y,1-Z DFIX 0.85 O1 H1 L.S. 20 PLAN 6 SIZE 0.17 0.11 0.06 TEMP 19.85 CONF BIND Br3 Br4 BIND Br1 Br1_$2 BIND Br4 Br4_$1 BOND list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.018600 EXTI 0.011088 FVAR 0.41986 BR2 3 0.067453 0.459166 0.305153 11.00000 0.05155 0.04178 = 0.05931 0.00758 0.00149 0.01851 BR3 3 -0.181674 0.439796 0.152101 11.00000 0.06869 0.07724 = 0.05125 0.00131 -0.00807 0.04128 BR1 3 0.296879 0.476612 0.436794 11.00000 0.07880 0.05301 = 0.06621 0.00194 -0.02235 0.02656 BR4 3 -0.047548 0.122525 0.046133 11.00000 0.07795 0.07176 = 0.05924 0.01402 -0.02006 0.00693 O1 5 0.913730 0.887450 0.382124 11.00000 0.05614 0.07683 = 0.04655 -0.00108 -0.01047 0.04159 O2 5 0.789468 1.061265 0.483856 11.00000 0.05698 0.07197 = 0.03567 -0.01233 -0.00687 0.03551 N1 4 0.459521 0.821851 0.181092 11.00000 0.03889 0.04592 = 0.03518 -0.00019 -0.00414 0.01464 C2 1 0.629729 0.959715 0.331377 11.00000 0.02890 0.03977 = 0.03202 0.00605 -0.00301 0.01177 C6 1 0.787311 0.973596 0.406217 11.00000 0.03811 0.04445 = 0.04846 0.00478 -0.00200 0.02071 C1 1 0.603450 0.834158 0.248768 11.00000 0.03506 0.04520 = 0.04324 0.00417 -0.00228 0.01429 AFIX 43 H1A 2 0.685057 0.758027 0.239789 11.00000 -1.20000 AFIX 0 C4 1 0.364695 1.058151 0.273030 11.00000 0.04841 0.05260 = 0.05119 0.00401 -0.00186 0.03188 AFIX 43 H4 2 0.282856 1.134418 0.280155 11.00000 -1.20000 AFIX 0 C5 1 0.342142 0.930540 0.192779 11.00000 0.04512 0.06292 = 0.04091 0.00912 -0.00657 0.02353 AFIX 43 H5 2 0.243026 0.919298 0.145413 11.00000 -1.20000 AFIX 0 C3 1 0.509265 1.072557 0.342935 11.00000 0.04742 0.04416 = 0.03915 0.00233 0.00061 0.01851 AFIX 43 H3 2 0.525837 1.158505 0.398084 11.00000 -1.20000 AFIX 0 C7 1 0.427886 0.681621 0.094250 11.00000 0.07275 0.07708 = 0.04111 -0.01992 -0.01815 0.03417 AFIX 137 H7A 2 0.508370 0.600249 0.100281 11.00000 -1.50000 H7B 2 0.477346 0.763988 0.043741 11.00000 -1.50000 H7C 2 0.277369 0.589438 0.082258 11.00000 -1.50000 AFIX 0 H1 2 0.992055 0.879164 0.425612 11.00000 -1.50000 HKLF 4 REM shi_5164_igfr_auto_a.res in P-1 REM wR2 = 0.0740, GooF = S = 1.012, Restrained GooF = 1.012 for all data REM R1 = 0.0470 for 1848 Fo > 4sig(Fo) and 0.0968 for all 3008 data REM 132 parameters refined using 1 restraints END WGHT 0.0186 0.0000 REM Highest difference peak 0.543, deepest hole -0.474, 1-sigma level 0.105 Q1 1 0.0264 0.0739 0.0819 11.00000 0.05 0.53 Q2 1 0.1370 0.2190 0.1471 11.00000 0.05 0.44 Q3 1 -0.0479 0.3168 0.3200 11.00000 0.05 0.42 Q4 1 -0.1049 0.0313 -0.0263 11.00000 0.05 0.41 Q5 1 -0.1075 0.5630 0.1270 11.00000 0.05 0.38 Q6 1 -0.2978 0.4590 0.1145 11.00000 0.05 0.38 ; _shelx_res_checksum 