The new N5+ salt, N5+ SbF6-, was prepared from N2F+ SbF6-and HN3 in anhydrous HF solution. The white solid is surprisingly stable, decomposing only at 70° C, and is relatively insensitive to impact. Its vibrational spectrum exhibits all nine fundamentals with frequencies that are in excellent agreement with the theoretical calculations for a five-atomic V-shaped ion of C 2 v symmetry. The N5+ Sb2F11-salt was also prepared, and its crystal structure ...