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

DOI: 10.1039/D2CP03928A DOI Help

Authors: Nathalie K. Fernando (University College London) , Hanna L. B. Bostroem (Max Planck Institute for Solid State Research) , Claire A. Murray (Diamond Light Source) , Robin L. Owen (Diamond Light Source) , Amber L. Thompson (University of Oxford) , Joshua L. Dickerson (University of Oxford) , Elspeth F. Garman (University of Oxford) , Andrew B. Cairns (University of Oxford) , Anna Regoutz (University College London)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Physical Chemistry Chemical Physics , VOL 84

State: Published (Approved)
Published: November 2022
Diamond Proposal Number(s): 23209

Open Access Open Access

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.

Subject Areas: Chemistry, Technique Development

Instruments: I11-High Resolution Powder Diffraction

Added On: 20/11/2022 15:56


Discipline Tags:

Physical Chemistry Technique Development - Chemistry Catalysis Chemistry Organometallic Chemistry

Technical Tags:

Diffraction X-ray Powder Diffraction