Abstract
Reaction of Na7H[Nb6O19]·15H2O with NaVO3·2H2O at 220 °C in the presence of NaHCO3 gives new bicapped α-Keggin vanadododecaniobate [VNb12O40{NbO(CO3)}2]13-, isolated and structurally characterized as Na9H4[VNb12O40{NbO(CO3)}2]·37H2O (1). According to 51V NMR and ESI-MS data, this anion equilibrates in solution with [VNb12O40]15- and oligomeric species that result from dissociation of the {NbO(CO3)}+ fragments. In the presence of potassium, the same reaction gives [VxNb24O76]n- (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 51V MAS NMR and ESI-MS data.
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