Direct phase determination and refinement in the electron crystallography of small structures

Abstract

The use of electron diffraction intensity data for quantitative determination of crystal structures was largely pioneered by Vainshtein, Pinsker and their co-workers, as recently reviewed, and was shown to produce results consistent with more typical X-ray structure analyses. Despite these encouraging results for a number of representative inorganic and organic materials, it is accurate to say that the technique has not been widely accepted by the crystallographic community. This is probably because, in several of the early analyses, contemporary X-ray structure results were used to provide heavy atom positions, thus providing much of the crystallographic phase information. Since it is also known that correct phases, combined with even scrambled structure factor amplitudes, will lead to a Fourier map that appears to be ’correct’, it is commonly (but incorrectly) thought that noab initioelectron diffraction determinations have been carried out for previously unsolved structures. In addition, the very complexity of n-beam dynamical scattering theory compared to ’primary extinction’ corrections has dampened enthusiasm to continue this work.