Synthesis, Structures, and Assembly of Geodesic Phenine Frameworks with Isoreticular Networks of [ n]Cyclo- para-phenylenes.
Sun, Zhe; Mio, Tatsuru; Ikemoto, Koki; Sato, Sota; Isobe, Hiroyuki; The Journal of organic chemistry 84 (2019) 3500–3507; doi:10.1021/acs.joc.9b00085

data_4033950
_publ_section_title
;
 Synthesis, Structures, and Assembly of Geodesic Phenine Frameworks with
 Isoreticular Networks of [ n]Cyclo- para-phenylenes.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3500
_journal_page_last               3507
_journal_paper_doi               10.1021/acs.joc.9b00085
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C208 H216, 3(C70), 7(C6 H5 Cl)'
_chemical_formula_sum            'C460 H251 Cl7'
_chemical_formula_weight         6025.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                81.65(3)
_cell_angle_beta                 78.06(3)
_cell_angle_gamma                77.99(3)
_cell_formula_units_Z            2
_cell_length_a                   19.820(4)
_cell_length_b                   20.510(4)
_cell_length_c                   38.690(8)
_cell_measurement_reflns_used    53146
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.575
_cell_measurement_theta_min      1.221
_cell_volume                     14965(6)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'SPring-8 BSS'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD MX225HE (Rayonix)'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.85000
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            267246
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.575
_diffrn_reflns_theta_max         26.575
_diffrn_reflns_theta_min         1.221
_diffrn_source                   'SPring-8 BL38B1 bending magnet beamline'
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       pillar
_exptl_crystal_F_000             6260
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.140
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.621
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5189
_refine_ls_number_reflns         35805
_refine_ls_number_restraints     13813
_refine_ls_restrained_S_all      1.445
_refine_ls_R_factor_all          0.1772
_refine_ls_R_factor_gt           0.1330
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.001
_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          0.3685
_refine_ls_wR_factor_ref         0.4073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23332
_reflns_number_total             35805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00085_si_008.cif
_cod_data_source_block           p-1
_cod_database_code               4033950
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              71335
_shelx_hkl_checksum              74547