Air-Stable Disilacyclopropene with a SiC Bond and Its Conversion to Disilacyclopropenylium Ion: Silicon-Carbon Hybrid 2π-Electron Systems
Masayasu Igarashi; Masaaki Ichinohe; Akira Sekiguchi; Journal of the American Chemical Society 129 (2007) 12660–12661; doi:10.1021/ja075740n

data_4110072
_publ_section_title
;
 Air-Stable Disilacyclopropene with a SiC Bond and Its Conversion to
 Disilacyclopropenylium Ion: Silicon-Carbon Hybrid 2\p-Electron Systems
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12660
_journal_page_last               12661
_journal_paper_doi               10.1021/ja075740n
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C47 H96 Si5'
_chemical_formula_weight         801.69
_chemical_name_systematic
; 
 3-(1-Adamantyl)-1,1,2-tris(tri-tert-butylsilyl)-
 1,2-disilacycloprop-2-ene 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   13.9010(2)
_cell_length_b                   20.7850(6)
_cell_length_c                   35.3310(9)
_cell_measurement_reflns_used    103446
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.04
_cell_volume                     10208.3(4)
_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      150.0(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.075
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            103446
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_description       cubic
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0052(4)
_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   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         12127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1819
_reflns_number_gt                8297
_reflns_number_total             12127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075740nsi20070801_030722.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               4110072