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_4105734
_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            'C35 H32 B F10 N O2'
_chemical_formula_weight         699.43
_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                 103.898(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.4261(7)
_cell_length_b                   10.3146(3)
_cell_length_c                   31.7887(11)
_cell_measurement_reflns_used    10112
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     6501.4(4)
_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 0.906
_diffrn_measured_fraction_theta_max 0.906
_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  0.117
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            55470
_diffrn_reflns_theta_full        67.61
_diffrn_reflns_theta_max         67.61
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.8976
_exptl_absorpt_correction_T_min  0.8789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         10652
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1585
_refine_ls_R_factor_gt           0.0795
_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^)+(0.1143P)^2^+7.4812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2058
_refine_ls_wR_factor_ref         0.2648
_reflns_number_gt                5332
_reflns_number_total             10652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1092369_si_009.cif
_cod_data_source_block           erk5505
_cod_database_code               4105734