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Salts of the tetrakis(pentafluoroethyl)aluminate anion [Al(C 2 F 5 ) 4 ] −  were obtained from AlCl 3  and LiC 2 F 5 . They were isolated with different counter‐cations and characterized by NMR and vibrational spectroscopy and mass spectrometry. Degradation of the [Al(C 2 F 5 ) 4 ] −  ion was found to proceed via 1,2‐fluorine shifts and stepwise loss of CF(CF 3 ) under formation of [(C 2 F 5 ) 4− n  AlF  n  ] −  ( n= 1–4) as assessed by NMR spectroscopy and mass spectrometry and supported by results of DFT calculations. In addition, the [(C 2 F 5 )AlF 3 ] −  ion was structurally characterized.

Pentafluoroethylaluminates: A Combined Synthetic, Spectroscopic, and Structural Study