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_4120124
_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         'C61 H60 B N P3 Si Ru, C6 H4 F'
_chemical_formula_sum            'C67 H64 B F N P3 Ru Si'
_chemical_formula_weight         1135.07
_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                75.370(3)
_cell_angle_beta                 84.383(4)
_cell_angle_gamma                70.341(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1029(11)
_cell_length_b                   13.4322(10)
_cell_length_c                   17.4919(12)
_cell_measurement_reflns_used    9710
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.337
_cell_measurement_theta_min      2.261
_cell_volume                     2804.9(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            128460
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       plate
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.432
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         10220
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+6.9383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                8236
_reflns_number_total             10220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404910h_si_002.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C67 H64 B F1 N P3 Ru Si'
_cod_database_code               4120124