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_4035393
_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         'C26 H32 O Si2'
_chemical_formula_sum            'C26 H32 O Si2'
_chemical_formula_weight         416.70
_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                 92.762(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4509(17)
_cell_length_b                   16.5070(17)
_cell_length_c                   8.0640(6)
_cell_measurement_reflns_used    2064
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.1750
_cell_measurement_theta_min      3.6370
_cell_volume                     2453.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11999
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    0.158
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0490P)^2^+0.0230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1320
_reflns_number_gt                3027
_reflns_number_total             4974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8b02018_si_001.cif
_cod_data_source_block           exp_5275
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4035393