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Crystal Structure AnalysisPrinciples and Practice$
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William Clegg, Alexander J Blake, Jacqueline M Cole, John S O Evans, Peter Main, Simon Parsons, and David J Watkin

Print publication date: 2009

Print ISBN-13: 9780199219469

Published to Oxford Scholarship Online: September 2009

DOI: 10.1093/acprof:oso/9780199219469.001.0001

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Crystal growth and evaluation

Crystal growth and evaluation

(p.27) 3 Crystal growth and evaluation
Crystal Structure Analysis

Alexander Blake

Oxford University Press

This chapter describes techniques for obtaining and handling single crystals suitable for X-ray diffraction, including solvent evaporation, cooling, liquid and vapour diffusion methods, slow reaction techniques, and sublimation. Crystal quality can depend critically on factors such as counterions, substituents, and solvent molecules incorporated in the crystal structure. Crystal quality can be conveniently assessed with a polarizing microscope, though the ultimate test is the appearance of the X-ray diffraction pattern. For diffraction measurements, a secure crystal mounting can use glass fibres, capillaries, and specialized mounts, with a variety of adhesives including vitrified oils if low-temperature facilities are employed, and incorporates alignment tools to keep the crystal in the X-ray beam during rotation and exposure. Air-sensitive and low-melting crystals need special handling techniques.

Keywords:   crystal growth, cooling, evaporation, diffusion, polarizing microscope, crystal quality, crystal mounting, crystal handling

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