Phosphinodi(benzylsilane) PhP{(o-C6H4CH2)SiMe2H}2: A Versatile "PSi2Hx" Pincer-Type Ligand at Ruthenium
Virginia Montiel-Palma; Miguel A. Muñoz-Hernández; Cynthia A. Cuevas-Chávez; Laure Vendier; Mary Grellier; Sylviane Sabo-Etienne; Inorganic Chemistry 52 (2013) 9798–9806; doi:10.1021/ic400703r

data_4335813
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_section_title
;
 Phosphinodi(benzylsilane) PhP{(o-C6H4CH2)SiMe2H}2: A Versatile "PSi2Hx"
 Pincer-Type Ligand at Ruthenium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9798
_journal_page_last               9806
_journal_paper_doi               10.1021/ic400703r
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C84 H132 P4 Ru2 Si4'
_chemical_formula_sum            'C84 H132 P4 Ru2 Si4'
_chemical_formula_weight         1580.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.930(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.6275(15)
_cell_length_b                   10.4778(3)
_cell_length_c                   20.726(5)
_cell_measurement_reflns_used    8279
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2933
_cell_measurement_theta_min      2.9199
_cell_measurement_wavelength     0.71073
_cell_volume                     8093(2)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0138349
_diffrn_orient_matrix_UB_12      -0.0047392
_diffrn_orient_matrix_UB_13      0.0268423
_diffrn_orient_matrix_UB_21      0.0128547
_diffrn_orient_matrix_UB_22      -0.007258
_diffrn_orient_matrix_UB_23      -0.0217484
_diffrn_orient_matrix_UB_31      0.0023653
_diffrn_orient_matrix_UB_32      0.0671485
_diffrn_orient_matrix_UB_33      -0.000459
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1123
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            79609
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.9975
_exptl_absorpt_correction_T_min  0.9520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         13787
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0191P)^2^+15.5285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                9681
_reflns_number_total             13787
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400703r_si_001_1.cif
_cod_data_source_block           Complex_3
_cod_database_code               4335813