Reaction of bis(o-phosphinophenyl)silane with M(PPh(3))(4) (M = Ni, Pd, Pt): synthesis and structural analysis of η(2)-(Si-H) metal(0) and pentacoordinate silyl metal(ii) hydride complexes of the Ni triad bearing a PSiP-pincer ligand.
Takaya, Jun; Iwasawa, Nobuharu; Dalton transactions (Cambridge, England : 2003) 40 (2011) 8814–8821; doi:10.1039/c1dt10526d

data_7016456
_publ_section_title
;
 Reaction of bis(o-phosphinophenyl)silane with M(PPh(3))(4) (M = Ni,
 Pd, Pt): synthesis and structural analysis of \h(2)-(Si-H) metal(0)
 and pentacoordinate silyl metal(ii) hydride complexes of the Ni triad
 bearing a PSiP-pincer ligand.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8814
_journal_page_last               8821
_journal_paper_doi               10.1039/c1dt10526d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C55 H47 P3 Pt Si'
_chemical_formula_weight         1024.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 116.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.567(3)
_cell_length_b                   12.9268(14)
_cell_length_c                   19.692(3)
_cell_measurement_reflns_used    14326
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.9418
_cell_measurement_theta_min      2.7953
_cell_volume                     4463.0(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       dtprofit.ref
_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  0.1177
_diffrn_reflns_av_sigmaI/netI    0.1128
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34473
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    3.316
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.5033
_exptl_absorpt_correction_type   Multi-scan'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         6.556
_refine_diff_density_min         -5.749
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         9956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0832
_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^)+(0.1223P)^2^+7.3400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2223
_reflns_number_gt                7292
_reflns_number_total             9956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10526d.txt
_cod_data_source_block           '__HPt(II)PSiP'
_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        4463.1(9)
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               7016456