Facile synthesis and characterization of aza-bridged all-benzenoid quinoidal figure-eight and cage molecules.
Dong, Shaoqiang; Han, Yi; Tong, Zekun; Wang, Jinfeng; Zhang, Yishan; Li, Aisen; Gopalakrishna, Tullimilli Y.; Tian, Hongkun; Chi, Chunyan; Chemical science 15 (2024) 9087–9095; doi:10.1039/d3sc02707d

data_1571763
_publ_section_title
;
 Facile synthesis and characterization of aza-bridged all-benzenoid
 quinoidal figure-eight and cage molecules.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9087
_journal_page_last               9095
_journal_paper_doi               10.1039/d3sc02707d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C204 H162 N6, 6(F6 Sb)'
_chemical_formula_sum            'C204 H162 F36 N6 Sb6'
_chemical_formula_weight         4111.96
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-06-05 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   24.0699(7)
_cell_length_b                   24.0699(7)
_cell_length_c                   29.1508(14)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.5421
_cell_measurement_theta_min      2.6059
_cell_volume                     14626.1(9)
_computing_cell_refinement       'SAINT-plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-plus (Bruker, 2007)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2354
_diffrn_reflns_av_unetI/netI     0.0822
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            132316
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.940
_diffrn_reflns_theta_max         66.940
_diffrn_reflns_theta_min         2.119
_exptl_absorpt_coefficient_mu    4.819
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.934
_exptl_crystal_description       block
_exptl_crystal_F_000             4116
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.001
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.16(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         8847
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      2.195
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.1543
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3581
_refine_ls_wR_factor_ref         0.3977
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4452
_reflns_number_total             8847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02707d2.cif
_cod_data_source_block           p-62c_sq
_cod_depositor_comments
'Adding full bibliography for 1571762--1571763.cif.'
_cod_original_cell_volume        14626.1(11)
_cod_database_code               1571763
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.446
_shelx_estimated_absorpt_t_max   0.644
_shelx_res_checksum              90980
_shelx_fab_checksum              32753