Reversible dimerization of decaniobate

Three different solvates of TBA6[Nb10O28] (TBA = tetra-n-butylammonium) were structurally characterized. The results revealed that two water molecules are hydrogen-bonded to the terminal oxygens of the [Nb10O28]6− anion in the same manner in all of the solvates. Decaniobate [Nb10O28]6− dimerizes by the action of HCl to form icosaniobate [Nb20O54]8−, while icosaniobate breaks up into decaniobate [Nb10O28]6− by the action of TBAOH. Decaniobate also dimerizes spontaneously to form icosaniobate [Nb20O54]8− in CH2Cl2 even if no acid is added to the solution. The reaction was followed by IR spectroscopy, and the results suggested the reaction is second order with respect to the concentration of [Nb10O28]6−.