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Automated diffraction tomography combined with electron precession: a new tool for ab initio nanostructure analysis

Published online by Cambridge University Press:  31 January 2011

Ute Kolb
Affiliation:, Johannes Gutenberg-University, Instiut for Physical Chemistry, Mainz, Germany
Tatiana Gorelik
Affiliation:, Johannes Gutenberg-University, Instiut for Physical Chemistry, Mainz, Germany
Enrico Mugnaioli
Affiliation:, Johannes Gutenberg-University, Instiut for Physical Chemistry, Mainz, Germany
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Three-dimensional electron diffraction data was collected with our recently developed module for automated diffraction tomography and used to solve inorganic as well as organic crystal structures ab initio. The diffraction data, which covers nearly the full relevant reciprocal space, was collected in the standard nano electron diffraction mode as well as in combination with the precession technique and was subsequently processed with a newly developed automated diffraction analysis and processing software package. Non-precessed data turned out to be sufficient for ab initio structure solution by direct methods for simple crystal structures only, while precessed data allowed structure solution and refinement in all of the studied cases.

Research Article
Copyright © Materials Research Society 2009

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1. O'Keefe, M. A., Microscopy and Microanalysis 10 (Suppl 2), 972 (2004).CrossRefGoogle Scholar
2. Zou, X., Hovmöller, A. and Hovmöller, S., Ultramicroscopy, 98, 187 (2004); J. Jansen, D. Tang, H. W. Zandbergen and H. Schenk, Acta Cryst. A54, 91 (1998); R. Kilaas, L. D. Marks and C. S. Own Ultramicroscopy 102, 233 (2005).CrossRefGoogle Scholar
3. Kolb, U., Gorelik, T., in: Weirich, Th. et al. (Eds.), Electron Crystallography, vol. 211, Kluwer Academic Publishers, Netherlands, NATO ASI Series E: Applied Sciences, 2005, p. 421.Google Scholar
4. Vainshtein, B. K., Structure Analysis by Electron Diffraction, Plenum, 1964.Google Scholar
5. Vincent, R., Midgley, P. A., Ultramicroscopy 53, 271 (1994).; C.S.Own, System design and verification of the precession electron diffraction technique, Ph. D. Dissertation, Northwestern University Evanston Illinois, 2005 /; A. Avilov, K. Kuligin, S. Nicolopoulos, M. Nickolskiy, K. Boulahya, J. Portillo, G. Lepeshov, B. Sobolev, J. P. Collette, N. Martin, A. C. Robins, P. Fischione, Ultramicroscopy 107, 431 (2007); M. Gemmi, S. Nicolopoulos, Ultramicroscopy 107, 483 (2007).CrossRefGoogle Scholar
6. Weirich, T. E., Rameau, R., Simon, A., Hovmöller, S., Zou, X. D., Nature 382, 144146, (1996); I. G. Voigt-Martin, Z. X. Zhang, U. Kolb, C. Gilmore, Ultramicroscopy 68, 43-59 (1997); D. L. Dorset, Structural Electron Crystallography, Plenum Press, New York, 1995.CrossRefGoogle Scholar
7. Kolb, U., Gaelic, T., Keble, C., Otten, M. T. and Hubert, D., Ultramicroscopy 107, 507 (2007)CrossRefGoogle Scholar
8. Kolb, U., Gaelic, T., Otten, M. T., Ultramicroscopy 108, 763 (2008).CrossRefGoogle Scholar
9. Dιéz, D. Castano, Seybert, A., Frangakis, A. S., J. Struct. Biol. 154, 195 (2006).CrossRefGoogle Scholar
10. Maslen, E. N., Streltsov, V. A., Streltsova, N. R. and Ishizawa, N., Acta Cryst. B51, 929 (1995).CrossRefGoogle Scholar
11. Jacobsen, S. D., Smyth, J. R., Swope, J., Can Miner. 36, 1053 (1998).Google Scholar
12. Mozharivsky, Y., Pecharsky, A. O., Bud’ko, S., and Miller, G. J.: Chem. Mater. 16, 1580 (2004).CrossRefGoogle Scholar
13. Rozhdestvenskaya, I. V., Kogure, T., and Drits, V. A., Abstracts of Meeting “Crystal chemistry and X-ray diffraction of Minerals”, Miass 2007, p. 4849.Google Scholar
14. Schmidt, M. U., Brühne, S., Wolf, A. K., Rech, A., Brüning, J., Alig, E., Fink, L., Buchsbaum, Ch., Glinnemann, J., Streek, J. van de, Gozzo, F., Brunelli, M., Stowasser, F., Gorelik, T., Mugnaioli, E. and Kolb, U. Acta Cryst. B65, 189 (2009).CrossRefGoogle Scholar
15. Kolb, U. and Matveeva, G. N., Zeitschrift für Kristallographie 218(4), 259 (2003), Special issue: Electron Crystallography.Google Scholar
16. Gorelik, T., Kolb, U., Matveeva, G., Schleuß, T., Kilbinger, A. F. M., Streek, J. van de, in preparation.Google Scholar
17.Basolite A100 purchased from Sigma Aldrich 688738.Google Scholar
18. Tahir, M. N. and Tremel, W., unpublished results.Google Scholar
19.Hielscher USA, Inc., 19, Forest Rd., NJ 07456, Ringwood, USA.Google Scholar
20.MRC: basic file format of the Medical Research Council, extended with additional headers for up to 1024 images.Google Scholar
21.UCSF Chimera package from the Resource for Biocomputing, Visualization, and Informatics at the University of California, San Francisco (supported by NIH P41 RR-01081).Google Scholar
22. Pettersen, E. F., Goddard, T. D., Huang, C. C., Couch, G. S., Greenblatt, D. M., Meng, E. C., and Ferrin, T. E., J. Comput. Chem. 25, 1605 (2004).CrossRefGoogle Scholar
23. Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., L. De Caro, Giacovazzo, C., Polidori, G., Diliqi, S., Spagna, R.: J. Appl. Cryst. 40, 609 (2007).CrossRefGoogle Scholar
24. Sheldrick, G. M., Acta Crystallogr. A64, 112122 (2008).CrossRefGoogle Scholar
25. Jacobsen, S. D., Smyth, J. R. and Swope, J., Can. Miner. 36 (1998) 1053 Google Scholar
26. Mugnaioli, E., Gorelik, T., Kolb, U., Ultramicroscopy, 109, 758 (2009).CrossRefGoogle Scholar
27. Mugnaioli, E., Gorelik, T., Panthoefer, M., Schade, Ch., Tremel, W. and Kolb, U., A combination of electron diffraction tomography and precession applied to Zn1+xSb nanophases, to be publishedGoogle Scholar
28. Putz, H., Schoen, J. C., Jansen, M., J. Appl. Cryst,. 32, 864 (1999).CrossRefGoogle Scholar
29. Schmidt, M. U., Hofmann, D. W. M., Buchsbaum, Ch., and Metz, H. J., Angew. Chem. Int. Ed,. 45, 1313 (2006).CrossRefGoogle Scholar
30. Georgieva, D. and Abrahams, J.-P., Leiden University, unpublished results.Google Scholar
31. Burla, M. C., Carrozzini, B., Cascarano, G. L., Giacovazzo, C. & Polidori, G. Z. Kristallogr. 217, 629 (2002).Google Scholar
32. Wilson, A. J. C. Acta Cryst.. 3, 397 (1950).CrossRefGoogle Scholar