Novel Pyromellitic Diimide-Based Macrocycle with a Linear π-Electronic System and Bis(phenylethynyl)pyromellitic Diimide: Syntheses, Structures, Photophysical Properties, and Redox Characteristics
Shin-ichiro Kato; Yasuhiro Nonaka; Toshiaki Shimasaki; Kenta Goto; Teruo Shinmyozu; Journal of Organic Chemistry 73 (2008) 4063–4075; doi:10.1021/jo800283r

data_4023440
_publ_section_title
;
 Novel Pyromellitic Diimide-Based Macrocycle with a Linear
 \p-Electronic System and Bis(phenylethynyl)pyromellitic Diimide:
 Syntheses, Structures, Photophysical Properties, and Redox
 Characteristics
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4063
_journal_page_last               4075
_journal_paper_doi               10.1021/jo800283r
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C50 H42 N4 O4'
_chemical_formula_weight         762.88
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.270(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.753(3)
_cell_length_b                   5.7366(11)
_cell_length_c                   27.350(5)
_cell_measurement_temperature    123(2)
_cell_volume                     1997.7(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            31375
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9968
_exptl_absorpt_correction_T_min  0.9730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+0.6777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                3510
_reflns_number_total             4562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo800283r-File006.cif
_cod_data_source_block           indole
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4023440