Synthesis of Single-Atom Catalysts with Reactive Oxygen Species-Scavenging Activity by the Dynamic Crystal Structure Transition of Coordination Polymers
Wei, Suosu; Zhang, Shengfeng; Xu, Zhong; Liao, Chen; Wei, Yongbiao; Deng, Chunxia; Song, Jian; Huang, Jin; Materials Horizons  (2025) –; doi:10.1039/D5MH01016K

data_1575586
_publ_section_title
;
 Synthesis of Single-Atom Catalysts with Reactive Oxygen
 Species-Scavenging Activity by the Dynamic Crystal Structure Transition
 of Coordination Polymers
;
_journal_name_full               'Materials Horizons'
_journal_paper_doi               10.1039/D5MH01016K
_journal_year                    2025
_chemical_formula_moiety         'C11 H9 Cu F4 N O6'
_chemical_formula_sum            'C11 H9 Cu F4 N O6'
_chemical_formula_weight         390.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-23 deposited with the CCDC.	2025-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                83.7118(18)
_cell_angle_beta                 71.617(2)
_cell_angle_gamma                75.087(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3193(2)
_cell_length_b                   9.6788(2)
_cell_length_c                   11.0000(2)
_cell_measurement_reflns_used    8079
_cell_measurement_temperature    297.75(10)
_cell_measurement_theta_max      75.5660
_cell_measurement_theta_min      4.2600
_cell_volume                     714.25(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.75(10)
_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 0.952
_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    -48.00 -18.00   0.50    0.30    --  -90.25  45.00   0.00   60
  2  \w    -68.00 -18.00   0.50    0.30    --  -90.25  61.00   0.00  100
  3  \w     14.00 117.00   0.50    0.12    --   43.18  77.00 150.00  206
  4  \w     34.00  59.00   0.50    0.30    --  109.26   0.00 150.00   50
  5  \w     72.00 178.00   0.50    0.30    --  109.26   0.00 150.00  212
  6  \w    -27.00  38.00   0.50    0.12    --  -43.18  19.00 -60.00  130
  7  \w    -51.00 -18.00   0.50    0.30    --  -90.25  45.00 -90.00   66
  8  \w    -51.00 -14.00   0.50    0.30    --  -90.25  45.00  90.00   74
  9  \w    -27.00  38.00   0.50    0.12    --  -43.18  19.00  60.00  130
 10  \w     51.00 117.00   0.50    0.12    --   43.18-158.00 -89.00  132
 11  \w     85.00 111.00   0.50    0.30    --  109.26-125.00 -30.00   52
 12  \w     42.00  81.00   0.50    0.30    --  109.26-125.00 -30.00   78
 13  \w     51.00 135.00   0.50    0.30    --  109.26-158.00 -89.00  168
 14  \w     77.00 103.00   0.50    0.30    --  109.26-125.00-150.00   52
 15  \w     39.00  74.00   0.50    0.30    --  109.26-125.00-150.00   70
 16  \w     30.00  93.00   0.50    0.12    --   43.18-118.00  64.00  126
 17  \w     34.00 110.00   0.50    0.30    --  109.26-118.00  64.00  152
 18  \w     80.00 105.00   0.50    0.30    --  109.26 -94.00 150.00   50
 19  \w     36.00  71.00   0.50    0.30    --  109.26 -61.00  90.00   70
 20  \w     35.00  68.00   0.50    0.30    --  109.26 -77.00  90.00   66
 21  \w     71.00  96.00   0.50    0.30    --  109.26 -77.00  90.00   50
 22  \w     38.00  89.00   0.50    0.30    --  109.26 -77.00  60.00  102
 23  \w     75.00 101.00   0.50    0.30    --  109.26 -77.00-150.00   52
 24  \w     39.00  70.00   0.50    0.30    --  109.26 -77.00-150.00   62
 25  \w     42.00  69.00   0.50    0.30    --  109.26 -61.00-150.00   54
 26  \w     37.00  63.00   0.50    0.30    --  109.26 -61.00-120.00   52
 27  \w     97.00 135.00   0.50    0.30    --  109.26 125.00  90.00   76
