Direct methods of crystal-structure determination

Author(s):  
Peter Main
1991 ◽  
Vol 24 (6) ◽  
pp. 1005-1008 ◽  
Author(s):  
P. G. Byrom ◽  
B. W. Lucas

In the past, crystal structure determination of solids consisting of molecules (or atom groups) whose geometry and size are known approximately has often been attempted using neutron powder diffraction profile refinement techniques, but without inclusion of this information. A method of structure solution has therefore been developed to include it. The proposed method does not require a set of structure factors and thus avoids the problems encountered in separating peaks in a powder diffraction scan. A successful test was conducted with a previously determined (yet treated as unknown) crystal structure, where direct methods had failed to solve the structure due to incorrect peak separation. Two computer programs, MODEL and PARAM, that implement the method are described.


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.


1995 ◽  
Vol 60 (8) ◽  
pp. 1333-1342 ◽  
Author(s):  
Jan Čejka ◽  
Jan Ondráček ◽  
Michal Hušák ◽  
Bohumil Kratochvíl ◽  
Alexandr Jegorov ◽  
...  

Dihydroergocristine methanesulfonate monohydrate crystallizes in orthorhorhombic space group P21212 (No. 18) with Z = 4, a = 12.736(2) Å, b = 39.089(5) Å, c = 7.130(1) Å, V = 3549.6(9) Å3. The indole moiety is nearly planar, both the ergoline ring C and the tripeptide ring F addopt an envelope E6 conformation. The ergoline ring D and the tripeptide ring E have a chair 1C4 conformation. The conformation of the ring G is between E1 and 5T1. The benzene ring H is planar. The structure was solved by direct methods and refined anisotropically to the final R value of 0.078 for 4219 statistically significant observed reflections [I o 1.96s(I)]. The absolute chirality was determined based on anomalous dispersion as: C4 (R), C8 (R), C6 (R), C17 (R), C25 (S), C24 (S), C19 (S).


1999 ◽  
Vol 32 (1) ◽  
pp. 115-119 ◽  
Author(s):  
Angela Altomare ◽  
Maria Cristina Burla ◽  
Mercedes Camalli ◽  
Giovanni Luca Cascarano ◽  
Carmelo Giacovazzo ◽  
...  

SIR97 is the integration of two programs,SIR92 andCAOS, the first devoted to the solution of crystal structures by direct methods, the second to refinementvialeast-squares–Fourier procedures. Several new features have been introduced inSIR97 with respect to the previous version,SIR92: greater automatization, increased efficiency of the direct methods section, and a powerful graphics interface. The program also provides publication tables and CIF files.


Science ◽  
1972 ◽  
Vol 176 (4037) ◽  
pp. 911-914 ◽  
Author(s):  
W. L. Duax ◽  
H. Hauptman ◽  
C. M. Weeks ◽  
D. A. Norton

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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