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_7720204
_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         'C76 H88 N12 O20 V4'
_chemical_formula_sum            'C76 H88 N12 O20 V4'
_chemical_formula_weight         1693.34
_chemical_name_systematic
'oxo-n-pentoxo-[N''-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonato]vanadium(v) polymer'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-09
_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                78.5350(10)
_cell_angle_beta                 76.5900(10)
_cell_angle_gamma                76.5310(10)
_cell_formula_units_Z            1
_cell_length_a                   10.32720(10)
_cell_length_b                   14.26200(10)
_cell_length_c                   14.42770(10)
_cell_measurement_reflns_used    41641
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.7970
_cell_measurement_theta_min      3.1910
_cell_volume                     1986.54(3)
_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 0.985
_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    -69.00 -34.00   0.50    0.39    --  -46.80 -37.00  18.00   70
  2  \w   -120.00 -94.00   0.50    0.39    --  -46.80 -37.00  18.00   52
  3  \w     34.00  67.00   0.50    0.39    --   46.80  37.00 174.00   66
  4  \w    -24.00  36.00   0.50    0.39    --   46.80 -37.00  18.00  120
  5  \w   -141.00-116.00   0.50    1.56    --  -86.25 -37.00  18.00   50
  6  \w    -41.00 -16.00   0.50    1.56    --  -86.25  37.00 174.00   50
  7  \w    112.00 137.00   0.50    1.56    --  107.75  37.00 174.00   50
  8  \w   -103.00 -35.00   0.50    0.39    --  -46.80 -19.00  60.00  136
  9  \w    -20.00  27.00   0.50    0.39    --  -46.80  19.00-120.00   94
 10  \w    -27.00  25.00   0.50    0.39    --  -46.80  37.00 174.00  104
 11  \w     92.00 118.00   0.50    0.39    --   46.80  19.00 -60.00   52
 12  \w     87.00 119.00   0.50    0.39    --   46.80  66.00 110.87   64
 13  \w     34.00  84.00   0.50    0.39    --   46.80  19.00 -60.00  100
 14  \w     37.00  69.00   0.50    0.39    --   46.80  57.00   0.00   64
 15  \w     85.00 110.00   0.50    0.39    --   46.80  64.00 -40.70   50
 16  \w     29.00  62.00   0.50    0.39    --   46.80  64.00 -40.70   66
 17  \w     32.00  57.00   0.50    0.39    --   46.80  57.00 -60.00   50
 18  \w     81.00 118.00   0.50    0.39    --   46.80  64.00  70.52   74
 19  \w     84.00 115.00   0.50    0.39    --   46.80  63.00-175.61   62
 20  \w     33.00  65.00   0.50    0.39    --   46.80  57.00-120.00   64
 21  \w     35.00  94.00   0.50    0.39    --   46.80-125.00 -30.00  118
 22  \w     50.00  95.00   0.50    0.39    --   46.80-125.00-150.00   90
 23  \w     29.00  72.00   0.50    0.39    --   46.80  64.00  70.52   86
 24  \w     34.00  63.00   0.50    0.39    --   46.80  57.00 -90.00   58
 25  \w     31.00  60.00   0.50    0.39    --   46.80  62.00 152.76   58
 26  \w     87.00 113.00   0.50    0.39    --   46.80  62.00 152.76   52
 27  \w     33.00  64.00   0.50    0.39    --   46.80  57.00  30.00   62
 28  \w     75.00 100.00   0.50    0.39    --   46.80  57.00-120.00   50
 29  \w     29.00  62.00   0.50    0.39    --   46.80  66.00 110.87   66
 30  \w     30.00  55.00   0.50    0.39    --   46.80  62.00  58.49   50
 31  \w     30.00  79.00   0.50    0.39    --   46.80  63.00-175.61   98
 32  \w   -109.00 -70.00   0.50    1.56    --  -86.25 -64.00 -41.82   78
 33  \w   -102.00 -69.00   0.50    1.56    --  -86.25 -63.00 158.29   66
