Crystal structure of 4,4'-(diazenediyl)dipyridinium nitrate perchlorate
Qiu, Qi-Ming; Song, Jian-Biao; Dong, Ai-Guo; Li, Chuan-Tao; Zheng, Zhi-Yuan; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022007885

data_2244143
_publ_section_title
;
 Crystal structure of 4,4'-(diazenediyl)dipyridinium nitrate perchlorate
;
_journal_coeditor_code           YK2173
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022007885
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C10 H10 N4 2+, N O3 -, Cl O4 -'
_chemical_formula_moiety         'C10 H10 N4 2+, N O3 -, Cl O4 -'
_chemical_formula_sum            'C10 H10 Cl N5 O7'
_chemical_formula_weight         347.68
_chemical_name_systematic
;
4,4'-(Diazenediyl)dipyridinium nitrate perchlorate
;
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                116.966(3)
_cell_angle_beta                 105.481(2)
_cell_angle_gamma                92.8710(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3023(8)
_cell_length_b                   10.0792(9)
_cell_length_c                   10.1052(9)
_cell_measurement_reflns_used    1709
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.306
_cell_measurement_theta_min      2.314
_cell_volume                     711.77(12)
_computing_cell_refinement
;
SAINT (Bruker, 2006)
;
_computing_data_collection
;
SAINT (Bruker, 2006)
;
_computing_data_reduction
;
APEX2 (Bruker, 2006)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega continuous scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3625
_diffrn_reflns_theta_full        25.045
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_min         2.314
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  0.9042
_exptl_absorpt_correction_T_min  0.8725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.330
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.507
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1890P)^2^+0.2213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2330
_refine_ls_wR_factor_ref         0.2497
_reflns_number_gt                1896
_reflns_number_total             2466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2173sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        711.77(11)
_cod_database_code               2244143
_shelx_estimated_absorpt_t_min   0.871
_shelx_estimated_absorpt_t_max   0.903
_shelx_hkl_checksum              34481
_shelx_res_checksum              67163
_cod_database_fobs_code 2244143