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_4127456
_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            'C58.5 H30.5 Cl7.5'
_chemical_formula_weight         999.20
_chemical_name_systematic        Heptabenzo[a,d,g,j,m,p,s][7]circulene
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                69.6938(16)
_cell_angle_beta                 89.6815(15)
_cell_angle_gamma                80.3472(15)
_cell_formula_units_Z            2
_cell_length_a                   9.8876(5)
_cell_length_b                   13.0506(7)
_cell_length_c                   18.7229(10)
_cell_measurement_reflns_used    202
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     2230.1(2)
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            81187
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.324
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6009
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         8091
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.111
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1473P)^2^+3.3222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5660
_reflns_number_total             8091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03910_si_002.cif
_cod_data_source_block           hb7c
_cod_original_formula_sum        'C58.50 H30.50 Cl7.50'
_cod_database_code               4127456
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.860
_shelx_res_checksum              29012
_shelx_hkl_checksum              16794