Selective Silylation of Nitriles with an NHC-Stabilized Silylene to 1,2-Disilylimines and Subsequent Synthesis of Silaaziridines
Li, Jianfeng; Ma, Bing; Cui, Chunming; Organometallics 35 (2016) 1358–; doi:10.1021/acs.organomet.6b00152

data_4086508
_publ_section_title
;
 Selective Silylation of Nitriles with an NHC-Stabilized Silylene to
 1,2-Disilylimines and Subsequent Synthesis of Silaaziridines
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1358
_journal_paper_doi               10.1021/acs.organomet.6b00152
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C41 H60 N4 Si2, C4 H10 O'
_chemical_formula_sum            'C45 H70 N4 O Si2'
_chemical_formula_weight         739.23
_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                 98.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.804(3)
_cell_length_b                   20.954(4)
_cell_length_c                   15.085(3)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9183
_cell_measurement_theta_min      1.6764
_cell_volume                     4624.7(16)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_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      113(2)
_diffrn_detector_area_resol_mean 14.6
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rigaku Saturn 724CCD camera'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Multilayer
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42790
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9802
_exptl_absorpt_correction_T_min  0.9758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0064(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+1.1811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1781
_reflns_number_gt                7880
_reflns_number_total             10685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00152_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4625.0(16)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4086508