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_7718149
_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         'C14 H11 N3 O5 V, 2(H2 O)'
_chemical_formula_sum            'C14 H15 N3 O7 V'
_chemical_formula_weight         388.23
_chemical_name_systematic
'dioxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v) dihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                107.183(4)
_cell_angle_beta                 97.280(3)
_cell_angle_gamma                91.817(4)
_cell_formula_units_Z            2
_cell_length_a                   7.2890(3)
_cell_length_b                   10.4109(5)
_cell_length_c                   10.5800(4)
_cell_measurement_reflns_used    6378
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.9630
_cell_measurement_theta_min      4.4200
_cell_volume                     758.82(6)
_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      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_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   -111.00 -31.00   0.50    0.34    --  -47.16 -59.00 -38.00  160
  2  \w     32.00 118.00   0.50    0.34    --   47.16  59.00 101.00  172
  3  \w    -23.00  16.00   0.50    0.34    --   47.16 -59.00 -38.00   78
  4  \w     25.00  53.00   0.50    0.34    --   47.16 -59.00 -38.00   56
  5  \w    -47.00 -20.00   0.50    1.36    --  -86.25  59.00 101.00   54
  6  \w   -139.00-114.00   0.50    1.36    --  -86.25 -59.00 -38.00   50
  7  \w    119.00 162.00   0.50    1.36    --  107.75  59.00 101.00   86
  8  \w     36.00  65.00   0.50    1.36    --  107.75 -59.00 -38.00   58
  9  \w   -114.00 -89.00   0.50    0.34    --  -47.16 -77.00-150.00   50
 10  \w    -10.00  17.00   0.50    0.34    --  -47.16  59.00 101.00   54
 11  \w    -61.00 -18.00   0.50    0.34    --  -47.16  59.00 101.00   86
 12  \w     57.00  95.00   0.50    0.34    --   47.16-125.00 150.00   76
 13  \w     37.00  88.00   0.50    0.34    --   47.16-125.00  30.00  102
 14  \w    -50.00 -14.00   0.50    1.36    --  -86.25  45.00 -90.00   72
 15  \w    -49.00 -16.00   0.50    1.36    --  -86.25  45.00 -60.00   66
 16  \w     96.00 175.00   0.50    1.36    --  107.75 125.00 150.00  158
 17  \w     41.00  88.00   0.50    1.36    --  107.75 -95.00 -90.00   94
 18  \w     35.00  71.00   0.50    1.36    --  107.75 -61.00 150.00   72
 19  \w    118.00 144.00   0.50    1.36    --  107.75 125.00-180.00   52
 20  \w    147.00 174.00   0.50    1.36    --  107.75 125.00-180.00   54
 21  \w    110.00 178.00   0.50    1.36    --  107.75  45.00-120.00  136
 22  \w     41.00  66.00   0.50    1.36    --  107.75 -61.00-180.00   50
 23  \w     71.00 110.00   0.50    1.36    --  107.75-125.00 -90.00   78
 24  \w     39.00  67.00   0.50    1.36    --  107.75-125.00 120.00   56
 25  \w     36.00  61.00   0.50    1.36    --  107.75-125.00 -90.00   50
 26  \w     42.00  67.00   0.50    1.36    --  107.75 -77.00-150.00   50
 27  \w     79.00 104.00   0.50    1.36    --  107.75 -77.00-120.00   50
 28  \w     78.00 108.00   0.50    1.36    --  107.75-125.00 120.00   60
 29  \w     94.00 120.00   0.50    1.36    --  107.75  77.00 -90.00   52
 30  \w    132.00 158.00   0.50    1.36    --  107.75  77.00 -90.00   52
 31  \w    102.00 128.00   0.50    1.36    --  107.75  77.00-180.00   52
 32  \w    136.00 178.00   0.50    1.36    --  107.75  77.00-180.00   84
 33  \w     73.00 102.00   0.50    1.36    --  107.75-125.00-120.00   58
 34  \w     89.00 150.00   0.50    1.36    --  107.75  77.00 120.00  122
 35  \w     78.00 103.00   0.50    1.36    --  107.75 -95.00  90.00   50
