Synthesis and structure of stable base-free dialkylsilanimines
Iwamoto, Takeaki; Ohnishi, Nobuyoshi; Gui, Zhenyu; Ishida, Shintaro; Isobe, Hiroyuki; Maeda, Satoshi; Ohno, Koichi; Kira, Mitsuo; New Journal of Chemistry 34 (2010) 1637–; doi:10.1039/c0nj00121j

data_7053519
_publ_section_title
;
 Synthesis and structure of stable base-free dialkylsilanimines
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1637
_journal_paper_doi               10.1039/c0nj00121j
_journal_volume                  34
_journal_year                    2010
_chemical_formula_sum            'C23 H47 N Si5'
_chemical_formula_weight         478.07
_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                115.304(2)
_cell_angle_beta                 95.635(2)
_cell_angle_gamma                107.048(2)
_cell_formula_units_Z            2
_cell_length_a                   10.844(2)
_cell_length_b                   11.874(3)
_cell_length_c                   13.349(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1435.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13815
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_correction_T_min  0.9499
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0462P)^2^+0.6223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                4087
_reflns_number_total             5027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00121j.txt
_cod_data_source_block           N-benzylsilanimines
_cod_original_cell_volume        1435.1(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053519