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We report the results of complementary high-resolution powder diffraction studies by neutron and synchrotron radiation of the solid phases of C, H,: C, F, including the ab-ini-ti0 structure determination of the lowest temperature phase IV. Although in the last few years powder diffraction has been used to solve the structures of inorganic materials or compounds containing second-row or heavier elements,'" 21 we believe that this work represents a significant achievement by demonstrating that moderately complicated structures of organic compounds can be solved directly by powder methods for those cases where single-crystal techniques are not applicable.