A tetra-n-butylammonium (TBA) salt of [Ta10O28](6-) was synthesized by heating TBA6[H2Ta6O19] in toluene for a prolonged period. X-ray structural analysis of TBA6[Ta10O28]·6H2O revealed that the anion has the decametalate structure and is isostructural with the decavanadate and decaniobate anions [a = 15.8517(8) Å, b = 19.364(1) Å, c = 21.935(1) Å, β = 93.638(1)°, V = 6719.4(6) Å(3), Z = 2, and space group P2(1)/n at 292(2) K].
A tetra-n-butylammonium (TBA) salt of [H(4.5)(Ta(6)O(19))](3.5-) was synthesized by reacting hydrous tantalum oxide with TBAOH. X-ray structural analysis of TBA(3.5)[H(4.5)(Ta(6)O(19))]·2THF·5.5H(2)O (THF = tetrahydrofuran) revealed that this compound consists of a hydrogen-bonded, rod-shaped tetramer of hexatantalate that is almost 30 Å long together with TBA cations and solvent molecules of crystallization [a = 20.6354(5) Å, b = 25.5951(7) Å, c = 37.2058(8) Å, α = 77.092(1)°, β = 86.177(1)°, γ = 88.683(1)°, V = 19110.9(8) Å(3), Z = 8, and space group P ̅1]. (1)H NMR spectra showed that this tetrameric structure is maintained in solution.
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