Palladium-Catalyzed Catellani-Type Bis-silylation and Bis-germanylation of Aryl Iodides and Norbornenes.
Lv, Weiwei; Yu, Jia; Ge, Bailu; Wen, Si; Cheng, Guolin; The Journal of organic chemistry 83 (2018) 12683–12693; doi:10.1021/acs.joc.8b02018

data_4035394
_publ_section_title
;
 Palladium-Catalyzed Catellani-Type Bis-silylation and Bis-germanylation
 of Aryl Iodides and Norbornenes.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12683
_journal_page_last               12693
_journal_paper_doi               10.1021/acs.joc.8b02018
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C23 H32 O Si2'
_chemical_formula_sum            'C23 H32 O Si2'
_chemical_formula_weight         380.67
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 102.55(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.589(4)
_cell_length_b                   9.963(2)
_cell_length_c                   17.419(3)
_cell_measurement_reflns_used    2676
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6960
_cell_measurement_theta_min      4.0330
_cell_volume                     2302.0(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0924
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13753
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.67
_exptl_absorpt_coefficient_mu    0.163
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                2550
_reflns_number_total             4656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8b02018_si_002.cif
_cod_data_source_block           exp_5274
_cod_original_cell_volume        2301.9(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4035394