Nicotinoyl hydrazone-directed vanadium assemblies: metallosupramolecular isomerism, polymorphism, and catalytic oxidation performance.
Topić, Edi; Sarjanović, Josipa; Kuzman, Dino; Cocut, Andrea; Hrenar, Tomica; Pisk, Jana; Vrdoljak, Višnja; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4237–4249; doi:10.1039/d5dt03088a

data_7720201
_publ_section_title
;
 Nicotinoyl hydrazone-directed vanadium assemblies: metallosupramolecular
 isomerism, polymorphism, and catalytic oxidation performance.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4237
_journal_page_last               4249
_journal_paper_doi               10.1039/d5dt03088a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         '0.25(C68 H72 N12 O20 V4)'
_chemical_formula_sum            'C17 H18 N3 O5 V'
_chemical_formula_weight         395.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-02
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-28 deposited with the CCDC.	2026-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.686(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.4796(2)
_cell_length_b                   24.2950(6)
_cell_length_c                   14.3185(3)
_cell_measurement_reflns_used    3633
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      79.5600
_cell_measurement_theta_min      3.6470
_cell_volume                     3569.95(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_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_environment      N~2~
_diffrn_ambient_temperature      169.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_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    -81.00  13.00   0.50    1.00    --  -47.74 102.00 -40.00  188
  2  \w     15.00  56.00   0.50    1.00    --   47.74-102.00-143.00   82
  3  \w    -75.00 -50.00   0.50    4.00    --  -91.75 102.00 -40.00   50
  4  \w   -145.00-119.00   0.50    4.00    --  -91.75-102.00-143.00   52
  5  \w     70.00 106.00   0.50    4.00    --  113.25-102.00-143.00   72
  6  \w    107.00 162.00   0.50    4.00    --  113.25 102.00 -40.00  110
  7  \w   -115.00 -89.00   0.50    1.00    --  -47.74 -77.00-150.00   52
  8  \w   -119.00 -89.00   0.50    1.00    --  -47.74 -77.00 -30.00   60
  9  \w   -116.00 -90.00   0.50    1.00    --  -47.74 -77.00 -90.00   52
 10  \w   -115.00 -89.00   0.50    1.00    --  -47.74 -77.00-120.00   52
 11  \w    -26.00  22.00   0.50    1.00    --  -47.74  19.00 -90.00   96
 12  \w     88.00 116.00   0.50    1.00    --   47.74  77.00  30.00   56
 13  \w    -46.00 -21.00   0.50    4.00    --  -91.75  45.00-180.00   50
 14  \w    -51.00 -20.00   0.50    4.00    --  -91.75  45.00-120.00   62
 15  \w    -51.00 -26.00   0.50    4.00    --  -91.75  45.00 150.00   50
 16  \w     42.00  67.00   0.50    4.00    --  113.25 -61.00 -90.00   50
 17  \w     46.00  71.00   0.50    4.00    --  113.25 -77.00 -60.00   50
 18  \w    153.00 178.00   0.50    4.00    --  113.25  30.00  90.00   50
 19  \w     49.00 107.00   0.50    4.00    --  113.25-125.00   0.00  116
 20  \w    100.00 176.00   0.50    4.00    --  113.25  15.00 -90.00  152
 21  \w    133.00 176.00   0.50    4.00    --  113.25  15.00  60.00   86
 22  \w     42.00  68.00   0.50    4.00    --  113.25 -61.00  90.00   52
 23  \w    102.00 130.00   0.50    4.00    --  113.25  15.00  60.00   56
 24  \w    142.00 168.00   0.50    4.00    --  113.25  45.00 -60.00   52
 25  \w    103.00 141.00   0.50    4.00    --  113.25  45.00 -60.00   76
 26  \w     42.00  68.00   0.50    4.00    --  113.25 -61.00 -30.00   52
 27  \w    102.00 178.00   0.50    4.00    --  113.25  45.00-180.00  152
 28  \w    105.00 140.00   0.50    4.00    --  113.25  30.00  90.00   70
 29  \w     48.00  95.00   0.50    4.00    --  113.25 -95.00-120.00   94
 30  \w     42.00 104.00   0.50    4.00    --  113.25 -77.00-120.00  124
 31  \w     46.00  71.00   0.50    4.00    --  113.25 -61.00-180.00   50
 32  \w     79.00 105.00   0.50    4.00    --  113.25 -77.00 -60.00   52
 33  \w    125.00 151.00   0.50    4.00    --  113.25 125.00  30.00   52
 34  \w     70.00  96.00   0.50    4.00    --  113.25 -95.00-180.00   52
 35  \w     44.00  69.00   0.50    4.00    --  113.25 -95.00 -90.00   50
 36  \w     77.00 106.00   0.50    4.00    --  113.25 -95.00 -90.00   58
 37  \w     42.00  68.00   0.50    4.00    --  113.25 -61.00 120.00   52
 38  \w     42.00  67.00   0.50    4.00    --  113.25 -61.00  30.00   50
 39  \w    108.00 134.00   0.50    4.00    --  113.25  30.00   0.00   52
 40  \w     43.00  69.00   0.50    4.00    --  113.25 -61.00   0.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0000982000
_diffrn_orient_matrix_UB_12      0.0020783000
_diffrn_orient_matrix_UB_13      -0.1075407000
_diffrn_orient_matrix_UB_21      -0.0437947000
_diffrn_orient_matrix_UB_22      0.0606146000
_diffrn_orient_matrix_UB_23      -0.0030668000
_diffrn_orient_matrix_UB_31      0.1435944000
_diffrn_orient_matrix_UB_32      0.0185092000
_diffrn_orient_matrix_UB_33      0.0222691000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31775
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.990
_diffrn_reflns_theta_min         3.639
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.948
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
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    1.471
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0441P)^2^+0.8281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6902
_reflns_number_total             7614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           exp_7381
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720201
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'V C N O'
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.544
_diffrn_oxdiff_digest_hkl
;
01b6207f9a87771f6ddf324d4c368c0a6f36ed
;
_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.a Ternary CH refined with riding coordinates:
 C15(H15), C32(H32)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C21(H21), C13(H13), C11(H11), C20(H20), C22(H22), C24(H24),
 C12(H12), C23(H23), C30(H30), C6(H6), C28(H28), C29(H29), C4(H4), C5(H5)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              6329
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.741