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_7718148
_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         'C19 H22 N3 O5 V'
_chemical_formula_sum            'C19 H22 N3 O5 V'
_chemical_formula_weight         423.33
_chemical_name_systematic
pentoxo-oxo-(N'-(3-methoxy-2-oxo-benzylidene)isonicotinoylhydrazonato)vanadium(v)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-02-19
_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                   11.8119(5)
_cell_length_b                   14.9558(6)
_cell_length_c                   10.9912(6)
_cell_measurement_reflns_used    5410
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.9810
_cell_measurement_theta_min      4.7540
_cell_volume                     1941.67(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.982
_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     50.00  75.00   0.50    0.30    --   47.03  66.00  25.00   50
  2  \w    106.00 132.00   0.50    1.20    --  107.75  80.00 140.00   52
  3  \w    133.00 175.00   0.50    1.20    --  107.75  80.00 140.00   84
  4  \w    105.00 178.00   0.50    1.20    --  107.75  66.00  25.00  146
  5  \w    104.00 134.00   0.50    1.20    --  107.75  45.00 -60.00   60
  6  \w    144.00 172.00   0.50    1.20    --  107.75  45.00 -60.00   56
  7  \w     99.00 175.00   0.50    1.20    --  107.75  76.00-104.00  152
  8  \w    -79.00 -42.00   0.50    0.30    --  -47.03 -38.00   0.00   74
  9  \w   -115.00 -82.00   0.50    0.30    --  -47.03 -38.00   0.00   66
 10  \w    -42.00 -16.00   0.50    1.20    --  -86.25  45.00-150.00   52
 11  \w   -113.00 -74.00   0.50    0.30    --  -47.03-125.00-180.00   78
 12  \w   -120.00 -86.00   0.50    0.30    --  -47.03-125.00 -30.00   68
 13  \w     35.00  81.00   0.50    1.20    --  107.75 -95.00 120.00   92
 14  \w     47.00  75.00   0.50    1.20    --  107.75 -77.00 -60.00   56
 15  \w     38.00  63.00   0.50    1.20    --  107.75 -61.00 -60.00   50
 16  \w     35.00  88.00   0.50    1.20    --  107.75 -77.00  30.00  106
 17  \w     42.00  67.00   0.50    1.20    --  107.75 -61.00  30.00   50
 18  \w    -26.00   6.00   0.50    0.30    --   47.03 -19.00-120.00   64
 19  \w     35.00  60.00   0.50    1.20    --  107.75 -61.00-180.00   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  0.0694
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8648
_diffrn_reflns_point_group_measured_fraction_full 0.815
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.158
_diffrn_reflns_theta_min         2.955
_exptl_absorpt_coefficient_mu    4.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       needle
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.033(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0905P)^2^+1.5530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1793
_reflns_Friedel_coverage         0.502
_reflns_Friedel_fraction_full    0.609
_reflns_Friedel_fraction_max     0.551
_reflns_number_gt                2778
_reflns_number_total             3226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00105f2.cif
_cod_data_source_block           exp_2480_auto
_cod_depositor_comments
'Adding full bibliography for 7718146--7718153.cif.'
_cod_database_code               7718148
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.509
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.967(16)
 0.033(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Restrained distances
 C27A-C28
 1.52 with sigma of 0.02
 C26-C27
 1.52 with sigma of 0.02
 C24-C25
 1.52 with sigma of 0.01
 C25-C26
 1.52 with sigma of 0.01
 C27-C28
 1.52 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C25A, C26A, C27A, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H24A(0.333333) H24B(0.333333) H24C(0.666667) H24D(0.666667)
 C25A(0.333333) H25A(0.333333) H25B(0.333333) C26A(0.333333) H26A(0.333333)
 H26B(0.333333) C27A(0.333333) H27A(0.333333) H27B(0.333333) C25(0.666667)
 H25C(0.666667) H25D(0.666667) C27(0.666667) H27C(0.666667) H27D(0.666667)
 H28A(0.333333) H28B(0.333333) H28C(0.333333) H28D(0.666667) H28E(0.666667)
 H28F(0.666667) C26(0.666667) H26C(0.666667) H26D(0.666667)
6.a Free rotating group:
 C24(C25A,C26A,C27A)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C24(H24C,H24D), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27A,
 H27B), C25(H25C,H25D), C27(H27C,H27D), C26(H26C,H26D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C17(H17), C11(H11), C12(H12), C16(H16), C15(H15), C18(H18), C14(H14)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C28(H28D,H28E,H28F)
;
_shelx_res_checksum              73612
_shelx_hkl_checksum              87106
_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
;