Abstract

The novel dimeric phosphotungstate, [P 2W 18Cd 4(H 2O) 2O 68] 10−, has been synthesized by an unusual reaction of A-β-Na 8HPW 9O 34 with cadmium nitrate under controlled pH conditions. This compound has also been synthesized by the reaction of B-α-Na 8HPW 9O 34 with cadmium nitrate. The unambiguous characterization of B-α-[P 2W 18Cd 4(H 2O) 2O 68] 10− was accomplished by means of elemental analysis, IR, 31P and 113Cd NMR spectroscopy, and confirmed by a single crystal X-ray structural analysis of the NH 4 + salt. The heteropolyanion consist of two lacunary B-α-[PW 9O 34] 9− Keggin moieties linked via a rhomboid Cd 4O 16 group leading to a sandwich-type structure. Acidification of this anion, like other P 2W 18M 4O 68 10− (M=Co, Zn, …) species, forms the PW 12O 40 3− anions as the main product.

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