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_4070496
_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            'C60 H55 P3 Pd Si'
_chemical_formula_weight         1003.44
_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                78.139(9)
_cell_angle_beta                 84.032(11)
_cell_angle_gamma                79.523(9)
_cell_formula_units_Z            2
_cell_length_a                   12.462(3)
_cell_length_b                   12.602(3)
_cell_length_c                   16.283(3)
_cell_measurement_temperature    123(2)
_cell_volume                     2455.0(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  CCDC
_diffrn_measurement_method       'omega and phi scans'
_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  0.1534
_diffrn_reflns_av_sigmaI/netI    0.4249
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16666
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prim
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.794
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8437
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.794
_refine_ls_R_factor_all          0.2430
_refine_ls_R_factor_gt           0.0743
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                2643
_reflns_number_total             8437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900874p_si_002.cif
_cod_data_source_block           iwasawa4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2455.0(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070496