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_4132758
_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 H80 N8'
_chemical_formula_sum            'C74 H80 N8'
_chemical_formula_weight         1081.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                94.624(7)
_cell_angle_beta                 93.167(7)
_cell_angle_gamma                97.221(7)
_cell_formula_units_Z            4
_cell_length_a                   15.6996(14)
_cell_length_b                   18.0988(15)
_cell_length_c                   22.340(2)
_cell_measurement_reflns_used    19533
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.09
_cell_measurement_theta_min      3.03
_cell_volume                     6263.2(10)
_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    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.977
_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  0.1000
_diffrn_reflns_av_unetI/netI     0.1099
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.977
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_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            116075
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         3.032
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2320.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1589
_refine_ls_number_reflns         22370
_refine_ls_number_restraints     296
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0900P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10133
_reflns_number_total             22370
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8b06079_si_003.cif
_cod_data_source_block           20150827_2
_cod_original_cell_volume        6263.2(9)
_cod_database_code               4132758
_shelx_res_checksum              39765
_shelx_hkl_checksum              75644
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