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_7720195
_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         '0.5(C36 H40 N6 O10 V2)'
_chemical_formula_sum            'C18 H20 N3 O5 V'
_chemical_formula_weight         409.31
_chemical_name_systematic
'oxo-n-butoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer form alpha'
_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                 100.0760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8876(2)
_cell_length_b                   15.6647(2)
_cell_length_c                   13.37440(10)
_cell_measurement_reflns_used    14950
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      76.5940
_cell_measurement_theta_min      2.5160
_cell_volume                     3689.76(7)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_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    -61.00  24.00   0.50    0.75    --  -46.80  57.00-100.00  170
  2  \w   -117.00 -61.00   0.50    0.75    --  -46.80 -57.00 118.00  112
  3  \w    -25.00  41.00   0.50    0.75    --   46.80 -57.00 118.00  132
  4  \w     51.00  76.00   0.50    0.75    --   46.80  57.00-100.00   50
  5  \w    -66.00 -41.00   0.50    3.00    --  -86.25  57.00-100.00   50
  6  \w   -139.00-114.00   0.50    3.00    --  -86.25 -57.00 118.00   50
  7  \w     98.00 178.00   0.50    3.00    --  106.38  57.00-100.00  160
  8  \w     35.00  64.00   0.50    3.00    --  106.38 -57.00 118.00   58
  9  \w   -118.00 -80.00   0.50    0.75    --  -46.80-125.00 -90.00   76
 10  \w   -115.00 -84.00   0.50    0.75    --  -46.80-125.00  60.00   62
 11  \w    -40.00 -14.00   0.50    3.00    --  -86.25  38.00  90.00   52
 12  \w    -86.00 -25.00   0.50    3.00    --  -86.25 125.00   0.00  122
 13  \w    -40.00 -15.00   0.50    3.00    --  -86.25  38.00   0.00   50
 14  \w     34.00 106.00   0.50    3.00    --  106.38 -99.00  90.00  144
 15  \w     34.00  59.00   0.50    3.00    --  106.38 -57.00  30.00   50
 16  \w     34.00  59.00   0.50    3.00    --  106.38 -57.00 150.00   50
 17  \w     34.00  66.00   0.50    3.00    --  106.38 -57.00-120.00   64
 18  \w    111.00 178.00   0.50    3.00    --  106.38  38.00   0.00  134
 19  \w     35.00  60.00   0.50    3.00    --  106.38 -57.00  60.00   50
 20  \w    103.00 140.00   0.50    3.00    --  106.38 125.00 -60.00   74
 21  \w    143.00 178.00   0.50    3.00    --  106.38 125.00 -60.00   70
 22  \w     34.00  66.00   0.50    3.00    --  106.38 -57.00 -30.00   64
 23  \w     57.00 105.00   0.50    3.00    --  106.38 -77.00   0.00   96
 24  \w     37.00  64.00   0.50    3.00    --  106.38 -57.00-150.00   54
 25  \w     37.00  62.00   0.50    3.00    --  106.38 -57.00  90.00   50
 26  \w    127.00 174.00   0.50    3.00    --  106.38  19.00  30.00   94
 27  \w     35.00  64.00   0.50    3.00    --  106.38 -57.00-180.00   58
 28  \w     63.00  89.00   0.50    3.00    --  106.38 -77.00 -90.00   52
 29  \w     36.00  61.00   0.50    3.00    --  106.38 -57.00   0.00   50
;
_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      0.0113828000
_diffrn_orient_matrix_UB_12      -0.0651391000
_diffrn_orient_matrix_UB_13      0.0876357000
_diffrn_orient_matrix_UB_21      -0.0867194000
_diffrn_orient_matrix_UB_22      -0.0107277000
_diffrn_orient_matrix_UB_23      -0.0115037000
_diffrn_orient_matrix_UB_31      0.0026084000
_diffrn_orient_matrix_UB_32      -0.0728797000
_diffrn_orient_matrix_UB_33      -0.0766248000
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.296
_diffrn_reflns_theta_min         2.509
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
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    1.474
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0502P)^2^+2.4989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6889
_reflns_number_total             7555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           4alpha
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720195
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V C N O'
_chemical_oxdiff_usercomment     '  '
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C16A(H16A,H16B), C15(H15C,H15D), C16(H16C,H16D), C17A(H17A,
 H17B), C17(H17C,H17D)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C10A(H10A), C2(H2), C13(H13), C12(H12), C11(H11), C11A(H11A),
 C2A(H2A), C6(H6), C8(H8), C13A(H13A), C7(H7), C12A(H12A), C8A(H8A), C6A(H6A),
 C7A(H7A)
2.c Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C18A(H18A,H18B,H18C), C14(H14D,H14E,H14F), C18(H18D,
 H18E,H18F)
;
_shelx_res_checksum              31640
_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 1.217
_oxdiff_exptl_absorpt_empirical_full_min 0.826