#------------------------------------------------------------------------------ #$Date: 2024-07-13 04:57:40 +0300 (Sat, 13 Jul 2024) $ #$Revision: 293406 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312553.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_2312553 loop_ _publ_author_name 'Qin, Qiaoqi' 'Liu, Jiamin' 'Luan, Xinyu' 'Xu, Jianqiao' 'Jiang, Long' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of two iHOFs based on CH...NC hydrogen bonding. ; _journal_coeditor_code JX3084 _journal_issue 8 _journal_name_full 'Acta crystallographica. Section C, Structural chemistry' _journal_paper_doi 10.1107/S2053229624005850 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C14 H10 N3 +, Br -' _chemical_formula_moiety 'C14 H10 N3 +, Br -' _chemical_formula_sum 'C14 H10 Br N3' _chemical_formula_weight 300.16 _chemical_name_systematic ; 4-Cyano-N-(4-cyanobenzyl)pyridinium bromide ; _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7734(4) _cell_length_b 7.0554(3) _cell_length_c 19.7544(10) _cell_measurement_reflns_used 6776 _cell_measurement_temperature 150.00 _cell_measurement_theta_max 59.421 _cell_measurement_theta_min 3.893 _cell_volume 1222.79(10) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX2 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) and Mercury (Macrae et al., 2020) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150.00 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON III' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34138 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_unetI/netI 0.0229 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 15238 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 59.421 _diffrn_reflns_theta_min 3.894 _diffrn_source MetalJet _diffrn_source_current 3.57 _diffrn_source_power 0.24947160000000 _diffrn_source_voltage 69.88 _exptl_absorpt_coefficient_mu 2.936 _exptl_absorpt_correction_T_max 0.7516 _exptl_absorpt_correction_T_min 0.6572 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2016) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.630 _exptl_crystal_description block _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.827 _refine_diff_density_min -0.586 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 97 _refine_ls_number_reflns 1461 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0282 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+1.2992P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.0687 _reflns_number_gt 1245 _reflns_number_total 1461 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jx3084sup1.cif _cod_data_source_block iHOFI _cod_database_code 2312553 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.758 _shelx_estimated_absorpt_t_max 0.867 _shelx_hkl_file ; 0 1 0 0.10 0.50 0 -1 0 -0.20 3.70 0 1 0 -5.10 4.30 0 -1 0 0.20 2.20 0 1 0 4.20 3.80 0 1 0 -0.40 0.60 0 -1 0 -2.30 5.30 0 1 0 0.60 4.80 0 -1 0 0.20 0.50 0 -1 0 0.30 1.20 0 1 0 0.10 0.80 0 -1 0 0.60 1.20 0 2 0 7541.85 261.97 0 2 0 7270.67 259.87 0 -2 0 7640.54 279.17 0 2 0 7443.76 272.87 0 -2 0 7315.17 262.17 0 -3 0 -4.70 14.50 0 3 0 0.60 1.50 0 -3 0 -0.70 2.10 0 3 0 5.40 9.40 0 -3 0 1.80 2.50 0 -3 0 6.30 6.10 0 -3 0 10.40 24.10 0 3 0 12.10 16.70 0 3 0 4.10 8.90 0 -3 0 -0.30 0.90 0 -4 0 4241.78 145.79 0 4 0 4098.19 193.48 0 4 0 3945.51 162.68 0 -4 0 4402.96 165.08 0 4 0 4458.05 167.18 0 -4 0 4041.70 215.18 0 -4 0 4302.57 146.09 0 4 0 4400.36 144.49 0 -5 0 -3.60 2.80 0 5 0 -8.80 21.50 0 5 0 -34.80 16.20 0 -5 0 -5.70 12.50 0 -5 0 10.70 23.40 0 -5 0 0.00 4.00 0 6 0 5036.30 206.88 0 -6 0 5075.59 174.48 0 -6 0 4960.10 172.38 0 7 0 0.80 2.70 0 7 0 -45.90 74.69 0 8 0 594.84 23.90 0 9 0 -2.90 3.00 -1 0 0 -3.90 6.90 -1 0 0 -1.10 0.70 1 0 0 -1.90 1.80 -1 0 0 -5.00 4.80 1 0 0 0.10 0.30 1 0 0 -0.40 0.40 1 0 0 0.30 0.40 1 0 0 1.80 2.90 -1 -1 0 -4.20 4.40 1 1 0 2.80 4.20 1 -1 0 0.30 0.50 1 1 0 0.30 0.70 1 -1 0 -3.10 8.10 -1 -1 0 -0.90 0.90 1 1 0 -1.60 4.50 1 -1 0 0.40 4.90 1 1 0 2.00 6.40 1 -1 0 1.90 