Hydrodefluorination and Other Hydrodehalogenation of Aliphatic Carbon-Halogen Bonds Using Silylium Catalysis
Christos Douvris; C. M. Nagaraja; Chun-Hsing Chen; Bruce M. Foxman; Oleg V. Ozerov; Journal of the American Chemical Society 132 (2010) 4946–4953; doi:10.1021/ja100605m

data_4102215
_publ_section_title
;
 Hydrodefluorination and Other Hydrodehalogenation of Aliphatic
 Carbon-Halogen Bonds Using Silylium Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4946
_journal_page_last               4953
_journal_paper_doi               10.1021/ja100605m
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C7 H21 B11 Cl6 Si1'
_chemical_formula_sum            'C7 H21 B11 Cl6 Si'
_chemical_formula_weight         464.97
_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
_audit_creation_date             08-01-25
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                109.622(4)
_cell_angle_beta                 96.022(4)
_cell_angle_gamma                92.315(4)
_cell_formula_units_Z            4
_cell_length_a                   7.5885(4)
_cell_length_b                   15.7841(10)
_cell_length_c                   18.8905(11)
_cell_measurement_reflns_used    5046
_cell_measurement_temperature    120
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     2112.6(2)
_computing_cell_refinement       'Apex2, (Bruker AXS, 2006)'
_computing_data_collection       'Apex2, (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2, (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24099
_diffrn_reflns_theta_full        25.166
_diffrn_reflns_theta_max         26.490
_diffrn_reflns_theta_min         1.154
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker AXS, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.04
_refine_diff_density_min         -1.01
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9400
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000495
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.45P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0882
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0882
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5550
_reflns_number_total             8140
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.58
_oxford_diffrn_Wilson_scale      58.47
_oxford_refine_ls_r_factor_ref   0.0766
_oxford_refine_ls_scale          0.13281(3)
_oxford_reflns_number_all        8140
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ135_0m in P-1'
_cod_data_source_file            ja100605m_si_002.cif
_cod_data_source_block           OZ135
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C7 H21 B11 Cl6 Si1'
_cod_database_code               4102215