Silyl-Substituted 1,4-Disila(Dewar benzene): New Synthesis and Unexpected Insertion of CO into the Si−Si Bond To Form a Disilyl Ketone
Nakata, Norio; Oikawa, Toru; Matsumoto, Takeshi; Kabe, Yoshio; Sekiguchi, Akira; Organometallics 24 (2005) 3368–; doi:10.1021/om050261n

data_4075896
_publ_section_title
;
 Silyl-Substituted 1,4-Disila(Dewar benzene):&#x00A0; New Synthesis and
 Unexpected Insertion of CO into the Si&#x2212;Si Bond To Form a Disilyl
 Ketone
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3368
_journal_paper_doi               10.1021/om050261n
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C31 H62 O Si4'
_chemical_formula_weight         563.17
_chemical_name_common            Disilylketone
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.6070(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8570(4)
_cell_length_b                   25.9730(9)
_cell_length_c                   15.8440(6)
_cell_measurement_temperature    120(2)
_cell_volume                     3527.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8053
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.9282
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0798P)^2^+0.2765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                6416
_reflns_number_total             8053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050261nsi20050519_093355.cif
_cod_data_source_block           Si2CO
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4075896