5.40 -1 1 0 -10.30 7.20 -1 -1 0 2.80 5.80 1 -1 0 0.80 0.60 -1 1 0 -5.30 4.10 -1 1 0 -0.90 0.90 -1 1 0 0.30 0.70 1 1 0 0.30 0.70 -1 -1 0 -2.60 4.90 -1 1 0 -0.40 3.00 -1 2 0 0.30 1.00 1 -2 0 -10.30 15.80 1 -2 0 -0.40 0.80 -1 2 0 2.00 1.40 1 -2 0 1.90 1.50 1 -2 0 -0.20 1.10 1 2 0 1.20 0.90 -1 -2 0 -4.80 5.00 -1 2 0 -9.70 4.50 1 2 0 6.30 7.70 1 2 0 14.30 11.10 -1 -2 0 -1.10 1.90 -1 -2 0 0.40 1.10 -1 -2 0 -1.70 4.80 1 2 0 0.80 8.60 -1 -2 0 0.40 1.20 -1 2 0 -1.00 7.30 1 -2 0 2.40 5.90 1 2 0 -1.30 1.00 1 -2 0 -14.00 9.30 -1 2 0 2.50 10.40 -1 3 0 9.50 8.40 -1 -3 0 -4.60 6.20 -1 3 0 12.10 8.70 -1 3 0 -25.70 15.30 1 3 0 -4.40 9.80 1 -3 0 4.60 21.80 1 3 0 -1.80 28.50 -1 -3 0 0.30 1.20 -1 -3 0 4.10 20.80 -1 -3 0 -0.10 1.50 1 -3 0 -6.70 14.50 1 -3 0 -5.40 7.30 -1 3 0 -3.40 1.50 1 -3 0 1.30 0.90 1 3 0 0.20 1.20 1 3 0 1.60 0.90 -1 -3 0 -15.40 13.80 -1 3 0 0.40 1.20 -1 -4 0 -2.10 1.40 -1 -4 0 -1.50 10.70 -1 -4 0 -4.00 2.30 1 -4 0 0.30 1.10 -1 4 0 16.60 20.40 -1 4 0 0.60 1.40 1 4 0 -0.10 1.20 1 4 0 -20.10 34.50 -1 4 0 2.10 1.70 1 4 0 -0.90 15.20 1 -4 0 -16.90 53.59 -1 4 0 0.50 32.00 -1 -4 0 63.59 46.40 -1 4 0 -2.90 10.60 -1 -4 0 34.60 43.20 1 4 0 -4.30 13.10 1 -4 0 3.90 2.80 1 -4 0 -5.60 3.00 1 -4 0 -1.40 9.50 -1 -5 0 -10.70 23.40 1 -5 0 9.10 23.90 1 -5 0 -4.20 4.20 1 -5 0 0.60 3.00 1 5 0 25.10 21.70 -1 5 0 -0.50 2.10 -1 -5 0 0.10 1.70 -1 5 0 5.70 14.40 -1 -5 0 -7.00 16.40 -1 5 0 22.30 20.10 -1 -5 0 4.10 3.60 1 5 0 22.30 27.70 1 6 0 0.30 2.10 1 -6 0 -3.00 3.30 1 -6 0 1.70 6.20 1 6 0 -0.50 33.30 -1 -6 0 -1.20 2.30 -1 6 0 -10.40 22.80 -1 6 0 -2.20 2.50 -1 7 0 3.10 2.50 1 7 0 -59.59 69.49 1 7 0 0.30 2.50 1 -7 0 5.50 3.50 1 -7 0 -2.00 4.40 -1 7 0 -16.40 55.29 1 8 0 -1.10 3.30 -1 8 0 -0.30 3.10 -1 9 0 -6.80 5.30 1 9 0 -4.70 3.10 2 0 0 113.19 4.30 -2 0 0 114.19 5.00 -2 0 0 124.39 30.70 2 0 0 103.79 9.30 2 0 0 107.99 4.20 2 0 0 109.29 4.40 2 0 0 129.99 12.20 -2 0 0 103.59 16.70 2 0 0 123.49 10.00 -2 1 0 2740.53 124.49 2 -1 0 2539.95 129.89 -2 -1 0 2732.13 114.89 -2 1 0 2884.91 97.49 -2 -1 0 2795.92 102.39 -2 -1 0 2693.03 93.49 2 -1 0 2638.84 100.49 -2 1 0 2840.12 98.39 -2 -1 0 3024.50 102.59 -2 1 0 2548.45 93.09 2 -1 0 2980.40 99.49 -2 1 0 2708.83 93.49 2 1 0 2719.03 102.39 2 1 0 2728.63 100.39 2 1 0 2600.94 116.89 2 2 0 3706.73 157.88 -2 -2 0 3730.83 139.59 2 -2 0 3669.33 174.88 2 -2 0 3700.63 125.79 2 -2 0 3688.03 136.59 2 2 0 3736.03 125.69 -2 -2 0 3785.92 136.29 2 -2 0 3707.33 125.59 -2 -2 0 3815.32 158.48 2 2 0 3740.43 139.29 -2 2 0 3803.22 134.39 2 -2 0 3637.94 140.19 -2 2 0 3737.13 132.69 -2 2 0 3561.04 125.79 -2 -2 0 3594.14 125.99 -2 2 0 3830.52 161.08 -2 -3 0 599.24 35.10 2 -3 0 618.74 37.40 -2 3 0 638.24 22.40 2 -3 0 612.94 22.00 2 -3 0 547.15 79.19 -2 3 0 654.23 34.40 2 -3 0 591.84 22.20 -2 -3 0 613.24 61.79 -2 -3 0 574.24 46.70 2 3 0 648.24 36.90 2 3 0 579.04 59.79 2 3 0 603.04 21.70 2 3 0 620.14 39.10 -2 3 0 597.24 31.70 -2 3 0 549.25 56.49 -2 -3 0 574.44 21.80 -2 3 0 600.14 21.50 2 -3 0 620.44 54.99 2 4 0 1061.29 61.29 2 -4 0 941.41 35.20 -2 4 0 999.20 50.69 2 4 0 961.20 57.19 -2 -4 0 1008.30 56.99 2 4 0 1042.90 35.70 2 -4 0 1104.09 143.69 2 4 0 936.71 100.29 2 -4 0 988.60 37.00 -2 4 0 1045.80 36.60 2 -4 0 1044.20 37.20 -2 -4 0 1009.30 35.90 -2 -4 0 920.31 109.79 -2 4 0 1063.29 52.89 2 -5 0 795.82 67.99 -2 5 0 941.01 58.59 -2 -5 0 1005.30 35.30 -2 5 0 1021.50 36.00 2 5 0 836.42 73.99 2 5 0 953.50 69.99 2 -5 0 1001.50 37.90 -2 5 0 1024.10 57.89 2 -5 0 992.10 37.10 2 5 0 971.60 34.60 -2 -5 0 825.42 69.49 2 5 0 1030.90 35.50 -2 6 0 0.90 2.80 2 6 0 -0.50 2.00 2 -6 0 -2.40 8.00 -2 -6 0 -0.80 2.60 2 -6 0 4.40 4.20 2 6 0 39.50 41.60 -2 6 0 -6.60 23.90 -2 7 0 680.83 71.79 -2 7 0 514.45 20.80 2 7 0 506.55 21.10 2 7 0 558.74 92.89 2 -7 0 504.25 23.80 2 -8 0 327.67 18.30 2 8 0 293.27 14.00 -2 8 0 308.67 14.00 3 0 0 -1.30 0.80 -3 0 0 -2.80 13.10 3 0 0 -0.20 4.90 3 0 0 0.80 0.70 3 0 0 -0.20 6.10 -3 0 0 1.40 23.60 3 0 0 -0.50 4.60 3 0 0 0.20 0.90 3 0 0 0.70 6.20 -3 0 0 -1.20 1.60 3 -1 0 3.90 9.00 3 1 0 -2.60 16.50 3 1 0 -0.60 0.90 -3 -1 0 -7.30 8.30 -3 1 0 -5.20 16.50 3 1 0 1.40 1.20 3 -1 0 0.10 0.80 -3 -1 0 -2.90 2.60 3 -1 0 8.20 5.20 3 1 0 1.70 0.90 -3 -1 0 1.70 1.70 -3 -1 0 -11.90 12.10 3 -1 0 32.70 33.00 3 -1 0 0.80 0.90 3 1 0 1.10 6.60 -3 1 0 -0.60 1.20 3 -2 0 -2.30 6.20 3 2 0 -0.90 17.00 3 -2 0 19.00 18.50 -3 -2 0 5.30 10.10 3 2 0 -0.30 1.00 -3 2 0 -5.70 4.10 -3 2 0 1.90 1.30 -3 2 0 -0.40 1.50 -3 -2 0 -1.10 5.50 -3 -2 0 5.50 21.10 -3 2 0 1.90 5.40 3 2 0 0.30 1.10 3 2 0 3.00 9.50 3 -2 0 15.00 33.10 3 2 0 -5.60 5.10 -3 -2 0 1.20 1.50 3 -2 0 0.40 1.00 -3 2 0 16.10 21.60 3 2 0 0.30 1.10 3 -3 0 3.10 10.30 3 -3 0 -28.80 49.70 3 3 0 -8.10 10.80 -3 3 0 -4.20 5.40 3 3 0 -1.00 1.10 -3 -3 0 0.50 1.50 -3 -3 0 -2.90 14.50 -3 3 0 3.10 7.80 3 3 0 0.40 1.00 3 3 0 -4.20 29.10 3 -3 0 -0.20 1.60 -3 -3 0 14.90 32.10 3 3 0 -0.50 12.10 -3 3 0 -1.00 1.70 3 3 0 -0.40 1.20 -3 -3 0 -9.80 18.50 3 -3 0 1.20 1.50 3 4 0 -0.50 1.40 -3 4 0 34.80 47.50 3 4 0 0.00 1.30 3 -4 0 -15.40 18.40 -3 -4 0 1.70 1.80 3 4 0 -20.60 17.50 -3 4 0 1.90 8.90 3 4 0 -18.80 61.09 -3 4 0 8.10 11.00 3 -4 0 66.89 91.69 3 -4 0 3.00 3.60 -3 4 0 1.00 2.40 3 4 0 2.80 20.50 3 -4 0 0.10 1.40 -3 -4 0 8.10 13.00 3 -4 0 2.10 3.30 -3 -4 0 -20.60 58.69 3 5 0 14.00 29.60 3 5 0 2.10 2.00 -3 -5 0 -0.50 2.10 3 5 0 8.80 42.20 -3 5 0 40.50 28.20 3 5 0 2.10 1.60 3 -5 0 -6.00 6.80 3 -5 0 -7.10 3.40 -3 5 0 -1.30 2.40 3 -5 0 -38.10 41.20 -3 5 0 -7.80 11.90 3 6 0 44.70 50.69 -3 6 0 1.70 3.50 3 -6 0 -2.60 14.40 -3 6 0 -2.60 32.80 3 6 0 1.00 2.40 3 -6 0 -2.20 3.60 3 7 0 61.19 153.28 -3 7 0 55.59 100.99 3 -8 0 -5.40 6.30 3 8 0 -0.60 2.80 -3 8 0 0.70 3.70 -4 0 0 751.32 66.39 4 0 0 727.23 36.80 4 0 0 718.53 39.90 4 0 0 657.33 38.20 -4 0 0 875.31 89.49 4 0 0 721.63 25.60 4 0 0 694.53 25.20 -4 0 0 793.32 27.60 4 0 0 733.83 25.50 4 1 0 644.54 23.40 4 1 0 689.53 23.70 4 1 0 693.63 40.00 -4 1 0 662.43 24.10 4 1 0 684.83 23.50 4 -1 0 684.43 34.50 4 1 0 613.94 35.60 4 -1 0 670.13 23.50 -4 -1 0 662.73 61.19 4 -1 0 649.34 43.40 -4 1 0 614.14 62.79 4 -1 0 674.13 23.40 -4 -2 0 1393.56 46.90 4 -2 0 1164.08 130.39 4 -2 0 1298.57 45.80 4 -2 0 1318.67 45.60 4 -2 0 1373.56 61.59 4 2 0 1371.16 63.39 -4 -2 0 1242.28 93.59 4 2 0 1413.56 108.49 -4 2 0 1347.47 46.60 4 2 0 1325.57 45.70 -4 2 0 1309.07 45.90 4 2 0 1324.27 65.99 -4 2 0 1241.28 118.19 -4 -2 0 1216.28 68.69 -4 -2 0 1344.07 61.09 4 2 0 1299.47 45.90 4 -3 0 1265.97 44.30 4 3 0 1210.18 44.00 -4 3 0 1304.17 44.90 -4 -3 0 1151.08 115.29 -4 -3 0 1350.96 64.69 4 3 0 1305.97 44.10 4 -3 0 1295.07 44.00 4 3 0 1255.57 123.19 4 3 0 1250.17 69.69 4 3 0 1103.29 63.49 4 -3 0 1217.18 66.19 -4 -3 0 1300.27 44.80 -4 3 0 1261.97 55.49 -4 3 0 1196.08 53.99 4 3 0 1257.17 43.60 4 4 0 897.71 31.70 4 4 0 847.32 65.29 -4 4 0 916.61 33.10 4 4 0 852.21 67.79 4 -4 0 902.51 33.10 -4 4 0 810.42 48.20 4 -4 0 922.71 32.90 4 4 0 867.61 32.00 4 -4 0 897.21 68.19 4 -4 0 843.62 31.70 -4 -4 0 880.91 32.50 -4 4 0 922.01 46.70 -4 5 0 329.47 33.00 4 5 0 299.37 12.30 -4 5 0 307.37 14.10 -4 -5 0 284.47 13.30 4 5 0 314.57 13.10 4 5 0 244.78 49.70 4 -5 0 315.87 15.60 4 -5 0 290.07 18.20 -4 6 0 274.37 13.30 4 6 0 289.47 12.70 4 -6 0 255.87 15.10 -4 6 0 211.18 35.40 4 6 0 197.18 88.19 4 -6 0 258.37 24.50 -4 7 0 171.58 9.20 4 -7 0 209.08 13.80 -4 7 0 159.18 10.00 4 7 0 174.78 10.30 4 -7 0 188.18 18.30 4 -8 0 256.37 15.50 4 8 0 260.67 12.00 -5 0 0 -1.80 2.40 5 0 0 0.30 1.10 5 0 0 -0.10 1.10 5 0 0 7.00 13.50 5 0 0 -7.60 6.70 5 0 0 -0.20 1.00 5 0 0 -21.60 42.80 -5 0 0 5.50 38.00 5 0 0 -10.30 7.10 5 -1 0 1.30 1.20 -5 -1 0 7.80 39.20 5 1 0 -0.50 7.20 5 -1 0 -12.50 11.30 5 1 0 -6.70 11.80 5 1 0 -4.50 13.20 5 -1 0 -12.00 11.00 5 1 0 -1.00 1.10 5 -1 0 8.40 11.20 -5 -1 0 95.69 65.79 -5 -1 0 -3.70 2.10 5 1 0 -0.30 1.00 5 1 0 9.50 12.10 5 1 0 0.00 1.10 -5 1 0 -55.59 55.89 -5 1 0 -0.70 1.70 -5 2 0 -2.30 1.70 -5 -2 0 72.39 51.99 5 -2 0 2.70 16.20 5 2 0 -92.79 63.09 5 -2 0 -0.20 1.30 -5 2 0 -8.50 50.09 5 2 0 0.60 1.30 5 -2 0 -0.80 1.20 5 2 0 -0.80 1.20 -5 -2 0 -0.50 2.10 5 2 0 