Abstract
Two novel octanuclear mixed-metal clusters M 2[Mo 3O 4(O 4CEt) 8Cr 2(O 2CEt) 8O 4Mo 3] · n(HO 2CEt) [M = K, n = 2 ( 1); M = Li, n = 0 ( 2)] have been synthesized and characterized by X-ray crystallographic structure determinations. Compound 1 is soluble in EtOH and N,N′-dimethylformamide solution, while compound 2 is insoluble. Both compounds contain a novel cyclic anion formed by two triangular trinuclear molybdenum cluster anions [Mo 3O 4(O 2CEt) 8] 4− and two chromium atoms as bridges connecting the two triangular molybdenum cluster anions. The potassium atom in compound I is coordinated to six oxygen atoms, including one oxygen atom from a weakly bound terminal HO 2CEt ligand. The lithium atom in compound 2 is five-coordinate. The weakly bound terminal ligand is responsible for the solubility of compound 1. Cyclic voltammetry shows a quasireversible redox couple for compound 1 at −0.97/−0.75 V/SCE and an irreversible oxidation peak at −0.52 V/SCE. The EPR spectrum of compound 1 suggests strong delocalization of electrons in this compound.
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