High-valent oxovanadium metallosupramolecular species as catalysts for the oxidation of benzyl alcohol derivatives.
Topić, Edi; Sarjanović, Josipa; Musija, Danijela; Mandarić, Mirna; Hrenar, Tomica; Pisk, Jana; Vrdoljak, Višnja; RSC advances 15 (2025) 3547–3561; doi:10.1039/d4ra09073j

data_7249904
_publ_section_title
;
 High-valent oxovanadium metallosupramolecular species as catalysts for
 the oxidation of benzyl alcohol derivatives.
;
_journal_issue                   5
_journal_name_full               'RSC advances'
_journal_page_first              3547
_journal_page_last               3561
_journal_paper_doi               10.1039/d4ra09073j
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C17 H18 N3 O4 V'
_chemical_formula_sum            'C17 H18 N3 O4 V'
_chemical_formula_weight         379.28
_chemical_name_systematic
'[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](n-butoxo)oxovanadium(v)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.5068(2)
_cell_length_b                   11.70940(10)
_cell_length_c                   23.1275(3)
_cell_measurement_reflns_used    11889
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.5380
_cell_measurement_theta_min      3.8310
_cell_volume                     3386.96(8)
_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 2018/3 (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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -32.00  18.00   0.50    1.27    --  -46.91  50.00 -95.00  100
  2  \w    -42.00 -13.00   0.50    5.00    --  -86.25 113.00 133.00   58
  3  \w   -136.00-110.00   0.50    5.00    --  -86.25 -73.00 -74.00   52
  4  \w    -56.00 -31.00   0.50    5.00    --  -86.25  50.00 -95.00   50
  5  \w     97.00 133.00   0.50    5.00    --  107.75  50.00 -95.00   72
  6  \w    130.00 156.00   0.50    5.00    --  107.75 113.00 133.00   52
  7  \w     40.00  65.00   0.50    5.00    --  107.75 -73.00 -74.00   50
  8  \w   -119.00 -93.00   0.50    1.27    --  -46.91-125.00-120.00   52
  9  \w    -24.00  26.00   0.50    1.27    --  -46.91  19.00  60.00  100
 10  \w   -111.00 -84.00   0.50    1.27    --  -46.91-125.00-150.00   54
 11  \w   -106.00 -73.00   0.50    1.27    --  -46.91-125.00-180.00   66
 12  \w    111.00 137.00   0.50    5.00    --  107.75 125.00   0.00   52
 13  \w     37.00  63.00   0.50    5.00    --  107.75 -61.00-180.00   52
 14  \w     98.00 124.00   0.50    5.00    --  107.75  77.00 -90.00   52
 15  \w     36.00  88.00   0.50    5.00    --  107.75 -95.00  90.00  104
 16  \w     95.00 177.00   0.50    5.00    --  107.75  30.00-150.00  164
 17  \w     41.00  74.00   0.50    5.00    --  107.75-125.00  60.00   66
 18  \w    148.00 174.00   0.50    5.00    --  107.75 125.00  60.00   52
 19  \w    148.00 174.00   0.50    5.00    --  107.75  77.00 -90.00   52
 20  \w    106.00 134.00   0.50    5.00    --  107.75  45.00 -30.00   56
 21  \w    137.00 177.00   0.50    5.00    --  107.75  45.00 -30.00   80
 22  \w    153.00 178.00   0.50    5.00    --  107.75  30.00 120.00   50
 23  \w    145.00 174.00   0.50    5.00    --  107.75  45.00 -60.00   58
 24  \w    108.00 146.00   0.50    5.00    --  107.75  30.00 120.00   76
 25  \w     38.00  64.00   0.50    5.00    --  107.75 -95.00 -60.00   52
 26  \w     35.00  66.00   0.50    5.00    --  107.75 -61.00 -30.00   62
 27  \w     99.00 124.00   0.50    5.00    --  107.75  45.00 -60.00   50
 28  \w     67.00 105.00   0.50    5.00    --  107.75 -77.00 -60.00   76
 29  \w     38.00  85.00   0.50    5.00    --  107.75 -95.00  60.00   94
 30  \w     53.00  79.00   0.50    5.00    --  107.75 -77.00  30.00   52
 31  \w     35.00  71.00   0.50    5.00    --  107.75 -61.00 120.00   72
 32  \w    105.00 146.00   0.50    5.00    --  107.75  45.00  30.00   82
 33  \w     42.00  68.00   0.50    5.00    --  107.75 -61.00  90.00   52
;
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24059
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.813
_diffrn_reflns_theta_min         3.823
_exptl_absorpt_coefficient_mu    5.143
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.508
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0704P)^2^+3.7488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3295
_reflns_number_total             3604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra09073j2.cif
_cod_data_source_block           exp_3517
_cod_database_code               7249904
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.434
_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:
 C14(H14A,H14B), C16(H16A,H16B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C5(H5), C3(H3), C4(H4), C13(H13), C10(H10), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              98990
_shelx_hkl_checksum              19027
_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
;