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_4033947
_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'
_chemical_formula_sum            'C208 H216'
_chemical_formula_weight         2715.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.560(6)
_cell_length_b                   35.210(7)
_cell_length_c                   22.180(4)
_cell_measurement_reflns_used    54922
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.001
_cell_measurement_theta_min      2.519
_cell_volume                     23866(8)
_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-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'CCD MX225HE (Rayonix)'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.900
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            117139
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        30.001
_diffrn_reflns_theta_max         30.001
_diffrn_reflns_theta_min         1.465
_diffrn_source                   'SPring-8 BL38B1 bending magnet beamline'
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.756
_exptl_crystal_description       plate
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8211
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1793P)^2^+28.0144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2758
_refine_ls_wR_factor_ref         0.2870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6772
_reflns_number_total             8211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00085_si_006.cif
_cod_data_source_block           ccca_sq
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4033947
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              12040
_shelx_hkl_checksum              49876
_shelx_fab_checksum              54419