A stable sulfate-pillared metal triazolate framework with a gating effect for highly efficient dehydration of bioethanol.
Tian, Wen-Jiang; Hu, Ding-Yi; Fang, Zi-Luo; Zhong, Xiao-Feng; Xue, Ming; Zhou, Hao-Long; Zhou, Dong-Dong; Chen, Xiao-Ming; Chemical communications (Cambridge, England) 61 (2025) 15461–15464; doi:10.1039/d5cc04344a

data_7134929
_publ_section_title
;
 A stable sulfate-pillared metal triazolate framework with a gating effect
 for highly efficient dehydration of bioethanol.
;
_journal_issue                   79
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15461
_journal_page_last               15464
_journal_paper_doi               10.1039/d5cc04344a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C8 H12 N6 O4 S Zn2, 1.5(H2 O)'
_chemical_formula_sum            'C8 H15 N6 O5.5 S Zn2'
_chemical_formula_weight         446.06
_chemical_name_systematic        MAF-65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2025-08-25 deposited with the CCDC.	2025-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.166(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4653(5)
_cell_length_b                   9.7370(3)
_cell_length_c                   9.8807(2)
_cell_measurement_reflns_used    3233
_cell_measurement_temperature    298.0(3)
_cell_measurement_theta_max      75.5580
_cell_measurement_theta_min      5.3050
_cell_volume                     1533.05(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.901
_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     55.00  83.00   0.50    0.10    --   46.30-121.00 119.00   56
  2  \w     37.00 105.00   0.50    0.60    --  108.76 -95.00 120.00  136
  3  \w     40.00 109.00   0.50    0.60    --  108.76-121.00 119.00  138
  4  \w     80.00 133.00   0.50    0.60    --  108.76-155.00 -38.00  106
  5  \w     40.00  65.00   0.50    0.60    --  108.76-155.00 -38.00   50
  6  \w    -30.00  21.00   0.50    0.10    --   46.30 -19.00-180.00  102
  7  \w    -30.00  23.00   0.50    0.10    --   46.30 -19.00 -60.00  106
  8  \w     57.00  89.00   0.50    0.10    --   46.30 155.00  -0.00   64
  9  \w    107.00 133.00   0.50    0.60    --  108.76 121.00-157.00   52
 10  \w    -54.00 -26.00   0.50    0.60    --  -97.00  45.00-150.00   56
 11  \w    -54.00 -26.00   0.50    0.60    --  -97.00  45.00-180.00   56
 12  \w    -72.00 -46.00   0.50    0.10    --  -46.30 121.00-157.00   52
 13  \w    -54.00 -28.00   0.50    0.60    --  -97.00  45.00 -60.00   52
 14  \w    -54.00 -28.00   0.50    0.60    --  -97.00  45.00  30.00   52
 15  \w   -170.00 -81.00   0.50    0.60    --  -97.00 -45.00 -60.00  178
 16  \w   -150.00-125.00   0.50    0.60    --  -97.00-121.00 119.00   50
 17  \w   -170.00-118.00   0.50    0.60    --  -97.00 -95.00  60.00  104
 18  \w   -115.00 -89.00   0.50    0.60    --  -97.00 -95.00  60.00   52
 19  \w   -117.00 -62.00   0.50    0.10    --  -46.30-155.00 -38.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0542769000
_diffrn_orient_matrix_UB_12      -0.1480476000
_diffrn_orient_matrix_UB_13      -0.0024972000
_diffrn_orient_matrix_UB_21      0.1480515000
_diffrn_orient_matrix_UB_22      0.0527594000
_diffrn_orient_matrix_UB_23      0.0262190000
_diffrn_orient_matrix_UB_31      -0.0126010000
_diffrn_orient_matrix_UB_32      -0.0185559000
_diffrn_orient_matrix_UB_33      0.0929859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3913
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.937
_diffrn_reflns_theta_min         5.324
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic intense colourless'
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00025(7)
_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   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1471
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0415P)^2^+4.5953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1435
_reflns_number_total             1471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04344a2.cif
_cod_data_source_block           maf-65
_cod_depositor_comments          'Adding full bibliography for 7134929.cif.'
_cod_original_cell_volume        1533.05(7)
_cod_original_formula_sum        'C8 H15 N6 O5.50 S Zn2'
_cod_database_code               7134929
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'C H N O S Zn'
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.610
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 S1-O3 \\sim S1-O2
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
4. Others
 Fixed Sof: O2(0.5) O3(0.5) O4(0.75) H4D(0.75) H4E(0.75)
5.a Riding coordinates:
 O4(H4D), O4(H4E)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              11436
_shelx_hkl_checksum              94579
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.687
_oxdiff_exptl_absorpt_empirical_full_min 0.795