Reaction of Aminodihydropentalenes with HB(C6F5)2: The Crucial Role of Dihydrogen Elimination
Bao-Hua Xu; Gerald Kehr; Roland Fröhlich; Stefan Grimme; Gerhard Erker; Journal of the American Chemical Society 133 (2011) 3480–3491; doi:10.1021/ja1092369

data_4105733
_publ_section_title
;
 Reaction of Aminodihydropentalenes with HB(C6F5)2: The Crucial Role of
 Dihydrogen Elimination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3480
_journal_page_last               3491
_journal_paper_doi               10.1021/ja1092369
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C24.5 H20 B Cl2 F10 N'
_chemical_formula_weight         600.13
_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                88.834(4)
_cell_angle_beta                 78.248(3)
_cell_angle_gamma                74.602(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4976(5)
_cell_length_b                   12.4411(8)
_cell_length_c                   12.8064(8)
_cell_measurement_reflns_used    4340
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     1427.40(15)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19428
_diffrn_reflns_theta_full        67.12
_diffrn_reflns_theta_max         67.12
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    2.787
_exptl_absorpt_correction_T_max  0.8288
_exptl_absorpt_correction_T_min  0.3363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       column
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0061(14)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4792
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1811P)^2^+0.8419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2429
_refine_ls_wR_factor_ref         0.2608
_reflns_number_gt                3882
_reflns_number_total             4792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1092369_si_008.cif
_cod_data_source_block           erk5544
_cod_original_formula_sum        'C24.50 H20 B Cl2 F10 N'
_cod_database_code               4105733