The Isolable Cation Radical of Disilene: Synthesis, Characterization, and a Reversible One-Electron Redox System
Shigeyoshi Inoue; Masaaki Ichinohe; Akira Sekiguchi; Journal of the American Chemical Society 130 (2008) 6078–6079; doi:10.1021/ja801761w

data_4107770
_publ_section_title
;
 The Isolable Cation Radical of Disilene: Synthesis, Characterization, and
 a Reversible One-Electron Redox System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6078
_journal_page_last               6079
_journal_paper_doi               10.1021/ja801761w
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C72 H96 B F20 Si6'
_chemical_formula_weight         1520.84
_chemical_name_systematic
; 
 Tetrais(di-tert-butylmethylsilyl)disilene cation radical
 tetrakis(pentfluorophenyl)borate 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.0090(17)
_cell_length_b                   21.009
_cell_length_c                   36.1310(14)
_cell_measurement_reflns_used    58814
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.24
_cell_volume                     15947.4(14)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      120.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1120
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            58814
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red-brown
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       Cube
_exptl_crystal_F_000             6376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.00093(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1075P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1794
_reflns_number_gt                2023
_reflns_number_total             3506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801761w-file002.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'I 41/a c d '
_cod_database_code               4107770