Publication | Closed Access
Cation-Dependent Self-assembly of Vanadium Polyoxoniobates
34
Citations
40
References
2016
Year
Reaction of Na<sub>7</sub>H[Nb<sub>6</sub>O<sub>19</sub>]·15H<sub>2</sub>O with NaVO<sub>3</sub>·2H<sub>2</sub>O at 220 °C in the presence of NaHCO<sub>3</sub> gives new bicapped α-Keggin vanadododecaniobate [VNb<sub>12</sub>O<sub>40</sub>{NbO(CO<sub>3</sub>)}<sub>2</sub>]<sup>13-</sup>, isolated and structurally characterized as Na<sub>9</sub>H<sub>4</sub>[VNb<sub>12</sub>O<sub>40</sub>{NbO(CO<sub>3</sub>)}<sub>2</sub>]·37H<sub>2</sub>O (1). According to <sup>51</sup>V NMR and ESI-MS data, this anion equilibrates in solution with [VNb<sub>12</sub>O<sub>40</sub>]<sup>15-</sup> and oligomeric species that result from dissociation of the {NbO(CO<sub>3</sub>)}<sup>+</sup> fragments. In the presence of potassium, the same reaction gives [V<sub>x</sub>Nb<sub>24</sub>O<sub>76</sub>]<sup>n-</sup> (x = 4, n = 12 (2a); x = 3, n = 17 (2b)). The anions with x = 3 and 4 cocrystallize together, but exist as separate entities both in solid and in solution according to <sup>51</sup>V MAS NMR and ESI-MS data.
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