Enhancing Electron Accepting Ability of Triarylboron via π-Conjugation with 2,2'-Bipy and Metal Chelation: 5,5'-Bis(BMes2)-2,2'-bipy and Its Metal Complexes
Yi Sun; Nicole Ross; Shu-Bin Zhao; Krista Huszarik; Wen-Li Jia; Rui-Yao Wang; Donal Macartney; Suning Wang; Journal of the American Chemical Society 129 (2007) 7510–7511; doi:10.1021/ja0725652

data_4109549
_publ_section_title
;
 Enhancing Electron Accepting Ability of Triarylboron via \p-Conjugation
 with 2,2'-Bipy and Metal Chelation: 5,5'-Bis(BMes2)-2,2'-bipy and Its
 Metal Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7510
_journal_page_last               7511
_journal_paper_doi               10.1021/ja0725652
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C54 H66 B2 N2 O2'
_chemical_formula_weight         796.71
_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                 107.649(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.940(3)
_cell_length_b                   8.2549(18)
_cell_length_c                   20.299(4)
_cell_measurement_temperature    180(2)
_cell_volume                     2385.6(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.1469
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13228
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   'empirical (multi-scans)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .1
_platon_squeeze_details
;

Difference electron density maps revealed the presence of disordered 
THF solvate molecules, which were ultimately modeled through the
use of the SQUEEZE subroutine of the PLATON software suite. PLATON 
Reference: P. v.d. Sluis & A.L. Spek. Acta Cryst. (1990), A46, 194. 
One solvent accessible void per lattice were found, comprising a 
total volume of 578.4 A3 and contributing a total of 158.0 electrons. 
The void was thus assigned to 4 disordered THF molecules, which 
contribute 4x40 = 160 electrons, and ocuppy about 400 A3 in space. 
The larger volume of the void may be a result of the disorder. The
contributions have been included in all derived crystal quantities. 
;
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                1549
_reflns_number_total             4194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0725652si20070517_103403.cif
_cod_data_source_block           nicole1
_cod_database_code               4109549