Silane-Isocyanide Coupling Involving 1,1-Insertion of XylNC into the Si-H Bond of a σ-Silane Ligand
Mark C. Lipke; T. Don Tilley; Journal of the American Chemical Society 135 (2013) 10298–10301; doi:10.1021/ja404910h

data_4120125
_publ_section_title
;
 Silane-Isocyanide Coupling Involving 1,1-Insertion of XylNC into the Si-H
 Bond of a \s-Silane Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10298
_journal_page_last               10301
_journal_paper_doi               10.1021/ja404910h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C66 H60 B N P3 Ru Si'
_chemical_formula_sum            'C66 H60 B N P3 Ru Si'
_chemical_formula_weight         1100.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.192(6)
_cell_angle_beta                 81.260(7)
_cell_angle_gamma                62.614(6)
_cell_formula_units_Z            2
_cell_length_a                   12.1477(15)
_cell_length_b                   13.1112(15)
_cell_length_c                   20.504(2)
_cell_measurement_reflns_used    1551
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.06
_cell_measurement_theta_min      2.323
_cell_volume                     2853.1(6)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2637
_diffrn_reflns_av_sigmaI/netI    0.4377
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38927
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       plate
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10429
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.2493
_refine_ls_R_factor_gt           0.0978
_refine_ls_shift/su_max          0.367
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.2340
_reflns_number_gt                3472
_reflns_number_total             10429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404910h_si_003.cif
_cod_data_source_block           shelxl
_cod_database_code               4120125