Reactivity of Stable Heteroleptic Silylene PhC(NtBu)2SiNPh2toward Diazobenzene andN-Benzylidineaniline
Azhakar, Ramachandran; Roesky, Herbert W.; Wolf, Hilke; Stalke, Dietmar; Organometallics 31 (2012) 8608–; doi:10.1021/om300999e

data_4079727
_publ_section_title
;
 Reactivity of Stable Heteroleptic Silylene PhC(NtBu)2SiNPh2toward
 Diazobenzene andN-Benzylidineaniline
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              8608
_journal_paper_doi               10.1021/om300999e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C40 H44 N4 Si'
_chemical_formula_sum            'C40 H44 N4 Si'
_chemical_formula_weight         608.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 97.84(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.486(4)
_cell_length_b                   15.541(5)
_cell_length_c                   19.133(6)
_cell_measurement_reflns_used    6978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.101
_cell_measurement_theta_min      2.218
_cell_volume                     3383.4(19)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.4-1'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'INCOATEC Mo Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43791
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.397
_diffrn_reflns_theta_min         1.694
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.9343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/2, Sheldrick, Goettingen'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+1.8769P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5328
_reflns_number_total             6921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om300999e_si_002.cif
_cod_data_source_block           p21c_a
_cod_database_code               4079727
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.992
_diffrn_reflns_sigmai/neti       0.0381
_shelxl_version_number           2012-4
_shelx_res_checksum              49626
_shelx_hkl_checksum              76365