Investigation of the Thermal Properties of [Cu20Se13(PEt3)12]

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Abstract
The mixed‐valence cluster [Cu20Se13(PEt3)12] has been synthesized by the reaction of CuCl and PEt3with Se(SiMe3)2. A powder‐diffraction pattern has revealed its crystalline purity and UV/Vis reflectance spectra display an intervalence band around 1200 nm. The solid‐state conversion of the cluster upon heating yields, even at moderate temperatures of around 100 °C, α‐Cu2Se and not a Cu3Se2phase that should be favoured in terms of the Cu/Se ratio of 3.1:2 in the cluster complex. This thermogravimetric analysis, coupled with mass spectrometry, shows that in addition to the labile phosphane ligands selenium atoms are cleaved as SePEt3during the consolidation process. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)

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