Stereochemistry of Disilanylene-Containing Cyclic Compounds. Palladium-Catalyzed Reactions ofcis- andtrans-3,4-Benzo-1,2-diisopropyl-1,2-dimethyl-1,2-disilacyclobut-3-ene with Ethylene
Naka, Akinobu; Ohshita, Joji; Miyazaki, Eigo; Miura, Toshiko; Kobayashi, Hisayoshi; Ishikawa, Mitsuo; Organometallics 31 (2012) 3492–; doi:10.1021/om201061x

data_4078198
_publ_section_title
;
 Stereochemistry of Disilanylene-Containing Cyclic Compounds.
 Palladium-Catalyzed Reactions ofcis-
 andtrans-3,4-Benzo-1,2-diisopropyl-1,2-dimethyl-1,2-disilacyclobut-3-ene
 with Ethylene
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3492
_journal_paper_doi               10.1021/om201061x
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C30 H52 Si4 '
_chemical_formula_sum            'C30 H52 Si4'
_chemical_formula_weight         525.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 91.6079(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.4827(3)
_cell_length_b                   19.1784(4)
_cell_length_c                   29.1806(6)
_cell_measurement_reflns_used    85140
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.1
_cell_volume                     6423.6(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47086
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         47828
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.9420
_exptl_absorpt_correction_T_min  0.9238
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         14642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0446
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1545
_reflns_number_gt                12853
_reflns_number_total             14642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201061x_si_002.cif
_cod_data_source_block           Naka050412
_cod_database_code               4078198