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_7720199
_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         'C15 H14 N3 O5 V'
_chemical_formula_sum            'C15 H14 N3 O5 V'
_chemical_formula_weight         367.23
_chemical_name_systematic
'oxo-methoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer'
_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
_audit_creation_date             2025-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-22 deposited with the CCDC.	2026-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.323(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4973(7)
_cell_length_b                   10.8105(5)
_cell_length_c                   26.3388(19)
_cell_measurement_reflns_used    4029
_cell_measurement_temperature    298
_cell_measurement_theta_max      24.4900
_cell_measurement_theta_min      4.3430
_cell_volume                     3198.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.914
_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   -102.00  -8.00   1.00    2.00    --  -31.47 -57.00-180.00   94
  2  \w    -55.00  39.00   1.00    2.00    --  -31.47  57.00  30.00   94
  3  \w    -55.00  39.00   1.00    2.00    --  -31.47  57.00  90.00   94
  4  \w   -104.00   2.00   1.00    2.00    --  -31.47 -77.00 -90.00  106
  5  \w     34.00 109.00   1.00    2.00    --   28.65 179.00 -60.00   75
  6  \w   -102.00 -77.00   1.00    2.00    --  -31.47 -57.00  90.00   25
  7  \w   -102.00  -8.00   1.00    2.00    --  -31.47 -57.00  30.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0489397000
_diffrn_orient_matrix_UB_12      -0.0404958000
_diffrn_orient_matrix_UB_13      -0.0008184000
_diffrn_orient_matrix_UB_21      0.0039951000
_diffrn_orient_matrix_UB_22      0.0093522000
_diffrn_orient_matrix_UB_23      0.0269717000
_diffrn_orient_matrix_UB_31      -0.0397216000
_diffrn_orient_matrix_UB_32      0.0507514000
_diffrn_orient_matrix_UB_33      -0.0056452000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.1056
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            42682
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.800
_diffrn_reflns_theta_min         4.096
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504
_exptl_crystal_preparation
'Reaction between VANH and VO(acac)2 in methanol.'
_exptl_crystal_recrystallization_method
'Crystallization from methanol solution.'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         10849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1679
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4925
_reflns_number_total             10849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720199
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V2 C28 N6 O8'
_chemical_oxdiff_usercomment     Martina_vanNH+VOacac2-MeOH-sobna
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.696
_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 Aromatic/amide H refined with riding coordinates:
 C10(H10), C10A(H10A), C2A(H2A), C13A(H13A), C11A(H11A), C2(H2), C11(H11),
 C12A(H12A), C8A(H8A), C12(H12), C13(H13), C8(H8), C6(H6), C7(H7), C6A(H6A),
 C7A(H7A)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C14A(H14D,H14E,H14F), C15A(H15D,
 H15E,H15F)
;
_shelx_res_checksum              8393
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.100
_oxdiff_exptl_absorpt_empirical_full_min 0.944