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_4120126
_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         'C49 H50 B1 O1 P3 Ru1'
_chemical_formula_sum            'C49 H50 B O P3 Ru'
_chemical_formula_weight         859.68
_chemical_name_common            4
_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                 107.815(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.261(5)
_cell_length_b                   13.944(4)
_cell_length_c                   20.315(5)
_cell_measurement_reflns_used    6049
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.311
_cell_measurement_theta_min      2.389
_cell_volume                     4655(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.1827
_diffrn_reflns_av_sigmaI/netI    0.2320
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45953
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.623
_refine_diff_density_min         -1.959
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8528
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.2072
_refine_ls_R_factor_gt           0.1084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2887
_refine_ls_wR_factor_ref         0.3209
_reflns_number_gt                3484
_reflns_number_total             8528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404910h_si_004.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C49 H50 B1 O1 P3 Ru1'
_cod_database_code               4120126