Influence of ancillary ligands on the formation and functionality of oxovanadium(V) metallosupramolecular assemblies: advanced computational and catalytic analyses.
Topić, Edi; Sarjanović, Josipa; Musija, Danijela; Mandarić, Mirna; Cocut, Andrea; Hrenar, Tomica; Agustin, Dominique; Pisk, Jana; Vrdoljak, Višnja; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5532–5545; doi:10.1039/d5dt00105f

data_7718152
_publ_section_title
;
 Influence of ancillary ligands on the formation and functionality of
 oxovanadium(V) metallosupramolecular assemblies: advanced computational
 and catalytic analyses.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5532
_journal_page_last               5545
_journal_paper_doi               10.1039/d5dt00105f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C16 H17 Mo N3 O6'
_chemical_formula_sum            'C16 H17 Mo N3 O6'
_chemical_formula_weight         443.26
_chemical_name_systematic
(ethanol)-cis-(2-oxido-3-methoxybenzaldehydeisonicotinylhydrazonato)-dioxomolybdenum(vi)
_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   mixed
_audit_creation_date             2025-02-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-13 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                113.2670(4)
_cell_angle_beta                 96.4325(4)
_cell_angle_gamma                97.8303(4)
_cell_formula_units_Z            2
_cell_length_a                   7.28057(4)
_cell_length_b                   10.45368(5)
_cell_length_c                   12.64056(6)
_cell_measurement_reflns_used    26692
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      79.7270
_cell_measurement_theta_min      3.8590
_cell_volume                     860.915(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_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_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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    -12.00  14.00   0.50    0.05    --   18.00  96.00-152.97   52
  2  \w    -15.00  11.00   0.50    0.05    --   18.00 100.00 -59.87   52
  3  \w     11.00  36.00   0.50    0.05    --   34.00  77.00 -30.82   50
  4  \w     14.00  40.00   0.50    0.05    --   34.00  73.00 -87.03   52
  5  \w     17.00  44.00   0.50    0.05    --   38.00  73.00-172.10   54
  6  \w     17.00  42.00   0.50    0.05    --   38.00  73.00  -7.59   50
  7  \w     11.00  36.00   0.50    0.05    --   34.00  77.00  10.11   50
  8  \w    -12.00  13.00   0.50    0.05    --   18.00 100.00  59.33   50
  9  \w     11.00  36.00   0.50    0.05    --   34.00  77.00 138.51   50
 10  \w     18.00  43.00   0.50    0.05    --   38.00  71.00 129.21   50
 11  \w     17.00  42.00   0.50    0.05    --   38.00  72.00  77.12   50
 12  \w     29.00  55.00   0.50    0.05    --   46.00  65.00 134.51   52
 13  \w     93.00 118.00   0.50    0.05    --   46.00  65.00 134.51   50
 14  \w     68.00 121.00   0.50    0.05    --   48.10  19.00  60.00  106
 15  \w     60.00  88.00   0.50    0.05    --   42.00  67.00  30.78   56
 16  \w     27.00  53.00   0.50    0.05    --   42.00  67.00  30.78   52
 17  \w     38.00  65.00   0.50    0.05    --   48.10  19.00  60.00   54
 18  \w     17.00  42.00   0.50    0.05    --   38.00  72.00-129.06   50
 19  \w     36.00  66.00   0.50    0.05    --   48.10  57.00-150.00   60
 20  \w     67.00  92.00   0.50    0.05    --  113.25   0.00-150.00   50
 21  \w     91.00 125.00   0.50    0.05    --  113.25  77.00-180.00   68
 22  \w    137.00 177.00   0.50    0.05    --  113.25  77.00-180.00   80
 23  \w     92.00 148.00   0.50    0.05    --  113.25  77.00 -30.00  112
 24  \w    135.00 178.00   0.50    0.05    --  113.25  77.00   0.00   86
 25  \w     91.00 128.00   0.50    0.05    --  113.25  77.00   0.00   74
 26  \w     92.00 156.00   0.50    0.05    --  113.25  77.00  30.00  128
