Striking Stability of a Substituted Silicon(II) Bis(trimethylsilyl)amide and the Facile Si-Me Bond Cleavage without a Transition Metal Catalyst
Sakya S. Sen; Jakob Hey; Regine Herbst-Irmer; Herbert W. Roesky; Dietmar Stalke; Journal of the American Chemical Society 133 (2011) 12311–12316; doi:10.1021/ja205369h

data_4106536
_publ_section_title
;
 Striking Stability of a Substituted Silicon(II) Bis(trimethylsilyl)amide
 and the Facile Si-Me Bond Cleavage without a Transition Metal Catalyst
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12311
_journal_page_last               12316
_journal_paper_doi               10.1021/ja205369h
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C21 H41 N3 Si3'
_chemical_formula_weight         419.84
_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                95.67(2)
_cell_angle_beta                 103.27(3)
_cell_angle_gamma                93.68(2)
_cell_formula_units_Z            2
_cell_length_a                   8.439(2)
_cell_length_b                   10.943(2)
_cell_length_c                   14.350(3)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.163
_cell_measurement_theta_min      2.490
_cell_volume                     1278.3(5)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2008.11'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II with D8'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'INCOATEC I\mS microfocus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0094
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41035
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5420
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0368P)^2^+0.4754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                5141
_reflns_number_total             5420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205369h_si_002.cif
_cod_data_source_block           2
_cod_database_code               4106536