Melt-quenched synthesis of a manganese ZIF glass.
León-Alcaide, Luis; Fernández-Alarcón, Alberto; Calbo, Joaquín; Keen, David A.; Mínguez Espallargas, Guillermo; Chemical communications (Cambridge, England) 61 (2025) 11641–11644; doi:10.1039/d5cc02342d

data_7134770
_publ_section_title
;
 Melt-quenched synthesis of a manganese ZIF glass.
;
_journal_issue                   62
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11641
_journal_page_last               11644
_journal_paper_doi               10.1039/d5cc02342d
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C24 H26 Mn3 N16'
_chemical_formula_sum            'C24 H26 Mn3 N16'
_chemical_formula_weight         703.43
_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             2025-04-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.06 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-22 deposited with the CCDC.	2025-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.158(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7686(5)
_cell_length_b                   12.9029(6)
_cell_length_c                   10.6640(4)
_cell_measurement_reflns_used    5327
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      76.1960
_cell_measurement_theta_min      4.0580
_cell_volume                     1481.42(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.102a (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 0.998
_diffrn_measured_fraction_theta_max 0.961
_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    -58.00  23.00   0.50   10.00    --  -48.92   7.00 -62.00  162
  2  \w   -120.00 -40.00   0.50   10.00    --  -48.92  -7.00 122.00  160
  3  \w     40.00 120.00   0.50   10.00    --   48.92   7.00 -62.00  160
  4  \w    -22.00  58.00   0.50   10.00    --   48.92  -7.00 122.00  160
  5  \w   -112.00 -31.00   0.50   40.00    -- -103.00   7.00 -62.00  162
  6  \w   -174.00 -94.00   0.50   40.00    -- -103.00  -7.00 122.00  160
  7  \w     32.00 113.00   0.50   40.00    --  103.32  -7.00 122.00  162
  8  \w     94.00 175.00   0.50   40.00    --  103.32   7.00 -62.00  162
  9  \w     19.00  92.00   0.50   10.00    --   48.92-125.00 -60.00  146
 10  \w     19.00  92.00   0.50   10.00    --   48.92-125.00-180.00  146
 11  \w     34.00 106.00   0.50   40.00    --  103.32 -99.00 -60.00  144
 12  \w     32.00 111.00   0.50   40.00    --  103.32 -38.00 -60.00  158
 13  \w     35.00 112.00   0.50   40.00    --  103.32-125.00 120.00  154
 14  \w     35.00 112.00   0.50   40.00    --  103.32-125.00 120.00  154
 15  \w     32.00 124.00   0.50   40.00    --  103.32 -77.00 120.00  184
 16  \w     34.00 106.00   0.50   40.00    --  103.32 -99.00 -60.00  144
 17  \w     40.00 104.00   0.50   40.00    --  103.32 -99.00  30.00  128
;
_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      -0.1051394000
_diffrn_orient_matrix_UB_12      -0.0092544000
_diffrn_orient_matrix_UB_13      -0.0995378000
_diffrn_orient_matrix_UB_21      0.0969801000
_diffrn_orient_matrix_UB_22      -0.0060356000
_diffrn_orient_matrix_UB_23      -0.1039062000
_diffrn_orient_matrix_UB_31      0.0032021000
_diffrn_orient_matrix_UB_32      -0.1189071000
_diffrn_orient_matrix_UB_33      0.0131062000
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13940
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.738
_diffrn_reflns_theta_min         4.106
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.102a (Rigaku Oxford Diffraction, 2023)
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    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0827P)^2^+1.2333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2269
_reflns_number_total             2999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02342d2.cif
_cod_data_source_block           sx1228_auto
_cod_depositor_comments          'Adding full bibliography for 7134770.cif.'
_cod_database_code               7134770
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Mn3C10H10N10
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.568
_diffrn_oxdiff_ac3_digest_hkl    019384e56727bc2012541cc7c14307c4e8d486
_diffrn_oxdiff_digest_hkl
;
0128f7d79ccd51e7389cfee4bee32265fe1d2b
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C15(H15), C22(H22), C24(H24), C25(H25), C32(H32),
 C34(H34), C35(H35), C42(H42), N43(H43), C44(H44), C45(H45)
;
_shelx_res_checksum              26560
_shelx_hkl_checksum              33328
_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 2.266
_oxdiff_exptl_absorpt_empirical_full_min 0.560