A Trinuclear Niobium Cluster with Six Bridging Sulfates and Metal to Metal Bond Order of ⅔

Avi Bino*

*Corresponding author for this work

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26 Scopus citations

Abstract

Upon addition of K2SO4 to the red-brown solution produced by the electrochemical reduction of Nb(V) in 70% H2SO4, a red-brown, crystalline product is precipitated. X-ray crystallographic study has defined this substance as K4(H5O2)-[Nb3O2(SO4)6(H2O)3]-5H2O. It crystallizes in the monoclinic space group P21 with the cell dimensions a = 9.961 (2) Å,b= 18.088 (3) Å c = 10.036 (2) Å, β = 118.84 (2)°, V= 1584 (1) Å3, and Z = 2. The structure was refined by full-matrtix least-squares methods to residuals of R1 = 0.037 and R2 = 0.044. It consists of a discrete trinuclear, triangular niobium cluster of the type M3X17 that has been found in metal clusters of group 6 elements. The three niobium atoms in the [Nb3O2(SO4)6(H2O)3]5- ion are triply bridged by two μ3-O atoms, above and below the triangle plane, and each pair of Nb atoms is bridged by two μ-S042- groups. The trimer possesses a near D3h symmetry. The mean Nb-Nb distance is 2.885 (7) Å, and the average oxidation state of the Nb atom is +3⅔. Four electrons occupy M-M bonding orbitals, resulting in a bond order of ⅔.

Original languageEnglish
Pages (from-to)1917-1920
Number of pages4
JournalInorganic Chemistry
Volume21
Issue number5
DOIs
StatePublished - 1982

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