The synthesis of CF(3)C(O)OONO(2) is accomplished by the reaction of (CF(3)C(O))(2)O with H(2)O(2) and subsequent nitration of the resulting peracetic acid. The pure product is isolated by trap to trap condensation and removal of the byproducts by treatment with NaHCO(3). At room temperature CF(3)C(O)OONO(2) is stable for days in the gaseous or liquid state. The melting point is -92 degrees C and the boiling point is extrapolated to 42.5 degrees C from the expression ln p = -4045/T + 19.77 (p in mbar, T in K). The compound is characterized further by mass spectrometry and vibrational, NMR, and UV spectroscopy. According to the NMR spectra of CF(3)C(O)OONO(2) as well as CH(3)C(O)OONO(2), both molecules exist in one single conformeric form at room temperature.