Silylene Extrusion from Organosilanes via Double Geminal Si-H Bond Activation by a Cp*Ru(κ2-P,N)+ Complex: Observation of a Key Stoichiometric Step in the Glaser-Tilley Alkene Hydrosilylation Mechanism
Matthew A. Rankin; Darren F. MacLean; Gabriele Schatte; Robert McDonald; Mark Stradiotto; Journal of the American Chemical Society 129 (2007) 15855–15864; doi:10.1021/ja0768800

data_4110320
_publ_contact_author_address
; Department of Chemistry
  Dalhousie University
  Dalhousie, Nova Scotia B3H 4J3
  Canada
;
_publ_contact_author_email       mark.stradiotto@dal.ca
_publ_contact_author_fax         '001 902 494 1310'
_publ_contact_author_name        'Dr Mark Stradiotto'
_publ_contact_author_phone       '001 902 494 7190'
_publ_section_title
;
 Silylene Extrusion from Organosilanes via Double Geminal Si-H Bond
 Activation by a Cp*Ru(\k2-P,N)+ Complex: Observation of a Key
 Stoichiometric Step in the Glaser-Tilley Alkene Hydrosilylation Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15855
_journal_page_last               15864
_journal_paper_doi               10.1021/ja0768800
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C33 H48 N P Ru Si'
_chemical_formula_sum            'C33 H48 N P Ru Si'
_chemical_formula_weight         618.85
_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                 93.3721(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.8412(11)
_cell_length_b                   14.2390(11)
_cell_length_c                   32.135(2)
_cell_measurement_reflns_used    7933
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.37
_cell_volume                     6322.4(8)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w 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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            52274
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.7515
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       prism
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         14500
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+2.6836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                12268
_reflns_number_total             14500
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0768800si20070911_011953_1.cif
_cod_data_source_block           dal0747
_cod_original_cell_volume        6322.3(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4110320