Oligomeric AsN particles have been synthesized as a first step towards forming polymeric (AsN)x, which is expected to be the arsenic nitride with the most important applications. The synthesis is described and the characterization of the resulting oligomers by X‐ray powder diffraction, mass spectrometry and DSC is presented which leads to the proposed structure of (AsN)12(AsCl2)6Cl6 shown in the Figure. magnified image