 27  \w     91.00 140.00   0.50    0.05    --  113.25  77.00  90.00   98
 28  \w     93.00 173.00   0.50    0.05    --  113.25  77.00 120.00  160
 29  \w    141.00 167.00   0.50    0.05    --  113.25  77.00 150.00   52
 30  \w     91.00 129.00   0.50    0.05    --  113.25  77.00 150.00   76
 31  \w     96.00 122.00   0.50    0.05    --  113.25  77.00 -60.00   52
 32  \w    135.00 160.00   0.50    0.05    --  113.25  77.00 -60.00   50
 33  \w    128.00 177.00   0.50    0.05    --  113.25  77.00-120.00   98
 34  \w     94.00 120.00   0.50    0.05    --  113.25  77.00-120.00   52
 35  \w     93.00 119.00   0.50    0.05    --  113.25  77.00-150.00   52
 36  \w    124.00 149.00   0.50    0.05    --  113.25  77.00-150.00   50
 37  \w     91.00 157.00   0.50    0.05    --  113.25  75.00-133.81  132
 38  \w     95.00 142.00   0.50    0.05    --  113.25  77.00 -90.00   94
 39  \w    100.00 125.00   0.50    0.05    --  113.25  61.00-150.00   50
 40  \w     91.00 178.00   0.50    0.05    --  113.25  77.00  60.00  174
 41  \w    100.00 147.00   0.50    0.05    --  113.25  61.00  60.00   94
 42  \w     99.00 132.00   0.50    0.05    --  113.25  61.00  30.00   66
 43  \w     98.00 143.00   0.50    0.05    --  113.25  61.00  90.00   90
 44  \w     97.00 150.00   0.50    0.05    --  113.25  62.00 177.26  106
 45  \w     97.00 136.00   0.50    0.05    --  113.25  61.00 120.00   78
 46  \w    153.00 178.00   0.50    0.05    --  113.25  61.00  30.00   50
 47  \w    148.00 178.00   0.50    0.05    --  113.25  61.00-150.00   60
 48  \w    148.00 174.00   0.50    0.05    --  113.25  61.00 -90.00   52
 49  \w     98.00 144.00   0.50    0.05    --  113.25  61.00 -90.00   92
 50  \w     99.00 161.00   0.50    0.05    --  113.25  61.00 -60.00  124
 51  \w    102.00 134.00   0.50    0.05    --  113.25  61.00 -30.00   64
 52  \w    103.00 150.00   0.50    0.05    --  113.25  61.00   0.00   94
 53  \w    113.00 138.00   0.50    0.05    --  113.25  45.00  60.00   50
 54  \w    100.00 127.00   0.50    0.05    --  113.25  61.00 150.00   54
 55  \w    141.00 169.00   0.50    0.05    --  113.25  45.00 150.00   56
 56  \w    149.00 174.00   0.50    0.05    --  113.25  61.00  90.00   50
 57  \w    108.00 133.00   0.50    0.05    --  113.25  30.00 120.00   50
 58  \w    142.00 168.00   0.50    0.05    --  113.25  30.00  30.00   52
 59  \w    111.00 137.00   0.50    0.05    --  113.25  45.00 -90.00   52
 60  \w    122.00 148.00   0.50    0.05    --  113.25  45.00-120.00   52
 61  \w    107.00 166.00   0.50    0.05    --  113.25  45.00-150.00  118
 62  \w    117.00 143.00   0.50    0.05    --  113.25  30.00-120.00   52
 63  \w    118.00 178.00   0.50    0.05    --  113.25   0.00-150.00  120
 64  \w    139.00 165.00   0.50    0.05    --  113.25  30.00 -90.00   52
 65  \w    114.00 139.00   0.50    0.05    --  113.25  30.00 -30.00   50
 66  \w    153.00 178.00   0.50    0.05    --  113.25  30.00 -30.00   50
 67  \w    104.00 160.00   0.50    0.05    --  113.25  17.00  13.05  112
 68  \w    131.00 178.00   0.50    0.05    --  113.25 125.00 -30.00   94
 69  \w    124.00 177.00   0.50    0.05    --  113.25 125.00 -60.00  106
 70  \w    112.00 137.00   0.50    0.05    --  113.25 127.00 -28.00   50
 71  \w    115.00 145.00   0.50    0.05    --  113.25 125.00  30.00   60
 72  \w    151.00 178.00   0.50    0.05    --  113.25 125.00  30.00   54
 73  \w    153.00 178.00   0.50    0.05    --  113.25 125.00  90.00   50
 74  \w    104.00 140.00   0.50    0.05    --  113.25 145.00 139.00   72
 75  \w    116.00 159.00   0.50    0.05    --  113.25 125.00 150.00   86
 76  \w    119.00 151.00   0.50    0.05    --  113.25 125.00 120.00   64
 77  \w    111.00 138.00   0.50    0.05    --  113.25 125.00  90.00   54
 78  \w    117.00 163.00   0.50    0.05    --  113.25 125.00 -90.00   92
