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_7134569
_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 Ni20 O52 S20 V8, 5(C2 H6 O), 12(C3 H7 N O)'
_chemical_formula_sum            'C262 H375 Cl5 N12 Ni20 O69 S20 V8'
_chemical_formula_weight         7196.89
_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   mixed
_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                   26.771(2)
_cell_length_b                   26.771(2)
_cell_length_c                   23.0428(19)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.0090
_cell_measurement_theta_min      2.3323
_cell_volume                     16514(2)
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            75315
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.406
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6479
_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            Yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       Block
_exptl_crystal_F_000             7464
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.462(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         13127
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+34.2669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.794
_reflns_Friedel_fraction_max     0.794
_reflns_number_gt                12406
_reflns_number_total             13127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02007g2.cif
_cod_data_source_block           Ni20V8
_cod_depositor_comments
'Adding full bibliography for 7134568--7134570.cif.'
_cod_original_cell_volume        16515(3)
_cod_database_code               7134569
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.788
_shelx_res_checksum              30351
_shelx_hkl_checksum              6132
_shelx_fab_checksum              83415