Synthesis and Characterization of B-Heterocyclic π-Radical and Its Reactivity as a Boryl Radical
Yoshitaka Aramaki; Hideki Omiya; Makoto Yamashita; Koji Nakabayashi; Shin-ichi Ohkoshi; Kyoko Nozaki; Journal of the American Chemical Society 134 (2012) 19989–19992; doi:10.1021/ja3094372

data_4118987
_publ_section_title
;
 Synthesis and Characterization of B-Heterocyclic \p-Radical and Its
 Reactivity as a Boryl Radical
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19989
_journal_page_last               19992
_journal_paper_doi               10.1021/ja3094372
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C76 H110 B2 F2 N4 O2'
_chemical_formula_weight         1171.30
_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                 104.580(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.741(4)
_cell_length_b                   9.664(2)
_cell_length_c                   22.416(5)
_cell_measurement_reflns_used    9407
_cell_measurement_temperature    93.1500
_cell_measurement_theta_max      28.1117
_cell_measurement_theta_min      2.3071
_cell_volume                     3509.8(14)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'RIGAKU/MSC Saturn CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12734
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.103
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+1.4105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                3896
_reflns_number_total             6055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3094372_si_002_3.cif
_cod_data_source_block           4
_cod_original_cell_volume        3509.9(15)
_cod_database_code               4118987