6.60 17.70 5 2 0 -0.50 1.20 5 2 0 11.30 14.60 -5 3 0 9.80 11.50 5 -3 0 -7.00 28.10 -5 3 0 -0.70 2.40 5 -3 0 1.30 1.90 5 3 0 -0.30 1.30 5 3 0 -1.60 11.60 -5 -3 0 17.00 24.00 5 -3 0 -0.40 1.70 5 3 0 32.70 29.20 -5 -3 0 -0.20 10.30 5 3 0 -0.50 1.40 -5 -3 0 1.20 2.50 5 3 0 0.50 1.50 5 3 0 4.60 18.80 5 -4 0 -3.40 2.90 5 -4 0 -0.30 2.10 5 4 0 3.00 30.10 -5 -4 0 -1.20 2.70 -5 4 0 0.30 2.70 5 4 0 2.20 2.10 5 -4 0 -43.50 57.19 5 -4 0 3.10 3.10 5 4 0 -0.10 1.70 5 -5 0 1.80 5.10 5 5 0 99.19 59.29 5 -6 0 7.20 5.20 -5 6 0 4.00 3.50 5 6 0 0.70 2.70 5 -6 0 2.40 16.80 5 -7 0 -10.30 10.00 5 -7 0 4.70 5.60 -5 7 0 5.60 3.50 5 8 0 -4.40 2.90 5 -8 0 0.20 5.80 6 0 0 325.37 13.10 6 0 0 313.67 43.20 6 0 0 366.36 15.20 6 0 0 322.07 38.90 6 0 0 309.77 34.30 6 1 0 657.73 23.50 6 -1 0 645.14 23.20 6 1 0 615.64 44.20 6 1 0 613.74 53.89 -6 1 0 671.13 24.50 6 -1 0 638.34 48.10 6 1 0 573.84 24.50 6 -1 0 659.73 23.40 6 1 0 626.14 49.90 6 -1 0 676.83 54.89 6 -1 0 600.44 46.10 6 1 0 648.44 23.20 6 -2 0 574.14 21.80 6 2 0 613.24 21.60 6 2 0 612.14 57.79 6 2 0 590.54 22.00 6 2 0 591.24 21.70 6 2 0 579.04 56.29 6 -2 0 541.55 60.39 -6 2 0 599.84 23.10 -6 -2 0 608.94 23.90 6 2 0 500.85 43.70 6 -2 0 590.64 21.70 6 3 0 274.97 11.30 -6 3 0 278.07 13.10 6 -3 0 284.47 12.20 6 3 0 278.67 11.70 -6 -3 0 292.47 13.70 6 -3 0 281.87 12.40 6 3 0 298.07 12.00 6 -3 0 306.67 63.29 6 4 0 420.26 16.40 6 4 0 389.96 72.59 -6 4 0 412.56 18.10 6 -4 0 437.56 18.20 6 -4 0 394.16 17.10 6 4 0 405.96 16.60 6 -4 0 431.16 18.40 -6 -4 0 397.66 18.00 6 -5 0 256.27 14.80 6 5 0 236.58 11.60 -6 5 0 276.47 13.60 6 -5 0 260.07 25.60 -6 6 0 137.09 10.70 6 6 0 162.78 8.90 6 -6 0 166.08 21.70 6 -6 0 190.48 15.30 6 7 0 123.69 7.80 6 -7 0 154.68 17.00 -6 7 0 135.39 8.70 6 -7 0 146.79 12.40 7 0 0 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292.67 25.00 2 0 1 281.57 9.90 -2 0 1 284.37 10.60 -2 0 -1 193.98 40.80 -2 0 1 239.18 35.10 2 0 1 273.77 10.00 2 0 -1 272.97 10.00 2 0 -1 290.17 10.00 -2 0 -1 284.87 10.60 2 0 1 267.17 9.70 2 0 -1 281.07 10.10 2 1 1 961.80 34.10 -2 1 -1 1008.90 58.49 2 1 1 1010.60 55.79 2 1 1 1025.10 43.90 2 1 1 944.71 34.00 2 -1 -1 1019.10 34.10 -2 1 -1 998.90 34.40 2 -1 -1 1060.69 41.10 -2 -1 1 982.80 40.90 -2 -1 1 998.80 43.50 2 -1 -1 983.90 71.19 -2 1 -1 1050.89 37.70 2 -1 -1 999.10 42.90 -2 -1 1 962.60 55.29 2 1 1 985.10 34.30 2 1 1 1061.29 42.00 -2 -1 1 965.40 34.40 2 -1 -1 954.90 34.10 -2 1 -1 1053.19 38.50 -2 -1 -1 1030.10 53.89 2 -1 1 983.00 41.10 -2 1 1 1107.49 68.09 2 1 -1 962.80 34.10 -2 1 1 1061.09 40.60 -2 -1 -1 964.20 43.00 2 -1 1 954.50 33.90 2 -1 1 1057.39 39.50 2 1 -1 961.40 34.20 -2 -1 -1 971.40 40.60 -2 1 1 1006.70 39.20 2 -1 1 960.90 34.00 -2 -1 -1 967.30 34.50 2 1 -1 1014.40 41.40 -2 1 1 978.80 34.40 2 1 -1 977.80 34.20 2 -2 -1 1923.91 76.09 2 2 1 1918.21 75.49 2 2 1 1861.71 64.29 2 2 1 1870.51 95.09 -2 2 -1 1896.11 64.69 2 -2 -1 1883.41 79.89 2 2 1 1881.31 64.49 2 -2 -1 1934.11 64.29 2 -2 -1 1911.01 64.49 2 -2 -1 1910.41 113.69 -2 2 -1 1878.61 69.79 -2 2 -1 1964.80 71.89 -2 -2 1 1977.30 94.99 -2 -2 1 1849.31 64.39 -2 -2 1 1843.62 77.39 -2 -2 1 1954.00 74.69 2 2 1 1856.91 77.89 -2 2 -1 1973.50 92.99 -2 2 1 1843.32 73.79 2 2 -1 1758.32 64.29 2 -2 1 1900.81 78.49 -2 -2 -1 1825.32 92.89 -2 2 1 1914.51 100.39 -2 -2 -1 1781.32 64.49 2 -2 1 1950.60 108.79 -2 2 1 1787.42 63.99 2 -2 1 1914.11 63.99 2 2 -1 1848.32 74.49 -2 2 1 1876.61 64.69 -2 2 1 1916.61 64.39 2 -2 1 2043.90 75.09 -2 -2 -1 1928.31 64.99 -2 2 1 1809.02 71.89 2 2 -1 1641.14 98.19 2 2 -1 1877.41 64.09 2 -2 1 1890.01 64.19 2 2 -1 1908.11 77.39 2 2 -1 1870.61 64.29 -2 -2 -1 1941.11 74.79 -2 -3 1 45.90 3.00 2 3 1 39.70 3.10 2 -3 -1 44.30 15.50 2 -3 -1 53.79 4.20 2 3 1 43.60 12.10 2 -3 -1 108.19 47.90 -2 3 -1 43.90 3.70 2 3 1 62.09 28.40 -2 3 -1 51.29 9.90 -2 -3 1 24.70 19.40 -2 3 -1 46.90 10.60 -2 -3 1 42.10 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-20 0.60 5.90 -2 2 20 2.70 3.10 2 -3 -20 180.08 10.80 2 3 20 165.48 10.10 2 3 20 184.48 9.90 2 -3 -20 