Diphenylaminodiazidophosphane (C6H5)(2)NP(N-3)(2) was synthesized from the corresponding dihalides (C6H5)(2)NPX2 (X = F, Cl) and (CH3)(3)SiN3, and was characterized by vibrational and multinuclear NMR spectroscopy. The intermediate compound (C6H5)(2)NPF(N-3) was also observed by NMR spectroscopy in solution. Some physical properties and reactions of all these compounds are discussed.