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_1576668
_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         'C48 H34 O8, 2(C2 H6)'
_chemical_formula_sum            'C52 H46 O8'
_chemical_formula_weight         798.89
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-10
_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                   13.4088(7)
_cell_length_b                   14.1154(5)
_cell_length_c                   25.8758(9)
_cell_measurement_reflns_used    3083
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_cell_volume                     4897.5(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      150.02
_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 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_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  0.0802
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31907
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.573
_diffrn_reflns_theta_min         6.271
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.583
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.046(6)
_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   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4449
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.1547
_refine_ls_R_factor_gt           0.0978
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2836
_refine_ls_wR_factor_ref         0.3545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1938
_reflns_number_total             4449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08507a2.cif
_cod_data_source_block           150KC2H6@HOF_ZSTU_5a
_cod_depositor_comments
'Adding full bibliography for 1576665--1576670.cif.'
_cod_database_code               1576668
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-C22 = O2-C1
 1.33 with sigma of 0.01
 C26-C25 = C28-C27 = C30-C29
 1.54 with sigma of 0.001
 C2-C1 = C8-C5 = C16-C10 = C22-C19 = C6-C24 = C23-C21 = C17-C00Q = C4-C31
 1.5 with sigma of 0.01
 O1-C1 = O3-C22
 1.2 with sigma of 0.01
 C14-C13 = C15-C14
 1.39 with sigma of 0.001
3. Restrained planarity
 C5, C7, C2, C6, C3, C4, C24, C31
 with sigma of 0.1
 C16, C19, C18, C17, C21, C20, C00Q, C23
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.03 and sigma
for terminal atoms of 0.03 within 2A
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: C00Q(0.6) H00A(0.6) H00B(0.6) H00C(0.6) H6(0.5) H4A(0.5) H21(0.6)
 H17(0.4) C23(0.4) H23A(0.4) H23B(0.4) H23C(0.4) C24(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C27(0.25) H27A(0.25)
 H27B(0.25) H27C(0.25) C28(0.25) H28A(0.25) H28B(0.25) H28C(0.25) C29(0.25)
 H29A(0.25) H29B(0.25) H29C(0.25) C30(0.25) H30A(0.25) H30B(0.25) H30C(0.25)
6.a Riding coordinates:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4A), C3(H3), C9(H9), C14(H14), C15(H15), C21(H21),
 C20(H20), C18(H18), C17(H17)
6.c Fitted hexagon refined as free rotating group:
 C12(C11,C10,C9,C8,C13), C16(C21,C20,C19,C18,C17)
6.d Idealised Me refined as rotating group:
 C00Q(H00A,H00B,H00C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,
 H31C)
6.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
;
_shelx_res_checksum              76100
_olex2_submission_special_instructions 'No special instructions were received'