High resolution neutron powder diffraction: a case study of the structure of C 60

Abstract

High resolution time-of-flight neutron powder diffraction has been used to determine the detailed structure of C 60 as a function of temperature. Rapid data collection coupled with high resolution has enabled subtle aspects of the 86 K orientational glass transition and precursor effects of the 260 K order-disorder transition to be observed. This surveying capability complements traditional single crystal methods. The power of the Rietveld method of profile refinement is demonstrated in the elucidation of the detailed crystal structure of the orientationally-ordered low temperature phase and in the evaluation of the departure from isotropic scattering of the C 60 molecule in the disordered high temperature phase. The counter-intuitive success in obtaining high-order cubic-harmonic coefficients, albeit to poorer precision than single crystal X-ray measurements, confirms the efficacy of the Rietveld profile refinement method. The collapse of three dimensions of diffraction information on to the one dimension of a high resolution powder diffraction pattern can still lead to an impressive amount of structural information that substantiates the assertion made by W. H. Bragg ‘the second method [powder diffraction], first used independently by Debye and Hull, can be used when the crystal is in powder, and can, therefore be employed when no single crystal can be obtained of sufficient size. All the spectra of the different planes are thrown together on the same diagram or photograph, and must be disentangled. This is not as difficult as it may seem . . . ’.