Back-exchange of deuterium in neutron crystallography: characterization by IR spectroscopy

Author:

Yee Ai Woon,Blakeley Matthew P.ORCID,Moulin Martine,Haertlein Michael,Mitchell Edward,Forsyth V. Trevor

Abstract

The application of IR spectroscopy to the characterization and quality control of samples used in neutron crystallography is described. While neutron crystallography is a growing field, the limited availability of neutron beamtime means that there may be a delay between crystallogenesis and data collection. Since essentially all neutron crystallographic work is carried out using D2O-based solvent buffers, a particular concern for these experiments is the possibility of H2O back-exchange across reservoir or capillary sealants. This may limit the quality of neutron scattering length density maps and of the associated analysis. Given the expense of central facility beamtime and the effort that goes into the production of suitably sized (usually perdeuterated) crystals, a systematic method of exploiting IR spectroscopy for the analysis of back-exchange phenomena in the reservoirs used for crystal growth is valuable. Examples are given in which the characterization of D2O/H2O back-exchange in transthyretin crystals is described.

Funder

Engineering and Physical Sciences Research Council

Publisher

International Union of Crystallography (IUCr)

Subject

General Biochemistry, Genetics and Molecular Biology

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