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_7249902
_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         'C35.667 H28.5 N6 O8 V2'
_chemical_formula_sum            'C35.67 H28.5 N6 O8 V2'
_chemical_formula_weight         771.03
_chemical_name_systematic
'[N'-(2-oxobenzylidene)isonicotinoylhydrazonato](1-pentoxo)oxovanadium(v)'
_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                   21.2703(3)
_cell_length_b                   29.7362(4)
_cell_length_c                   22.5536(4)
_cell_measurement_reflns_used    33047
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      77.758
_cell_measurement_theta_min      4.123
_cell_volume                     14265.1(4)
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33047
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.758
_diffrn_reflns_theta_min         4.123
_exptl_absorpt_coefficient_mu    4.901
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.457
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             6312
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1305P)^2^+16.8622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5571
_reflns_number_total             7431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra09073j2.cif
_cod_data_source_block           exp_2986_twin1_hklf4
_cod_original_formula_sum        'C35.67 H28.50 N6 O8 V2'
_cod_database_code               7249902
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.792
_olex2_refinement_description
;
1. 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,H,H,H) groups
2. Restrained distances
 C17A-C16A
 1.5 with sigma of 0.02
 C19A-C17A
 1.5 with sigma of 0.02
 C19-C20
 1.5 with sigma of 0.02
 C20-C21
 1.5 with sigma of 0.02
 C17-C18
 1.5 with sigma of 0.02
 C14-C19
 1.5 with sigma of 0.02
 C18-C17 \\sim C16-C15 \\sim C14-C19 \\sim C20-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C20: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C20 \\sim C21: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C18A) = Uanis(C17A)
Uanis(C19) = Uanis(C14)
4. Others
 Fixed Sof: H16C(0.5) H16D(0.5) H16A(0.5) H16B(0.5) C15(0.6666) H19D(0.5)
 H19E(0.5) H19F(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C16(0.6666) C17(0.6666)
 C18A(0.5) H18A(0.5) H18B(0.5) C18(0.6666) C17A(0.5) H17A(0.5) C21(0.3334)
 C20(0.3334) C19(0.3334)
5.a Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B), C15A(H15A,H15B), C16A(H16C,H16D), C16A(H16A,H16B), C18A(H18A,
 H18B)
5.b Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C6A(H6A), C3A(H3A), C5A(H5A), C6(H6), C4(H4), C5(H5), C4A(H4A),
 C3(H3), C13A(H13A), C7(H7), C11A(H11A), C10A(H10A), C12A(H12A), C10(H10),
 C13(H13), C11(H11), C12(H12), C17A(H17A)
5.c Idealised Me refined as rotating group:
 C19A(H19D,H19E,H19F), C19A(H19A,H19B,H19C)
;
_shelx_res_checksum              97144
_shelx_hkl_checksum              26670
_olex2_submission_special_instructions 'No special instructions were received'