Solvent-free approach for the synthesis of heterometallic Fe–Zn-ZIF glass via a melt-quenched process
León-Alcaide, Luis; Castillo-Blas, Celia; Martin-Diaconescu, Vlad; da Silva, Ivan; Keen, David A.; Bennett, Thomas D.; Mínguez Espallargas, Guillermo; Chemical Science 16 (2025) 7946–7955; doi:10.1039/D5SC00767D

data_1574239
_publ_section_title
;
 Solvent-free approach for the synthesis of heterometallic Fe--Zn-ZIF
 glass via a melt-quenched process
;
_journal_issue                   18
_journal_name_full               'Chemical Science'
_journal_page_first              7946
_journal_page_last               7955
_journal_paper_doi               10.1039/D5SC00767D
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C12 H12 Fe0.667 N8 Zn1.333'
_chemical_formula_sum            'C12 H12 Fe0.67 N8 Zn1.33'
_chemical_formula_weight         392.69
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-07-24 deposited with the CCDC.	2025-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.4527(4)
_cell_length_b                   23.4527(4)
_cell_length_c                   12.5316(4)
_cell_measurement_reflns_used    11001
_cell_measurement_temperature    120.1(4)
_cell_measurement_theta_max      74.2750
_cell_measurement_theta_min      3.7290
_cell_volume                     6892.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.71a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.71a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.71a (Rigaku OD, 2023)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.1(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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   -111.00 -30.00   0.50   30.00    -- -103.00  29.00 116.00  162
  2  \w   -174.00 -95.00   0.50   30.00    -- -103.00 -29.00 -44.00  158
  3  \w     42.00 121.00   0.50   10.00    --   48.69  29.00 116.00  158
  4  \w     99.00 178.00   0.50   30.00    --  107.50  29.00 116.00  158
  5  \w   -121.00 -41.00   0.50   10.00    --  -48.69 -29.00 -44.00  160
  6  \w    -56.00  24.00   0.50   10.00    --  -48.69  29.00 116.00  160
  7  \w     35.00 116.00   0.50   30.00    --  107.50 -29.00 -44.00  162
  8  \w    -24.00  56.00   0.50   10.00    --   48.69 -29.00 -44.00  160
  9  \w     36.00 105.00   0.50   30.00    --  107.50 -95.00  90.00  138
 10  \w     36.00 105.00   0.50   30.00    --  107.50 -95.00 150.00  138
 11  \w     36.00 105.00   0.50   30.00    --  107.50 -95.00  30.00  138
 12  \w    -91.00 -65.00   0.50   30.00    -- -103.00  30.00-180.00   52
 13  \w     36.00  95.00   0.50   30.00    --  107.50 -30.00-150.00  118
 14  \w     42.00 127.00   0.50   30.00    --  107.50 -77.00 150.00  170
 15  \w     52.00 105.00   0.50   30.00    --  107.50 -95.00 120.00  106
 16  \w   -115.00 -75.00   0.50   10.00    --  -48.69-125.00  30.00   80
 17  \w     35.00  77.00   0.50   30.00    --  107.50 -15.00   0.00   84
 18  \w     80.00 113.00   0.50   30.00    --  107.50 -15.00   0.00   66
 19  \w   -118.00 -73.00   0.50   10.00    --  -48.69-125.00 -90.00   90
 20  \w    103.00 129.00   0.50   30.00    --  107.50  45.00 -30.00   52
 21  \w    143.00 178.00   0.50   30.00    --  107.50  45.00 -30.00   70
 22  \w     88.00 135.00   0.50   30.00    --  107.50  77.00 150.00   94
 23  \w     59.00  85.00   0.50   30.00    --  107.50 -61.00  30.00   52
 24  \w     95.00 121.00   0.50   30.00    --  107.50 -61.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0199514000
_diffrn_orient_matrix_UB_12      0.0239073000
_diffrn_orient_matrix_UB_13      -0.1082604000
_diffrn_orient_matrix_UB_21      -0.0147791000
_diffrn_orient_matrix_UB_22      0.0571457000
_diffrn_orient_matrix_UB_23      0.0538016000
_diffrn_orient_matrix_UB_31      0.0608301000
_diffrn_orient_matrix_UB_32      0.0217953000
_diffrn_orient_matrix_UB_33      -0.0223773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34407
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.154
_diffrn_reflns_theta_min         3.769
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.71a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             3157
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.33(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3653
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0724P)^2^+9.6057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                3061
_reflns_number_total             3653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00767d2.cif
_cod_data_source_block           MUV-25_zni
_cod_depositor_comments
'Adding full bibliography for 1574239--1574240.cif.'
_cod_database_code               1574239
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.610
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.67(3)
 0.33(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Shared sites
{Zn1, Fe1}
{Zn2, Fe2}
4. Uiso/Uaniso restraints and constraints
Uanis(Zn1) = Uanis(Fe1)
Uanis(Zn2) = Uanis(Fe2)
5. Others
 Fixed Sof: Zn1(0.66667) Fe1(0.33333) Zn2(0.66667) Fe2(0.33333)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C12(H12), C14(H14), C15(H15), C22(H22), C24(H24),
 C25(H25), C32(H32), C34(H34), C35(H35)
;
_shelx_res_checksum              46128
_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 2.630
_oxdiff_exptl_absorpt_empirical_full_min 0.480