Dibenzosilanorbornadienyl Cations and Their Fragmentation into Silyliumylidenes
Claudia Gerdes; Wolfgang Saak; Detlev Haase; Thomas Müller; Journal of the American Chemical Society 135 (2013) 10353–10361; doi:10.1021/ja400306h

data_4120092
_publ_section_title
;
 Dibenzosilanorbornadienyl Cations and Their Fragmentation into
 Silyliumylidenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10353
_journal_page_last               10361
_journal_paper_doi               10.1021/ja400306h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C76 H38 B F32 N Si'
_chemical_formula_weight         1611.97
_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                90.417(3)
_cell_angle_beta                 102.865(3)
_cell_angle_gamma                105.219(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2363(4)
_cell_length_b                   18.2469(9)
_cell_length_c                   19.1570(9)
_cell_measurement_reflns_used    2971
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      19.19
_cell_measurement_theta_min      2.40
_cell_volume                     3357.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1201
_diffrn_reflns_av_sigmaI/netI    0.1734
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50210
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_correction_T_min  0.9497
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         15448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.2057
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                5889
_reflns_number_total             15448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400306h_si_004.cif
_cod_data_source_block           CG073I
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4120092