North-HollandUltramicr°sc°py 52(1993)436-444 ultramicroscopy
Quantitative electron diffraction - new features in the program
system ELD
Xiaodong Zou, Yuri Sukharev and Sven Hovm611er
Structural Chemistry, Stockholm University, S-10691 Stockholm, Sweden
Received 5 January 1993
Dedicated to Professor John M. Cowley on the occasion of his seventieth birthday
Accurate quantitative intensities from electron diffraction patterns can be obtained by the program system ELD. Such
data is needed for solving or refining crystal structures. ELD runs on a personal computer. The quality of normal (i.e. not
slow-scan) CCD cameras is sufficient for giving quite accurate structure factor amplitudes from electron diffraction patterns.
Several factors which affect the intensity evaluation are discussed and some algorithms in ELD concerned with the problems
of extracting high quality quantitative structure factors from electron diffraction patterns are described.
1. Introduction
Structure determination of single crystals con-
sists of two steps: first solving and then refining
the structures. In X-ray crystallography, only the
amplitude parts of the structure factors are ex-
perimentally available. Various methods have
been developed for solving the phase problem,
for example, the Patterson method and the so-
called direct methods. A structural model can be
deduced once the phase information is available,
and then subjected to a least-squares refinement
against the experimental amplitudes.
Crystallographic image processing (CIP) has
been developed for solving structures from high
resolution electron microscopy (HREM) images
[1-3]. In HREM images, both amplitude and
phase information from the structure factors are
already present, although distorted. After digiti-
zation of the image, the Fourier transform is
calculated. By correcting for the optical distor-
tions and imposing the crystallographic symmetry
on the amplitudes and phases, a nearly distor-
tion-free map of projected potential can be re-
constructed by an inverse Fourier transformation.
Atomic coordinates, at least for heavier atoms,
can be obtained with an accuracy of 0.1 A and
these are good enough to serve as a starting
model for the next step, the structure refinement.
The resolution of electron diffraction (ED)
from inorganic crystals usually extends up to 1
or better. A complete three-dimensional data set
can be obtained by merging ED patterns from
several zone axes of a crystal (fig. 1). Despite the
strong scattering of electrons causing multiple
scattering, the data can be utilized for refinement
of the structure if the crystal is sufficiently thin.
o
For a resolution of about 1 A, the number of ED
amplitudes is large enough to allow all the vari-
ables to be refined. The refinement procedure is
similar to that used in X-ray crystallography,
combining the Fourier and the least-squares
methods. More accurate heavy-atom positions and
the coordinates for light atoms are the results of
the refinement. If the quality of the ED intensi-
ties is good, phases can also be deduced from the
intensities, by the same procedures as those used
in X-ray crystallography [4].
We are developing a computer program system
for structure determination by electron crystallog-
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