Accuracy of linear polymer crystal structures determined from electron diffraction intensities: Problems with zonal data

Abstract

In contrast to analyses based on X-ray and neutron diffraction intensity data, electron crystal structure determination for organic materials is only a crudely-developed procedure. Although the pioneering work of Vainshtein and co-workers has been very important for realization of the technique's advantages, self-consistent procedures based on earlier-derived diffraction theory have only recently emerged, enabling a reasonable estimate of what structural information might be obtained from a given microcrystalline organic specimen and how this might be best achieved. Problems which are unresolved include the optimal refinement procedure for an unknown structure and also the adequate identification of the correct crystal structure during this refinement process.The behavior of the crystallographic residual(R) during structure refinement is manifested by various minima in a multidimensional parameter space. The description of this space is more complicated for electron diffraction than for X-ray diffraction, although both cases include atomic position, atomic thermal vibration, atomic occupancy, “extinction”, and crystal distortion.