3.4,5-Triamino-1.2.4-triazolium 5-nitrotetrazolate (2) was synthesized in high yield from 3.4.5-triamino-1,2,4-triazole (guanazine) (1) and ammonium 5-nitrotetrazolate. ne new compound 2 was characterized by vibrational (IR and Raman) and multinuclear NMR spectroscopy (H-1, C-13, N-15), elemental analysis and single crystal X-ray diffraction (triclinic, P(-1), a=0.7194(5), b= 0.8215(5), c=0.8668(5) nm, alpha=75.307(5), beta-70.054(5), gamma = 68.104(5)degrees, V=0.4421(5) nm(3), Z=2, rho=1.722 g cm(-1), R-1 = 0.0519 [F > 4 sigma(F)], wR(2)(all data)= 0.1154). The N-15 NMR spec trum and X-ray crystal structure (triclinic, P-1, a-0.5578(5), b-0.6166(5), c= 0.7395(5) nm, alpha-114.485(5)degrees, beta=90.810(5)degrees, gamma = 97.846(5)degrees, V-0.2286(3) nm(3), Z = 2, rho-1.658 g cm(-1), R-1 = 0.0460 [F > 4 rho(F)], wR(2)(all data) = 0.1153) of 1 were also determined.