Facile Synthesis of a 20‐Membered Macrocyclic Magnesium Sulfide Complex

Abstract

Deprotonation of 2,3‐pyrazyl‐linked bis(thiophosphorano)methane {CH2(iPr2P=S)}2(C4H2N2‐2,3) (2) with one equivalent of nBu2Mg in THF afforded a 20‐membered macrocyclic magnesium complex [Mg{CH(iPr2P–S)}2(C4H2N2‐2,3)]4 (4a). The structure of 4a has been characterized by X‐ray crystallography and NMR spectroscopy.

Recent Developments in the Preparation and Chemistry of Metallacycles and Metallacages via Coordination

“…132 A magnesium-based metallocrown, unique in its use of a main-group element, was reported by Leung and co-workers wherein four Mg(II) ions were joined by a 2,3-pyrazyl-linked bis(thiophosphorano)methane ligand (Figure 30). 133 The neutral ligand was deprotonated with n-Bu 2 Mg, resulting in metallacycle formation with each Mg(II) node bound by two sulfur atoms and two N atoms of the pyrazyl rings. The structure, confirmed by X-ray crystallography, was reportedly preserved in solution on the basis of 31 P NMR analysis.…”