Facile Access to the Functionalized N-Donor Stabilized Silylenes PhC(NtBu)2SiX (X = PPh2, NPh2, NCy2, NiPr2, NMe2, N(SiMe3)2, OtBu)
Azhakar, Ramachandran; Ghadwal, Rajendra S.; Roesky, Herbert W.; Wolf, Hilke; Stalke, Dietmar; Organometallics 31 (2012) 4588–; doi:10.1021/om3003762

data_4078595
_publ_section_title
;
 Facile Access to the Functionalized N-Donor Stabilized Silylenes
 PhC(NtBu)2SiX (X = PPh2, NPh2, NCy2, NiPr2, NMe2, N(SiMe3)2, OtBu)
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              4588
_journal_paper_doi               10.1021/om3003762
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C27 H33 N2 P Si'
_chemical_formula_sum            'C27 H33 N2 P Si'
_chemical_formula_weight         444.61
_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                89.190(10)
_cell_angle_beta                 86.06(2)
_cell_angle_gamma                72.470(10)
_cell_formula_units_Z            2
_cell_length_a                   8.384(3)
_cell_length_b                   9.073(3)
_cell_length_c                   17.254(4)
_cell_measurement_reflns_used    9715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.279
_cell_measurement_theta_min      2.354
_cell_volume                     1248.5(7)
_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  'SHELXS in SHELXTL Version 2008/4'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode (TXS)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0104
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42389
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_correction_T_min  0.9827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/2, Sheldrick, Goettingen'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         6185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0394P)^2^+0.5038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                5753
_reflns_number_total             6185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003762_si_001.cif
_cod_data_source_block           hilke
_cod_database_code               4078595