185.78 11.30 -2 3 20 176.38 10.30 -2 3 20 184.28 10.80 -2 -3 -20 177.18 11.60 -2 -3 -20 178.78 12.40 2 4 20 3.30 3.40 2 -4 -20 -1.60 3.80 2 4 20 2.30 3.40 2 -4 -20 0.90 4.30 -2 4 20 5.00 4.20 -2 4 20 2.20 4.30 -2 -4 -20 0.10 4.30 -2 -4 -20 -2.90 5.00 2 -5 -20 63.59 8.90 2 5 20 57.99 6.70 2 5 20 76.89 6.50 2 -5 -20 62.49 7.60 -2 5 20 41.00 7.40 -2 -5 -20 75.39 7.90 -2 -5 -20 43.60 8.10 3 0 20 1.40 2.10 3 0 -20 2.20 3.60 3 -1 -20 36.50 6.40 3 1 20 46.60 6.80 3 1 -20 36.60 6.80 -3 -1 -20 48.70 10.00 -3 1 20 49.00 5.60 -3 -1 -20 33.90 10.30 3 2 20 -1.70 2.70 3 -2 -20 -1.80 3.20 3 2 20 -0.50 2.50 -3 -2 -20 4.10 4.90 -3 -2 -20 -2.30 4.00 -3 2 20 1.10 3.10 3 -3 -20 139.79 10.00 3 3 20 139.99 8.40 3 3 20 166.18 9.20 -3 -3 -20 143.69 10.90 -3 3 20 138.49 9.30 -3 3 20 147.49 9.80 -3 -3 -20 142.79 11.10 3 4 20 -5.60 2.90 3 -4 -20 4.70 4.70 3 -4 -20 1.00 3.90 3 4 20 -1.10 2.50 -3 4 20 3.20 4.10 -3 4 20 8.70 4.90 -3 -4 -20 1.90 4.20 -3 -4 -20 -1.90 4.50 3 -5 -20 19.70 6.50 3 5 20 7.90 4.50 3 -5 -20 17.00 4.80 3 5 20 13.40 3.80 -3 5 20 26.50 5.90 -3 -5 -20 15.20 5.20 4 0 20 28.20 3.50 4 0 -20 25.60 4.70 4 1 20 49.70 4.80 4 1 20 39.50 4.50 4 -1 -20 57.39 6.80 -4 1 20 55.49 5.70 4 1 -20 52.19 6.50 -4 -1 -20 57.29 8.00 4 -2 -20 67.09 7.30 4 2 20 49.70 5.00 4 2 20 48.60 4.80 -4 2 20 53.49 6.50 -4 -2 -20 60.89 8.00 4 3 20 27.90 4.10 4 -3 -20 15.30 4.60 4 3 20 12.30 5.10 -4 3 20 13.10 4.70 -4 -3 -20 21.30 6.20 -4 3 20 17.90 4.50 4 4 20 28.00 4.00 4 4 20 43.40 5.30 4 -4 -20 29.00 4.80 -4 4 20 33.70 5.70 -4 -4 -20 44.10 8.10 5 0 -20 30.00 5.20 5 0 20 27.90 3.50 5 -1 -20 6.50 3.90 5 1 20 5.80 2.60 5 -1 20 10.70 2.70 -5 -1 -20 -4.00 7.30 5 1 -20 5.60 5.00 -5 1 20 7.20 3.30 5 -2 -20 -0.70 5.20 5 2 20 12.50 2.70 -5 -2 -20 5.20 5.60 -5 2 20 4.30 5.70 5 3 20 0.80 2.40 5 3 20 -0.50 2.70 5 -3 -20 0.80 3.70 -5 -3 -20 1.30 4.80 -5 3 20 0.50 3.80 6 0 -20 65.59 6.50 6 0 20 60.39 4.60 6 1 20 22.20 3.10 6 -1 -20 24.10 4.60 -6 1 20 22.20 4.10 6 2 20 54.79 4.80 6 2 20 66.69 5.00 6 -2 -20 53.69 6.60 -6 -2 -20 38.90 7.60 -6 2 20 41.00 5.90 0 0 21 -0.30 2.30 0 0 -21 -2.60 3.20 0 1 21 82.39 7.30 0 -1 -21 88.89 9.20 0 2 21 -2.40 2.30 0 2 21 2.70 3.00 0 -2 -21 2.20 4.40 0 3 21 92.39 7.60 0 -3 -21 77.49 8.90 0 -3 -21 91.69 8.20 0 3 21 77.99 6.80 0 4 21 -2.40 3.40 0 -4 -21 -2.00 4.20 0 4 21 -3.50 5.30 0 -4 -21 7.10 4.40 0 -5 -21 31.10 5.90 0 5 21 35.50 5.40 0 -5 -21 20.00 4.90 1 0 21 2.30 3.00 -1 0 21 6.70 2.60 -1 0 -21 4.70 5.20 1 0 -21 7.10 6.10 -1 1 21 50.19 6.90 1 -2 -21 144.99 10.30 1 2 21 146.29 9.00 1 2 21 136.69 8.20 -1 -2 -21 131.69 12.40 -1 -2 -21 138.79 10.60 -1 2 21 136.29 8.80 1 3 21 60.09 6.40 1 -3 -21 38.80 7.60 1 -3 -21 60.49 7.90 1 3 21 52.49 5.90 -1 3 21 58.19 6.60 -1 3 21 61.39 6.80 -1 -3 -21 59.19 7.70 1 -4 -21 77.09 8.50 1 4 21 90.59 7.30 1 4 21 79.79 7.10 -1 4 21 74.79 7.60 -1 -4 -21 78.29 8.70 -1 4 21 90.29 8.20 -1 -4 -21 58.99 7.20 1 5 21 14.10 4.90 1 -5 -21 10.60 4.70 1 -5 -21 11.60 11.40 -1 -5 -21 7.30 4.70 -1 -5 -21 23.70 7.30 -2 0 -21 72.89 7.80 2 0 -21 80.59 7.40 2 0 21 78.69 5.90 2 -1 -21 2.00 4.00 2 1 21 9.80 3.20 2 1 21 4.40 2.50 -2 -1 -21 5.10 4.60 -2 1 21 5.50 3.00 2 -2 -21 58.59 7.40 2 2 21 62.09 5.50 2 2 21 48.90 5.60 -2 2 21 45.70 5.50 -2 -2 -21 59.19 8.10 -2 -2 -21 47.10 6.90 2 3 21 1.80 3.00 2 3 21 7.20 3.40 2 -3 -21 -0.30 4.10 -2 3 21 5.30 3.60 -2 3 21 3.40 3.60 -2 -3 -21 4.70 4.90 2 -4 -21 22.20 7.10 2 4 21 26.70 4.40 2 -4 -21 37.60 6.10 2 4 21 32.30 4.70 -2 -4 -21 23.90 5.20 -2 4 21 41.10 5.60 -2 4 21 29.50 5.60 -2 -4 -21 19.10 5.60 3 0 -21 115.59 8.80 3 0 21 119.39 6.60 3 -1 -21 -2.90 3.80 3 1 21 4.10 2.60 3 1 21 1.70 3.00 -3 1 21 4.90 2.90 -3 -1 -21 -1.70 4.10 3 -2 -21 10.60 4.90 3 2 21 2.70 2.60 3 2 21 6.90 3.10 -3 -2 -21 0.80 4.70 -3 2 21 5.80 3.30 -3 -2 -21 1.70 7.40 3 3 21 8.70 5.30 3 -3 -21 6.50 4.50 -3 3 21 11.80 5.20 -3 -3 -21 15.90 5.60 -3 3 21 11.80 4.20 -3 -3 -21 9.30 5.50 3 4 21 2.30 3.10 3 -4 -21 8.40 4.30 3 4 21 5.70 2.90 -3 4 21 2.50 4.30 -3 -4 -21 -4.80 7.40 4 0 -21 28.30 