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_1574240
_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         'C24 H26 Fe N16 Zn2'
_chemical_formula_sum            'C24 H26 Fe N16 Zn2'
_chemical_formula_weight         725.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-24 deposited with the CCDC.	2025-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.38840(10)
_cell_length_b                   13.2702(2)
_cell_length_c                   10.44280(10)
_cell_measurement_reflns_used    17432
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      77.3370
_cell_measurement_theta_min      4.2580
_cell_volume                     1438.17(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 1.5 (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_environment      N~2~
_diffrn_ambient_temperature      120(2)
_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 0.985
_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   -119.00 -72.00   0.50    7.00    --  -48.73-128.00-171.00   94
  2  \w   -121.00 -62.00   0.50    7.00    --  -48.73-142.00  17.00  118
  3  \w   -103.00 -22.00   0.50    7.00    --  -48.73 142.00  73.00  162
  4  \w     28.00 104.00   0.50    7.00    --   48.73-142.00  17.00  152
  5  \w     68.00 121.00   0.50    7.00    --   48.73 142.00  73.00  106
  6  \w     21.00  95.00   0.50    7.00    --   48.73-128.00-171.00  148
  7  \w   -124.00 -31.00   0.50   10.00    -- -103.00 142.00  73.00  186
  8  \w   -114.00 -33.00   0.50   10.00    -- -103.00 128.00 -97.00  162
  9  \w   -173.00 -72.00   0.50   10.00    -- -103.00-128.00-171.00  202
 10  \w     38.00 114.00   0.50   10.00    --  107.50-128.00-171.00  152
 11  \w     36.00 124.00   0.50   10.00    --  107.50-142.00  17.00  176
 12  \w     78.00 178.00   0.50   10.00    --  107.50 128.00 -97.00  200
 13  \w   -118.00 -73.00   0.50    7.00    --  -48.73-125.00-120.00   90
 14  \w    -56.00  23.00   0.50    7.00    --  -48.73  38.00-180.00  158
 15  \w    -95.00 -14.00   0.50    7.00    --  -48.73 128.00 -97.00  162
 16  \w   -118.00 -73.00   0.50    7.00    --  -48.73-125.00  30.00   90
 17  \w   -121.00 -36.00   0.50    7.00    --  -48.73 -57.00-150.00  170
 18  \w    -23.00  56.00   0.50    7.00    --   48.73 -38.00 -30.00  158
 19  \w    -70.00 -35.00   0.50   10.00    -- -103.00 125.00-120.00   70
 20  \w   -173.00-112.00   0.50   10.00    -- -103.00 -30.00   0.00  122
 21  \w   -173.00-147.00   0.50   10.00    -- -103.00 -15.00-120.00   52
 22  \w   -174.00-101.00   0.50   10.00    -- -103.00 -62.00 -82.85  146
 23  \w   -124.00 -53.00   0.50   10.00    -- -103.00 141.00 -70.31  142
 24  \w   -129.00 -96.00   0.50   10.00    -- -103.00 -15.00-120.00   66
 25  \w   -107.00 -70.00   0.50   10.00    -- -103.00  30.00 150.00   74
 26  \w     43.00  81.00   0.50   10.00    --  107.50 -87.00 -26.95   76
 27  \w     39.00 109.00   0.50   10.00    --  107.50-125.00  90.00  140
 28  \w     84.00 168.00   0.50   10.00    --  107.50 125.00-150.00  168
 29  \w     41.00  81.00   0.50   10.00    --  107.50-125.00-120.00   80
 30  \w     73.00  98.00   0.50   10.00    --  107.50 -95.00   0.00   50
 31  \w    133.00 171.00   0.50   10.00    --  107.50  45.00   0.00   76
 32  \w     94.00 126.00   0.50   10.00    --  107.50 -77.00   0.00   64
 33  \w     90.00 117.00   0.50   10.00    --  107.50 -61.00 150.00   54
 34  \w     61.00  88.00   0.50   10.00    --  107.50 -77.00   0.00   54
 35  \w     99.00 178.00   0.50   10.00    --  107.50  30.00 150.00  158
 36  \w     85.00 111.00   0.50   10.00    --  107.50-125.00-120.00   52
 37  \w     39.00 111.00   0.50   10.00    --  107.50-125.00 150.00  144
 38  \w    100.00 177.00   0.50   10.00    --  107.50  45.00  30.00  154
 39  \w     37.00  71.00   0.50   10.00    --  107.50 -61.00 150.00   68
 40  \w    103.00 129.00   0.50   10.00    --  107.50  45.00   0.00   52
 41  \w     78.00 104.00   0.50   10.00    --  107.50 -95.00 -90.00   52
 42  \w     84.00 111.00   0.50   10.00    --  107.50 -87.00 -26.95   54
 43  \w     56.00 105.00   0.50   10.00    --  107.50-125.00 -90.00   98
 44  \w     72.00 116.00   0.50   10.00    --  107.50 -45.00-180.00   88
 45  \w     39.00  68.00   0.50   10.00    --  107.50 -45.00-180.00   58
 46  \w     75.00 104.00   0.50   10.00    --  107.50 -95.00-120.00   58
 47  \w     64.00 105.00   0.50   10.00    --  107.50 -95.00-180.00   82
 48  \w     41.00  79.00   0.50   10.00    --  107.50-125.00   0.00   76
 49  \w     39.00  82.00   0.50   10.00    --  107.50-125.00 -30.00   86
 50  \w     96.00 121.00   0.50   10.00    --  107.50 142.00  73.00   50
;
_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      -0.1300175000
_diffrn_orient_matrix_UB_12      -0.0541448000
_diffrn_orient_matrix_UB_13      0.0125409000
_diffrn_orient_matrix_UB_21      -0.0116825000
_diffrn_orient_matrix_UB_22      0.0455131000
_diffrn_orient_matrix_UB_23      0.1346969000
_diffrn_orient_matrix_UB_31      -0.0706387000
_diffrn_orient_matrix_UB_32      0.0920609000
_diffrn_orient_matrix_UB_33      -0.0592421000
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28704
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.393
_diffrn_reflns_theta_min         4.260
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.331
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85867
_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    1.675
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0396P)^2^+1.2692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2880
_reflns_number_total             3054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00767d2.cif
_cod_data_source_block           MUV-25
_cod_depositor_comments
'Adding full bibliography for 1574239--1574240.cif.'
_cod_database_code               1574240
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.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), N33(H33), C34(H34), C35(H35)
;
_shelx_res_checksum              68136
_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 1.922
_oxdiff_exptl_absorpt_empirical_full_min 0.568