Abstract
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.
Similar content being viewed by others
References
M. A. O'Keefe, Microscopy and Microanalysis 10 (Suppl 2), 972 (2004).
X. Zou, A. Hovmöller and S. Hovmöller, 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).
U. Kolb, T. Gorelik, in: Th. Weirich {etet al}. (Eds.), Electron Crystallography, vol. 211, Kluwer Academic Publishers, Netherlands, NATO ASI Series E: Applied Sciences, 2005, p. 421.
B. K. Vainshtein, Structure Analysis by Electron Diffraction, Plenum, 1964.
R. Vincent, P. A. Midgley, 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 /http://www.numis.northwestern.edu/Research/Current/precessions; 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).
T. E. Weirich, R. Rameau, A. Simon, S. Hovmöller, X. D. Zou, Nature 382, 144–146, (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.
U. Kolb, T. Gaelic, C. Keble, M. T. Otten and D. Hubert, Ultramicroscopy 107, 507 (2007)
U. Kolb, T. Gaelic, M. T. Otten, Ultramicroscopy 108, 763 (2008).
D. Castano Dιéz, A. Seybert, A. S. Frangakis, J. Struct. Biol. 154, 195 (2006).
E. N. Maslen, V. A. Streltsov, N. R. Streltsova and N. Ishizawa, Acta Cryst. B51, 929 (1995).
S. D. Jacobsen, J. R. Smyth, J. Swope, Can Miner. 36, 1053 (1998).
Y. Mozharivsky, A. O. Pecharsky, S. Bud’ko, and G. J. Miller: Chem. Mater. 16, 1580 (2004).
I. V. Rozhdestvenskaya, T. Kogure, and V. A. Drits, Abstracts of Meeting “Crystal chemistry and X-ray diffraction of Minerals”, Miass 2007, p. 48–49.
M. U. Schmidt, S. Brühne, A. K. Wolf, A. Rech, J. Brüning, E. Alig, L. Fink, Ch. Buchsbaum, J. Glinnemann, J. van de Streek, F. Gozzo, M. Brunelli, F. Stowasser, T. Gorelik, E. Mugnaioli and U. Kolb Acta Cryst. B65, 189 (2009).
U. Kolb and G. N. Matveeva, Zeitschrift für Kristallographie 218(4), 259 (2003), Special issue: Electron Crystallography.
T. Gorelik, U. Kolb, G. Matveeva, T. Schleuß, A. F. M. Kilbinger, J. van de Streek, in preparation.
Basolite A100 purchased from Sigma Aldrich 688738.
M. N. Tahir and W. Tremel, unpublished results.
Hielscher USA, Inc., 19, Forest Rd., NJ 07456, Ringwood, USA.
MRC: basic file format of the Medical Research Council, extended with additional headers for up to 1024 images.
UCSF Chimera package from the Resource for Biocomputing, Visualization, and Informatics at the University of California, San Francisco (supported by NIH P41 RR-01081).
E. F. Pettersen, T. D. Goddard, C. C. Huang, G. S. Couch, D. M. Greenblatt, E. C. Meng, and T. E. Ferrin, J. Comput. Chem. 25, 1605 (2004).
M. C. Burla, R. Caliandro, M. Camalli, B. Carrozzini, G. L. Cascarano, L. De Caro, C. Giacovazzo, G. Polidori, S. Diliqi, R. Spagna: J. Appl. Cryst. 40, 609 (2007).
G. M. Sheldrick, Acta Crystallogr. A64, 112–122 (2008).
S. D. Jacobsen, J. R. Smyth and J. Swope, Can. Miner. 36 (1998) 1053
E. Mugnaioli, T. Gorelik, U. Kolb, Ultramicroscopy, 109, 758 (2009).
E. Mugnaioli, T. Gorelik, M. Panthoefer, Ch. Schade, W. Tremel and U. Kolb, A combination of electron diffraction tomography and precession applied to Zn1+xSb nanophases, to be published
H. Putz, J. C. Schoen, M. Jansen, J. Appl. Cryst,. 32, 864 (1999).
M. U. Schmidt, D. W. M. Hofmann, Ch. Buchsbaum, and H. J. Metz, Angew. Chem. Int. Ed,. 45, 1313 (2006).
D. Georgieva and J.-P. Abrahams, Leiden University, unpublished results.
M. C. Burla, B. Carrozzini, G. L. Cascarano, C. Giacovazzo & G. Z. Polidori Kristallogr. 217, 629 (2002).
A. J. C. Wilson Acta Cryst.. 3, 397 (1950).
Acknowledgments
This work has been supported by the Deutsche Forschungsgemeinschaft within its Sonderforschungsbereich 625.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Kolb, U., Gorelik, T. & Mugnaioli, E. Automated diffraction tomography combined with electron precession: a new tool for ab initio nanostructure analysis. MRS Online Proceedings Library 1184, 38–50 (2009). https://doi.org/10.1557/PROC-1184-GG01-05
Published:
Issue Date:
DOI: https://doi.org/10.1557/PROC-1184-GG01-05