C-60(CO2)(x), where x = 0.2 or 0.95, has been synthesized from solutions of C-60 in conventional organic solvents using antisolvent precipitation with supercritical CO2. The technique requires much lower pressures and temperatures than current routes to C-60(CO2)(x) and, for small quantities, is quicker. Products were characterized by SEM, IRI, C-13 solid-state NMR, and powder XRD. Reitveld refinement of the powder XRD shows CO2 to be located in the octahedral interstitial sites of the C-60 lattice. The cell lattice parameter is observed to increase for higher occupancies of CO2. Experimental conditions can be varied to generate radically different morphologies of C-60(CO2)x Using rapid antisolvent precipitation, irregular aggregates of ca, 200 nm particles are formed, where x = 0.2. With slower, diffusion-controlled precipitation, regular, highly crystalline, octahedral-shaped particles (1-70 mu m) can be formed, where x = 0.95. All products were precipitated completely free from the original organic solvent, and we conclude that CO2 has entered the lattice during crystallization.