5.10 4 0 21 34.30 4.20 4 -1 -21 51.99 6.70 4 1 21 44.80 4.50 -4 1 21 47.10 5.60 4 2 21 24.20 4.90 4 -2 -21 39.70 10.20 4 2 21 23.70 3.50 -4 -2 -21 29.50 6.80 -4 2 21 27.50 5.30 4 -3 -21 10.80 4.60 4 3 21 7.80 2.80 4 3 21 12.30 3.40 -4 -3 -21 8.80 6.80 -4 3 21 6.00 3.70 -4 3 21 6.10 4.80 5 0 21 14.70 2.80 5 0 -21 14.50 4.40 5 1 21 114.59 6.60 5 -1 -21 111.39 8.50 -5 1 21 126.39 8.30 5 -2 -21 2.00 3.40 5 2 21 4.50 2.60 -5 2 21 2.50 3.90 -5 -2 -21 8.60 7.00 -5 2 21 0.80 7.30 5 3 21 102.29 6.60 5 -3 -21 101.59 8.20 5 3 21 107.49 6.60 -5 3 21 102.69 8.60 6 0 -21 25.50 6.10 6 0 21 17.70 3.00 6 1 21 15.20 2.90 6 -1 -21 18.80 4.40 -6 1 21 14.40 4.20 0 0 22 129.79 7.70 0 0 -22 139.99 10.10 0 1 22 2.10 2.90 0 -1 -22 0.50 4.30 0 -1 22 5.60 3.50 0 2 22 133.19 7.90 0 -2 -22 119.19 10.10 0 2 22 125.19 8.40 0 3 22 -4.70 3.50 0 3 22 2.40 4.60 0 -3 -22 -4.50 4.00 0 -4 -22 84.39 8.60 0 -4 -22 53.79 9.30 0 4 22 92.39 7.50 0 4 22 66.59 7.70 1 0 22 23.30 3.90 -1 0 22 26.90 3.70 1 0 -22 18.50 4.80 1 -1 -22 71.29 8.10 1 1 22 70.49 6.40 -1 -1 -22 58.59 7.60 -1 1 22 76.89 6.40 1 2 22 5.80 2.90 1 2 22 0.90 3.00 1 -2 -22 8.90 4.70 -1 2 22 0.00 2.70 -1 2 22 1.50 3.00 -1 -2 -22 6.70 5.20 1 3 22 12.80 4.90 1 3 22 7.00 5.80 1 -3 -22 9.10 5.90 -1 3 22 2.10 5.70 -1 -3 -22 2.00 6.50 1 4 22 0.40 3.30 1 -4 -22 3.50 4.30 1 4 22 1.10 3.90 -1 4 22 -1.90 4.30 -1 -4 -22 4.30 4.70 -1 -4 -22 6.00 5.80 -1 4 22 -1.90 3.80 -2 0 22 21.70 3.50 2 0 -22 25.70 5.30 2 1 22 32.10 4.00 2 1 22 27.20 4.30 2 -1 -22 24.70 5.40 -2 -1 -22 16.90 5.40 -2 1 22 22.20 3.90 2 -2 -22 22.50 5.00 2 2 22 27.90 4.60 2 2 22 34.00 4.20 -2 -2 -22 33.40 6.60 -2 2 22 19.20 4.00 2 3 22 25.80 4.30 2 -3 -22 25.90 5.40 2 3 22 33.40 4.50 -2 -3 -22 15.20 10.30 -2 3 22 26.50 4.60 -2 -3 -22 21.30 6.00 -2 3 22 19.00 4.40 2 -4 -22 27.20 8.20 2 4 22 8.90 3.70 -2 4 22 5.80 5.20 -2 -4 -22 12.10 6.50 -2 4 22 12.50 7.40 -2 -4 -22 16.20 6.10 -3 0 22 19.70 3.40 3 0 22 15.20 3.60 3 0 -22 18.50 5.60 3 -1 -22 52.39 9.00 3 1 22 54.29 5.10 -3 1 22 57.59 5.70 3 -2 -22 6.20 4.40 3 2 22 3.30 2.80 3 2 22 4.50 3.50 3 -3 -22 89.99 8.20 3 3 22 90.39 6.50 3 3 22 93.69 6.70 -3 3 22 84.09 8.80 -3 3 22 91.49 7.80 -4 0 22 33.30 4.70 4 0 -22 32.10 5.80 4 0 22 27.80 3.60 4 1 22 7.40 2.80 4 -1 -22 4.60 4.20 -4 1 22 7.60 3.20 4 -2 -22 61.89 7.30 4 2 22 57.69 5.40 -4 2 22 61.59 7.10 -4 2 22 70.39 6.60 4 3 22 15.40 3.40 4 3 22 8.80 3.10 4 -3 -22 3.20 4.40 -4 3 22 15.50 4.60 5 0 22 10.10 2.90 -5 0 22 13.20 3.20 5 0 -22 16.30 6.70 5 1 22 4.40 2.90 5 -1 -22 9.10 4.50 -5 1 22 5.00 3.90 5 -2 -22 12.80 4.20 -5 2 22 20.10 7.40 0 1 23 58.79 8.60 0 -2 -23 0.00 4.60 0 2 23 1.10 3.00 0 3 23 36.90 4.80 0 3 23 40.30 5.00 0 -3 -23 27.80 5.70 -1 0 23 0.90 3.50 1 1 23 43.60 7.20 1 -1 -23 24.10 6.20 1 1 23 33.20 4.10 -1 -1 23 34.80 4.00 -1 1 23 31.00 4.70 -1 -1 -23 26.10 6.00 1 2 23 23.60 4.30 1 -2 -23 28.00 5.80 1 2 23 38.60 4.80 -1 2 23 31.90 5.00 -1 -2 -23 20.90 6.10 -1 2 23 36.70 5.10 1 3 23 77.89 6.90 1 3 23 92.79 7.10 1 -3 -23 76.29 8.70 -1 3 23 91.19 7.50 -1 -3 -23 69.29 8.70 -1 3 23 82.29 7.00 -2 0 23 52.89 6.60 2 0 23 47.20 4.60 2 -1 -23 9.50 4.90 2 1 23 25.90 4.00 -2 -1 23 16.70 3.20 -2 1 23 24.90 6.50 -2 -1 -23 17.00 5.60 2 2 23 41.00 5.10 2 -2 -23 29.50 5.70 2 2 23 45.20 5.20 -2 2 23 49.30 5.80 -2 -2 -23 49.90 7.00 -2 2 23 46.50 5.70 2 -3 -23 14.80 5.10 2 3 23 17.70 4.00 -2 3 23 12.60 4.50 -2 3 23 22.30 6.30 -2 -3 -23 17.80 6.30 3 0 23 83.29 5.70 -3 0 23 87.09 6.30 3 1 23 24.20 3.60 3 -1 -23 20.50 5.20 -3 1 23 23.80 4.10 3 2 23 121.19 7.20 3 -2 -23 133.99 10.50 -3 2 23 119.19 8.30 -3 2 23 118.49 7.90 -4 0 23 19.00 3.70 4 -1 -23 6.90 4.30 4 1 23 3.10 3.40 -4 1 23 -3.60 3.20 4 -2 -23 4.00 4.30 4 2 23 9.80 3.00 -4 2 23 12.10 4.00 -4 2 23 10.10 4.60 0 -1 -24 1.40 6.00 0 1 24 -2.10 2.40 0 1 24 7.50 3.70 0 2 24 5.20 6.00 0 2 24 17.50 3.80 0 -2 -24 17.60 6.10 -1 0 24 93.19 7.00 1 -1 -24 -5.60 5.80 1 1 24 11.00 3.10 -1 1 24 6.00 3.30 1 2 24 29.50 5.50 1 -2 -24 19.30 5.90 1 2 24 35.10 4.50 -1 2 24 28.60 6.10 -1 -2 -24 34.00 6.60 -1 2 24 32.40 4.50 -2 0 24 -0.20 3.10 2 1 24 49.99 4.90 2 -1 -24 32.40 6.10 -2 -1 24 46.60 5.30 -2 1 24 40.30 4.90 2 2 24 1.10 3.60 2 -2 -24 -5.60 4.60 2 2 24 6.20 3.30 -2 2 24 -2.10 4.80 -2 2 24 -2.00 4.10 3 0 24 -2.20 2.80 -3 0 24 0.90 3.50 3 1 24 27.30 3.70 -3 -1 24 19.50 3.70 -3 1 24 21.50 4.40 0 1 25 12.60 3.40 0 1 25 9.90 5.00 1 0 25 79.99 5.90 1 1 25 41.70 4.90 -1 1 25 27.80 5.40 -1 1 25 30.80 4.10 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 93697 _shelx_res_file ; TITL iHOFI.res in Pnma iHOFI.res created by SHELXL-2018/3 at 16:15:43 on 28-Apr-2024 REM Old TITL __TMP__ in Pnma REM SHELXT solution in Pnma REM R1 0.096, Rweak 0.001, Alpha 0.023, Orientation as input REM Formula found by SHELXT: C14 N3 Br CELL 1.34139 8.7734 7.0554 19.7544 90 90 90 ZERR 4 0.0004 0.0003 0.001 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Br N DISP Br -0.9338 1.0006 7840.1 DISP C 0.0137 0.0067 57.1 DISP H -0 0 0.6481 DISP N 0.0241 0.0134 109.9 UNIT 56 40 4 12 EQIV $1 1.5-X,1-Y,-0.5+Z EQIV $2 -0.5+X,1.5-Y,0.5-Z EQIV $3 -0.5+X,0.5-Y,0.5-Z EQIV $4 1.5-X,1-Y,0.5+Z L.S. 10 PLAN 5 SIZE 0.05 0.08 0.1 TEMP -123.15 CONF HTAB C2 N3_$1 HTAB C1 Br1_$2 HTAB C5 Br1_$3 HTAB C5 Br1_$2 HTAB C8 N2_$4 BOND $H list 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.025200 1.299200 FVAR 0.44630 BR1 3 0.653492 0.750000 0.244493 10.50000 0.02063 0.01648 = 0.03671 0.00000 -0.00149 0.00000 N1 4 0.368226 0.250000 0.199812 10.50000 0.01648 0.01927 = 0.02157 0.00000 -0.00249 0.00000 N2 4 0.717119 0.250000 -0.019652 10.50000 0.04619 0.02876 = 0.03155 0.00000 0.00721 0.00000 N3 4 0.779124 0.250000 0.530032 10.50000 0.03940 0.03379 = 0.03165 0.00000 -0.00543 0.00000 C1 1 0.411974 0.417658 0.172680 11.00000 0.02403 0.01818 = 0.02719 -0.00001 -0.00153 0.00163 AFIX 43 H1 2 0.379092 0.533022 0.192725 11.00000 -1.20000 AFIX 0 C2 1 0.503758 0.421800 0.116260 11.00000 0.02657 0.01749 = 0.02564 0.00083 -0.00271 -0.00164 AFIX 43 H2 2 0.535449 0.538883 0.097130 11.00000 -1.20000 AFIX 0 C3 1 0.549153 0.250000 0.087828 10.50000 0.01954 0.02310 = 0.01969 0.00000 -0.00302 0.00000 C4 1 0.644585 0.250000 0.028130 10.50000 0.03231 0.02071 = 0.02605 0.00000 -0.00286 0.00000 C5 1 0.277609 0.250000 0.263527 10.50000 0.01700 0.01907 = 0.02757 0.00000 0.00330 0.00000 AFIX 23 H5A 2 0.211507 0.136349 0.264955 10.50000 -1.20000 H5B 2 0.211507 0.363651 0.264955 10.50000 -1.20000 AFIX 0 C6 1 0.382643 0.250000 0.323561 10.50000 0.01798 0.01902 = 0.02277 0.00000 0.00446 0.00000 C7 1 0.433159 0.421043 0.350917 11.00000 0.02641 0.01700 = 0.03097 0.00151 0.00238 -0.00066 AFIX 43 H7 2 0.397935 0.537574 0.332593 11.00000 -1.20000 AFIX 0 C8 1 0.534251 0.421743 0.404572 11.00000 0.03005 0.02087 = 0.02829 -0.00274 0.00107 -0.00285 AFIX 43 H8 2 0.568918 0.538316 0.423071 11.00000 -1.20000 AFIX 0 C9 1 0.585037 0.250000 0.431380 10.50000 0.02096 0.02577 = 0.02321 0.00000 0.00436 0.00000 C10 1 0.692515 0.250000 0.486837 10.50000 0.03124 0.02404 = 0.02749 0.00000 0.00674 0.00000 HKLF 4 REM iHOFI.res in Pnma REM wR2 = 0.0687, GooF = S = 1.088, Restrained GooF = 1.088 for all data REM R1 = 0.0282 for 1245 Fo > 4sig(Fo) and 0.0375 for all 1461 data REM 97 parameters refined using 0 restraints END WGHT 0.0252 1.2996 REM Highest difference peak 0.827, deepest hole -0.586, 1-sigma level 0.073 Q1 1 0.6413 0.7500 0.2804 10.50000 0.05 0.83 Q2 1 0.3521 0.2500 0.2896 10.50000 0.05 0.52 Q3 1 0.4411 0.4130 0.1382 11.00000 0.05 0.39 Q4 1 0.5045 0.4037 0.3695 11.00000 0.05 0.33 Q5 1 0.6572 0.7500 0.1783 10.50000 0.05 0.32 ; _shelx_res_checksum 32633 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.65349(4) 0.750000 0.24449(2) 0.02461(12) Uani d 1 . . N N1 0.3682(3) 0.250000 0.19981(12) 0.0191(5) Uani d 1 . . N N2 0.7171(4) 0.250000 -0.01965(15) 0.0355(7) Uani d 1 . . N N3 0.7791(4) 0.250000 0.53003(14) 0.0349(7) Uani d 1 . . C C1 0.4120(2) 0.4177(3) 0.17268(10) 0.0231(5) Uani d 1 . . H H1 0.379092 0.533022 0.192725 0.028 Uiso calc 1 . . C C2 