Reactivity of a Disilyne RSi\τbSiR (R = SiiPr[CH(SiMe3)2]2) toward π-Bonds: Stereospecific Addition and a New Route to an Isolable 1,2-Disilabenzene
Rei Kinjo; Masaaki Ichinohe; Akira Sekiguchi; Nozomi Takagi; Michinori Sumimoto; Shigeru Nagase; Journal of the American Chemical Society 129 (2007) 7766–7767; doi:10.1021/ja072759h

data_4109583
_publ_section_title
;
 Reactivity of a Disilyne RSi\\tbSiR (R = SiiPr[CH(SiMe3)2]2) toward
 \p-Bonds: Stereospecific Addition and a New Route to an Isolable
 1,2-Disilabenzene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7766
_journal_page_last               7767
_journal_paper_doi               10.1021/ja072759h
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C38 H98 Si12'
_chemical_formula_weight         892.24
_chemical_name_systematic
; 
 trans-1,2-Bis{bis[bis(trimethylsilyl)methyl]isopropylsilyl}-
 3,4-dimethyl-1,2-disilacyclobutene
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 90.886(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8790(3)
_cell_length_b                   16.2050(6)
_cell_length_c                   29.3670(9)
_cell_measurement_reflns_used    29754
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.13
_cell_volume                     5652.4(3)
_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      120.0(1)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            29754
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_description       needle
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(11)
_refine_ls_extinction_coef       0.0031(3)
_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   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6687
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+3.7108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                6314
_reflns_number_total             6687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072759hsi20070420_125312.cif
_cod_data_source_block           disilacyclobutene
_cod_original_sg_symbol_H-M      'C c '
_cod_database_code               4109583