Synthesis of substituent-free dioxadiaza[8]circulene to investigate intermolecular interactions and photophysical properties.
Nakagawa, Aoi; Ota, Wataru; Ehara, Takumi; Matsuo, Yusuke; Miyata, Kiyoshi; Onda, Ken; Sato, Tohru; Seki, Shu; Tanaka, Takayuki; Chemical communications (Cambridge, England) 60 (2024) 14770–14773; doi:10.1039/d4cc05539j

data_7133955
_publ_section_title
;
 Synthesis of substituent-free dioxadiaza[8]circulene to investigate
 intermolecular interactions and photophysical properties.
;
_journal_issue                   99
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14770
_journal_page_last               14773
_journal_paper_doi               10.1039/d4cc05539j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C56 H58 N2 O2'
_chemical_formula_sum            'C56 H58 N2 O2'
_chemical_formula_weight         791.04
_chemical_name_common
tetra-tert-butyl-N,N-diphenylethyl-opp-dioxadiaza[8]circulene
_chemical_name_systematic
tetra-tert-butyl-N,N-diphenylethyldioxadiaza[8]circulene
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-10-17 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.86080(10)
_cell_length_b                   13.42840(10)
_cell_length_c                   27.87400(10)
_cell_measurement_reflns_used    40778
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      74.1940
_cell_measurement_theta_min      3.2160
_cell_volume                     4439.13(5)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    CrystalMakerX
_computing_publication_material  CrystalMakerX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0084
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.515
_diffrn_reflns_theta_min         3.654
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.9950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8260
_reflns_number_total             8973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05539j2.cif
_cod_data_source_block           210705nakagawa
_cod_depositor_comments
'Adding full bibliography for 7133954--7133956.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7133955
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              27592
_shelx_hkl_checksum              87418