Surface engineering on a microporous metal-organic framework to boost ethane/ethylene separation under humid conditions.
Xie, Xiao-Jing; Wang, Ying; Cao, Qi-Yun; Krishna, Rajamani; Zeng, Heng; Lu, Weigang; Li, Dan; Chemical science 14 (2023) 11890–11895; doi:10.1039/d3sc04119k

data_1570090
_publ_section_title
;
 Surface engineering on a microporous metal-organic framework to boost
 ethane/ethylene separation under humid conditions.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              11890
_journal_page_last               11895
_journal_paper_doi               10.1039/d3sc04119k
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C5.001 H4 N2 O2.25 Zn1'
_chemical_formula_sum            'C5 H4 N2 O2.25 Zn'
_chemical_formula_weight         193.49
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-21 deposited with the CCDC.	2023-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   20.15260(14)
_cell_length_b                   20.15260(14)
_cell_length_c                   20.15260(14)
_cell_measurement_reflns_used    1792
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3130
_cell_measurement_theta_min      7.2400
_cell_volume                     8184.52(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -31.00  -5.00   0.50    2.76    --   -0.90 -77.00  64.00   52
  2  \w    137.00 162.00   0.50   11.03    --  105.10  49.00  50.00   50
  3  \w      3.00  37.00   0.50    2.76    --    0.90  82.00-120.00   68
  4  \w     83.00 183.00   0.50   11.03    --  105.10  82.00 -90.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2558
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.433
_diffrn_reflns_theta_min         7.289
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         465
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0888P)^2^+99.1468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                441
_reflns_number_total             465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04119k2.cif
_cod_data_source_block           JNU-6-CH3
_cod_depositor_comments
'Adding full bibliography for 1570090--1570092.cif.'
_cod_original_cell_volume        8184.52(17)
_cod_database_code               1570090
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.751
_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
2. Restrained distances
 C3-C1
 1.5 with sigma of 0.005
 O2-C3 = C3-O0AA
 1.22 with sigma of 0.005
 O0AA-O2
 2.22 with sigma of 0.02
 Zn1-N2 = N0AA-Zn1_$1
 2 with sigma of 0.02
 C1AA-C0AA
 1.53 with sigma of 0.02
 C2-C3 \\sim C3-C0AA
 with sigma of 0.02
 O2-C1 \\sim C1-O0AA
 with sigma of 0.02
 C1-C1AA \\sim C1AA-N2
 with sigma of 0.02
3. Restrained planarity
 N2, C1, C0AA, N0AA, C2, O2, O0AA, C3
 with sigma of 0.001
4. Rigid bond restraints
 N2, C2, C1, C0AA, O2, O0AA, C3, C1AA, N0AA
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N2 \\sim C2 \\sim C1 \\sim C0AA \\sim O2 \\sim O0AA \\sim C3 \\sim C1AA \\sim
N0AA: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C0AA)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O0AA) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C1AA) \\sim Ueq, Uanis(N0AA) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C3) = Uanis(O2)
6. Rigid body (RIGU) restrains
 C1AA, C0AA, N2, N0AA, C2, C1, C3, O0AA, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
7. Others
 Fixed Sof: N2(0.1667) N0AA(0.1667) C2(0.1667) H2(0.1667) C1(0.1667)
 C0AA(0.1667) O2(0.1667) O0AA(0.1667) C3(0.1667) C1AA(0.16667) H1AA(0.16667)
 H1AB(0.16667) H1AC(0.16667)
8.a Aromatic/amide H refined with riding coordinates:
 C2(H2)
8.b Fitted pentagon refined as free rotating group:
 N2(N0AA,C2,C1,C0AA)
8.c Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              41450
_shelx_fab_checksum              65070
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;