High Electrophilicity at Silicon in η3-Silane σ-Complexes: Lewis Base Adducts of a Silane Ligand, Featuring Octahedral Silicon and Three Ru-H-Si Interactions
Mark C. Lipke; T. Don Tilley; Journal of the American Chemical Society 133 (2011) 16374–16377; doi:10.1021/ja207169e

data_4106970
_publ_section_title
;
 High Electrophilicity at Silicon in \h3-Silane \s-Complexes: Lewis Base
 Adducts of a Silane Ligand, Featuring Octahedral Silicon and Three
 Ru-H-Si Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16374
_journal_page_last               16377
_journal_paper_doi               10.1021/ja207169e
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C64 H64 B1 N2 P3 Ru Si, C7 H7'
_chemical_formula_sum            'C71 H71 B N2 P3 Ru Si'
_chemical_formula_weight         1185.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.752(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4177(16)
_cell_length_b                   24.646(3)
_cell_length_c                   20.125(2)
_cell_measurement_reflns_used    69994
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      25.367
_cell_measurement_theta_min      2.250
_cell_volume                     6621.7(13)
_computing_cell_refinement       'Bruker SAINT v. 7.07'
_computing_data_collection       'Bruker APEX2 v.2.1-4'
_computing_data_reduction        'Bruker SAINT v. 7.07'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      158(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX I'
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            113677
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_platon_squeeze_details
;
;
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         12131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+11.9240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                10877
_reflns_number_total             12131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja207169e_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        6621.5(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C71 H71 B1 N2 P3 Ru Si'
_cod_database_code               4106970