Thiacalixarene-supported M20V8 (M = Fe, Co, Ni) square pyramid nanocages for visible light photothermal catalysis
Li, Qiqi; Zou, Yuhan; Mao, Dongao; Tian, Hongrui; Hang, Xinxin; Bi, Yanfeng; Chemical Communications 61 (2025) 9266–9269; doi:10.1039/D5CC02007G

data_7134568
_publ_section_title
;
 Thiacalixarene-supported M20V8 (M = Fe, Co, Ni) square pyramid nanocages
 for visible light photothermal catalysis
;
_journal_issue                   51
_journal_name_full               'Chemical Communications'
_journal_page_first              9266
_journal_page_last               9269
_journal_paper_doi               10.1039/D5CC02007G
_journal_volume                  61
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C216 H260 Cl5 Fe20 O52 S20 V8, 12(C3 H7 N O)(C2 H6 O)'
_chemical_formula_sum            'C254 H351 Cl5 Fe20 N12 O65 S20 V8'
_chemical_formula_weight         6955.42
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2025-05-08 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.9722(13)
_cell_length_b                   26.9722(13)
_cell_length_c                   22.8711(14)
_cell_measurement_reflns_used    9483
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0029
_cell_measurement_theta_min      2.3878
_cell_volume                     16638.7(15)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Diamond 3.2K'
_computing_publication_material  'Adobe Photoshop CS6 and POV-Ray v3.7'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            94058
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.434
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       Block
_exptl_crystal_F_000             7176
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(2)
_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     735
_refine_ls_number_reflns         14257
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1005P)^2^+36.2742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.938
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                13241
_reflns_number_total             14257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02007g2.cif
_cod_data_source_block           Fe20V8
_cod_depositor_comments
'Adding full bibliography for 7134568--7134570.cif.'
_cod_original_cell_volume        16638.7(19)
_cod_database_code               7134568
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.811
_shelx_estimated_absorpt_t_max   0.821
_shelx_res_checksum              54122
_shelx_hkl_checksum              13524
_shelx_fab_checksum              24805