Abstract
Solid state reduction of NbCl5, with excess NaCl, by Ga2Cl4 under lower-temperature (175°) kinetic control yields a brown powder from which the green, incomplete cubane cluster compound [Nb3(µ3-Cl)(µ-Cl)3(NCCH3)9]4+, with GaCl4 − anions, can be extracted by acetonitrile in 51 % isolated yield. This seven valence electron discrete cluster is a moderately-soluble coordination complex of the known, seven electron, extended structure (Nb3Cl8)x. The solid state structure consists of a triangular cluster with one face-capping µ3-Cl, three edge-bridging µ-Cl ligands on the opposite face, and three terminal N-bonded CH3CN ligands per Nb. The average Nb–Nb, Nb–(µ3-Cl), and Nb–(µ-Cl) distances for one of the four independent cluster cores in the unit cell are 2.811[1] A, 2.438[9] A, and 2.427[3] A, respectively, and the average Nb–(µ-Cl)–Nb angle is 70.8[1]°. These values are compared to those of other discrete triniobium clusters and triniobium chloride extended structures with the Nb3(µ3-X)(µ-X)3XnL9−n incomplete metallacubane structure.
Published Version
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