Hydrogen-Substituted Osmium Silylene Complexes: Effect of Charge Localization on Catalytic Hydrosilation
Paul G. Hayes; Chad Beddie; Michael B. Hall; Rory Waterman; T. Don Tilley; Journal of the American Chemical Society 128 (2006) 428–429; doi:10.1021/ja057494q

data_4110374
_publ_section_title
;
 Hydrogen-Substituted Osmium Silylene Complexes: Effect of Charge
 Localization on Catalytic Hydrosilation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              428
_journal_page_last               429
_journal_paper_doi               10.1021/ja057494q
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C34 H61 Os P Si'
_chemical_formula_weight         719.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.7370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.326(3)
_cell_length_b                   9.2322(8)
_cell_length_c                   24.865(2)
_cell_measurement_temperature    135(2)
_cell_volume                     6970.2(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      135(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0873
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14967
_diffrn_reflns_theta_full        24.75
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    3.759
_exptl_absorpt_correction_T_max  0.7284
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.698
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                4023
_reflns_number_total             5758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057494qsi20051102_052435.cif
_cod_data_source_block           ph01m
_cod_original_cell_volume        6970.3(11)
_cod_database_code               4110374