Characterization of reactive organometallic species via MicroED

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 ultra-sensitive 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 or diamagnetic transition metal complexes.

Sterically Invariant Carborane-Based Ligands for the Morphological and Electronic Control of Metal–Organic Chalcogenolate Assemblies

“…This work therefore further establishes the utility of MicroED for hybrid material structure elucidation when reaching the limitations of more traditional structural determination methods. [81][82][83][84] This study furthermore highlights how the use of bulky, organomimetic, boron cluster ligands can lead to the formation of hybrid materials with unique structures and properties. 35-57, 59-65, 85-100 ASSOCIATED CONTENT Crystallographic data are available from the Cambridge Crystallographic Data Centre, under the reference number: CCDC 2121247 (A)…”