Polycyclic π-Electron System with Boron at Its Center
Shohei Saito; Kyohei Matsuo; Shigehiro Yamaguchi; Journal of the American Chemical Society 134 (2012) 9130–9133; doi:10.1021/ja3036042

data_4118034
_publ_section_title
;
 Polycyclic \p-Electron System with Boron at Its Center
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9130
_journal_page_last               9133
_journal_paper_doi               10.1021/ja3036042
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         '2(C30 H17 B S2), C2 H4 Cl2'
_chemical_formula_sum            'C62 H38 B2 Cl2 S4'
_chemical_formula_weight         1003.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 97.9550(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.584(7)
_cell_length_b                   20.312(8)
_cell_length_c                   26.769(10)
_cell_measurement_reflns_used    8930
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.9975
_cell_measurement_theta_min      2.0549
_cell_volume                     9469(6)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  VariMax
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            78085
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1335
_refine_ls_number_reflns         16390
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.1048
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+17.7077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2376
_refine_ls_wR_factor_ref         0.2569
_reflns_number_gt                12438
_reflns_number_total             16390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3036042_si_005.cif
_cod_data_source_block           compound_8a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4118034