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Watching Photochemistry Happen: Recent Developments in Dynamic Single-Crystal X-Ray Diffraction Studies

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21st Century Challenges in Chemical Crystallography I

Part of the book series: Structure and Bonding ((STRUCTURE,volume 185))

Abstract

Photoresponsive materials are an important contemporary research area with applications in, for example, energy and catalysis. Mechanistic information on solid-state photochemical reactions has traditionally come from spectroscopy and modelling, with crystallography limited to snapshots of endpoints and long-lived intermediates. Recent advances in X-ray sources and detectors have made it possible to follow solid-state reactions in situ with dynamic single-crystal X-ray diffraction (SCXRD) methods, allowing a full set of atomic positions to be determined over the course of the reaction. These experiments provide valuable structural information that can be used to interpret spectroscopic measurements and to inform materials design and optimisation.

Solid-state linkage isomers, where small-molecule ligands such as NO, NO2−, N2 and SO2 show photo-induced changes in binding to a transition metal centre, have played a leading role in the development of dynamic SCXRD methodology, since the movement of whole atoms and the predictable temperature dependence of the excited-state lifetimes make them ideal test systems. The field of “photocrystallography”, pioneered by Coppens in the late 1990s, has developed alongside advances in instrumentation and computing and can now provide the 3D structures of species with lifetimes down to femtoseconds.

In this chapter, we will review the development of photocrystallography experiments against linkage isomer systems, from the early identification of metastable species under continuous illumination, through measuring kinetics at low temperature, to recent experiments studying species with sub-second lifetimes. We will discuss the advances in X-ray sources and instrumentation that have made dynamic SCXRD experiments possible, and we will highlight the role of kinetic modelling and complementary spectroscopy in designing experiments. Finally, we will discuss possible directions for future development and identify some of the outstanding challenges that remain to be addressed.

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Abbreviations

2D:

Two-dimensional

3D:

Three-dimensional

bipy:

2,2′-Bipyridine

BPh4:

Tetraphenylborate

Bu4dien:

N,N,N′,N′-Tetrabutyldiethylenetriamine

CCD:

Charge-coupled device

CMOS:

Complementary metal-oxide-semiconductor

dcpe :

1,2-Bis(dicyclohexylphosphino)ethane

dppe :

1,2-Bis(diphenylphosphino)ethane

ES:

Excited state

Et4dien:

N,N,N′,N′-Tetraethyldiethylenetriamine

GS :

Ground state

JMAK:

Johnson-Mehl-Avrami-Kolmogorov

LED :

Light-emitting diode

MS1:

Metastable state 1

MS2 :

Metastable state 2

MX:

Macromolecular crystallography

OTf:

Trifluoromethanesulfonate

SCXRD :

Single-crystal X-ray diffraction

SFX:

Serial femtosecond crystallography

SNP :

Sodium nitroprusside

TR :

Time resolved

XFEL:

X-ray free-electron laser

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Author information

Authors and Affiliations

  1. School of Chemistry, Cardiff University, Cardiff, UK

    Lauren E. Hatcher

  2. Diamond Light Source Ltd., Diamond House, Harwell Science and Innovation Campus, Didcot, UK

    Mark R. Warren & Lucy K. Saunders

  3. School of Chemical and Process Engineering, University of Leeds, Leeds, UK

    Anuradha R. Pallipurath

  4. Department of Chemistry, University of Manchester, Manchester, UK

    Jonathan M. Skelton

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  1. Lauren E. Hatcher
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  2. Mark R. Warren
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  4. Lucy K. Saunders
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  5. Jonathan M. Skelton
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Correspondence to Jonathan M. Skelton .

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Editors and Affiliations

  1. Inorganic Chemistry Laboratory, University of Oxford, Oxford, UK

    D. Michael P. Mingos

  2. Department of Chemistry, University of Bath, Bath, UK

    Paul R. Raithby

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Hatcher, L.E., Warren, M.R., Pallipurath, A.R., Saunders, L.K., Skelton, J.M. (2020). Watching Photochemistry Happen: Recent Developments in Dynamic Single-Crystal X-Ray Diffraction Studies. In: Mingos, D.M.P., Raithby, P.R. (eds) 21st Century Challenges in Chemical Crystallography I. Structure and Bonding, vol 185. Springer, Cham. https://doi.org/10.1007/430_2020_78

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