Investigating discontinuous X-ray irradiation as a damage mitigation strategy for [M(COD)Cl]2 catalysts
File(s)
Published version
Author(s)
Type
Journal Article
Abstract
With the advent of ever more intense and focused X-ray sources, including in laboratories, at synchrotrons, and at X-ray free electron lasers, radiation-induced sample change and damage are becoming increasingly challenging. Therefore, the exploration of possible mitigation strategies is crucial to continue to allow the collection of robust and repeatable data. One mitigation approach is the introduction of short, X-ray-free “dark” periods. However, it is unclear whether this strategy minimises damage or, in actuality, promotes it through a phenomenon called “dark progression”, i.e. the increase or progression of radiation damage that occurs after the X-ray beam is turned off. This work discusses the influence of introducing dark periods and their duration on the radiation-induced changes in two model small-molecule catalysts, [Ir(COD)Cl]2 and [Rh(COD)Cl]2, exposed to X-ray radiation in synchrotron powder diffraction (PXRD) and laboratory photoelectron spectroscopy (XPS) experiments. This provides, for the first time, insights into how damage progresses under varying radiation regimes and allows the distinction between the processes that affect the unit cell itself, the individual molecular units, and the respective atomic chemical environments. Furthermore, it provides the basis for informed decision-making in the design of future experiments where the need to minimise radiation-induced damage is crucial.
Date Issued
2025-05-14
Date Acceptance
2025-04-09
Citation
Physical Chemistry Chemical Physics, 2025, 27 (18), pp.9417-9428
ISSN
1463-9076
Publisher
Royal Society of Chemistry
Start Page
9417
End Page
9428
Journal / Book Title
Physical Chemistry Chemical Physics
Volume
27
Issue
18
Copyright Statement
This journal is © the Owner Societies 2025. This article is licensed under a Creative Commons Attribution 3.0 Unported Licence.
License URL
Identifier
10.1039/d5cp00089k
Publication Status
Published
Date Publish Online
2025-04-09