A Novel Niobium Cluster Aqua Ion with Capping μ₄‐Se Ligand

Abstract

The aqueous solution chemistry of niobium is underexplored, and well characterized aqua complexes are scarce. In this contribution, a new niobium aqua complex was obtained by treatment of Zn‐reduced ethanolic solution of NbCl5 with HCl in the presence of a selenide source (ZnSe). This is the first example of selenium containing aqua complex of niobium. The yellow‐green aqua complex was isolated by cation‐exchange chromatography and transformed into corresponding isothiocyanate complex by ligand exchange, which was crystallized as (PyH)4.5[H1.5Nb4SeO5(NCS)10]·0.5H2O. X‐ray structural analysis revealed a metal‐metal bonded tetranuclear {Nb4(μ4‐Se)(μ2‐O)5}4+ core with a capping μ4‐Se ligand.