NO(HSO4), a Fairly Ionic Solid

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.