Synthesis, structure and redox reactions of a new crowded benzodithiolium salt: first isolation and characterization of a stable dithiolyl radical with a 7π electron framework
Ogawa, Satoshi; Kikuchi, Mieko; Sato, Ryu; Kawai, Yasushi; Niizuma, Shigeya; Chemical Communications  (1999) 1891–; doi:10.1039/a905276c

data_7115189
_publ_section_title
;
 Synthesis, structure and redox reactions of a new crowded benzodithiolium
 salt: first isolation and characterization of a stable dithiolyl radical
 with a 7\p electron framework
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1891
_journal_paper_doi               10.1039/a905276c
_journal_year                    1999
_chemical_formula_moiety         'C22 H27 S2 1+, B F4 1-, C6 H6'
_chemical_formula_sum            'C28 H33 B F4 S2'
_chemical_formula_weight         520.49
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     'direct methods'
_atom_sites_solution_secondary   'Fourier techniques'
_audit_creation_date             'Thu Jul  26 22:03:01 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 122.91(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.387(8)
_cell_length_b                   13.177(7)
_cell_length_c                   19.851(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      13.6
_cell_volume                     5795(4)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SAPI92
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01579
_diffrn_orient_matrix_UB_12      -0.05946
_diffrn_orient_matrix_UB_13      -0.01446
_diffrn_orient_matrix_UB_21      0.00400
_diffrn_orient_matrix_UB_22      0.04352
_diffrn_orient_matrix_UB_23      -0.03814
_diffrn_orient_matrix_UB_31      0.04210
_diffrn_orient_matrix_UB_32      0.01817
_diffrn_orient_matrix_UB_33      0.04402
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  filter
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.105
_diffrn_reflns_av_sigmaI/netI    0.187
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4659
_diffrn_reflns_theta_max         60.07
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        3.44
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.003
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   '\DF (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2192.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.225
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     316
_refine_ls_number_reflns         2083
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.1049
_refine_ls_shift/esd_max         0.0759
_refine_ls_shift/esd_mean        0.0046
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.01000|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1514
_reflns_number_observed          2083
_reflns_number_total             4544
_reflns_observed_criterion       >1.5sigma(I)
_cod_data_source_file            905276c.txt
_cod_data_source_block           Benzodithiolium
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.01000|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.01000|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5794(4)
_cod_original_sg_symbol_H-M      'C 2/c        '
_cod_original_formula_sum        'C28 H33 B F4 S2 '
_cod_database_code               7115189