Fully Fused Quinoidal/Aromatic Carbazole Macrocycles with Poly-radical Characters.
Das, Soumyajit; Herng, Tun Seng; Zafra, José L; Burrezo, Paula Mayorga; Kitano, Masaaki; Ishida, Masatoshi; Gopalakrishna, Tullimilli Y.; Hu, Pan; Osuka, Atsuhiro; Casado, Juan; Ding, Jun; Casanova, David; Wu, Jishan; Journal of the American Chemical Society 138 (2016) 7782–7790; doi:10.1021/jacs.6b04539

data_4130555
_publ_section_title
;
 Fully Fused Quinoidal/Aromatic Carbazole Macrocycles with Poly-radical
 Characters.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7782
_journal_page_last               7790
_journal_paper_doi               10.1021/jacs.6b04539
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C123 H114 N6 O6'
_chemical_formula_sum            'C123 H114 N6 O6'
_chemical_formula_weight         1772.29
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   38.5230(6)
_cell_length_b                   38.5230(6)
_cell_length_c                   14.3978(3)
_cell_measurement_reflns_used    1452
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      1.50
_cell_volume                     21366.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.32a (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.32a (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.109
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.109
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            97346
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.109
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         68.913
_diffrn_reflns_theta_min         1.766
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.32a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7536.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.343
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1350
_refine_ls_number_reflns         22146
_refine_ls_number_restraints     926
_refine_ls_R_factor_all          0.1733
_refine_ls_R_factor_gt           0.1179
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3424
_refine_ls_wR_factor_ref         0.3812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12905
_reflns_number_total             19696
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja6b04539_si_003.cif
_cod_data_source_block           SX15R032
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4130555
_shelx_res_checksum              71256
_shelx_hkl_checksum              20281
_platon_squeeze_void_probe_radius 1.20