Synthesis and crystal structure of bis(12-crown-4)lithium bis[N,N′-bis(trimethylsilyl)benzenesulphinamidino]lithiate(1–-); the first observation of three different lithium-7 environments in high-resolution solid-state NMR spectroscopy

Abstract

[Li(12-crown-4)₂]⁺[Li({N(SiMe₃)}₂SPh)₂]^–1 is the product of the reaction of Me₃SiNSNSiMe₃ with phenyllithium using 12-crown-4 as a donor and has an ion-separated structure which is unique for alkali metal sulphinamidino derivatives; at room temperature 1 undergoes a phase transformation, and a preliminary examination of this process by high-resolution solid-state ⁷Li NMR spectroscopy shows, for the first time, the presence of three resolvable resonances.