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_4109550
_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            'C79 H124 B2 Cl2 F2 N4'
_chemical_formula_weight         1260.34
_chemical_name_systematic
;
 ?
;
_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                78.656(3)
_cell_angle_beta                 77.688(3)
_cell_angle_gamma                72.650(3)
_cell_formula_units_Z            2
_cell_length_a                   11.402(3)
_cell_length_b                   17.934(5)
_cell_length_c                   21.197(5)
_cell_measurement_reflns_used    3311
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      19.33
_cell_measurement_theta_min      2.28
_cell_volume                     4000.7(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0822
_diffrn_reflns_av_sigmaI/netI    0.1535
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35977
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_correction_T_min  0.9570
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;

Difference electron density maps revealed the presence of disordered 
lattice 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 was found, comprising a 
total volume of 449.3 A3 and contributing a total of 72.3 electrons. 
The void was thus assigned to 2 disordered CH2Cl2 molecules, which 
contribute 2x42 = 84 electrons, and ocuppy about 120 A3 in space. 
The smaller electron numbers and larger volume of the void may be 
a result of the disorder. The contributions have been included in 
all derived crystal quantities although the precise composition 
of the lattice solvate is somewhat speculative.
;
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0075(12)
_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   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         14060
_refine_ls_number_restraints     454
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1936
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2551
_refine_ls_wR_factor_ref         0.2949
_reflns_number_gt                5463
_reflns_number_total             14060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0725652si20070517_103453.cif
_cod_data_source_block           sun4sqz
_cod_original_cell_volume        4000.7(17)
_cod_database_code               4109550