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_4106128
_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            'C30.25 H31 B S'
_chemical_formula_weight         437.42
_chemical_melting_point          384.9
_chemical_name_common            cmpd3
_chemical_name_systematic
; 
 (benzothieno)(benzo)borole
;
_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                71.525(13)
_cell_angle_beta                 77.197(15)
_cell_angle_gamma                76.333(12)
_cell_formula_units_Z            4
_cell_length_a                   12.580(3)
_cell_length_b                   14.116(4)
_cell_length_c                   16.020(4)
_cell_measurement_reflns_used    6029
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.5050
_cell_measurement_theta_min      2.9098
_cell_volume                     2588.4(12)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0636
_diffrn_reflns_av_sigmaI/netI    0.1003
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16894
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.9930
_exptl_absorpt_correction_T_min  0.9861
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         8857
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1184P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2308
_reflns_number_gt                5239
_reflns_number_total             8857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2019977_si_004.cif
_cod_data_source_block           ai-bs
_cod_original_cell_volume        2588.4(11)
_cod_database_code               4106128