Two-Step Synthesis of Boron-Fused Double Helicenes.
Katayama, Takazumi; Nakatsuka, Soichiro; Hirai, Hiroki; Yasuda, Nobuhiro; Kumar, Jatish; Kawai, Tsuyoshi; Hatakeyama, Takuji; Journal of the American Chemical Society 138 (2016) 5210–5213; doi:10.1021/jacs.6b01674

data_4125028
_publ_section_title
;
 Two-Step Synthesis of Boron-Fused Double Helicenes.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5210
_journal_page_last               5213
_journal_paper_doi               10.1021/jacs.6b01674
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C30 H16 B2 O4'
_chemical_formula_sum            'C30 H16 B2 O4'
_chemical_formula_weight         462.05
_chemical_name_systematic
; 
 TerarylB2O4-1  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.036(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3686(4)
_cell_length_b                   25.6303(12)
_cell_length_c                   9.8925(4)
_cell_measurement_reflns_used    10933
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.86
_cell_volume                     2121.84(17)
_computing_cell_refinement       'RIGAKU RAPID AUTO'
_computing_data_collection       'RIGAKU RAPID AUTO'
_computing_data_reduction        'RIGAKU RAPID AUTO'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 29
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_radiation_monochromator  'Si (111) Channel Cut'
_diffrn_radiation_source         'Synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78202
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10933
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.9450
_exptl_absorpt_correction_T_min  0.9450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' ABSCOR (T. Higashi, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.007(2)
_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   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0370P)^2^+0.7532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                2718
_reflns_number_total             3607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b01674_si_002.cif
_cod_data_source_block           B2O4
_cod_depositor_comments          'Adding full bibliography for 4125028.cif.'
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4125028