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Instruments / Technical Area	Publication Details	Published	Actions
I11-High Resolution Powder Diffraction I19-Small Molecule Single Crystal Diffraction	Structural and electronic effects of X-ray irradiation on prototypical [M(COD)Cl]2 catalysts Nathalie K. Fernando , Andrew B. Cairns , Claire A. Murray , Amber L. Thompson , Joshua L. Dickerson , Elspeth F. Garman , Nayera Ahmed , Laura E. Ratcliff , Anna Regoutz The Journal Of Physical Chemistry A DOI: 10.1021/acs.jpca.1c05759 Diamond Proposal Number(s): [19420, 22705] Show Abstract ▼ Abstract: X-ray characterization techniques are invaluable for probing material characteristics and properties, and have been instrumental in discoveries across materials research. However, there is a current lack of understanding of how X-ray-induced effects manifest in small molecular crystals. This is of particular concern as new X-ray sources with ever-increasing brilliance are developed. In this paper, systematic studies of X-ray–matter interactions are reported on two industrially important catalysts, [Ir(COD)Cl]2 and [Rh(COD)Cl]2, exposed to radiation in X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) experiments. From these complementary techniques, changes to structure, chemical environments, and electronic structure are observed as a function of X-ray exposure, allowing comparisons of stability to be made between the two catalysts. Radiation dose is estimated using recent developments to the RADDOSE-3D software for small molecules and applied to powder XRD and XPS experiments. Further insights into the electronic structure of the catalysts and changes occurring as a result of the irradiation are drawn from density functional theory (DFT). The techniques combined here offer much needed insight into the X-ray-induced effects in transition-metal catalysts and, consequently, their intrinsic stabilities. There is enormous potential to extend the application of these methods to other small molecular systems of scientific or industrial relevance.	Aug 2021
I19-Small Molecule Single Crystal Diffraction	Radiation damage in small-molecule crystallography: fact not fiction Jeppe Christensen , Peter N. Horton , Charles S. Bury , Joshua L. Dickerson , Helena Taberman , Elspeth F. Garman , Simon J. Coles Iucrj 6 DOI: 10.1107/S2052252519006948 Diamond Proposal Number(s): [15762] Open Access Show Abstract ▼ Abstract: Traditionally small-molecule crystallographers have not usually observed or recognized significant radiation damage to their samples during diffraction experiments. However, the increased flux densities provided by third-generation synchrotrons have resulted in increasing numbers of observations of this phenomenon. The diversity of types of small-molecule systems means it is not yet possible to propose a general mechanism for their radiation-induced sample decay, however characterization of the effects will permit attempts to understand and mitigate it. Here, systematic experiments are reported on the effects that sample temperature and beam attenuation have on radiation damage progression, allowing qualitative and quantitative assessment of their impact on crystals of a small-molecule test sample. To allow inter-comparison of different measurements, radiation-damage metrics (diffraction-intensity decline, resolution fall-off, scaling B-factor increase) are plotted against the absorbed dose. For ease-of-dose calculations, the software developed for protein crystallography, RADDOSE-3D, has been modified for use in small-molecule crystallography. It is intended that these initial experiments will assist in establishing protocols for small-molecule crystallographers to optimize the diffraction signal from their samples prior to the onset of the deleterious effects of radiation damage.	Jul 2019

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