0.5038(2) 0.4218(3) 0.11626(10) 0.0232(4) Uani d 1 . . H H2 0.535449 0.538883 0.097130 0.028 Uiso calc 1 . . C C3 0.5492(3) 0.250000 0.08783(14) 0.0208(6) Uani d 1 . . C C4 0.6446(4) 0.250000 0.02813(15) 0.0264(7) Uani d 1 . . C C5 0.2776(3) 0.250000 0.26353(14) 0.0212(6) Uani d 1 . . H H5A 0.211507 0.136349 0.264955 0.025 Uiso calc 0.5 . . H H5B 0.211507 0.363651 0.264955 0.025 Uiso calc 0.5 . . C C6 0.3826(3) 0.250000 0.32356(14) 0.0199(6) Uani d 1 . . C C7 0.4332(2) 0.4210(3) 0.35092(11) 0.0248(5) Uani d 1 . . H H7 0.397935 0.537574 0.332593 0.030 Uiso calc 1 . . C C8 0.5343(3) 0.4217(3) 0.40457(11) 0.0264(5) Uani d 1 . . H H8 0.568918 0.538316 0.423071 0.032 Uiso calc 1 . . C C9 0.5850(3) 0.250000 0.43138(15) 0.0233(7) Uani d 1 . . C C10 0.6925(4) 0.250000 0.48684(16) 0.0276(7) Uani 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 0.02063(17) 0.01648(17) 0.03671(19) 0.000 -0.00149(13) 0.000 N1 0.0165(12) 0.0193(13) 0.0216(11) 0.000 -0.0025(9) 0.000 N2 0.0462(18) 0.0288(17) 0.0315(15) 0.000 0.0072(13) 0.000 N3 0.0394(17) 0.0338(18) 0.0317(15) 0.000 -0.0054(13) 0.000 C1 0.0240(10) 0.0182(12) 0.0272(10) 0.0016(9) -0.0015(8) 0.0000(8) C2 0.0266(11) 0.0175(11) 0.0256(10) -0.0016(9) -0.0027(8) 0.0008(8) C3 0.0195(14) 0.0231(17) 0.0197(13) 0.000 -0.0030(11) 0.000 C4 0.0323(17) 0.0207(17) 0.0261(15) 0.000 -0.0029(14) 0.000 C5 0.0170(13) 0.0191(14) 0.0276(15) 0.000 0.0033(11) 0.000 C6 0.0180(14) 0.0190(16) 0.0228(14) 0.000 0.0045(10) 0.000 C7 0.0264(11) 0.0170(12) 0.0310(11) -0.0007(9) 0.0024(9) 0.0015(8) C8 0.0301(12) 0.0209(12) 0.0283(10) -0.0029(10) 0.0011(9) -0.0027(8) C9 0.0210(15) 0.0258(18) 0.0232(14) 0.000 0.0044(11) 0.000 C10 0.0312(17) 0.0240(18) 0.0275(16) 0.000 0.0067(13) 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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 -0.9338 1.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0134 '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 C1 N1 C1 7_565 . 121.7(3) ? C1 N1 C5 . . 119.08(13) ? C1 N1 C5 7_565 . 119.07(13) ? N1 C1 H1 . . 119.8 ? N1 C1 C2 . . 120.3(2) ? C2 C1 H1 . . 119.8 ? C1 C2 H2 . . 120.8 ? C1 C2 C3 . . 118.4(2) ? C3 C2 H2 . . 120.8 ? C2 C3 C2 7_565 . 120.8(3) ? C2 C3 C4 . . 119.60(13) ? C2 C3 C4 7_565 . 119.60(13) ? N2 C4 C3 . . 178.6(4) ? N1 C5 H5A . . 109.7 ? N1 C5 H5B . . 109.7 ? N1 C5 C6 . . 109.9(2) ? H5A C5 H5B . . 108.2 ? C6 C5 H5A . . 109.7 ? C6 C5 H5B . . 109.7 ? C7 C6 C5 7_565 . 120.07(14) ? C7 C6 C5 . . 120.07(14) ? C7 C6 C7 . 7_565 119.8(3) ? C6 C7 H7 . . 119.9 ? C8 C7 C6 . . 120.3(2) ? C8 C7 H7 . . 119.9 ? C7 C8 H8 . . 120.2 ? C7 C8 C9 . . 119.5(2) ? C9 C8 H8 . . 120.2 ? C8 C9 C8 7_565 . 120.5(3) ? C8 C9 C10 . . 119.73(14) ? C8 C9 C10 7_565 . 119.73(14) ? N3 C10 C9 . . 179.0(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 C1 7_565 1.354(3) ? N1 C1 . 1.354(3) ? N1 C5 . 1.489(4) ? N2 C4 . 1.138(4) ? N3 C10 . 1.143(4) ? C1 H1 . 0.9500 ? C1 C2 . 1.375(3) ? C2 H2 . 0.9500 ? C2 C3 . 1.394(3) ? C3 C4 . 1.446(4) ? C5 H5A . 0.9900 ? C5 H5B . 0.9900 ? C5 C6 . 1.502(4) ? C6 C7 . 1.395(3) ? C6 C7 7_565 1.395(3) ? C7 H7 . 0.9500 ? C7 C8 . 1.382(3) ? C8 H8 . 0.9500 ? C8 C9 . 1.395(3) ? C9 C10 . 1.445(5) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C1 H1 Br1 4_465 0.95 2.79 3.649(2) 150.5 yes C2 H2 N3 2_664 0.95 2.57 3.448(3) 153.3 yes C5 H5A Br1 4_455 0.99 2.78 3.6953(9) 154.1 yes C5 H5B Br1 4_465 0.99 2.78 3.6953(9) 154.1 yes C8 H8 N2 2_665 0.95 2.65 3.516(3) 151.4 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 C1 C2 C3 . . . . 0.4(3) ? N1 C5 C6 C7 . . . . 89.1(2) ? N1 C5 C6 C7 . . . 7_565 -89.1(2) ? C1 N1 C1 C2 7_565 . . . -0.3(4) ? C1 N1 C5 C6 . . . . -88.1(2) ? C1 N1 C5 C6 7_565 . . . 88.1(2) ? C1 C2 C3 C2 . . . 7_565 -0.6(4) ? C1 C2 C3 C4 . . . . 179.5(2) ? C5 N1 C1 C2 . . . . 175.9(2) ? C5 C6 C7 C8 . . . . -177.6(2) ? C6 C7 C8 C9 . . . . -0.2(4) ? C7 C6 C7 C8 7_565 . . . 0.7(4) ? C7 C8 C9 C8 . . . 7_565 -0.2(4) ? C7 C8 C9 C10 . . . . 179.1(2) ? _cod_database_fobs_code 2312553