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Application of δ recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes

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δ Recycling is a simple procedure for directly extracting phase information from Patterson‐type functions [Rius (2012). Acta Cryst. A68, 399–400]. This new phasing method has a clear theoretical basis and was developed with ideal single‐crystal X‐ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507–513]. When combined with precession electron diffraction, it delivers quasi‐kinematical intensity data even for complex inorganic compounds, so that single‐crystal diffraction data of nanometric volumes are now available for structure determination by direct methods. To check the tolerance of δ recycling to missing data‐collection corrections and to deviations from kinematical behaviour of ADT intensities, δ recycling has been applied to differently shaped nanocrystals of various inorganic materials. The results confirm that it can phase ADT data very efficiently. In some cases even more complete structure models than those derived from conventional direct methods and least‐squares refinement have been found. During this study it has been demonstrated that the Wilson‐plot scaling procedure is largely insensitive to sample thickness variations and missing absorption corrections affecting electron ADT intensities.
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Document Type: Research Article

Publication date: July 1, 2013

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