LED-pump-X-ray-multiprobe crystallography for sub-second timescales

DOI: 10.1038/s42004-022-00716-1

Authors: Lauren E. Hatcher (University of Bath; Cardiff University) , Mark R. Warren (Diamond Light Source) , Jonathan M. Skelton (University of Bath; University of Manchester) , Anuradha R. Pallipurath (University of Bath; University of Leeds) , Lucy K. Saunders (Diamond Light Source) , David R. Allan (Diamond Light Source) , Paul Hathaway (Diamond Light Source) , Giulio Crevatin (Diamond Light Source) , David Omar (Diamond Light Source) , Ben. H. Williams (Diamond Light Source) , Ben A. Coulson (Cardiff University) , Chick C. Wilson (University of Bath) , Paul R. Raithby (University of Bath)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Communications Chemistry , VOL 5

State: Published (Approved)
Published: August 2022
Diamond Proposal Number(s): 17306 , 19670

Abstract: The visualization of chemical processes that occur in the solid-state is key to the design of new functional materials. One of the challenges in these studies is to monitor the processes across a range of timescales in real-time. Here, we present a pump-multiprobe single-crystal X-ray diffraction (SCXRD) technique for studying photoexcited solid-state species with millisecond-to-minute lifetimes. We excite using pulsed LEDs and synchronise to a gated X-ray detector to collect 3D structures with sub-second time resolution while maximising photo-conversion and minimising beam damage. Our implementation provides complete control of the pump-multiprobe sequencing and can access a range of timescales using the same setup. Using LEDs allows variation of the intensity and pulse width and ensures uniform illumination of the crystal, spreading the energy load in time and space. We demonstrate our method by studying the variable-temperature kinetics of photo-activated linkage isomerism in [Pd(Bu4dien)(NO2)][BPh4] single-crystals. We further show that our method extends to following indicative Bragg reflections with a continuous readout Timepix3 detector chip. Our approach is applicable to a range of physical and biological processes that occur on millisecond and slower timescales, which cannot be studied using existing techniques.

Subject Areas: Technique Development, Chemistry


Instruments: I19-Small Molecule Single Crystal Diffraction

Added On: 01/09/2022 09:35

Documents:
s42004-022-00716-1.pdf

Discipline Tags:

Technique Development - Chemistry Chemistry

Technical Tags:

Diffraction Single Crystal X-ray Diffraction (SXRD)