 34  \w    -96.00 -70.00   0.50    1.56    --  -86.25 -60.00 -81.02   52
 35  \w    -95.00 -69.00   0.50    1.56    --  -86.25 -63.00  97.02   52
 36  \w   -103.00 -69.00   0.50    1.56    --  -86.25 -66.00 -12.46   68
 37  \w    -96.00 -70.00   0.50    1.56    --  -86.25 -59.00  23.14   52
 38  \w    -95.00 -69.00   0.50    1.56    --  -86.25 -64.00  56.59   52
 39  \w    -95.00 -69.00   0.50    1.56    --  -86.25 -65.00-129.22   52
 40  \w   -143.00 -68.00   0.50    1.56    --  -86.25 -66.00-154.39  150
 41  \w   -102.00 -70.00   0.50    1.56    --  -86.25 -59.00 138.27   64
 42  \w    -94.00 -69.00   0.50    1.56    --  -86.25 -66.00 -88.63   50
 43  \w    -94.00 -68.00   0.50    1.56    --  -86.25 -66.00  44.34   52
 44  \w   -150.00-125.00   0.50    1.56    --  -86.25 -62.00 174.89   50
 45  \w   -102.00 -71.00   0.50    1.56    --  -86.25 -61.00 -30.00   62
 46  \w   -145.00-120.00   0.50    1.56    --  -86.25 -59.00  23.14   50
 47  \w    -94.00 -69.00   0.50    1.56    --  -86.25 -63.00 109.68   50
 48  \w    -94.00 -69.00   0.50    1.56    --  -86.25 -62.00  -9.47   50
 49  \w   -158.00-115.00   0.50    1.56    --  -86.25 -64.00 -41.82   86
 50  \w    -95.00 -69.00   0.50    1.56    --  -86.25 -62.00 174.89   52
 51  \w    -93.00 -68.00   0.50    1.56    --  -86.25 -66.00-104.52   50
 52  \w   -154.00-124.00   0.50    1.56    --  -86.25 -63.00  97.02   60
 53  \w   -154.00-128.00   0.50    1.56    --  -86.25 -63.00 109.68   52
 54  \w    -96.00 -71.00   0.50    1.56    --  -86.25 -56.00  57.87   50
 55  \w    -95.00 -70.00   0.50    1.56    --  -86.25 -60.00   9.45   50
 56  \w    -93.00 -68.00   0.50    1.56    --  -86.25 -66.00 -57.95   50
 57  \w    -96.00 -70.00   0.50    1.56    --  -86.25 -64.00   4.59   52
 58  \w   -104.00 -68.00   0.50    1.56    --  -86.25 -65.00 128.05   72
 59  \w    -97.00 -69.00   0.50    1.56    --  -86.25 -62.00-125.52   56
 60  \w    -94.00 -68.00   0.50    1.56    --  -86.25 -66.00-138.88   52
 61  \w    -95.00 -69.00   0.50    1.56    --  -86.25 -63.00-167.37   52
 62  \w    -94.00 -69.00   0.50    1.56    --  -86.25 -63.00  79.78   50
 63  \w     88.00 143.00   0.50    1.56    --  107.75  77.00  60.00  110
 64  \w     35.00  61.00   0.50    1.56    --  107.75 -77.00-180.00   52
 65  \w    101.00 130.00   0.50    1.56    --  107.75  45.00-120.00   58
 66  \w     81.00 112.00   0.50    1.56    --  107.75-125.00-180.00   62
 67  \w     52.00 112.00   0.50    1.56    --  107.75-125.00   0.00  120
 68  \w     78.00 104.00   0.50    1.56    --  107.75 -77.00-180.00   52
 69  \w     36.00  71.00   0.50    1.56    --  107.75 -61.00  30.00   70
 70  \w     35.00  71.00   0.50    1.56    --  107.75 -77.00 150.00   72
 71  \w     88.00 176.00   0.50    1.56    --  107.75  77.00 -90.00  176
 72  \w     91.00 146.00   0.50    1.56    --  107.75  61.00 120.00  110
 73  \w     91.00 137.00   0.50    1.56    --  107.75  61.00  30.00   92
 74  \w     89.00 178.00   0.50    1.56    --  107.75  70.00 137.98  178
 75  \w     37.00  62.00   0.50    1.56    --  107.75-125.00-180.00   50
 76  \w     78.00 108.00   0.50    1.56    --  107.75-110.00 -78.36   60
 77  \w     91.00 161.00   0.50    1.56    --  107.75  61.00-150.00  140
 78  \w    129.00 154.00   0.50    1.56    --  107.75  77.00-150.00   50
 79  \w    153.00 178.00   0.50    1.56    --  107.75  61.00-120.00   50
 80  \w     91.00 139.00   0.50    1.56    --  107.75  61.00 -90.00   96
