Abstract A series of m, n′-diazidodiphenyl ethers (m≤ n, m= 3, 4; n= 3, 4) was photolyzed at 77 K in frozen, glassy 2-methyltetrahydrofuran matrices to generate the corresponding diphenyl ether m, n′-dinitrenes for study by electron spin resonance (ESR) spectroscopy. 3, 4′-Diazidodiphenyl ether gave an ESR spectrum dominated by a mononitrene peak with∣ D/hc∣= 0· 972 cm− 1, and also showed a weak dinitrene quintet spectrum with∣ D/hc∣= ...