Preparation of hydrofullerenes by hydrogen radical induced hydrogenation

Fullerite (a mix of crude C[sub 60] and C[sub 70]) has been hydrogenated using hydrogen radical species (H[sup [sm bullet]]) at elevated temperatures (400[degrees]C) and hydrogen pressures (6.9 MPa (cold)). Iodoethane was employed as the hydrogen radical promoter. Analysis of the reduced fullerite by fast atom bombardment mass spectrometry revealed a mixture of hydrofullerenes comprising mainly C[sub 60]H[sub 36] and C[sub 70]H[sub 36]. No spectral evidence for the ethylation or iodination of the fullerite was found. Prepared under these conditions, the product is only sparingly soluble in common solvents. Solid-state [sup 13]C nuclear magnetic resonance spectroscopy and infrared spectroscopy were used to characterize the reduced fullerite. The structure of the C[sub 60]H[sub 36] produced under these conditions is of lower symmetry than T[sub h] and most likely D[sub 3d] or C[sub 3i] symmetry. 18 refs., 3 figs.