Stable Ni(II)-based metal-organic framework nanoparticles for efficient photocatalytic C-N coupling reaction.
Wang, Yuhao; Zhong, Jinping; Feng, Fada; Zeng, Yikui; Yan, Dengfeng; Li, Xudong; Nanoscale 17 (2025) 25868–25876; doi:10.1039/d5nr03175c

data_1575918
_publ_section_title
;
 Stable Ni(II)-based metal-organic framework nanoparticles for efficient
 photocatalytic C-N coupling reaction.
;
_journal_issue                   44
_journal_name_full               Nanoscale
_journal_page_first              25868
_journal_page_last               25876
_journal_paper_doi               10.1039/d5nr03175c
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'C14 H15 N Ni O8'
_chemical_formula_sum            'C14 H15 N Ni O8'
_chemical_formula_weight         383.98
_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   mixed
_audit_creation_date             2024-08-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-09-30 deposited with the CCDC.	2025-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.252(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.3586(2)
_cell_length_b                   33.0345(12)
_cell_length_c                   10.7307(9)
_cell_measurement_reflns_used    3129
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8960
_cell_measurement_theta_min      4.3210
_cell_volume                     1888.24(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.990
_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   -108.00 -83.00   0.50    0.50    --  -39.95-155.00 149.00   50
  2  \w    -83.00 -58.00   0.50    0.50    --  -39.95 155.00-171.00   50
  3  \w    -71.00 -46.00   0.50    0.50    --  -39.95 120.00  31.00   50
  4  \w     60.00  96.00   0.50    0.50    --   39.95-120.00 -53.00   72
  5  \w     60.00  85.00   0.50    0.50    --   39.95-155.00 149.00   50
  6  \w    -65.00 -30.00   0.50    2.00    --  -94.50 155.00-171.00   70
  7  \w   -150.00-118.00   0.50    2.00    --  -94.50-120.00 -53.00   64
  8  \w     70.00 110.00   0.50    2.00    --  108.87-120.00 -53.00   80
  9  \w    106.00 132.00   0.50    2.00    --  108.87-155.00 149.00   52
 10  \w    107.00 137.00   0.50    2.00    --  108.87 155.00-171.00   60
 11  \w     80.00 105.00   0.50    2.00    --  108.87 155.00-171.00   50
 12  \w    -26.00   4.00   0.50    0.50    --  -39.95  19.00   0.00   60
 13  \w    -27.00  46.00   0.50    0.50    --  -39.95  19.00-150.00  146
 14  \w    -34.00  27.00   0.50    0.50    --   39.95 -19.00-180.00  122
 15  \w    -21.00  12.00   0.50    0.50    --   39.95 -19.00  30.00   66
 16  \w    -48.00 -17.00   0.50    2.00    --  -94.50  45.00 -90.00   62
 17  \w    -51.00 -15.00   0.50    2.00    --  -94.50  45.00 150.00   72
 18  \w    -50.00 -15.00   0.50    2.00    --  -94.50  45.00-120.00   70
 19  \w    -50.00 -15.00   0.50    2.00    --  -94.50  45.00-150.00   70
 20  \w    -50.00 -23.00   0.50    2.00    --  -94.50  45.00-180.00   54
 21  \w    -71.00 -46.00   0.50    2.00    --  -94.50  61.00 150.00   50
 22  \w   -123.00 -98.00   0.50    2.00    --  -94.50-155.00 149.00   50
 23  \w    138.00 177.00   0.50    2.00    --  108.87  30.00-150.00   78
 24  \w     82.00 125.00   0.50    2.00    --  108.87  30.00-150.00   86
 25  \w     34.00  71.00   0.50    2.00    --  108.87-125.00   0.00   74
 26  \w    141.00 167.00   0.50    2.00    --  108.87 125.00 -90.00   52
 27  \w    102.00 128.00   0.50    2.00    --  108.87 125.00 -90.00   52
 28  \w     34.00  59.00   0.50    2.00    --  108.87 -61.00 -60.00   50
 29  \w     35.00  60.00   0.50    2.00    --  108.87 -61.00 -90.00   50
 30  \w     38.00  63.00   0.50    2.00    --  108.87 -61.00 120.00   50
 31  \w     37.00  63.00   0.50    2.00    --  108.87 -61.00  90.00   52
 32  \w     35.00  94.00   0.50    2.00    --  108.87-125.00 -30.00  118
 33  \w     79.00 105.00   0.50    2.00    --  108.87 -94.00 120.00   52
 34  \w     48.00  74.00   0.50    2.00    --  108.87 -94.00 120.00   52
 35  \w     79.00 110.00   0.50    2.00    --  108.87-125.00   0.00   62
 36  \w     38.00  63.00   0.50    2.00    --  108.87 -61.00 -30.00   50
;
_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      -0.0362553000
_diffrn_orient_matrix_UB_12      -0.0458257000
_diffrn_orient_matrix_UB_13      0.0177660000
_diffrn_orient_matrix_UB_21      -0.0157409000
_diffrn_orient_matrix_UB_22      0.0067521000
_diffrn_orient_matrix_UB_23      0.1410253000
_diffrn_orient_matrix_UB_31      -0.2863962000
_diffrn_orient_matrix_UB_32      0.0054008000
_diffrn_orient_matrix_UB_33      -0.0258959000
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10873
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.534
_diffrn_reflns_theta_min         2.675
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.829
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.49a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3305
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.1545
_refine_ls_R_factor_gt           0.1361
_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^)+(0.1013P)^2^+22.1293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3267
_refine_ls_wR_factor_ref         0.3371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2703
_reflns_number_total             3305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr03175c2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1575918.cif.'
_cod_database_code               1575918
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O N Fe Cl'
_reflns_odcompleteness_completeness 98.81
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3.a Rotating group:
 O8(H8A,H8B), O6(H6A,H6B), O5(H5A,H5B), O7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C6(H6), C10(H10), C13(H13), C11(H11), C12(H12)
;
_shelx_res_checksum              70177
_shelx_fab_checksum              7988
_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 2.194
_oxdiff_exptl_absorpt_empirical_full_min 0.571