Bis(o-phosphinophenyl)silane as a Scaffold for Dynamic Behavior of H−Si and C−Si Bonds with Palladium(0)
Takaya, Jun; Iwasawa, Nobuharu; Organometallics 28 (2009) 6636–; doi:10.1021/om900874p

data_4070495
_publ_section_title
;
 Bis(o-phosphinophenyl)silane as a Scaffold for Dynamic Behavior of
 H&#x2212;Si and C&#x2212;Si Bonds with Palladium(0)
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6636
_journal_paper_doi               10.1021/om900874p
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C55 H47 P3 Pd Si'
_chemical_formula_weight         935.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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                 93.252(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.617(6)
_cell_length_b                   10.690(4)
_cell_length_c                   25.340(8)
_cell_measurement_reflns_used    10160
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      1.23
_cell_volume                     4494(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      83(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode UX-18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0988
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            58040
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         10160
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0241P)^2^+5.0394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                8418
_reflns_number_total             10160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900874p_si_002.cif
_cod_data_source_block           iwasawa2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4070495