Efficient Synthesis of Diborylalkenes from Alkenes and Diboron by a New PSiP-Pincer Palladium-Catalyzed Dehydrogenative Borylation
Jun Takaya; Naohiro Kirai; Nobuharu Iwasawa; Journal of the American Chemical Society 133 (2011) 12980–12983; doi:10.1021/ja205186k

data_4106629
_publ_contact_author_email       niwasawa@chem.titech.ac.jp
_publ_contact_author_name        'Nobuharu Iwasawa'
_publ_section_title
;
 Efficient Synthesis of Diborylalkenes from Alkenes and Diboron by a New
 PSiP-Pincer Palladium-Catalyzed Dehydrogenative Borylation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12980
_journal_page_last               12983
_journal_paper_doi               10.1021/ja205186k
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C43 H43 B O2 P2 Pd Si'
_chemical_formula_weight         799.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.629(3)
_cell_angle_beta                 85.393(3)
_cell_angle_gamma                79.455(3)
_cell_formula_units_Z            6
_cell_length_a                   8.5513(6)
_cell_length_b                   22.4101(16)
_cell_length_c                   32.205(3)
_cell_measurement_reflns_used    15814
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      3.0038
_cell_volume                     6007.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            74880
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9252
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.848
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1403
_refine_ls_number_reflns         27365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0800P)^2^+17.9834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1726
_reflns_number_gt                21882
_reflns_number_total             27365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205186k_si_002.cif
_cod_data_source_block           crystalclear
_cod_database_code               4106629