Abstract
Ab-initio structure analysis by electron diffraction is hampered by two major problems: insufficient number of reflections sampled and an intensity alteration by dynamical scattering contribution or beam damage. Thus, in recent years the principles of automated diffraction tomography (ADT) allowing systematic reciprocal space sampling and automated data analysis were developed. Here the basic ideas of ADT and its general applicability will be discussed along with some examples of solved structures.
Keywords
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.
This is a preview of subscription content, log in via an institution.
Buying options
Tax calculation will be finalised at checkout
Purchases are for personal use only
Learn about institutional subscriptionsReferences
Vainshtein BK (1964) Structure analysis by electron diffraction. Pergamon Press, New York
Kolb U, Gorelik T, Kübel C, Otten MT, Hubert D (2007) Towards automated diffraction tomography: part I – data acquisition. Ultramicroscopy 107:507–513. doi:10.1016/j.ultramic.2006.10.007
Peng LM, Dudarev SL, Whelan MJ (2004) High-energy electron diffraction and microscopy. Oxford University Press, New York
Fultz B, Howe JM (2008) Transmission electron microscopy and diffractometry of materials. Springer, Berlin
Van Dyck D, Coene W (1984) The real space method for dynamical electron diffraction calculations in high resolution electron microscopy: I. Principles of the method. Ultramicroscopy 15:29–40. doi:10.1016/0304-3991(84)90072-X
Tanaka M, Terauchi M, Kaneyama T, Tsuda M, Saitoh K (1985) Convergent beam electron diffraction, vol I–IV. JEOL, Tokyo
Sung CM, Williams DB (1991) A bibliography of CBED papers from 1939–1990. J Electron Micro Tech 17:95–118
Gorelik TE, Stewart AA, Kolb U (2011) Structure solution with automated electron diffraction tomography data: different instrumental approaches. J Microsc 244:325–331
Palatinus L, Klementová M, Dřínek V, Jarošová M, Petříček V (2011) An incommensurately modulated structure of η’-phase of Cu3+xSi determined by quantitative electron diffraction tomography. Inorg Chem 50:3743–3751
Dorset DL (1995) Structural electron crystallography. Plenum Press, New York
Williams DB, Carter CB (1996) Transmission electron microscopy, vol II. Plenum Press, New York
Vincent R, Midgley PA (1994) Double conical beam-rocking system for measurement of integrated electron diffraction intensities. Ultramicroscopy 53:271–282
Arndt UW, Champness JN, Phizackerley RP, Wonacott AJ (1973) A single-crystal oscillation camera for large unit cells. J Appl Crystallogr 6:457–463
Monaco HL (1994) Experimental methods in X-ray crystallography. In: Giacovazzo C (ed) Fundamentals of crystallography. Oxford University Press, New York, pp 229–318
Kolb U, Gorelik T, Otten MT (2008) Towards automated diffraction tomography. Part II – cell parameter determination. Ultramicroscopy 108:763–772
Hauptman H, Karle J (1953) The solution of the phase problem, I. The centrosymmetric crystal. Polycrystal Book Service, Pittsburgh
Wilson JAC (1949) The probability distribution of X-ray intensities. Acta Crystallogr 2:318–321
Giacovazzo C (1980) Direct methods in crystallography. Academic, London
Dorset DL, Gilmore CJ (2000) Prospects for kinematical least-squares refinement in polymer electron crystallography. Acta Crystallogr A 56:62–67
Burla MC, Caliandro R, Camalli M, Carrozzini B, Cascarano GL, De Caro L, Giacovazzo C, Polidori G, Siliqi D, Spagna R (2007) IL MILIONE: a suite of computer programs for crystal structure solution of proteins. J Appl Crystallogr 40:609–613
Sheldrick GM (2008) A short history of SHELX. Acta Crystallogr A 64:112–122
Gilmore GJ (1996) Maximum entropy and Bayesian statistics in crystallography: a review of practical applications. Acta Crystallogr A 52:561–589
Gilmore CJ, Bricogne G (1997) The mice computer program. Methods Enzymol 277:65–78
Palatinus L, Chapuis G (2007) Superflip – a computer program for the solution of crystal structures by charge flipping in arbitrary dimensions. J Appl Crystallogr 40:786–790
Brandenburg K, Putz H (2009) Endeavour – structure solution from powder diffraction. http://www.crystalimpact.com/endeavour/Default.htm
Coelho A (2007) TOPAS-academic V4.1, Brisbane. http://www.topas-academic.net
Favre-Nicolin V, Černý R (2002) FOX, ‘free objects for crystallography’: a modular approach to ab initio structure determination from powder diffraction. J Appl Crystallogr 35:734–743
Favre-Nicolin V (2008) Fox, free objects for crystallography. http://objcryst.sourceforge.net
David WIF, Shankland K, Van De Streek J, Pidcock E, Motherwell WDS, Cole JC (2002) DASH: a program for crystal structure determination from powder diffraction data. J Appl Crystallogr 39:910–915
