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_4078596
_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_sum            'C27 H45 N3 Si'
_chemical_formula_weight         439.75
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 111.70(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.040(4)
_cell_length_b                   11.542(4)
_cell_length_c                   16.516(6)
_cell_measurement_temperature    100(2)
_cell_volume                     2663.9(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            60239
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.9979
_exptl_absorpt_correction_T_min  0.9791
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0383P)^2^+1.1391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                4601
_reflns_number_total             5422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3003762_si_002.cif
_cod_data_source_block           sad_a
_cod_original_cell_volume        2663.9(15)
_cod_database_code               4078596