Tritungsten(IV) cluster compounds with hydroxo ligands. Preparation and structure of [W3O2(O2CCH3)6(H2O)(OH)2]·16H2O and [W3O2(O2CCH3)6(H2O)(OH)2]·KBr·15H2O

Avi Bino*, Dan Gibson

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

4 Scopus citations

Abstract

The trinuclear tritungsten(IV) cluster ion, [W3O2(OAc)6(H2O)3]2+ acts as a polyprotic acid in aqueous solution. If the pH of the solution is about 6, brown yellow crystals of [W3O2(OAc)6(H2O)·(OH)2]· 16H2O, 2, are obtained. In the presence of KBr, crystals of the double salt, [W3O2(OAc)6(H2O)(OH)2]· KBr·15H2O, 3, precipitate upon evaporation of the solution. X-ray structural analyses of the two compounds revealed that compound 2 is monoclinic, space group C2/m with a = 18.845(2) Å, b = 19.001(3) Å, c = 10.862(1) Å, β = 95.60(3)°, V = 3871(1) Å3 and Z = 4. Compound 3 is monoclinic, space group P21/c with a = 10.984(1) Å, b = 18.440(2) Å c = 19.305(2) Å, β = 95.63(2)° V = 3891(1) Å3 and Z = 4. The structures were refined by a full-matrix least-squares technique, using 2996 and 3871 reflections to R values of 3.7% and 4.6% respectively. In both structures the presence of the two hydroxo ligands in the cluster causes a considerable increase in the WW bond lengths relative to the triaqua complex. In 3, the potassium cation is bonded to two hydroxo oxygen atoms from neighbouring clusters, forming infinite chains of ··O(H)W3O(H)⋯K⋯O(H)W3O(H)⋯ units in the crystal.

Original languageEnglish
Pages (from-to)155-160
Number of pages6
JournalInorganica Chimica Acta
Volume104
Issue number3
DOIs
StatePublished - 1 Nov 1985

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