A Pentacoordinate Boron-Containing π-Electron System with Cl-B-Cl Three-Center Four-Electron Bonds
Chuandong Dou; Shohei Saito; Shigehiro Yamaguchi; Journal of the American Chemical Society 135 (2013) 9346–9349; doi:10.1021/ja404724f

data_4119997
_publ_contact_author_address
'Nagoya University, Furo, Chikusa, Nagoya, Japan'
_publ_contact_author_email       yamaguchi@chem.nagoya-u.c.jp
_publ_contact_author_fax         +81-52-789-5947
_publ_contact_author_name        'Shigehiro Yamaguchi'
_publ_contact_author_phone       +81-52-789-2291
_publ_section_title
;
 A Pentacoordinate Boron-Containing \p-Electron System with Cl-B-Cl
 Three-Center Four-Electron Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9346
_journal_page_last               9349
_journal_paper_doi               10.1021/ja404724f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C76 H62 B2 Cl4 O4, 3(C H Cl3)'
_chemical_formula_sum            'C79 H65 B2 Cl13 O4'
_chemical_formula_weight         1560.78
_chemical_name_systematic
;
6,13-Bis(1,8-dichloro-4,5-dimesityloxyanthr-9-yl)-
6,13-dihydro-6,13-diboraanthracene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-05-04 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 106.1668(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.553(4)
_cell_length_b                   14.752(3)
_cell_length_c                   17.366(4)
_cell_measurement_reflns_used    7659
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.9975
_cell_measurement_theta_min      1.4565
_cell_volume                     3580.8(15)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30391
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.160
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6498
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0839
_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^)+(0.1402P)^2^+9.8757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2311
_refine_ls_wR_factor_ref         0.2393
_reflns_number_gt                5750
_reflns_number_total             6498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404724f_si_001_1.cif
_cod_data_source_block           compound4
_cod_database_code               4119997