C60F36 has been obtained by fluorination of [60]fullerene with MnF3 at 350 °C under vacuum. HPLC separation involving elution first with toluene (to separate highly polar C60F18which has a much longer retention time, and in one run, C60F20 which has a retention time similar to that of C60F18), then with toluene–hexane mixtures, and finally hexane, produces two main fractions of C60F36, each giving a 1404 amu mass spectrum. The 19F NMR spectrum of the first fraction (which is also the major and more volatile component) consists of 12 lines of equal intensity showing it to have C3 symmetry. The spectrum of the second fraction consists of three lines of equal intensity, indicating it to be the T isomer, confirmed by 13C NMR spectroscopy which shows two lines of equal intensity in the sp2 region; the ratio of the two fractions is ca. 3∶1, respectively. Both the T isomer and a low energy C3 isomer contain the C60F18 moiety as a subset. A reason for the failure to observe any of the predicted D3d isomer is conjectured. The mass spectrum of purified C60F36 shows the presence of a trace of C60F38 (which is more volatile).