The synthesis of FC(O)OONO2 is accomplished by the photolysis of a mixture of (FCO)2, NO2, and O2. The pure product is isolated after trap-to-trap condensation and the removal of byproducts by treatment of the crude product with O3 and AsF5. The colorless liquid freezes at −105 °C; its boiling point is 32 °C. At 20 °C and a few millibars, FC(O)OONO2 decomposes in the gas phase with a half-life of 20 h. FC(O)OONO2 is characterized by vapor pressure measurements, vibrational, 19F NMR, 13C NMR and UV spectroscopies as well as by mass spectrometry. According to the vibrational and NMR spectra, the compound exists at room temperature only as a syn conformer. The molecular structure of FC(O)OONO2 is determined by gas electron diffraction. The molecule possesses a skew structure with a dihedral angle of φ(COON) = 86.2(14)°. The short O−O bond (1.420(6) Å) and the long N−O bond (1.514(6) Å) are consistent with the chemical properties of this compound. The experimental geometry is reproduced reasonably well by quantum chemical.

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