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Stabilization of the + IV oxidation state in siloxide supported terbium compounds.

The synthesis of lanthanides, other than cerium, in the oxidation state +IV has remained for a long time a desirable but unmet target. Here we report the third example of a molecular complex of terbium(IV) which was isolated and characterized by EPR, UV-vis spectroscopy, SQUID magnetometry, and cyclic voltammetry. The supporting tetrakis(triphenylsiloxide) ligand environment does not saturate the coordination sphere of Tb(IV) in the six-coordinate complex [TbIV(OSiPh3)4(MeCN)2], 2-TbPh, but 2-TbPh shows high stability. Computational studies suggest that such stability is due to a strong π(O-Tb) interaction which is greater than in the previously reported Tb(IV) complexes.Importantly, non-binding counterions contribute to the Tb(IV) solution stability by destabilizing the +III oxidation state, while alkali ions promote Tb(IV)/Tb(III) electron-transfer. These results provide key information for the isolation of stable lanthanide(IV) ions. Reactivity studies of 2-TbPh with phosphinoxide ligands led to the synthesis of the stable complexes [TbIV(OSiPh3)4(Et3PO)], 3 and [TbIV(OSiPh3)4(Ph3PO)], 4.