Four-Step Synthesis of B<sub>2</sub>N<sub>2</sub>-Embedded Corannulene.
Nakatsuka, Soichiro; Yasuda, Nobuhiro; Hatakeyama, Takuji; Journal of the American Chemical Society 140 (2018) 13562–13565; doi:10.1021/jacs.8b08197

data_4133054
_publ_section_title
;
 Four-Step Synthesis of B<sub>2</sub>N<sub>2</sub>-Embedded Corannulene.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13562
_journal_page_last               13565
_journal_paper_doi               10.1021/jacs.8b08197
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C32 H18 B2 N2'
_chemical_formula_sum            'C32 H18 B2 N2'
_chemical_formula_weight         452.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.216(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3734(4)
_cell_length_b                   18.3383(6)
_cell_length_c                   11.1315(4)
_cell_measurement_reflns_used    11530
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.115
_cell_measurement_theta_min      1.22
_cell_volume                     2052.70(13)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7813
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15943
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        27.497
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.539
_diffrn_source                   'SPring-8 BL40XU beamline'
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   1.000000
_exptl_transmission_factor_min   0.856431
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+2.3241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2604
_reflns_number_total             3508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08197_si_002.cif
_cod_data_source_block           B2N2TBC
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4133054
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              26509
_shelx_hkl_checksum              34610