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_4033946
_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_absolute_configuration unk
_chemical_formula_moiety         'C260 H270'
_chemical_formula_sum            'C260 H270'
_chemical_formula_weight         3394.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 96.72(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.570(3)
_cell_length_b                   42.930(9)
_cell_length_c                   57.470(12)
_cell_measurement_reflns_used    88035
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      23.240
_cell_measurement_theta_min      0.753
_cell_volume                     40600(14)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'KEK ugui'
_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    'SHELXD-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD Q315r (ADSC)'
_diffrn_measurement_method       'oscillation method, \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.75000
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            359350
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        23.240
_diffrn_reflns_theta_max         23.240
_diffrn_reflns_theta_min         0.753
_diffrn_source
'Aichi Synchrotron Radiation Research Center BL2S1'
_exptl_absorpt_coefficient_mu    0.031
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.555
_exptl_crystal_description       block
_exptl_crystal_F_000             7320
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 18122 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5319
_refine_ls_number_reflns         98006
_refine_ls_number_restraints     3911
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.023
_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          0.2568
_refine_ls_wR_factor_ref         0.3055
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                51504
_reflns_number_total             98006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b00085_si_007.cif
_cod_data_source_block           p21_sq
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4033946
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              3310
_shelx_hkl_checksum              86167
_shelx_fab_checksum              48210
_platon_squeeze_void_probe_radius 1.20