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_7249903
_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         'C28 H24 N6 O8 V2, 0.5[CH4O]'
_chemical_formula_sum            'C28.5 H26 N6 O8.5 V2'
_chemical_formula_weight         690.43
_chemical_name_systematic
'[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](methoxo)oxovanadium(v) methanol solvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I 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            16
_cell_length_a                   22.0687(2)
_cell_length_b                   20.5886(2)
_cell_length_c                   26.8420(3)
_cell_measurement_reflns_used    18194
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      76.9860
_cell_measurement_theta_min      3.2950
_cell_volume                     12196.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.986
_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   -101.00 -34.00   0.50    1.00    --  -47.29 -63.00  -7.00  134
  2  \w    -74.00 -49.00   0.50    5.50    --  -86.25  64.00 -83.00   50
  3  \w     45.00  71.00   0.50    5.50    --  107.75-102.00 -96.00   52
  4  \w     36.00  70.00   0.50    5.50    --  107.75 -63.00  -7.00   68
  5  \w     92.00 175.00   0.50    5.50    --  107.75  63.00 129.00  166
  6  \w    126.00 151.00   0.50    5.50    --  107.75  64.00 -83.00   50
  7  \w     35.00  60.00   0.50    5.50    --  107.75 -64.00 140.00   50
  8  \w    -25.00  20.00   0.50    1.00    --  -47.29  19.00 -90.00   90
  9  \w   -115.00 -90.00   0.50    1.00    --  -47.29 -77.00 -60.00   50
 10  \w     89.00 119.00   0.50    1.00    --   47.29  77.00  60.00   60
 11  \w     80.00 111.00   0.50    5.50    --  107.75-125.00   0.00   62
 12  \w     37.00  63.00   0.50    5.50    --  107.75 -95.00  60.00   52
 13  \w     44.00  70.00   0.50    5.50    --  107.75 -61.00  30.00   52
 14  \w     54.00 111.00   0.50    5.50    --  107.75-125.00 -30.00  114
 15  \w     68.00 106.00   0.50    5.50    --  107.75-125.00-180.00   76
 16  \w    107.00 137.00   0.50    5.50    --  107.75 125.00 150.00   60
 17  \w     38.00 107.00   0.50    5.50    --  107.75-125.00-150.00  138
 18  \w     36.00  67.00   0.50    5.50    --  107.75 -61.00  60.00   62
 19  \w    133.00 167.00   0.50    5.50    --  107.75  30.00  60.00   68
 20  \w     39.00  67.00   0.50    5.50    --  107.75-125.00 -60.00   56
 21  \w     75.00 107.00   0.50    5.50    --  107.75-125.00 -60.00   64
 22  \w     97.00 122.00   0.50    5.50    --  107.75 125.00  30.00   50
 23  \w    142.00 176.00   0.50    5.50    --  107.75 125.00  30.00   68
 24  \w     35.00  60.00   0.50    5.50    --  107.75 -61.00 -60.00   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  0.0315
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34430
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.725
_diffrn_reflns_theta_min         4.006
_exptl_absorpt_coefficient_mu    5.668
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.151
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             5648
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+11.9058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5950
_reflns_number_total             6412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra09073j2.cif
_cod_data_source_block           exp_4327
_cod_original_formula_sum        'C28.50 H26 N6 O8.50 V2'
_cod_database_code               7249903
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.359
_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. Others
 Fixed Sof: C14A(0.75) H14D(0.75) H14E(0.75) H14F(0.75) C15A(0.25) H15A(0.25)
 H15B(0.25) H15C(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C6(H6), C3A(H3A), C4(H4), C3(H3), C4A(H4A), C5A(H5A),
 C13(H13), C7A(H7A), C6A(H6A), C10(H10), C12(H12), C11(H11), C13A(H13A),
 C11A(H11A), C10A(H10A), C12A(H12A)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15A(H15A,H15B,H15C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 176 electrons were 
found in a volume of 1296\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[CH4O] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3626
_shelx_hkl_checksum              68467
_shelx_fab_checksum              33248
_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
;