Dinuclear Palladium and Platinum Complexes with Bridging Silylene Ligands. Preparation Using (Aminosilyl)boronic Ester as the Ligand Precursor and Their Reactions with Alkynes
Tanabe, Makoto; Jiang, Jian; Yamazawa, Hideto; Osakada, Kohtaro; Ohmura, Toshimichi; Suginome, Michinori; Organometallics 30 (2011) 3981–; doi:10.1021/om200156g

data_4064519
_publ_section_title
;
 Dinuclear Palladium and Platinum Complexes with Bridging Silylene
 Ligands. Preparation Using (Aminosilyl)boronic Ester as the Ligand
 Precursor and Their Reactions with Alkynes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3981
_journal_paper_doi               10.1021/om200156g
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C47.50 H52 P2 Pd Si2'
_chemical_formula_sum            'C47.5 H52 P2 Pd Si2'
_chemical_formula_weight         847.45
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.812(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.1130(14)
_cell_length_b                   20.167(3)
_cell_length_c                   21.381(3)
_cell_measurement_reflns_used    10754
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     4329.8(11)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33888
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.510
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9841
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                7738
_reflns_number_total             9841
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om200156g_si_001.cif
_cod_data_source_block           complex6
_cod_original_cell_volume        4329.7(11)
_cod_original_formula_sum        'C47.50 H52 P2 Pd Si2'
_cod_database_code               4064519