Reminiscences and discoveries, the introduction of Fourier methods into crystal-structure determination

1. The nature of X-rays X-rays were discovered in 1895 by Rontgen in Wurtzburg. For the next 17 years the nature of these rays was one of the dominant questions in physics: were they particles or were they waves? W.H. Bragg, of Adelaide, found indisputable evidence that they were particles; C.G. Barkla, of Liverpool and Edinburgh, found even more indisputable evidence that they were waves. The decisive experiment was carried out by Friedrich and Knipping (1) in 1912 in Munich, under the guidance of von Laue; they passed a fine beam of X-rays through a crystal of copper sulphate, hoping that it would behave as a diffraction grating. It did! The background was emotionally described bv von Laue in 1948 (2). * W.H. Bragg had a son, W.L. Bragg, who was a research student under J.J. Thomson at Cambridge. He was, as he himself said later, rather upset that his father seemed to have been proved wrong, and he tried to think up an alternative explanation of particles travelling through tunnels in the crystal. But he soon realized that the wave explanation had to be accepted.

1985 ◽  
Vol 38 (3) ◽  
pp. 263 ◽  
Author(s):  
CA Beevers ◽  
H Lipson

Fourier methods for the determination of crystal structures were first suggested by Bragg in 1929, and were then successfully used by Beevers and Lipson for determining the structure of CuS04.5H20 in 1934. It was necessary for methods of summation to be devised, and after some experimentation the Beevers-Lipson strips became established as the best device for the work. They enabled increasingly complicated structures to be derived, but ultimately more elaborate and automatic devices based on digital computers had to be introduced. At the same time, isomorphous-replacement, heavy-atom and direct methods were also developed and these have enabled structures of enormous complexity to be successfully determined.


Author(s):  
Douglas L. Dorset ◽  
Anthony J. Hancock

Lipids containing long polymethylene chains were among the first compounds subjected to electron diffraction structure analysis. It was only recently realized, however, that various distortions of thin lipid microcrystal plates, e.g. bends, polar group and methyl end plane disorders, etc. (1-3), restrict coherent scattering to the methylene subcell alone, particularly if undistorted molecular layers have well-defined end planes. Thus, ab initio crystal structure determination on a given single uncharacterized natural lipid using electron diffraction data can only hope to identify the subcell packing and the chain axis orientation with respect to the crystal surface. In lipids based on glycerol, for example, conformations of long chains and polar groups about the C-C bonds of this moiety still would remain unknown.One possible means of surmounting this difficulty is to investigate structural analogs of the material of interest in conjunction with the natural compound itself. Suitable analogs to the glycerol lipids are compounds based on the three configurational isomers of cyclopentane-1,2,3-triol shown in Fig. 1, in which three rotameric forms of the natural glycerol derivatives are fixed by the ring structure (4-7).


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