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The formation of the gaseous species LiCl, Li2Cl2, AlCl3 and LiAlCl4 was shown by mass spectrometric studies of the reaction of solid LiCl with gaseous AlCl3 at 575 °C. Besides AlCl3 and Al2Cl6, the gas complexes LiAlCl4, Li2AlCl5 and LiAl2Cl7 were formed during the evaporation of liquefied LiAlCl4. The structures of the molecules under discussion were computed by quantum chemical DFT studies. Thermodynamic data of these molecules were determined by experimental methods (mass spectrometry), and the results were confirmed by theoretical calculations. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008)