Spatial pinning of globally inert pores in a superhydrophobic hydrogen-bonded organic framework for inverse ethane/ethylene separation.
Cai, Youlie; Li, Jing-Hong; Xiao, Xiaoyan; Wei, Runzhi; Lin, Rui-Biao; Chen, Banglin; Gao, Junkuo; Chemical science 17 (2026) 4256–4267; doi:10.1039/d5sc08507a

data_1576666
_publ_section_title
;
 Spatial pinning of globally inert pores in a superhydrophobic
 hydrogen-bonded organic framework for inverse ethane/ethylene separation.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              4256
_journal_page_last               4267
_journal_paper_doi               10.1039/d5sc08507a
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C28 H19.5 O6, C20 H14.5 O2, 2(C6 H12)'
_chemical_formula_sum            'C60 H58 O8'
_chemical_formula_weight         907.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-12 deposited with the CCDC.	2025-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9347(7)
_cell_length_b                   14.1589(5)
_cell_length_c                   25.2455(8)
_cell_measurement_reflns_used    7672
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_cell_volume                     5338.4(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_data_collection       'APEX4 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2025/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 VENTURE'
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '0.60\ % \ w and 0.6\ % \ f scans'
_diffrn_radiation_collimation    '0.5 mm double- pinhole'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35521
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.396
_diffrn_reflns_theta_min         4.586
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00031(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2025/1 (Sheldrick 2025)'
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         4750
_refine_ls_number_restraints     3611
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.1477
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2725
_refine_ls_wR_factor_ref         0.2872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2688
_reflns_number_total             4750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08507a2.cif
_cod_data_source_block           hof_zstu_5
_cod_depositor_comments
'Adding full bibliography for 1576665--1576670.cif.'
_cod_database_code               1576666
_shelx_shelxl_version_number     2025/1
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C9B-C14B = C15B-C14B
 1.39 with sigma of 0.001
 C9A-C14A = C15A-C14A
 1.39 with sigma of 0.001
 C22A-C19A = C16A-C11A = C8A-C5A = C2A-C1A = C22B-C19B = C16B-C11B = C8B-C5B =
 C2B-C1B
 1.5 with sigma of 0.01
 C23A-C17A = C23B-C17B = C6A-C24A = C6B-C24
 1.54 with sigma of 0.01
 O1A-C1A = O1B-C1B = O4B-C22A = O4A-C22B
 1.25 with sigma of 0.01
 O3B-C22A = O3A-C22B = O2B-C1B = O2A-C1A
 1.33 with sigma of 0.01
 C26-C25 = C27-C26 = C28-C27 = C29-C28 = C30-C29 = C30-C25
 1.54 with sigma of 0.001
 C13A-C13A_$1 = C13B-C13B_$1
 1.39 with sigma of 0.001
 C22B-C18B \\sim C22A-C20A \\sim C22B-C20B \\sim C22A-C18A \\sim C7A-C1A \\sim
C3B-C1B \\sim C3A-C1A ~
 C7B-C1B
 with sigma of 0.02
 O2A-C2A \\sim O1B-C2B \\sim O1A-C2A \\sim O2B-C2B \\sim O3A-C19B \\sim
O4B-C19A \\sim O4A-C19B \\sim O3B-
 C19A
 with sigma of 0.02
3. Restrained planarity
 C12A, C13A, C9A, C14A, C15A, C12A_$1, C13A_$1, C9A_$1, C14A_$1, C15A_$1
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.03 and sigma
for terminal atoms of 0.03 within 3.8A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.03 and sigma
for terminal atoms of 0.03
5. Others
 Fixed Sof: O1B(0.75) O2B(0.75) H2B(0.75) O3A(0.75) H3A(0.75) O4A(0.75)
 C1B(0.75) C2B(0.75) C3B(0.75) H3B(0.75) C4B(0.75) H4B(0.75) C5B(0.75)
 C6B(0.75) C7B(0.75) H7B(0.75) C13B(0.5) C9B(0.5) C8B(0.5) C10B(0.5) H10B(0.5)
 C11B(0.5) C12B(0.5) C14B(0.5) H14B(0.5) C15B(0.5) H15B(0.5) C19B(0.5)
 C20B(0.5) H20B(0.5) C21B(0.5) H21B(0.5) C16B(0.5) C17B(0.5) C18B(0.5)
 H18B(0.5) C22B(0.75) C23B(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C24(0.5)
 H24A(0.5) H24B(0.5) H24C(0.5) O2A(0.25) H2A(0.25) O1A(0.25) O4B(0.25)
 O3B(0.25) H3BA(0.25) C1A(0.25) C6A(0.25) C5A(0.25) C4A(0.25) H4A(0.25)
 C3A(0.25) H3AA(0.25) C2A(0.25) C7A(0.25) H7A(0.25) C8A(0.5) C10A(0.5)
 H10A(0.5) C11A(0.5) C12A(0.5) C13A(0.5) C9A(0.5) C14A(0.5) H14A(0.5) C15A(0.5)
 H15A(0.5) C16A(0.5) C21A(0.5) H21A(0.5) C20A(0.5) H20A(0.5) C19A(0.5)
 C18A(0.5) H18A(0.5) C17A(0.5) C22A(0.25) C23A(0.5) H23D(0.5) H23E(0.5)
 H23F(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C25(H25A,H25B), C26(H26A,H26B), C29(H29A,H29B), C28(H28A,
 H28B), C27(H27A,H27B)
6.b Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C4B(H4B), C7B(H7B), C10B(H10B), C14B(H14B), C15B(H15B), C20B(H20B),
 C21B(H21B), C18B(H18B), C4A(H4A), C3A(H3AA), C7A(H7A), C10A(H10A), C14A(H14A),
 C15A(H15A), C21A(H21A), C20A(H20A), C18A(H18A)
6.c Fitted hexagon refined as free rotating group:
 C2B(C3B,C4B,C5B,C6B,C7B), C13B(C9B,C8B,C10B,C11B,C12B), C19B(C20B,C21B,C16B,
 C17B,C18B), C6A(C5A,C4A,C3A,C2A,C7A), C8A(C10A,C11A,C12A,C13A,C9A), C16A(C21A,
 C20A,C19A,C18A,C17A)
6.d Idealised Me refined as rotating group:
 C23B(H23A,H23B,H23C), C24(H24A,H24B,H24C), C23A(H23D,H23E,H23F), C24A(H24D,
 H24E,H24F)
6.e Idealised tetrahedral OH refined as rotating group:
 O2B(H2B), O3A(H3A), O2A(H2A), O3B(H3BA)
;
_shelx_res_checksum              12940
_olex2_submission_special_instructions 'No special instructions were received'