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_4118033
_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
'C66 H69 B F K N2 O8 S2, 0.53(C6 H6), 0.35(C6 H14)'
_chemical_formula_sum            'C142.64 H154.28 B2 F2 K2 N4 O16 S4'
_chemical_formula_weight         2446.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                74.793(12)
_cell_angle_beta                 73.353(12)
_cell_angle_gamma                62.6114(10)
_cell_formula_units_Z            2
_cell_length_a                   18.9618(4)
_cell_length_b                   19.21270(10)
_cell_length_c                   20.76030(10)
_cell_measurement_reflns_used    10777
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.5
_cell_volume                     6357.7(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63997
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2111
_refine_ls_number_reflns         22284
_refine_ls_number_restraints     2052
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1783
_refine_ls_R_factor_gt           0.1107
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2914
_refine_ls_wR_factor_ref         0.3887
_reflns_number_gt                10851
_reflns_number_total             22284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3036042_si_004.cif
_cod_data_source_block           compound_5FKcryptand
_cod_original_cell_volume        6357.72(41)
_cod_database_code               4118033