Photocatalytic oxidation of various C–H bonds by a polyoxometalate nanocluster-dominated compartmentalized metal–organic framework
Jiao, Jiachen; Zhang, Chuanbao; Sun, Hui; Hu, Haina; Xu, Ziqing; Zhao, Junwei; Han, Qiuxia; Ma, Pengtao; Green Chemistry 27 (2025) 7608–7619; doi:10.1039/D5GC00269A

data_7250442
_publ_section_title
;
 Photocatalytic oxidation of various C--H bonds by a polyoxometalate
 nanocluster-dominated compartmentalized metal--organic framework
;
_journal_issue                   25
_journal_name_full               'Green Chemistry'
_journal_page_first              7608
_journal_page_last               7619
_journal_paper_doi               10.1039/D5GC00269A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety
'C27 H18 N9 Ni2 O46 W12, C18 H12 N6 Ni O5, 5(O)'
_chemical_formula_sum            'C45 H30 N15 Ni3 O56 W12'
_chemical_formula_weight         4059.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-16 deposited with the CCDC.	2025-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.9440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.284(4)
_cell_length_b                   20.5520(17)
_cell_length_c                   26.903(2)
_cell_measurement_reflns_used    6563
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.20
_cell_volume                     19127(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Helios multilayer optic'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            49671
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.152
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_type              Microfocus
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.039
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1221 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.6147. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             14600
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.728
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         17047
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0645P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11941
_reflns_number_total             17047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5gc00269a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7250442.cif.'
_cod_database_code               7250442
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.266
_shelx_estimated_absorpt_t_min   0.123
_diffrn_source_source            'Incoatc Ius 3.0 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C44) \\sim Ueq, Uanis(O14W) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(O15W)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O13W(0.5) O17W(0.5) O18W(0.5) O19W(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C41(H41), C42(H42), C44(H44), C45(H45), C49(H49), C50(H50)
;
_shelx_res_checksum              80687
_shelx_hkl_checksum              91202
_shelx_fab_checksum              19278
_olex2_submission_special_instructions 'No special instructions were received'