51912 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -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_occupancy Br Br2 0.06745(8) 0.45917(8) 0.30515(3) 0.05120(19) Uani 1.000000 Br Br3 -0.18168(9) 0.43980(10) 0.15210(3) 0.0628(2) Uani 1.000000 Br Br1 0.29688(10) 0.47662(9) 0.43679(4) 0.0673(2) Uani 1.000000 Br Br4 -0.04755(10) 0.12253(10) 0.04613(3) 0.0781(3) Uani 1.000000 O O1 0.9137(6) 0.8874(6) 0.3821(2) 0.0564(10) Uani 1.000000 O O2 0.7895(5) 1.0613(5) 0.4839(2) 0.0540(10) Uani 1.000000 N N1 0.4595(6) 0.8218(6) 0.1811(2) 0.0420(10) Uani 1.000000 C C2 0.6297(7) 0.9597(7) 0.3314(3) 0.0348(12) Uani 1.000000 C C6 0.7873(8) 0.9736(8) 0.4062(3) 0.0430(13) Uani 1.000000 C C1 0.6035(7) 0.8341(7) 0.2488(3) 0.0423(13) Uani 1.000000 H H1a 0.6851(7) 0.7580(7) 0.2398(3) 0.0507(15) Uiso 1.000000 C C4 0.3646(8) 1.0582(8) 0.2730(3) 0.0477(13) Uani 1.000000 H H4 0.2828(8) 1.1345(8) 0.2802(3) 0.0572(16) Uiso 1.000000 C C5 0.3421(8) 0.9306(8) 0.1928(3) 0.0497(14) Uani 1.000000 H H5 0.2430(8) 0.9193(8) 0.1454(3) 0.0597(17) Uiso 1.000000 C C3 0.5093(8) 1.0726(8) 0.3430(3) 0.0444(13) Uani 1.000000 H H3 0.5259(8) 1.1585(8) 0.3981(3) 0.0533(16) Uiso 1.000000 C C7 0.4279(8) 0.6816(8) 0.0942(3) 0.0660(17) Uani 1.000000 H H7a 0.508(4) 0.600(4) 0.1002(9) 0.099(3) Uiso 1.000000 H H7b 0.2774(10) 0.589(4) 0.0823(13) 0.099(3) Uiso 1.000000 H H7c 0.477(5) 0.7640(9) 0.0437(5) 0.099(3) Uiso 1.000000 H H1 0.992(7) 0.879(9) 0.426(3) 0.099(3) Uiso 1.000000 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 Br2 0.0515(4) 0.0417(3) 0.0592(3) 0.0185(3) 0.0015(2) 0.0076(2) Br3 0.0686(4) 0.0771(5) 0.0512(3) 0.0412(3) -0.0081(3) 0.0013(3) Br1 0.0787(5) 0.0529(4) 0.0661(4) 0.0265(3) -0.0223(3) 0.0019(3) Br4 0.0779(5) 0.0717(5) 0.0592(4) 0.0069(4) -0.0200(3) 0.0140(3) O1 0.057(3) 0.077(3) 0.047(2) 0.042(2) -0.0104(17) -0.0010(19) O2 0.057(2) 0.072(3) 0.0359(18) 0.036(2) -0.0069(15) -0.0123(17) N1 0.039(3) 0.046(3) 0.036(2) 0.015(2) -0.0041(18) -0.0001(19) C2 0.029(3) 0.040(3) 0.032(2) 0.012(2) -0.0030(19) 0.006(2) C6 0.038(3) 0.045(3) 0.049(3) 0.021(3) -0.002(2) 0.005(3) C1 0.035(3) 0.045(3) 0.043(3) 0.014(2) -0.002(2) 0.004(2) C4 0.049(3) 0.053(3) 0.051(3) 0.032(3) -0.002(2) 0.004(3) C5 0.045(3) 0.063(4) 0.041(3) 0.024(3) -0.007(2) 0.009(3) C3 0.048(3) 0.044(3) 0.039(3) 0.019(3) 0.001(2) 0.002(2) C7 0.074(4) 0.078(4) 0.041(3) 0.034(3) -0.018(3) -0.020(3) loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Br 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090 41.43280 2.95570 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' -0.38188 2.46625 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' C 