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_1576667
_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         '2(C48 H34 O8), 0.8(C2 H6)'
_chemical_formula_sum            'C98 H74 O16'
_chemical_formula_weight         1507.57
_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
_audit_creation_date             2025-02-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-21 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            2
_cell_length_a                   13.444(3)
_cell_length_b                   14.142(3)
_cell_length_c                   25.861(5)
_cell_measurement_reflns_used    1063
_cell_measurement_temperature    273.0
_cell_measurement_theta_max      44.47
_cell_measurement_theta_min      20.37
_cell_volume                     4916.8(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38486
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        58.916
_diffrn_reflns_theta_max         58.916
_diffrn_reflns_theta_min         4.745
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.6554
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0966 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.8720.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.018
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0155(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3513
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0735
_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^)+(0.1712P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2140
_refine_ls_wR_factor_ref         0.2661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1722
_reflns_number_total             3513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08507a2.cif
_cod_data_source_block           RTC2H6@HOF_ZSTU_5a
_cod_depositor_comments
'Adding full bibliography for 1576665--1576670.cif.'
_cod_original_cell_volume        4917.0(17)
_cod_database_code               1576667
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.921
_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
 C40-C36
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H00J(0.4) H00L(0.6) H00M(0.6) H00N(0.4) C36(0.2) H36A(0.2)
 H36B(0.2) H36C(0.2) C40(0.2) H40A(0.2) H40B(0.2) H40C(0.2) C0AA(0.6) H0AA(0.6)
 H0AB(0.6) H0AC(0.6) C4(0.4) H4A(0.4) H4B(0.4) H4C(0.4) C1AA(0.6) H1AA(0.6)
 H1AB(0.6) H1AC(0.6) C2(0.4) H2A(0.4) H2B(0.4) H2C(0.4)
6.a Riding coordinates:
 C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C0AA(H0AA,H0AB,H0AC), C4(H4A,H4B,
 H4C), C1AA(H1AA,H1AB,H1AC), C2(H2A,H2B,H2C)
6.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00D(H00D), C00F(H00F), C00G(H00G), C00I(H00I), C00J(H00J),
 C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P)
6.c Idealised tetrahedral OH refined as rotating group:
 O002(H002), O004(H004)
;
_shelx_res_checksum              27973
_olex2_submission_special_instructions 'No special instructions were received'