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_7720194
_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         'C18 H20 N3 O5 V'
_chemical_formula_sum            'C18 H20 N3 O5 V'
_chemical_formula_weight         409.31
_chemical_name_systematic
'oxo-t-butoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   62.1004(15)
_cell_length_b                   16.0479(6)
_cell_length_c                   7.9027(3)
_cell_measurement_reflns_used    2694
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      78.3300
_cell_measurement_theta_min      2.8470
_cell_volume                     7875.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 41.123a 64-bit (release 20-01-2022))'
_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 2019/3 (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 0.994
_diffrn_measured_fraction_theta_max 0.972
_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   -122.00 -34.98   0.38   10.00    --  -47.74 -27.00 -36.00  229
  2  \w    -64.00 -27.14   0.38   40.00    --  -91.75  97.00 -96.00   97
  3  \w   -140.00-113.78   0.38   40.00    --  -91.75 -27.00 -36.00   69
  4  \w    100.00 126.22   0.38   40.00    --  113.25-149.00  98.00   69
  5  \w     42.00  97.86   0.38   40.00    --  113.25 -97.00 155.00  147
  6  \w   -117.00 -89.64   0.38   10.00    --  -47.74-125.00 120.00   72
  7  \w     -5.00  40.22   0.38   10.00    --   47.74 -38.00 150.00  119
  8  \w    111.00 138.74   0.38   40.00    --  113.25  30.00   0.00   73
  9  \w     44.00 104.80   0.38   40.00    --  113.25 -95.00-150.00  160
 10  \w     62.00  97.34   0.38   40.00    --  113.25 -77.00-150.00   93
 11  \w    146.00 175.64   0.38   40.00    --  113.25  30.00   0.00   78
 12  \w     49.00  74.08   0.38   40.00    --  113.25 -77.00 150.00   66
 13  \w    115.00 174.66   0.38   40.00    --  113.25  15.00 -90.00  157
 14  \w    101.00 143.94   0.38   40.00    --  113.25 125.00 -60.00  113
 15  \w    146.00 170.70   0.38   40.00    --  113.25 125.00 -60.00   65
 16  \w     43.00  68.08   0.38   40.00    --  113.25 -61.00-150.00   66
 17  \w     42.00  91.02   0.38   40.00    --  113.25-125.00 150.00  129
 18  \w     43.00  94.30   0.38   40.00    --  113.25 -95.00  30.00  135
 19  \w     42.00  67.08   0.38   40.00    --  113.25 -61.00 -60.00   66
;
_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      0.0063444000
_diffrn_orient_matrix_UB_12      -0.0507879000
_diffrn_orient_matrix_UB_13      0.1577960000
_diffrn_orient_matrix_UB_21      0.0063658000
_diffrn_orient_matrix_UB_22      0.0810019000
_diffrn_orient_matrix_UB_23      0.0916560000
_diffrn_orient_matrix_UB_31      -0.0231218000
_diffrn_orient_matrix_UB_32      0.0084530000
_diffrn_orient_matrix_UB_33      0.0686840000
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -78
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9373
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.910
_diffrn_reflns_theta_min         2.846
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94025
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.035(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3502
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0606P)^2^+9.2603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.561
_reflns_Friedel_fraction_full    0.702
_reflns_Friedel_fraction_max     0.632
_reflns_number_gt                3272
_reflns_number_total             3502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           4tert
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720194
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V C N O'
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.840
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.965(8)
 0.035(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C10(H10), C2(H2), C7(H7), C6(H6), C8(H8)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              57905
_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 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.842