An Isolable NHC-Stabilized Silylene Radical Cation: Synthesis and Structural Characterization
Hiroaki Tanaka; Masaaki Ichinohe; Akira Sekiguchi; Journal of the American Chemical Society 134 (2012) 5540–5543; doi:10.1021/ja301180v

data_4117745
_publ_section_title
;
 An Isolable NHC-Stabilized Silylene Radical Cation: Synthesis and
 Structural Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5540
_journal_page_last               5543
_journal_paper_doi               10.1021/ja301180v
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C94 H138.5 B F18.5 N2 Si7'
_chemical_formula_weight         1855.51
_chemical_name_systematic
; 
 (1,1,1,3,3,3-hexa-tert-butyltrisilane-2-yl-2-ylium 
 1,3,4,5-tetramthylimidazole-2,2-diyl)-
 tetrakis[4-(tert-butyldimethylsilyl)-2,3,5,6-tetrafluorophenyl]borate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.2500(10)
_cell_angle_beta                 96.718(2)
_cell_angle_gamma                90.447(2)
_cell_formula_units_Z            2
_cell_length_a                   15.260(2)
_cell_length_b                   16.593(2)
_cell_length_c                   20.617(3)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.28
_cell_volume                     5129.3(12)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120.0(1)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1816
_diffrn_reflns_av_sigmaI/netI    0.1304
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57840
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9715
_exptl_absorpt_correction_T_min  0.9292
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0005(3)
_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   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1124
_refine_ls_number_reflns         22911
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+8.0350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2283
_refine_ls_wR_factor_ref         0.2450
_reflns_number_gt                18730
_reflns_number_total             22911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301180v_si_003.cif
_cod_data_source_block           si2sinhctsfpb_0m
_cod_original_cell_volume        5129.4(12)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4117745