A B-B Bond-Containing Polycyclic π-Electron System: Dithieno-1,2-dihydro-1,2-diborin and Its Dianion
Atsushi Wakamiya; Kenji Mori; Takafumi Araki; Shigehiro Yamaguchi; Journal of the American Chemical Society 131 (2009) 10850–10851; doi:10.1021/ja905007s

data_4104864
_publ_section_title
;
 A B-B Bond-Containing Polycyclic \p-Electron System:
 Dithieno-1,2-dihydro-1,2-diborin and Its Dianion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10850
_journal_page_last               10851
_journal_paper_doi               10.1021/ja905007s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C54 H96 B2 K2 N6 O13.5 S2'
_chemical_formula_weight         1209.31
_chemical_melting_point_gt       573
_chemical_name_systematic
; 
Bis[potassium[2.2.2]cryptand]salt of 
1,2-bis(dimethylamino)[3,2-c:2',3'-e]
dithieno-1,2-dihydro-1,2-diborin
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 99.229(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.835(4)
_cell_length_b                   24.235(7)
_cell_length_c                   38.188(11)
_cell_measurement_reflns_used    8664
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0043
_cell_volume                     12638(6)
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            50088
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_correction_T_min  0.9462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             5200
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         11126
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0740
_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/[?^2^(Fo^2^)+(0.0898P)^2^+27.8385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.1945
_reflns_number_gt                9380
_reflns_number_total             11126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905007s_si_002_2.cif
_cod_data_source_block           comp1-dianion
_cod_original_cell_volume        12639(6)
_cod_original_formula_sum        'C54 H96 B2 K2 N6 O13.50 S2'
_cod_database_code               4104864