Experimental and Computational Study on the Structure and Properties of Herz Cations and Radicals: 1,2,3-Benzodithiazolium, 1,2,3-Benzodithiazolyl, and Their Se Congeners
Alexander Yu. Makarov; Frank Blockhuys; Irina Yu. Bagryanskaya; Yuri V. Gatilov; Makhmut M. Shakirov; Andrey V. Zibarev; Inorganic Chemistry 52 (2013) 3699–3710; doi:10.1021/ic302203t

data_4334285
_publ_contact_author_email       bagryan@nioch.nsc.ru
_publ_contact_author_name        'Dr. I. Yu. Bagryanskaya'
_publ_section_title
;
 Experimental and Computational Study on the Structure and Properties of
 Herz Cations and Radicals: 1,2,3-Benzodithiazolium,
 1,2,3-Benzodithiazolyl, and Their Se Congeners
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3699
_journal_page_last               3710
_journal_paper_doi               10.1021/ic302203t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C6 H4 N S2 1+, B F4 1-'
_chemical_formula_sum            'C6 H4 B F4 N S2'
_chemical_formula_weight         241.03
_chemical_melting_point          418
_chemical_name_systematic
; 
 1,2,3-benzodithiazolium tetrafluoroborate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.309(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.6946(11)
_cell_length_b                   5.5482(4)
_cell_length_c                   21.652(2)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      12.02
_cell_measurement_theta_min      1.87
_cell_volume                     1765.2(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            1981
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        2.3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.8432
_exptl_absorpt_correction_T_min  0.5054
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black-dark_red
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         1909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+6.1616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                1517
_reflns_number_total             1909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302203t_si_001_4.cif
_cod_data_source_block           zm-bf4
_cod_original_cell_volume        1765.2(3)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4334285