Synthesis, Structures, and Properties of Heptabenzo[7]circulene and Octabenzo[8]circulene.
Pun, Sai Ho; Wang, Yujing; Chu, Ming; Chan, Chi Kit; Li, Yuke; Liu, Zhifeng; Miao, Qian; Journal of the American Chemical Society 141 (2019) 9680–9686; doi:10.1021/jacs.9b03910

data_4127457
_publ_section_title
;
 Synthesis, Structures, and Properties of Heptabenzo[7]circulene and
 Octabenzo[8]circulene.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9680
_journal_page_last               9686
_journal_paper_doi               10.1021/jacs.9b03910
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C82 H64 S4'
_chemical_formula_weight         1177.57
_chemical_name_systematic
'2,11,18,27-Tetra(tert-butyl)octabenzo[a, d, g, j, m, p, s, v][8]circulene'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 96.355(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4908(14)
_cell_length_b                   20.5122(14)
_cell_length_c                   29.522(2)
_cell_measurement_reflns_used    631
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     12332.2(15)
_computing_cell_refinement       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_collection       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_reduction        'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER D8VENTURE DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            201847
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.104
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6097
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             4960
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         11179
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1776
_refine_ls_R_factor_gt           0.1505
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1225P)^2^+117.9246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3529
_refine_ls_wR_factor_ref         0.3719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8531
_reflns_number_total             11179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03910_si_003.cif
_cod_data_source_block           tbuob8c
_cod_original_cell_volume        12332.4(15)
_cod_database_code               4127457
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.942
_shelxl_version_number           2014/6
_shelx_res_checksum              13887
_shelx_hkl_checksum              92770