Chemical crystallography by serial femtosecond X-ray diffraction

Journal Article · Wed Jan 19 00:00:00 EST 2022 · Nature (London)

DOI:https://doi.org/10.1038/s41586-021-04218-3· OSTI ID:1862303

Schriber, Elyse A.; Paley, Daniel W.; Bolotovsky, Robert; Rosenberg, Daniel J.; Sierra, Raymond G.; Aquila, Andrew; Mendez, Derek; Poitevin, Frédéric; Blaschke, Johannes P.; Bhowmick, Asmit; Kelly, Ryan P.; Hunter, Mark; Hayes, Brandon; Popple, Derek C.; Yeung, Matthew; Pareja-Rivera, Carina; Lisova, Stella; Tono, Kensuke; Sugahara, Michihiro; Owada, Shigeki ; Kuykendall, Tevye; Yao, Kaiyuan; Schuck, P. James; Solis-Ibarra, Diego; Sauter, Nicholas K.; Brewster, Aaron S.; Hohman, J. Nathan

AbstractInorganic–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.

• Research Organization: SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States); Univ. of Connecticut, Storrs, CT (United States)
• Sponsoring Organization: USDOE Office of Science (SC), Advanced Scientific Computing Research (ASCR); USDOE Office of Science (SC), Basic Energy Sciences (BES)
• Grant/Contract Number: AC02-76SF00515; SC0022215
• OSTI ID: 1862303
• Alternate ID(s): OSTI ID: 1864674
• Journal Information: Nature (London), Journal Name: Nature (London) Journal Issue: 7893 Vol. 601; ISSN 0028-0836
• Publisher: Nature Publishing Group
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
mithrene
mocha
self-assembly
xfel
crystallography