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870 51.65120 0.21560 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' 0.00313 0.00162 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' H 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236 57.79970 0.00304 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' N 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750 0.58260 -11.52900 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' 0.00612 0.00332 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' O 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390 32.90890 0.25080 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' 0.01085 0.00610 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 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 Br1 Br2 Br3 . . 178.04(3) ? Br4 Br3 Br2 . . 90.37(2) ? Br1 Br1 Br2 2_666 . 162.42(4) ? Br4 Br4 Br3 2 . 176.22(3) ? H1 O1 C6 . . 116(4) ? C5 N1 C1 . . 120.7(4) ? C7 N1 C1 . . 119.4(4) ? C7 N1 C5 . . 119.8(4) ? C1 C2 C6 . . 120.3(5) ? C3 C2 C6 . . 120.6(4) ? C3 C2 C1 . . 119.2(4) ? O2 C6 O1 . . 125.2(4) ? C2 C6 O1 . . 114.6(4) ? C2 C6 O2 . . 120.1(5) ? C2 C1 N1 . . 120.0(5) ? H1a C1 N1 . . 120.0(3) ? H1a C1 C2 . . 120.0(3) ? C5 C4 H4 . . 120.4(3) ? C3 C4 H4 . . 120.4(3) ? C3 C4 C5 . . 119.2(5) ? C4 C5 N1 . . 121.2(4) ? H5 C5 N1 . . 119.4(3) ? H5 C5 C4 . . 119.4(3) ? C4 C3 C2 . . 119.8(4) ? H3 C3 C2 . . 120.1(3) ? H3 C3 C4 . . 120.1(3) ? H7a C7 N1 . . 109.5 ? H7b C7 N1 . . 109.5 ? H7b C7 H7a . . 109.5 ? H7c C7 N1 . . 109.5 ? H7c C7 H7a . . 109.5 ? H7c C7 H7b . . 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 Br2 Br3 . 2.7307(7) ? Br2 Br1 . 2.4095(7) ? Br3 Br4 . 3.0625(10) ? Br1 Br1 2_666 3.1813(12) ? Br4 Br4 2 2.4002(15) ? O1 C6 . 1.290(6) ? O1 H1 . 0.845(19) ? O2 C6 . 1.228(5) ? N1 C1 . 1.348(5) ? N1 C5 . 1.332(6) ? N1 C7 . 1.476(5) ? C2 C6 . 1.483(6) ? C2 C1 . 1.380(6) ? C2 C3 . 1.373(6) ? C1 H1a . 0.9300 ? C4 H4 . 0.9300 ? C4 C5 . 1.365(6) ? C4 C3 . 1.370(6) ? C5 H5 . 0.9300 ? C3 H3 . 0.9300 ? C7 H7a . 0.9600 ? C7 H7b . 0.9600 ? C7 H7c . 0.9600 ? 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 O1 H1 O2 2_776 0.80(7) 1.89(7) 2.668(5) 164(7) yes C1 H1A Br3 1_655 0.93 2.96 3.838(5) 158.1 yes C5 H5 Br4 2_565 0.93 2.99 3.881(5) 160.0 yes C7 H7A Br3 1_655 0.96 2.92 3.857(6) 166.0 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 O1 C6 C2 C1 . . . . 9.9(5) ? O1 C6 C2 C3 . . . . -169.6(4) ? O2 C6 C2 C1 . . . . -169.9(4) ? O2 C6 C2 C3 . . . . 10.6(5) ? N1 C1 C2 C6 . . . . 179.8(4) ? N1 C1 C2 C3 . . . . -0.6(5) ? N1 C5 C4 C3 . . . . -0.7(6) ? C2 C3 C4 C5 . . . . 0.3(5) ?