000 02887 am a22003133u 4500
042 _adc
100 1 0 _aFernando, Nathalie K.
_eauthor
_92452
700 1 0 _aBostrom, Hanna L. B.
_eauthor
_92453
700 1 0 _aMurray, Claire A.
_eauthor
_92454
700 1 0 _aOwen, Robin L.
_eauthor
_92455
700 1 0 _aThompson, Amber L.
_eauthor
_92456
700 1 0 _aDickerson, Joshua L.
_eauthor
_92457
700 1 0 _aGarman, Elspeth F.
_eauthor
_92458
700 1 0 _aCairns, Andrew B.
_eauthor
_92459
700 1 0 _aRegoutz, Anna
_eauthor
_92460
245 0 0 _aVariability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters†
260 _c2022-11-30.
500 _a/pmc/articles/PMC7614095/
500 _a/pubmed/36399064
520 _aX-ray characterisation methods have undoubtedly enabled cutting-edge advances in all aspects of materials research. Despite the enormous breadth of information that can be extracted from these techniques, the challenge of radiation-induced sample change and damage remains prevalent. This is largely due to the emergence of modern, high-intensity X-ray source technologies and the growing potential to carry out more complex, longer duration in situ or in operando studies. The tunability of synchrotron beamlines enables the routine application of photon energy-dependent experiments. This work explores the structural stability of [Rh(COD)Cl](2), a widely used catalyst and precursor in the chemical industry, across a range of beamline parameters that target X-ray energies of 8 keV, 15 keV, 18 keV and 25 keV, on a powder X-ray diffraction synchrotron beamline at room temperature. Structural changes are discussed with respect to absorbed X-ray dose at each experimental setting associated with the respective photon energy. In addition, the X-ray radiation hardness of the catalyst is discussed, by utilising the diffraction data collected at the different energies to determine a dose limit, which is often considered in protein crystallography and typically overlooked in small molecule crystallography. This work not only gives fundamental insight into how damage manifests in this organometallic catalyst, but will encourage careful consideration of experimental X-ray parameters before conducting diffraction on similar radiation-sensitive organometallic materials.
540 _a
540 _ahttps://creativecommons.org/licenses/by/4.0/This work is licensed under a CC BY 4.0 (https://creativecommons.org/licenses/by/4.0/) International license.
540 _ahttps://creativecommons.org/licenses/by/3.0/This article is licensed under a Creative Commons Attribution 3.0 Unported Licence (https://creativecommons.org/licenses/by/3.0/) .
546 _aen
690 _aArticle
655 7 _aText
_2local
786 0 _nPhys Chem Chem Phys
856 4 1 _uhttp://dx.doi.org/10.1039/d2cp03928a
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999 _c918
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