Abstract

The colourless solid NO(HSO4), known as “lead‐chamber crystals”, was investigated ever since its first preparation more than two centuries ago. Its overall ionic nature now is confirmed by X‐ray crystallography [Pna21, a = 7.3558(4), b = 6.8924(3), c = 7.7017(3) Å, Z = 4]. The next neighbours of the NO+ cations are four hydrogensulfate oxygen atoms, forming a distorted square at a distance of about 2.5 Å from the nitrogen atom. The square pattern next to the nitrogen atom is the most widespread coordination figure about an NO+ ion in a nitrosyl salt. Depending on the anion, the interaction goes along with a decrease of the N–O stretch's excitation energy.

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