#------------------------------------------------------------------------------ #$Date: 2026-01-20 17:28:07 +0000 (Tue, 20 Jan 2026) $ #$Revision: 304194 $ #$URL: svn://www.crystallography.net/cod/cif/3/50/01/3500150.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3500150 loop_ _publ_author_name 'Thierry Maris' _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _publ_section_title ; Hydrazinium Bromide at 150 K ; _journal_name_full 'Personal communication to COD' _journal_year 2026 _chemical_formula_moiety 'H5 N2, Br' _chemical_formula_sum 'Br H5 N2' _chemical_formula_weight 112.97 _chemical_name_systematic 'Hydrazinium Bromide' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2025-01-07 _cell_angle_alpha 90 _cell_angle_beta 110.499(1) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 12.7636(5) _cell_length_b 4.5286(2) _cell_length_c 12.0133(5) _cell_measurement_reflns_used 9966 _cell_measurement_temperature 150 _cell_measurement_theta_max 73.596 _cell_measurement_theta_min 6.146 _cell_volume 650.41(5) _computing_cell_refinement ; SAINT (2013) V8.41; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_collection ; APEX 4 (2022) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction ; SAINT (2013) V8.41; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150 _diffrn_detector 'CMOS Area detector' _diffrn_detector_area_resol_mean 10.42 _diffrn_detector_type 'Bruker CMOS Photon III ' _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device 'k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker Venture Metaljet' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Helios MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Ga K\a' _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_unetI/netI 0.0204 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 11296 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 73.536 _diffrn_reflns_theta_min 6.442 _diffrn_source 'Metal Jet' _diffrn_source_current 3.57 _diffrn_source_power 0.2488647 _diffrn_source_target Ga _diffrn_source_type 'Gallium Liquid Metal Jet Source' _diffrn_source_voltage 69.71 _exptl_absorpt_coefficient_mu 9.918 _exptl_absorpt_correction_T_max 0.1727 _exptl_absorpt_correction_T_min 0.0591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1662 before and 0.0931 after correction. The Ratio of minimum to maximum transmission is 0.3422. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 2.307 _exptl_crystal_description platelet _exptl_crystal_F_000 432 _exptl_crystal_recrystallization_method 'crystallised from MeOH' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Venture diffractometer equipped with a Photon III CMOS Detector, a Helios MX optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 1024 x 1024 pixel mode. ; _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _refine_diff_density_max 0.791 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.129 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.205 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 43 _refine_ls_number_reflns 989 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.205 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0282 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+3.9982P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.0851 _refine_special_details ; 1. Fixed Uiso At 1.5 times of: All N(H,H) groups, All N(H,H,H) groups ; _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 967 _reflns_number_total 989 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file nitbr1.cif _cod_data_source_block nitbr1 _cod_database_code 3500150 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _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 _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.60036(3) 0.91055(8) 0.41752(3) 0.02899(14) Uani 1 1 d . . . . . N1 N 0.3508(3) 0.5900(7) 0.3657(3) 0.0292(6) Uani 1 1 d . . . . . H1A H 0.284(5) 0.690(13) 0.337(5) 0.044 Uiso 1 1 d . U . . . H1B H 0.346(4) 0.497(13) 0.438(5) 0.044 Uiso 1 1 d . U . . . H1C H 0.405(5) 0.698(13) 0.396(5) 0.044 Uiso 1 1 d . U . . . N2 N 0.3570(3) 0.3861(7) 0.2752(3) 0.0297(6) Uani 1 1 d . . . . . H2A H 0.416(5) 0.272(13) 0.309(5) 0.045 Uiso 1 1 d . U . . . H2B H 0.381(5) 0.478(13) 0.217(5) 0.045 Uiso 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0286(2) 0.0313(2) 0.0273(2) 0.00054(12) 0.01007(14) -0.00031(12) N1 0.0278(14) 0.0311(14) 0.0274(13) -0.0021(11) 0.0080(11) -0.0027(11) N2 0.0298(14) 0.0308(14) 0.0307(14) -0.0009(11) 0.0133(12) -0.0005(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0241 0.0134 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 H1A N1 H1B 101(4) . . H1A N1 H1C 114(5) . . H1B N1 H1C 100(5) . . N2 N1 H1A 109(3) . . N2 N1 H1B 115(3) . . N2 N1 H1C 117(4) . . N1 N2 H2A 107(4) . . N1 N2 H2B 113(4) . . H2A N2 H2B 99(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 N1 H1A 0.92(6) . N1 H1B 0.99(6) . N1 H1C 0.82(6) . N1 N2 1.449(4) . N2 H2A 0.89(6) . N2 H2B 0.95(6) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1A Br1 0.92(6) 3.10(5) 3.558(3) 113(4) 3_445 yes N1 H1A N2 0.92(6) 2.04(6) 2.925(5) 162(5) 4 yes N1 H1B Br1 0.99(6) 2.46(6) 3.343(3) 148(4) 5_666 yes N1 H1C Br1 0.82(6) 2.60(6) 3.354(3) 154(5) . yes N1 H1C Br1 0.82(6) 2.88(6) 3.339(3) 117(5) 5_676 yes N2 H2A Br1 0.89(6) 2.79(6) 3.673(3) 180(5) 1_545 yes N2 H2B Br1 0.95(6) 2.60(6) 3.490(3) 155(5) 2_655 yes _cod_database_fobs_code 3500150