The preparation of the MF6- (M = As, Sb) salts of 1,4-benzoquinodal bridged bis-1,3,2-dithiazolylium utilizing the cycloaddition and oxidative dehydrogenation chemistry of SNSMF6 and observation of a hybrid semiquinoidal-thiazyl radical-cation by EPR.
Decken, Andreas; Mailman, Aaron; Passmore, Jack; Chemical communications (Cambridge, England)  (2009) 6077–6079; doi:10.1039/b910338d

data_7104927
_publ_section_title
;
 The preparation of the MF6- (M = As, Sb) salts of 1,4-benzoquinodal
 bridged bis-1,3,2-dithiazolylium utilizing the cycloaddition and
 oxidative dehydrogenation chemistry of SNSMF6 and observation of a
 hybrid semiquinoidal-thiazyl radical-cation by EPR.
;
_journal_issue                   40
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6077
_journal_page_last               6079
_journal_paper_doi               10.1039/b910338d
_journal_year                    2009
_chemical_formula_moiety         'C6 H4 N O2 S2, C6 H4 O2, F6 Sb'
_chemical_formula_sum            'C12 H8 F6 N O4 S2 Sb'
_chemical_formula_weight         530.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.500(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0959(5)
_cell_length_b                   12.9028(7)
_cell_length_c                   14.3415(8)
_cell_measurement_reflns_used    6373
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.627
_cell_measurement_theta_min      2.582
_cell_volume                     1680.02(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8267
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  0.8271
_exptl_absorpt_correction_T_min  0.5058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         2856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0203
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.9181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                2672
_reflns_number_total             2856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b910338d.txt
_cod_data_source_block           jp040304
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7104927