 81  \w     88.00 114.00   0.50    1.56    --  107.75  77.00-150.00   52
 82  \w     36.00  84.00   0.50    1.56    --  107.75 -77.00-120.00   96
 83  \w     91.00 138.00   0.50    1.56    --  107.75  61.00-120.00   94
 84  \w    126.00 152.00   0.50    1.56    --  107.75  77.00  90.00   52
 85  \w     89.00 178.00   0.50    1.56    --  107.75  77.00   0.00  178
 86  \w    120.00 168.00   0.50    1.56    --  107.75  77.00 -60.00   96
 87  \w     81.00 108.00   0.50    1.56    --  107.75-110.00-112.66   54
 88  \w     38.00  66.00   0.50    1.56    --  107.75-110.00 -78.36   56
 89  \w    118.00 177.00   0.50    1.56    --  107.75  30.00  90.00  118
 90  \w     88.00 113.00   0.50    1.56    --  107.75  77.00 -60.00   50
 91  \w     81.00 111.00   0.50    1.56    --  107.75-125.00 -30.00   60
 92  \w     37.00  77.00   0.50    1.56    --  107.75-110.00-112.66   80
 93  \w     36.00  62.00   0.50    1.56    --  107.75-125.00 -30.00   52
 94  \w    134.00 160.00   0.50    1.56    --  107.75  61.00 -60.00   52
 95  \w     91.00 120.00   0.50    1.56    --  107.75  61.00 -60.00   58
 96  \w    151.00 178.00   0.50    1.56    --  107.75  61.00  90.00   54
 97  \w     78.00 104.00   0.50    1.56    --  107.75 -77.00 -30.00   52
 98  \w     37.00  75.00   0.50    1.56    --  107.75 -77.00 -30.00   76
 99  \w     46.00  72.00   0.50    1.56    --  107.75-107.00-149.68   52
100  \w     82.00 107.00   0.50    1.56    --  107.75-107.00-149.68   50
101  \w     91.00 128.00   0.50    1.56    --  107.75  61.00  90.00   74
102  \w    138.00 174.00   0.50    1.56    --  107.75  77.00 150.00   72
103  \w     88.00 116.00   0.50    1.56    --  107.75  77.00  90.00   56
104  \w     89.00 131.00   0.50    1.56    --  107.75  77.00 150.00   84
105  \w     88.00 148.00   0.50    1.56    --  107.75  77.00 120.00  120
106  \w     80.00 112.00   0.50    1.56    --  107.75-125.00-150.00   64
107  \w     35.00  61.00   0.50    1.56    --  107.75-125.00-150.00   52
108  \w    101.00 136.00   0.50    1.56    --  107.75 125.00 -90.00   70
109  \w    141.00 177.00   0.50    1.56    --  107.75 125.00 -90.00   72
110  \w     37.00  95.00   0.50    1.56    --  107.75 -95.00 120.00  116
111  \w     77.00 112.00   0.50    1.56    --  107.75-125.00 120.00   70
112  \w     36.00  69.00   0.50    1.56    --  107.75-125.00 120.00   66
113  \w    144.00 170.00   0.50    1.56    --  107.75  61.00   0.00   52
114  \w     88.00 178.00   0.50    1.56    --  107.75  77.00  30.00  180
115  \w     88.00 157.00   0.50    1.56    --  107.75  77.00-180.00  138
116  \w     91.00 127.00   0.50    1.56    --  107.75  61.00   0.00   72
117  \w     83.00 112.00   0.50    1.56    --  107.75-125.00  30.00   58
118  \w    123.00 148.00   0.50    1.56    --  107.75  77.00-120.00   50
119  \w     37.00  62.00   0.50    1.56    --  107.75-125.00  30.00   50
120  \w     88.00 113.00   0.50    1.56    --  107.75  77.00-120.00   50
121  \w     38.00  92.00   0.50    1.56    --  107.75 -77.00 -60.00  108
122  \w     92.00 163.00   0.50    1.56    --  107.75  61.00  60.00  142
123  \w     75.00 100.00   0.50    1.56    --  107.75 -77.00 150.00   50
124  \w     40.00  75.00   0.50    1.56    --  107.75 -87.00  16.36   70
125  \w     89.00 125.00   0.50    1.56    --  107.75 -87.00  16.36   72
126  \w     91.00 151.00   0.50    1.56    --  107.75  61.00-180.00  120
127  \w    120.00 156.00   0.50    1.56    --  107.75 125.00 150.00   72