Birkel CS, Mugnaioli E, Gorelik T, Kolb U, Panthöfer M, Tremel W (2010) Solution synthesis of a new thermoelectric Zn1+x Sb nanophase and its structure determination using automated electron diffraction tomography. J Am Chem Soc 132:9881–9889
Kolb U, Gorelik T, Mugnaioli E (2009) Automated diffraction tomography combined with electron precession: a new tool for ab initio nanostructure analysis. In: Moeck P, Hovmoeller S, Nicolopoulos S, Rouvimov S, Petrok V, Gateshki M, Fraundorf P (eds) Electron crystallography for materials research and quantitative characterization of nanostructured materials, Materials Research Society Symposia Proceedings, vol 1184, Warrendale, PA, GG01-05
Mugnaioli E, Gorelik T, Kolb U (2009) “Ab initio” structure solution from electron diffraction data obtained by a combination of automated diffraction tomography and precession technique. Ultramicroscopy 109:758–765
Mugnaioli E, Kolb U (2012) Applications of automated diffraction tomography (ADT) on nanocrystalline porous materials. Micropor Mesopor Mater (in press), doi:10.1016/j.micromeso.2012.02.024
Gemmi M, Fischer J, Merlini M, Poli S, Fumagalli P, Mugnaioli E, Kolb U (2011) A new hydrous Al-bearing pyroxene as a water carrier in subduction zones. Earth Planet Sci Lett 310:422–428
Mugnaioli E, Gorelik TE, Stewart A, Kolb U (2011) “Ab-initio” structure solution of nano-crystalline minerals and synthetic materials by automated electron tomography. In: Krivovichev SV (ed) Minerals as advanced materials II. Springer, Berlin/Heidelberg, pp 41–54
Kolb U, Mugnaioli E, Gorelik TE (2011) Automated electron diffraction tomography – a new tool for nano crystal structure analysis. Cryst Res Technol 6:542–554
Mugnaioli E, Sedlmaier SJ, Oekler O, Kolb U, Schnick W (2012) Ba6P12N17O9Br3 – a column-type phosphate structure solved from single-nanocrystal data obtained by automated electron diffraction tomography. Eur J Inorg Chem 2012:121–125
Andrusenko I, Mugnaioli E, Gorelik TE, Koll D, Panthöfer M, Tremel W, Kolb U (2011) Structure analysis of titanate nanorods by automated electron diffraction tomography. Acta Crystallogr B 67:218–225
Sedlmaier SJ, Mugnaioli E, Oekler O, Kolb U, Schnick W (2011) SrP3N5O: a highly condensed layer phosphate structure solved from a nanocrystal by automated electron diffraction tomography. Chem Eur J 17:11258–11265
Jiang J, Jorda JL, Yu J, Baumes LA, Mugnaioli E, Diaz-Cabanas MJ, Kolb U, Corma A (2011) Synthesis and structure determination of the hierarchical meso-microporous zeolite ITQ-43. Science 333:1131–1134
Rozhdestvenskaya I, Mugnaioli E, Czank M, Depmeier W, Kolb U, Merlino S (2011) Essential features of the polytypic charoite-96 structure compared to charoite-90. Mineral Mag 75:2833–2846
Rozhdestvenskaya I, Mugnaioli E, Czank M, Depmeier W, Kolb U, Reinholdt A, Weirich T (2010) The structure of charoite, (K,Sr,Ba,Mn)15–16(Ca,Na)32[(Si70(O,OH)180)] (OH,F)4.0*nH2O, solved by conventional and automated electron diffraction. Mineral Mag 74:159–177
Kolb U, Gorelik TE, Mugnaioli E, Stewart A (2010) Structural characterization of organics using manual and automated electron diffraction. Polym Rev 50:385–409
Gorelik TE, van de Streek J, Kilbinger AFM, Brunklaus G, Kolb U (2012) Ab-initio crystal structure analysis and refinement approaches of oligo p-benzamides based on electron diffraction data. Acta Crystallogr B 68:171–181
Denysenko D, Grzywa M, Tonigold M, Schmitz B, Krkljus I, Hirscher M, Mugnaioli E, Kolb U, Hanss J, Volkmer D (2011) Elucidating gating effects for hydrogen sorption in MHU-4 type triazolate-based MOFs featuring different pore sizes. Chem Eur J 17:1837–1848
Bellussi G, Montanari E, Di Paola E, Millini R, Carati A, Rizzo C, O’Neil Parker WJ, Gemmi M, Mugnaioli E, Kolb U, Zanardi S (2012) ECS-3: a crystalline hybrid organic–inorganic aluminosilicate with open porosity. Angew Chem 51:666–669
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2012 Springer Science+Business Media Dordrecht
About this paper
Cite this paper
Kolb, U. (2012). Automated Electron Diffraction Tomography. In: Kolb, U., Shankland, K., Meshi, L., Avilov, A., David, W. (eds) Uniting Electron Crystallography and Powder Diffraction. NATO Science for Peace and Security Series B: Physics and Biophysics. Springer, Dordrecht. https://doi.org/10.1007/978-94-007-5580-2_29
Download citation
DOI: https://doi.org/10.1007/978-94-007-5580-2_29
Published:
Publisher Name: Springer, Dordrecht
Print ISBN: 978-94-007-5579-6
Online ISBN: 978-94-007-5580-2
eBook Packages: Physics and AstronomyPhysics and Astronomy (R0)