Thiophene-Fused Ladder Boroles with High Antiaromaticity
Azusa Iida; Shigehiro Yamaguchi; Journal of the American Chemical Society 133 (2011) 6952–6955; doi:10.1021/ja2019977

data_4106127
_publ_contact_author_address
;Department of chemistry, Graduate school of science, Nagoya university
Furo, Chikusa, Nagoya, 464-8602, Japan
;
_publ_contact_author_email       yamaguchi.shigehiro@b.mbox.nagoya-u.ac.jp
_publ_contact_author_fax         +81527895947
_publ_contact_author_name        'Yamaguchi Shigehiro'
_publ_contact_author_phone       +81527892291
_publ_section_title
;
 Thiophene-Fused Ladder Boroles with High Antiaromaticity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6952
_journal_page_last               6955
_journal_paper_doi               10.1021/ja2019977
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C29 H43 B S2 Si2'
_chemical_formula_weight         522.74
_chemical_melting_point          411.1
_chemical_name_common            cmpd2
_chemical_name_systematic
; 
 dithienoborole
;
_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                101.036(3)
_cell_angle_beta                 106.603(3)
_cell_angle_gamma                105.435(3)
_cell_formula_units_Z            2
_cell_length_a                   10.698(4)
_cell_length_b                   11.602(4)
_cell_length_c                   14.185(5)
_cell_measurement_reflns_used    3604
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.5050
_cell_measurement_theta_min      3.0357
_cell_volume                     1556.7(10)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'ORTEP 3 for windows'
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.1018
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10529
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       plate
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1472
_reflns_number_gt                3538
_reflns_number_total             5365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2019977_si_003.cif
_cod_data_source_block           ai-sbs
_cod_original_cell_volume        1556.6(9)
_cod_database_code               4106127