 28  \w     96.00 127.00   0.50    0.30    --  109.26 125.00 120.00   62
 29  \w    100.00 148.00   0.50    0.30    --  109.26 118.00 150.00   96
 30  \w    130.00 173.00   0.50    0.30    --  109.26 125.00 120.00   86
 31  \w    145.00 178.00   0.50    0.30    --  109.26 125.00  90.00   66
 32  \w     95.00 154.00   0.50    0.30    --  109.26 125.00-180.00  118
 33  \w     92.00 117.00   0.50    0.30    --  109.26 158.00 -55.00   50
 34  \w   -108.00 -30.00   0.50    0.12    --  -43.18 158.00 -55.00  156
 35  \w    -83.00  -8.00   0.50    0.12    --  -43.18 118.00 150.00  150
 36  \w    -83.00 -15.00   0.50    0.30    --  -90.25 118.00 150.00  136
 37  \w   -169.00 -66.00   0.50    0.30    --  -90.25 -30.00 -90.00  206
 38  \w   -109.00 -70.00   0.50    0.30    --  -90.25 -45.00 120.00   78
 39  \w   -166.00-132.00   0.50    0.30    --  -90.25 -45.00 120.00   68
 40  \w   -166.00 -78.00   0.50    0.30    --  -90.25-118.00  64.00  176
 41  \w   -163.00 -85.00   0.50    0.30    --  -90.25-125.00  90.00  156
 42  \w   -117.00 -51.00   0.50    0.12    --  -43.18-158.00 -89.00  132
 43  \w   -143.00 -51.00   0.50    0.30    --  -90.25-158.00 -89.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0617745000
_diffrn_orient_matrix_UB_12      -0.1550747000
_diffrn_orient_matrix_UB_13      -0.0448921000
_diffrn_orient_matrix_UB_21      -0.0822692000
_diffrn_orient_matrix_UB_22      -0.0528071000
_diffrn_orient_matrix_UB_23      0.1391818000
_diffrn_orient_matrix_UB_31      -0.2037559000
_diffrn_orient_matrix_UB_32      0.0179148000
_diffrn_orient_matrix_UB_33      -0.0203537000
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9715
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.694
_diffrn_reflns_theta_min         4.237
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       needle
_exptl_crystal_F_000             390
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0045(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         2826
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0565P)^2^+0.3007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2678
_reflns_number_total             2826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5mh01016k2.cif
_cod_data_source_block           20210906-hj-pw-cuf
_cod_database_code               1575586
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H8 Cu2 F8 N2 O10 '
_cell_oxdiff_angle_alpha         83.7118(18)
_cell_oxdiff_angle_beta          71.617(2)
_cell_oxdiff_angle_gamma         75.087(2)
_cell_oxdiff_length_a            7.3193(2)
_cell_oxdiff_length_b            9.6788(2)
_cell_oxdiff_length_c            11.0000(2)
_cell_oxdiff_measurement_reflns_used 8079
_cell_oxdiff_volume              714.25(3)
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 O19-C20A = O19-C20
 1.2 with sigma of 0.02
 N21A-C20A = N21-C20
 1.32 with sigma of 0.02
 N21A-C22A = N21-C23 = N21A-C23A = N21-C22
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C20 \\sim N21 \\sim N21A \\sim C20A \\sim C22A \\sim C23 \\sim C22 \\sim C23A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(C20A)=Sof(H20A)=Sof(N21A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(N21)=Sof(C20)=Sof(H20)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
5.a Rotating group:
 O18(H18A,H18B)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C20A(H20A)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C23A(H23D,H23E,H23F), C22A(H22D,
 H22E,H22F)
;
_shelx_res_checksum              73879
_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 1.743
_oxdiff_exptl_absorpt_empirical_full_min 0.515