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

✍ Scribed by Andreas Eichhöfer; Dieter Fenske; Petra Scheer

• Publisher: John Wiley and Sons
• Year: 2004
• Tongue: English
• Weight: 130 KB
• Volume: 2004
• Category: Article
• ISSN: 1434-1948
• DOI: 10.1002/ejic.200300263

✦ Synopsis

Abstract

The mixed‐valence cluster [Cu~20~Se~13~(PEt~3~)~12~] has been synthesized by the reaction of CuCl and PEt~3~ with Se(SiMe~3~)~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‐Cu~2~Se and not a Cu~3~Se~2~ phase 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 SePEt~3~ during the consolidation process. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)