 79  \w    131.00 157.00   0.50    0.05    --  113.25 125.00-120.00   52
 80  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00-120.00   50
 81  \w     61.00  90.00   0.50    0.05    --  113.25 -77.00-150.00   58
 82  \w     80.00 105.00   0.50    0.05    --  113.25 -77.00-120.00   50
 83  \w     42.00  77.00   0.50    0.05    --  113.25 -77.00-120.00   70
 84  \w     60.00  98.00   0.50    0.05    --  113.25 -77.00 -60.00   76
 85  \w     73.00  98.00   0.50    0.05    --  113.25 -77.00 120.00   50
 86  \w     43.00  85.00   0.50    0.05    --  113.25 -77.00  90.00   84
 87  \w     42.00  70.00   0.50    0.05    --  113.25 -77.00 -30.00   56
 88  \w     42.00  68.00   0.50    0.05    --  113.25 -61.00 -90.00   52
 89  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00-180.00   50
 90  \w     91.00 140.00   0.50    0.05    --  113.25 -86.00-105.18   98
 91  \w     46.00  71.00   0.50    0.05    --  113.25-127.00-104.00   50
 92  \w     45.00  78.00   0.50    0.05    --  113.25-125.00-180.00   66
 93  \w     38.00  93.00   0.50    0.05    --   48.10-127.00-104.00  110
 94  \w     45.00  79.00   0.50    0.05    --  113.25-125.00 -30.00   68
 95  \w     87.00 125.00   0.50    0.05    --  113.25-145.00  87.00   76
 96  \w     48.00  91.00   0.50    0.05    --  113.25-125.00 120.00   86
 97  \w     46.00 107.00   0.50    0.05    --   48.10-145.00  87.00  122
 98  \w     48.00  76.00   0.50    0.05    --  113.25-125.00   0.00   56
 99  \w     76.00 105.00   0.50    0.05    --  113.25 -95.00  90.00   58
100  \w     57.00 111.00   0.50    0.05    --  113.25-125.00  90.00  108
101  \w     78.00 104.00   0.50    0.05    --  113.25 -95.00 150.00   52
102  \w     69.00 102.00   0.50    0.05    --  113.25 -95.00   0.00   66
103  \w     66.00  93.00   0.50    0.05    --  113.25 -95.00  60.00   54
104  \w     44.00  80.00   0.50    0.05    --  113.25-125.00-120.00   72
105  \w     45.00  80.00   0.50    0.05    --  113.25-125.00-150.00   70
106  \w     86.00 111.00   0.50    0.05    --  113.25-125.00-150.00   50
107  \w     81.00 106.00   0.50    0.05    --  113.25 -95.00-120.00   50
108  \w     43.00  73.00   0.50    0.05    --  113.25 -87.00  76.41   60
109  \w     92.00 118.00   0.50    0.05    --  113.25 -87.00  76.41   52
110  \w    -73.00 -31.00   0.50    0.05    --  -48.10 -62.00  70.63   84
111  \w    -58.00 -33.00   0.50    0.05    --  -48.10 -57.00 -60.00   50
112  \w    -75.00 -37.00   0.50    0.05    --  -48.10 -57.00-120.00   76
113  \w   -119.00 -86.00   0.50    0.05    --  -48.10 -57.00-120.00   66
114  \w   -117.00 -91.00   0.50    0.05    --  -48.10 -57.00 -60.00   52
115  \w   -114.00 -82.00   0.50    0.05    --  -48.10-127.00-104.00   64
116  \w   -141.00-116.00   0.50    0.05    --  -91.75-127.00-104.00   50
117  \w   -115.00 -88.00   0.50    0.05    --  -48.10-145.00  87.00   54
118  \w   -130.00-105.00   0.50    0.05    --  -91.75-145.00  87.00   50
119  \w    -94.00 -68.00   0.50    0.05    --  -82.00 -53.00 -31.89   52
120  \w    -76.00 -51.00   0.50    0.05    --  -70.00 -67.00 -54.45   50
121  \w   -104.00 -78.00   0.50    0.05    --  -91.75 -68.00-142.47   52
122  \w    -78.00 -52.00   0.50    0.05    --  -70.00 -67.00-149.25   52
123  \w   -101.00 -73.00   0.50    0.05    --  -91.75 -67.00 -93.39   56
124  \w   -101.00 -73.00   0.50    0.05    --  -91.75 -67.00 -39.36   56
125  \w    -85.00 -53.00   0.50    0.05    --  -70.00 -67.00 -40.47   64
126  \w    -91.00 -64.00   0.50    0.05    --  -82.00 -66.00 -77.73   54
127  \w   -141.00-114.00   0.50    0.05    --  -70.00 -67.00 -54.45   54
128  \w   -108.00 -73.00   0.50    0.05    --  -91.75 -67.00  51.97   70
129  \w    -80.00 -53.00   0.50    0.05    --  -70.00 -67.00 145.77   54
130  \w    -94.00 -68.00   0.50    0.05    --  -86.00 -66.00 140.47   52
131  \w   -108.00 -73.00   0.50    0.05    --  -91.75 -67.00 127.52   70
