Characterization of Reactive Organometallic Species via MicroED

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.