 36  \w     37.00  62.00   0.50    1.36    --  107.75-125.00 -60.00   50
 37  \w     79.00 111.00   0.50    1.36    --  107.75-125.00 -60.00   64
 38  \w     41.00  72.00   0.50    1.36    --  107.75-125.00  90.00   62
 39  \w    135.00 164.00   0.50    1.36    --  107.75 125.00 120.00   58
 40  \w    106.00 178.00   0.50    1.36    --  107.75  45.00 -30.00  144
 41  \w     39.00  64.00   0.50    1.36    --  107.75-125.00 -30.00   50
 42  \w    127.00 153.00   0.50    1.36    --  107.75 125.00 -90.00   52
 43  \w     77.00 112.00   0.50    1.36    --  107.75-125.00 -30.00   70
 44  \w     99.00 155.00   0.50    1.36    --  107.75  15.00  30.00  112
 45  \w     84.00 109.00   0.50    1.36    --  107.75-125.00-150.00   50
 46  \w     80.00 112.00   0.50    1.36    --  107.75-125.00  90.00   64
 47  \w     38.00  63.00   0.50    1.36    --  107.75-125.00-150.00   50
 48  \w     39.00  64.00   0.50    1.36    --  107.75 -61.00  60.00   50
 49  \w     58.00 112.00   0.50    1.36    --  107.75-125.00  30.00  108
 50  \w    127.00 169.00   0.50    1.36    --  107.75  45.00  60.00   84
 51  \w     58.00  84.00   0.50    1.36    --  107.75 -77.00   0.00   52
 52  \w     37.00  62.00   0.50    1.36    --  107.75 -77.00 120.00   50
 53  \w     67.00  96.00   0.50    1.36    --  107.75 -77.00 120.00   58
 54  \w     44.00  69.00   0.50    1.36    --  107.75 -95.00-180.00   50
 55  \w     38.00  99.00   0.50    1.36    --  107.75 -95.00 -30.00  122
 56  \w     52.00  98.00   0.50    1.36    --  107.75 -95.00  30.00   92
 57  \w    120.00 161.00   0.50    1.36    --  107.75 125.00   0.00   82
 58  \w     99.00 124.00   0.50    1.36    --  107.75 125.00  60.00   50
 59  \w    140.00 178.00   0.50    1.36    --  107.75 125.00  60.00   76
 60  \w    111.00 136.00   0.50    1.36    --  107.75  45.00 -60.00   50
 61  \w     97.00 149.00   0.50    1.36    --  107.75  15.00 -30.00  104
 62  \w     83.00 108.00   0.50    1.36    --  107.75 -82.00  18.99   50
 63  \w     39.00 105.00   0.50    1.36    --  107.75 -95.00 120.00  132
;
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11559
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.755
_diffrn_reflns_theta_min         4.419
_exptl_absorpt_coefficient_mu    5.908
_exptl_absorpt_correction_T_max  0.15308
_exptl_absorpt_correction_T_min  0.05224
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       irregular
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.031
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0592
_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^)+(0.1387P)^2^+0.0838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2869
_reflns_number_total             3175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00105f2.cif
_cod_data_source_block           exp_4139
_cod_depositor_comments
'Adding full bibliography for 7718146--7718153.cif.'
_cod_database_code               7718149
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.509
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H24A,H24B} of O24
 At 1.5 times of:
  All C(H,H,H) groups, {H25A,H25B} of O25
2. Others
 Fixed X: H24A(0.64222) H24B(0.74325)
 Fixed Y: H24A(0.03517) H24B(0.0902)
 Fixed Z: H24A(0.96929) H24B(1.0949)
3.a Free rotating group:
 O25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C9(H9), C7(H7), C5(H5), C19(H19), C6(H6), C16(H16), C18(H18)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              80560
_shelx_hkl_checksum              52353
_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
- Detector area scaling
;