Characterization of Reactive Organometallic Species via MicroED

Christopher G Jones; Matthew Asay; Lee Joon Kim; Jack F Kleinsasser; Ambarneil Saha; Tyler J Fulton; Kevin R Berkley; Duilio Cascio; Andrey G Malyutin; Matthew P Conley; Brian M Stoltz; Vincent Lavallo; José A Rodríguez; Hosea M Nelson

doi:10.1021/acscentsci.9b00403

Characterization of Reactive Organometallic Species via MicroED

ACS Cent Sci. 2019 Sep 25;5(9):1507-1513. doi: 10.1021/acscentsci.9b00403. Epub 2019 Sep 6.

Authors

Christopher G Jones¹, Matthew Asay¹, Lee Joon Kim¹, Jack F Kleinsasser², Ambarneil Saha^{1

1}, Tyler J Fulton³, Kevin R Berkley², Duilio Cascio^{1

1}, Andrey G Malyutin³, Matthew P Conley², Brian M Stoltz³, Vincent Lavallo², José A Rodríguez^{1

1}, Hosea M Nelson¹

Affiliations

¹ Department of Chemistry and Biochemistry and UCLA-DOE Institute for Genomics & Proteomics, University of California, Los Angeles, California 90095, United States.
² Department of Chemistry, University of California, Riverside, California 92521, United States.
³ The Warren and Katharine Schlinger Laboratory for Chemistry and Chemical Engineering, Division of Chemistry and Chemical Engineering and Beckman Institute, California Institute of Technology, Pasadena, California 91125, United States.

Abstract

Here we apply microcrystal electron diffraction (MicroED) to the structural determination of transition-metal complexes. We find that the simultaneous use of 300 keV electrons, very low electron doses, and an ultrasensitive camera allows for the collection of data without cryogenic cooling of the stage. This technique reveals the first crystal structures of the classic zirconocene hydride, colloquially known as "Schwartz's reagent", a novel Pd(II) complex not amenable to solution-state NMR or X-ray crystallography, and five other paramagnetic and diamagnetic transition-metal complexes.

Grants and funding

R35 GM128867/GM/NIGMS NIH HHS/United States