Li±Induced σ-Bond Metathesis: Aryl for Methyl Exchange on Boron in a Methylated Monocarbadodecaborate Anion
Zbyněk Janoušek; Uwe Lehmann; Jakub Častulík; Ivana Císařová; Josef Michl; Journal of the American Chemical Society 126 (2004) 4060–4061; doi:10.1021/ja0387857

data_4112387
_publ_section_title
;
 Li+-Induced \s-Bond Metathesis: Aryl for Methyl Exchange on Boron in a
 Methylated Monocarbadodecaborate Anion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4060
_journal_page_last               4061
_journal_paper_doi               10.1021/ja0387857
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_sum            'C25 H51 B12 Br N Na O3'
_chemical_formula_weight         646.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.6320(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7000(2)
_cell_length_b                   9.99600(10)
_cell_length_c                   23.4820(3)
_cell_measurement_reflns_used    8451
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     3531.02(7)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.038
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53478
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8059
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+4.4463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                6381
_reflns_number_total             8059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0387857si20040223_121554.cif
_cod_data_source_block           JA0387857
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4112387