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High-Pressure Single-Crystal Diffractometry with Laboratory X-Ray Sources

High-pressure structural determinations at home laboratories

  • Conference paper
High-Pressure Crystallography

Part of the book series: NATO Science Series ((NAII,volume 140))

Abstract

The invention of the diamond-anvil high-pressure cell (DAC) [ 1,2] coincided with the development of 4-circle diffractometers [3]. When the application of gaskets paved the way for the first single-crystal high-pressure studies in hydrostatic environment [4], diffractometers were still not considered indispensable for determining the crystal structures at high pressures. For example, the high-pressure crystal structure of chloroform was studied using a modified precession camera [5]. Nevertheless, soon after it was the use of 4-circle diffractometers that came to dominate the scarce high-pressure determinations. The diffractometers then were usually equipped with sealed or rotating-anode X-ray tubes and ‘single-point’ scintillator-photomultiplier detectors. Throughout the 1980’s, the first synchrotron-sources were applied for high-pressure studies, and at the synchrotrons, 2dimensional image-plate detectors started to be used for high-pressure determinations. Nowadays we are witnessing rapid development in the designs of high-pressure DAC’s and diffractometers, which are now routinely equipped with 2-dimensional CCD detectors. Thus, in this way, history has come full circle, in that researchers trained in photographic techniques have applied their experience to 2-dimensional detectors. The component parts of diffractometric equipment, which itself is constantly under development, include sophisticated detectors, X-ray sources, goniometers and their controlling software. At present it may appear that the main thrust of high-pressure research has moved to synchrotrons.

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Authors and Affiliations

  1. Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780, Poznań, Poland

    A. Katrusiak

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  1. A. Katrusiak
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Editors and Affiliations

  1. Faculty of Chemistry, Adam Mickiewicz University, Poznań, Poland

    Andrzej Katrusiak

  2. Department of Chemistry, University College London, UK

    Paul McMillan

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Katrusiak, A. (2004). High-Pressure Single-Crystal Diffractometry with Laboratory X-Ray Sources. In: Katrusiak, A., McMillan, P. (eds) High-Pressure Crystallography. NATO Science Series, vol 140. Springer, Dordrecht. https://doi.org/10.1007/978-1-4020-2102-2_4

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  • DOI: https://doi.org/10.1007/978-1-4020-2102-2_4

  • Publisher Name: Springer, Dordrecht

  • Print ISBN: 978-1-4020-1954-8

  • Online ISBN: 978-1-4020-2102-2

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