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_4113675
_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
;
  2,3-Diethyl-1,1-bis(tri-tert-butylsilyl)-1-silacycloprop-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                 90.131(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7820(2)
_cell_length_b                   17.3430(8)
_cell_length_c                   21.4700(10)
_cell_measurement_reflns_used    31089
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.23
_cell_volume                     3270.0(2)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31089
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0178(12)
_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   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         7563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+1.1549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                6110
_reflns_number_total             7563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020929e_1.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4113675