Intramolecular Halogen Stabilization of Silylium Ions Directs Gearing Dynamics
Paola Romanato; Simon Duttwyler; Anthony Linden; Kim K. Baldridge; Jay S. Siegel; Journal of the American Chemical Society 132 (2010) 7828–7829; doi:10.1021/ja9109665

data_4102552
_publ_contact_author_address
; Institute of Organic Chemistry
   University of Z\"urich
   Winterthurerstrasse 190
   CH-8057 Z\"urich
   Switzerland
;
_publ_contact_author_email       alinden@oci.uzh.ch
_publ_contact_author_fax         '41 44 635 6812'
_publ_contact_author_name        'Dr. Anthony Linden'
_publ_contact_author_phone       '41 44 635 4228'
_publ_section_title
;
 Intramolecular Halogen Stabilization of Silylium Ions Directs Gearing
 Dynamics
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7828
_journal_page_last               7829
_journal_paper_doi               10.1021/ja9109665
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'0.645(C24 H23 F4 O Si 1+), 1.355(C24 H25 F4 O Si 1+), 2(C24 B F20 1-), C6 H14'
_chemical_formula_sum            'C102 H62.71 B2 F48 O2 Si2'
_chemical_formula_weight         2310.03
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2009-12-11
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.7190(13)
_cell_angle_beta                 76.9370(11)
_cell_angle_gamma                79.5644(12)
_cell_formula_units_Z            2
_cell_length_a                   15.9428(4)
_cell_length_b                   17.3376(3)
_cell_length_c                   19.1253(3)
_cell_measurement_reflns_used    50720
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     4965.13(17)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 '65 mm CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       '\w scans with \k offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590 sealed tube generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            69174
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2321
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0037(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1425
_refine_ls_number_reflns         17366
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+1.1489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                12924
_reflns_number_total             17369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9109665_si_002.cif
_cod_data_source_block           1a.THF_1a.Et2O
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4102552