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_4120090
_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            'C53.5 H65 Cl Si'
_chemical_formula_weight         771.60
_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                96.1160(10)
_cell_angle_beta                 97.7080(10)
_cell_angle_gamma                100.8650(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0405(2)
_cell_length_b                   11.9574(2)
_cell_length_c                   21.3996(4)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.32
_cell_volume                     2230.57(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond 3.2 (Crystal Impact, 2010)'
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43021
_diffrn_reflns_theta_full        28.16
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.9546
_exptl_absorpt_correction_T_min  0.9406
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         10814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0664P)^2^+1.5411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                8378
_reflns_number_total             10814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400306h_si_002.cif
_cod_data_source_block           CG098
_cod_original_cell_volume        2230.57(7)
_cod_original_formula_sum        'C53.50 H65 Cl Si'
_cod_database_code               4120090