Synthesis, Structure, and Bonding of Stable Dialkylsilaketenimines
Takashi Abe; Takeaki Iwamoto; Chizuko Kabuto; Mitsuo Kira; Journal of the American Chemical Society 128 (2006) 4228–4229; doi:10.1021/ja057917o

data_4110497
_publ_section_title
;
 Synthesis, Structure, and Bonding of Stable Dialkylsilaketenimines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4228
_journal_page_last               4229
_journal_paper_doi               10.1021/ja057917o
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C29 H57 N Si5'
_chemical_formula_weight         560.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.5890(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.737(3)
_cell_length_b                   18.390(5)
_cell_length_c                   16.713(5)
_cell_measurement_reflns_used    8504
_cell_measurement_temperature    243.1500
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.2181
_cell_volume                     3546.0(17)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243.1500
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8077
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.1500
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         8077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0318P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                4400
_reflns_number_total             8077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057917osi20051122_034616.cif
_cod_data_source_block           dialkylsilylene-DIPNC
_cod_original_cell_volume        3545.9(17)
_cod_database_code               4110497