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_7718150
_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         'C64 H64 N12 O20 V4'
_chemical_formula_sum            'C64 H64 N12 O20 V4'
_chemical_formula_weight         1525.03
_chemical_name_systematic
tetrakis(ethoxo-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             2025-02-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-13 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                   17.6211(4)
_cell_length_b                   17.6211(4)
_cell_length_c                   21.2898(9)
_cell_measurement_reflns_used    6752
_cell_measurement_temperature    173.16(10)
_cell_measurement_theta_max      76.4740
_cell_measurement_theta_min      3.2480
_cell_volume                     6610.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_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     47.00  72.00   0.50    0.60    --   46.91  52.00-124.00   50
  2  \w    119.00 174.00   0.50    1.00    --  107.75  52.00-124.00  110
  3  \w    134.00 159.00   0.50    1.00    --  107.75  15.00 -90.00   50
  4  \w     83.00 109.00   0.50    0.60    --   46.91  52.00-124.00   52
  5  \w    -25.00  27.00   0.50    0.60    --  -46.91  19.00  60.00  104
  6  \w    -59.00 -34.00   0.50    1.00    --  -86.25  52.00-124.00   50
  7  \w   -118.00 -76.00   0.50    0.60    --  -46.91-125.00  30.00   84
  8  \w     41.00  67.00   0.50    1.00    --  107.75 -77.00 -60.00   52
  9  \w     75.00 101.00   0.50    1.00    --  107.75 -77.00 -90.00   52
 10  \w     47.00  89.00   0.50    1.00    --  107.75 -77.00-120.00   84
 11  \w     39.00  71.00   0.50    1.00    --  107.75 -77.00 -90.00   64
 12  \w     39.00  64.00   0.50    1.00    --  107.75 -61.00-150.00   50
 13  \w     75.00 100.00   0.50    1.00    --  107.75 -77.00 -60.00   50
 14  \w     39.00  64.00   0.50    1.00    --  107.75 -61.00 -30.00   50
 15  \w     43.00  70.00   0.50    1.00    --  107.75 -61.00  90.00   54
 16  \w     36.00  67.00   0.50    1.00    --  107.75 -61.00 120.00   62
 17  \w     35.00  61.00   0.50    1.00    --  107.75 -61.00 -90.00   52
 18  \w     79.00 104.00   0.50    1.00    --  107.75 -95.00 -90.00   50
 19  \w     74.00 102.00   0.50    1.00    --  107.75 -92.00-131.00   56
 20  \w     42.00  67.00   0.50    1.00    --  107.75 -95.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12910
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.872
_diffrn_reflns_theta_min         3.256
_exptl_absorpt_coefficient_mu    5.322
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.400
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0534P)^2^+15.2595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2963
_reflns_number_total             3437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00105f2.cif
_cod_data_source_block           exp_2911
_cod_depositor_comments
'Adding full bibliography for 7718146--7718153.cif.'
_cod_original_cell_volume        6610.5(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7718150
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.523
_shelx_estimated_absorpt_t_min   0.431
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C18(H18), C5(H5), C16(H16), C11(H11), C14(H14), C15(H15), C17(H17)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              6821
_shelx_hkl_checksum              31774
_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
;