Variability in X-ray induced effects in [Rh(COD)Cl]2 with changing experimental parameters
Author(s)
Type
Journal Article
Abstract
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.
Date Issued
2022-12-14
Date Acceptance
2022-11-11
Citation
Physical Chemistry Chemical Physics, 2022, 24 (46), pp.28444-28456
ISSN
1463-9076
Publisher
Royal Society of Chemistry
Start Page
28444
End Page
28456
Journal / Book Title
Physical Chemistry Chemical Physics
Volume
24
Issue
46
Copyright Statement
This journal is © the Owner Societies 2022. This article is licensed under a Creative Commons Attribution 3.0 Unported Licence.
License URL
Identifier
https://www.webofscience.com/api/gateway?GWVersion=2&SrcApp=PARTNER_APP&SrcAuth=LinksAMR&KeyUT=WOS:000886648900001&DestLinkType=FullRecord&DestApp=ALL_WOS&UsrCustomerID=a2bf6146997ec60c407a63945d4e92bb
Subjects
Chemistry
Chemistry, Physical
CRYSTALLOGRAPHY
DOSE DEPENDENCE
ENERGY
I11
Physical Sciences
Physics
Physics, Atomic, Molecular & Chemical
POWDER-DIFFRACTION
PROTEIN CRYSTALS
RADIATION-DAMAGE
REFINEMENT
Science & Technology
WAVELENGTH
Publication Status
Published
Date Publish Online
2022-11-12