Anthryl-Substituted 3-Silylene-2-silaaziridine Obtained by Isomerization of Disilacyclopropanimine: An Exocyclic Silene Showing a Distinct Intramolecular Charge Transfer Transition
Takeaki Iwamoto; Nobuyoshi Ohnishi; Naohiko Akasaka; Koichi Ohno; Shintaro Ishida; Journal of the American Chemical Society 135 (2013) 10606–10609; doi:10.1021/ja404045f

data_4120147
_publ_section_title
;
 Anthryl-Substituted 3-Silylene-2-silaaziridine Obtained by Isomerization
 of Disilacyclopropanimine: An Exocyclic Silene Showing a Distinct
 Intramolecular Charge Transfer Transition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10606
_journal_page_last               10609
_journal_paper_doi               10.1021/ja404045f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C39 H65 N Si6'
_chemical_formula_weight         716.46
_chemical_name_systematic
; 
 ? 
;
_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                108.521(4)
_cell_angle_beta                 106.022(3)
_cell_angle_gamma                103.615(3)
_cell_formula_units_Z            4
_cell_length_a                   11.687(2)
_cell_length_b                   20.969(4)
_cell_length_c                   21.104(5)
_cell_measurement_reflns_used    4035
_cell_measurement_temperature    273
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     4407.4(16)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21104
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.9788
_exptl_absorpt_correction_T_min  0.9583
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       prism
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.617
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         15228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+2.5784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                10503
_reflns_number_total             15228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404045f_si_002_2.cif
_cod_data_source_block           disilacyclopropanimine_2b_(naphthyl,no15)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4120147