Reactivity Studies of Heteroleptic Silylenes PhC(NtBu)2SiX (X = NPh2, NMe2) toward Selected Azides
Azhakar, Ramachandran; Roesky, Herbert W.; Holstein, Julian J.; Pröpper, Kevin; Dittrich, Birger; Organometallics 32 (2013) 358–; doi:10.1021/om301149q

data_4080005
_publ_section_title
;
 Reactivity Studies of Heteroleptic Silylenes PhC(NtBu)2SiX (X = NPh2,
 NMe2) toward Selected Azides
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              358
_journal_paper_doi               10.1021/om301149q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C27 H44 N4 Si'
_chemical_formula_sum            'C27 H44 N4 Si'
_chemical_formula_weight         452.75
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.587(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4541(10)
_cell_length_b                   11.4512(7)
_cell_length_c                   13.5293(9)
_cell_measurement_temperature    100(2)
_cell_volume                     2628.4(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2009)'
_computing_data_collection       'Apex2 (Bruker AXS, 2009)'
_computing_molecular_graphics    'shelXle (Huebschle et al, 2011)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 6000 CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'INCOATEC multilayer optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28606
_diffrn_reflns_theta_full        59.30
_diffrn_reflns_theta_max         59.30
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.9126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS version 2008/2, multi-scan. (G. M. Sheldrick, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3793
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0974
_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^)+(0.0186P)^2^+19.9356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2171
_refine_ls_wR_factor_ref         0.2341
_reflns_number_gt                2884
_reflns_number_total             3793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301149q_si_002.cif
_cod_data_source_block           compound8
_cod_database_code               4080005
_computing_refinement_gui        'shelXle (Huebschle et al, 2011)'