Chemical crystallography by serial femtosecond X-ray diffraction

Elyse A. Schriber, Daniel W. Paley, Robert Bolotovsky, Daniel J. Rosenberg, Raymond G. Sierra, Andrew Aquila, Derek Mendez, Frédéric Poitevin, Johannes P. Blaschke, Asmit Bhowmick, Ryan P. Kelly, Mark Hunter, Brandon Hayes, Derek C. Popple, Matthew Yeung, Carina Pareja-Rivera, Stella Lisova, Kensuke Tono, Michihiro Sugahara, Shigeki Owada, Tevye Kuykendall, Kaiyuan Yao, P. James Schuck, Diego Solis-Ibarra, Nicholas K. Sauter (), Aaron S. Brewster () and J. Nathan Hohman ()
Additional contact information
Elyse A. Schriber: University of Connecticut
Daniel W. Paley: Lawrence Berkeley National Laboratory
Robert Bolotovsky: Lawrence Berkeley National Laboratory
Daniel J. Rosenberg: Lawrence Berkeley National Laboratory
Raymond G. Sierra: SLAC National Accelerator Laboratory
Andrew Aquila: SLAC National Accelerator Laboratory
Derek Mendez: Lawrence Berkeley National Laboratory
Frédéric Poitevin: SLAC National Accelerator Laboratory
Johannes P. Blaschke: Lawrence Berkeley National Laboratory
Asmit Bhowmick: Lawrence Berkeley National Laboratory
Ryan P. Kelly: University of Connecticut
Mark Hunter: SLAC National Accelerator Laboratory
Brandon Hayes: SLAC National Accelerator Laboratory
Derek C. Popple: Lawrence Berkeley National Laboratory
Matthew Yeung: Massachusetts Institute of Technology
Carina Pareja-Rivera: Universidad Nacional Autónoma de México
Stella Lisova: Arizona State University
Kensuke Tono: Japan Synchrotron Radiation Research Institute
Michihiro Sugahara: RIKEN SPring-8 Center
Shigeki Owada: Japan Synchrotron Radiation Research Institute
Tevye Kuykendall: Lawrence Berkeley National Laboratory
Kaiyuan Yao: Columbia University
P. James Schuck: Columbia University
Diego Solis-Ibarra: Universidad Nacional Autónoma de México
Nicholas K. Sauter: Lawrence Berkeley National Laboratory
Aaron S. Brewster: Lawrence Berkeley National Laboratory
J. Nathan Hohman: University of Connecticut

Nature, 2022, vol. 601, issue 7893, 360-365

Abstract: Abstract Inorganic–organic hybrid materials represent a large share of newly reported structures, owing to their simple synthetic routes and customizable properties1. This proliferation has led to a characterization bottleneck: many hybrid materials are obligate microcrystals with low symmetry and severe radiation sensitivity, interfering with the standard techniques of single-crystal X-ray diffraction2,3 and electron microdiffraction4–11. Here we demonstrate small-molecule serial femtosecond X-ray crystallography (smSFX) for the determination of material crystal structures from microcrystals. We subjected microcrystalline suspensions to X-ray free-electron laser radiation12,13 and obtained thousands of randomly oriented diffraction patterns. We determined unit cells by aggregating spot-finding results into high-resolution powder diffractograms. After indexing the sparse serial patterns by a graph theory approach14, the resulting datasets can be solved and refined using standard tools for single-crystal diffraction data15–17. We describe the ab initio structure solutions of mithrene (AgSePh)18–20, thiorene (AgSPh) and tethrene (AgTePh), of which the latter two were previously unknown structures. In thiorene, we identify a geometric change in the silver–silver bonding network that is linked to its divergent optoelectronic properties20. We demonstrate that smSFX can be applied as a general technique for structure determination of beam-sensitive microcrystalline materials at near-ambient temperature and pressure.

Date: 2022
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DOI: 10.1038/s41586-021-04218-3

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