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_4080004
_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         'C37 H48 N4 Si, C7 H8'
_chemical_formula_sum            'C44 H56 N4 Si'
_chemical_formula_weight         669.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                97.5940(10)
_cell_angle_beta                 90.3320(10)
_cell_angle_gamma                117.1580(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8224(2)
_cell_length_b                   11.3612(2)
_cell_length_c                   17.1797(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1857.73(6)
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART 6000'
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            64943
_diffrn_reflns_theta_full        73.62
_diffrn_reflns_theta_max         73.62
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.9446
_exptl_absorpt_correction_T_min  0.8525
_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    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0525P)^2^+1.1269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                7012
_reflns_number_total             7283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301149q_si_002.cif
_cod_data_source_block           compound6
_cod_database_code               4080004
_computing_refinement_gui        'shelXle (Huebschle et al, 2011)'