132  \w    -90.00 -48.00   0.50    0.05    --  -66.00 -66.00 177.72   84
133  \w   -154.00-128.00   0.50    0.05    --  -86.00 -66.00 140.47   52
134  \w    -72.00 -42.00   0.50    0.05    --  -58.00 -65.00  40.45   60
135  \w    -95.00 -68.00   0.50    0.05    --  -86.00 -65.00 -28.71   54
136  \w    -85.00 -37.00   0.50    0.05    --  -54.00 -65.00   9.38   96
137  \w    -82.00 -56.00   0.50    0.05    --  -74.00 -65.00 -72.36   52
138  \w    -78.00 -52.00   0.50    0.05    --  -70.00 -65.00-110.55   52
139  \w    -80.00 -52.00   0.50    0.05    --  -70.00 -65.00-124.84   56
140  \w    -79.00 -53.00   0.50    0.05    --  -70.00 -63.00-137.97   52
141  \w    -99.00 -74.00   0.50    0.05    --  -91.75 -66.00-123.37   50
142  \w   -100.00 -75.00   0.50    0.05    --  -91.75 -62.00-157.89   50
143  \w    -83.00 -58.00   0.50    0.05    --  -74.00 -63.00-165.94   50
144  \w   -140.00-114.00   0.50    0.05    --  -70.00 -65.00-124.84   52
145  \w   -101.00 -75.00   0.50    0.05    --  -91.75 -62.00 -65.88   52
146  \w    -85.00 -57.00   0.50    0.05    --  -74.00 -62.00-105.79   56
147  \w   -140.00-113.00   0.50    0.05    --  -74.00 -62.00-105.79   54
148  \w   -102.00 -75.00   0.50    0.05    --  -91.75 -61.00-109.01   54
149  \w   -101.00 -75.00   0.50    0.05    --  -91.75 -61.00 -90.00   52
150  \w   -101.00 -75.00   0.50    0.05    --  -91.75 -61.00-120.00   52
151  \w   -101.00 -76.00   0.50    0.05    --  -91.75 -60.00-139.16   50
152  \w   -107.00 -75.00   0.50    0.05    --  -91.75 -62.00  17.79   64
153  \w    -78.00 -51.00   0.50    0.05    --  -66.00 -59.00  60.71   54
154  \w    -85.00 -59.00   0.50    0.05    --  -74.00 -58.00  42.50   52
155  \w   -111.00 -77.00   0.50    0.05    --  -91.75 -58.00  76.19   68
156  \w   -106.00 -76.00   0.50    0.05    --  -91.75 -58.00  94.53   60
157  \w   -126.00 -99.00   0.50    0.05    --  -66.00 -58.00  99.37   54
158  \w    -99.00 -64.00   0.50    0.05    --  -78.00 -57.00  36.05   70
159  \w    -85.00 -59.00   0.50    0.05    --  -74.00 -57.00  81.75   52
160  \w   -100.00 -69.00   0.50    0.05    --  -82.00 -56.00  19.18   62
161  \w    -84.00 -59.00   0.50    0.05    --  -74.00 -56.00   1.03   50
162  \w    -87.00 -60.00   0.50    0.05    --  -74.00 -55.00 -19.01   54
163  \w    -98.00 -63.00   0.50    0.05    --  -78.00 -56.00  95.20   70
164  \w    -78.00 -53.00   0.50    0.05    --  -66.00 -58.00  99.37   50
165  \w    -96.00 -64.00   0.50    0.05    --  -82.00 -64.00 163.18   64
166  \w    -89.00 -57.00   0.50    0.05    --  -74.00 -64.00 174.24   64
167  \w    -78.00 -53.00   0.50    0.05    --  -91.75 127.00 -28.00   50
168  \w    -63.00 -37.00   0.50    0.05    --  -48.10 127.00 -28.00   52
169  \w    -85.00 -58.00   0.50    0.05    --  -48.10 145.00 139.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.888
_diffrn_reflns_theta_min         3.871
_exptl_absorpt_coefficient_mu    6.596
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0137(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.3936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3675
_reflns_number_total             3703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00105f2.cif
_cod_data_source_block           exp_6176_auto
_cod_depositor_comments
'Adding full bibliography for 7718146--7718153.cif.'
_cod_database_code               7718152
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.446
_shelx_estimated_absorpt_t_min   0.275
_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:
 C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C6(H6), C11(H11), C13(H13), C12(H12), C18(H18), C21(H21), C20(H20)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              92293
_shelx_hkl_checksum              55106
_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
;