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_4117744
_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            'C35 H74 N2 O Si3'
_chemical_formula_weight         623.23
_chemical_name_systematic
; 
 1,1,1,3,3,3-hexa-tert-butyltrisilane-2,2-diyl 
 1',3',4',5'-tetramethyl-2',3'-dihydro-1'H-imidazole-2',2'-diyl complex 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   15.7355(7)
_cell_length_b                   16.2056(8)
_cell_length_c                   30.5406(14)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.24
_cell_volume                     7788.0(6)
_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(1)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            88783
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  0.9792
_exptl_absorpt_correction_T_min  0.9690
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.289
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.0000(2)
_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   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         17787
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1389P)^2^+2.8304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2032
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                14015
_reflns_number_total             17787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301180v_si_002.cif
_cod_data_source_block           reductsi2sinhc_0m
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4117744