Facile separation of cyclic aliphatic and aromatic vapors using crystalline thiacalixarene assemblies with preorganized channels.
Yamada, Manabu; Yoshizaki, Ruka; Uemura, Fumiya; Katagiri, Hiroshi; Kato, Sumio; Akimoto, Kazuhiko; Hamada, Fumio; Chemical communications (Cambridge, England) 59 (2023) 2604–2607; doi:10.1039/d2cc05647j

data_7131343
_publ_section_title
;
 Facile separation of cyclic aliphatic and aromatic vapors using
 crystalline thiacalixarene assemblies with preorganized channels.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2604
_journal_page_last               2607
_journal_paper_doi               10.1039/d2cc05647j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C36 H36 Br4 O4 S4, 1[C7H8]'
_chemical_formula_sum            'C43 H44 Br4 O4 S4'
_chemical_formula_weight         1072.66
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-17 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   31.2941(5)
_cell_length_b                   31.2941(5)
_cell_length_c                   24.1681(4)
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_cell_measurement_temperature    223
_cell_measurement_theta_max      28.6690
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_cell_volume                     20497.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'PLATON (Spek, 2020)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL2018 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT2014 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            92214
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.603
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       Prism
_exptl_crystal_F_000             9684
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5243
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0468P)^2^+50.5879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3666
_reflns_number_total             5243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05647j2.cif
_cod_data_source_block           20200810_yamada_no4_-50__sq
_cod_original_cell_volume        20497.4(7)
_cod_database_code               7131343
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.520
_shelx_estimated_absorpt_t_max   0.520
_oxdiff_exptl_absorpt_empirical_full_min 0.823
_oxdiff_exptl_absorpt_empirical_full_max 1.383
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              21384
_shelx_hkl_checksum              16237
_shelx_fab_checksum              32445