Synthesis, Structures, and Properties of Core-Expanded Azacoronene Analogue: A Twisted π-System with Two N-Doped Heptagons.
Oki, Kosuke; Takase, Masayoshi; Mori, Shigeki; Shiotari, Akitoshi; Sugimoto, Yoshiaki; Ohara, Keishi; Okujima, Tetsuo; Uno, Hidemitsu; Journal of the American Chemical Society 140 (2018) 10430–10434; doi:10.1021/jacs.8b06079

data_4132757
_publ_section_title
;
 Synthesis, Structures, and Properties of Core-Expanded Azacoronene
 Analogue: A Twisted \p-System with Two N-Doped Heptagons.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10430
_journal_page_last               10434
_journal_paper_doi               10.1021/jacs.8b06079
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C74 H96 N8'
_chemical_formula_sum            'C74 H96 N8'
_chemical_formula_weight         1097.63
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.950(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   21.3574(4)
_cell_length_b                   13.0173(2)
_cell_length_c                   23.8200(5)
_cell_measurement_reflns_used    52994
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.20
_cell_measurement_theta_min      3.40
_cell_volume                     6606.6(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            75034
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.205
_diffrn_reflns_theta_min         3.720
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384.00
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     783
_refine_ls_number_reflns         12073
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6369
_reflns_number_total             12073
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8b06079_si_002.cif
_cod_data_source_block           20150826
_cod_database_code               4132757
_shelx_res_checksum              13630
_shelx_hkl_checksum              89450