128  \w    138.00 164.00   0.50    1.56    --  107.75  45.00-120.00   52
129  \w     51.00  76.00   0.50    1.56    --  107.75-125.00  90.00   50
130  \w    136.00 178.00   0.50    1.56    --  107.75  77.00 -30.00   84
131  \w     46.00  90.00   0.50    1.56    --  107.75 -77.00 -90.00   88
132  \w     94.00 125.00   0.50    1.56    --  107.75  61.00 -30.00   62
133  \w     96.00 169.00   0.50    1.56    --  107.75  45.00 -90.00  146
134  \w     88.00 129.00   0.50    1.56    --  107.75  77.00 -30.00   82
135  \w     64.00  97.00   0.50    1.56    --  107.75 -95.00  30.00   66
136  \w     36.00  74.00   0.50    1.56    --  107.75 -77.00 120.00   76
137  \w     35.00  79.00   0.50    1.56    --  107.75 -95.00  90.00   88
138  \w    134.00 160.00   0.50    1.56    --  107.75  45.00 -30.00   52
139  \w     95.00 122.00   0.50    1.56    --  107.75  45.00 -30.00   54
140  \w     38.00  70.00   0.50    1.56    --  107.75-104.00 121.78   64
141  \w     80.00 106.00   0.50    1.56    --  107.75-104.00 121.78   52
142  \w     38.00  89.00   0.50    1.56    --  107.75 -95.00 -60.00  102
143  \w     80.00 112.00   0.50    1.56    --  107.75-125.00  90.00   64
144  \w     96.00 176.00   0.50    1.56    --  107.75  45.00 120.00  160
145  \w    101.00 145.00   0.50    1.56    --  107.75  45.00 -60.00   88
146  \w     97.00 156.00   0.50    1.56    --  107.75  45.00   0.00  118
147  \w    123.00 161.00   0.50    1.56    --  107.75  45.00  30.00   76
148  \w     38.00  63.00   0.50    1.56    --  107.75 -61.00-180.00   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      0.1459718000
_diffrn_orient_matrix_UB_12      0.0052422000
_diffrn_orient_matrix_UB_13      0.0037798000
_diffrn_orient_matrix_UB_21      0.0251998000
_diffrn_orient_matrix_UB_22      0.0409582000
_diffrn_orient_matrix_UB_23      -0.1083894000
_diffrn_orient_matrix_UB_31      -0.0501457000
_diffrn_orient_matrix_UB_32      0.1045378000
_diffrn_orient_matrix_UB_33      0.0240024000
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            74882
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.141
_diffrn_reflns_theta_min         3.186
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.482
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         8374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0474P)^2^+0.7527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7895
_reflns_number_total             8374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03088a2.cif
_cod_data_source_block           5alpha
_cod_depositor_comments
'Adding full bibliography for 7720194--7720204.cif.'
_cod_database_code               7720204
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'V2 C38 N6 O10'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.483
_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:
 C15(H15A,H15B), C17(H17A,H17B), C16(H16A,H16B), C16A(H16C,H16D), C15A(H15C,
 H15D), C17A(H17C,H17D), C18(H18A,H18B), C18A(H18C,H18D)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C2(H2), C10A(H10A), C11A(H11A), C13A(H13A), C8(H8), C12A(H12A),
 C13(H13), C2A(H2A), C6(H6), C11(H11), C7(H7), C6A(H6A), C12(H12), C8A(H8A),
 C7A(H7A)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C19(H19A,H19B,H19C), C19A(H19D,
 H19E,H19F)
;
_shelx_res_checksum              84036
_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 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.721