A novel two-step route for the synthesis of RhFe3N is presented that yields the target material with a significantly improved phase purity. Except from Fe0.5Rh0.5, the absence of other side products is exemplified on the basis of powder XRD, REM/EDX measurements, and Mo¨ssbauer investigations. As predicted from density-functional theory calculations, both Rietveld refinement and Mo¨ssbauer…