Two Reversible σ-Bond Metathesis Pathways for Boron-Palladium Bond Formation: Selective Synthesis of Isomeric Five-Coordinate Borylpalladium Complexes
Naohiro Kirai; Jun Takaya; Nobuharu Iwasawa; Journal of the American Chemical Society 135 (2013) 2493–2496; doi:10.1021/ja400294m

data_4119380
_publ_contact_author_email       niwasawa@chem.titech.ac.jp
_publ_contact_author_name        'Nobuharu Iwasawa'
_publ_section_title
;
 Two Reversible \s-Bond Metathesis Pathways for Boron-Palladium Bond
 Formation: Selective Synthesis of Isomeric Five-Coordinate Borylpalladium
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2493
_journal_page_last               2496
_journal_paper_doi               10.1021/ja400294m
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C63 H58 B O3 P3 Pd Si'
_chemical_formula_weight         1101.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 100.4611(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.922(3)
_cell_length_b                   13.0423(12)
_cell_length_c                   34.076(4)
_cell_measurement_reflns_used    13914
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      3.0058
_cell_volume                     10892(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            65437
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9076
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       prism
_exptl_crystal_F_000             4560
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.051
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         12445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+41.5846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                10765
_reflns_number_total             12445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400294m_si_004.cif
_cod_data_source_block           '_trans_BPdPSiP_PPh3_2b'
_cod_original_cell_volume        10892.1(19)
_cod_database_code               4119380