Influence of ancillary ligands on the formation and functionality of oxovanadium(V) metallosupramolecular assemblies: advanced computational and catalytic analyses.
Topić, Edi; Sarjanović, Josipa; Musija, Danijela; Mandarić, Mirna; Cocut, Andrea; Hrenar, Tomica; Agustin, Dominique; Pisk, Jana; Vrdoljak, Višnja; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5532–5545; doi:10.1039/d5dt00105f

data_7718151
_publ_section_title
;
 Influence of ancillary ligands on the formation and functionality of
 oxovanadium(V) metallosupramolecular assemblies: advanced computational
 and catalytic analyses.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5532
_journal_page_last               5545
_journal_paper_doi               10.1039/d5dt00105f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C60 H56 N12 O20 V4'
_chemical_formula_sum            'C60 H56 N12 O20 V4'
_chemical_formula_weight         1468.92
_chemical_name_systematic
tetrakis(methoxo-oxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v))
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-02-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-19 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5925(4)
_cell_length_b                   17.5925(4)
_cell_length_c                   21.6260(9)
_cell_measurement_reflns_used    3830
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.493
_cell_measurement_theta_min      4.282
_cell_volume                     6693.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1285
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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   -107.00 -78.00   1.00   40.00    --  -28.78-178.00 -30.00   29
  2  \w     12.00  99.00   1.00   40.00    --   30.34  37.00  90.00   87
  3  \w    -38.00  62.00   1.00   40.00    --   30.34 -37.00 -90.00  100
  4  \w     30.00  75.00   1.00   40.00    --   30.34 -99.00-150.00   45
  5  \w    -40.00  54.00   1.00   40.00    --   30.34 -57.00 150.00   94
  6  \w      7.00 101.00   1.00   40.00    --   30.34  57.00-180.00   94
  7  \w     35.00 110.00   1.00   40.00    --   30.34 178.00 150.00   75
  8  \w     -3.00  86.00   1.00   40.00    --   30.34  77.00 -30.00   89
  9  \w     -2.00 104.00   1.00   40.00    --   30.34  37.00 -60.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34740
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         4.282
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0623P)^2^+6.9113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2870
_reflns_number_total             3830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00105f2.cif
_cod_data_source_block           exp_4442
_cod_depositor_comments
'Adding full bibliography for 7718146--7718153.cif.'
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7718151
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.929
_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
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C5(H5), C15(H15), C16(H16), C6(H6), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              92163
_shelx_hkl_checksum              61194
_olex2_submission_special_instructions 'No special instructions were received'