Bis(tri-tert-butylsilyl)silylene: Triplet Ground State Silylene
Akira Sekiguchi; Takashi Tanaka; Masaaki Ichinohe; Kimio Akiyama; Shozo Tero-Kubota; Journal of the American Chemical Society 125 (2003) 4962–4963; doi:10.1021/ja020929e

data_4113677
_publ_section_title
;
 Bis(tri-tert-butylsilyl)silylene: Triplet Ground State Silylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4962
_journal_page_last               4963
_journal_paper_doi               10.1021/ja020929e
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C30 H64 Si3'
_chemical_formula_weight         509.08
_chemical_name_systematic
;
  4,4-Di-tert-butyl-2,3-diethyl-5,5-dimethyl-1-tri-tert-butylsilyl-
  1,4-disilacyclohex-2-ene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 91.7710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6610(2)
_cell_length_b                   25.8240(5)
_cell_length_c                   14.4820(2)
_cell_measurement_reflns_used    32671
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.11
_cell_volume                     3237.52(11)
_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    SIR92
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32671
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_description       cube
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0221(11)
_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   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         7742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+1.1198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                7256
_reflns_number_total             7742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020929e_3.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4113677