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_4120091
_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            'C36 H36 Si'
_chemical_formula_weight         496.74
_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                90.00
_cell_angle_beta                 96.848(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4831(4)
_cell_length_b                   16.0535(6)
_cell_length_c                   14.5104(5)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.54
_cell_volume                     2887.10(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond 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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1139
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63102
_diffrn_reflns_theta_full        30.12
_diffrn_reflns_theta_max         30.12
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.9577
_exptl_absorpt_correction_T_min  0.9468
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         8486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.9418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1765
_reflns_number_gt                5878
_reflns_number_total             8486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400306h_si_003.cif
_cod_data_source_block           cg141
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4120091