Cargando…

Variability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters†

X-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...

Descripción completa

Detalles Bibliográficos
Autores principales: Fernando, Nathalie K., Bostrom, Hanna L. B., Murray, Claire A., Owen, Robin L., Thompson, Amber L., Dickerson, Joshua L., Garman, Elspeth F., Cairns, Andrew B., Regoutz, Anna
Formato: Online Artículo Texto
Lenguaje:English
Publicado: 2022
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7614095/
https://www.ncbi.nlm.nih.gov/pubmed/36399064
http://dx.doi.org/10.1039/d2cp03928a
_version_ 1783605564068069376
author Fernando, Nathalie K.
Bostrom, Hanna L. B.
Murray, Claire A.
Owen, Robin L.
Thompson, Amber L.
Dickerson, Joshua L.
Garman, Elspeth F.
Cairns, Andrew B.
Regoutz, Anna
author_facet Fernando, Nathalie K.
Bostrom, Hanna L. B.
Murray, Claire A.
Owen, Robin L.
Thompson, Amber L.
Dickerson, Joshua L.
Garman, Elspeth F.
Cairns, Andrew B.
Regoutz, Anna
author_sort Fernando, Nathalie K.
collection PubMed
description X-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.
format Online
Article
Text
id pubmed-7614095
institution National Center for Biotechnology Information
language English
publishDate 2022
record_format MEDLINE/PubMed
spelling pubmed-76140952023-01-23 Variability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters† Fernando, Nathalie K. Bostrom, Hanna L. B. Murray, Claire A. Owen, Robin L. Thompson, Amber L. Dickerson, Joshua L. Garman, Elspeth F. Cairns, Andrew B. Regoutz, Anna Phys Chem Chem Phys Article X-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. 2022-11-30 2022-11-30 /pmc/articles/PMC7614095/ /pubmed/36399064 http://dx.doi.org/10.1039/d2cp03928a Text en https://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. https://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/) .
spellingShingle Article
Fernando, Nathalie K.
Bostrom, Hanna L. B.
Murray, Claire A.
Owen, Robin L.
Thompson, Amber L.
Dickerson, Joshua L.
Garman, Elspeth F.
Cairns, Andrew B.
Regoutz, Anna
Variability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters†
title Variability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters†
title_full Variability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters†
title_fullStr Variability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters†
title_full_unstemmed Variability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters†
title_short Variability in X-ray induced effects in [Rh(COD)Cl](2) with changing experimental parameters†
title_sort variability in x-ray induced effects in [rh(cod)cl](2) with changing experimental parameters†
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7614095/
https://www.ncbi.nlm.nih.gov/pubmed/36399064
http://dx.doi.org/10.1039/d2cp03928a
work_keys_str_mv AT fernandonathaliek variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters
AT bostromhannalb variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters
AT murrayclairea variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters
AT owenrobinl variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters
AT thompsonamberl variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters
AT dickersonjoshual variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters
AT garmanelspethf variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters
AT cairnsandrewb variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters
AT regoutzanna variabilityinxrayinducedeffectsinrhcodcl2withchangingexperimentalparameters