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The first transition metal iodato peroxido complex, K3[V2O2(O2)4(IO3)]·H2O (I), was prepared by crystallization from the KVO3 — KIO3 — H2O2 — H2O — ethanol (HNO3) solution. The dinuclear anion is immediately decomposed in aqueous solution; the 51V NMR spectrum exhibits signals corresponding to [VO(O2)2(H2O)]−, [V2O2(OH)(O2)4]3− and H2VO4− species only. The IR and Raman spectra contain all characteristic bands of the VO(O2)2 group and the coordinated IO3− ligand. Based on the positions of bands assigned to the vibrations of the VO(O2)2 groups a pentagonal pyramidal arrangement around the vanadium atoms can be supposed. The crystal structure was solved from X-ray synchrotron powder data by direct space method and refined by energy minimization in the solid state employing a hybrid PBE0 functional. This crystal and molecular structure, has confirmed the presence of hexacoordinated vanadium atoms and revealed asymmetric dinuclear structure of the [V2O2(O2)4(IO3)]3− ion. The coordination spheres of vanadium atoms are different — the IO3− anion is coordinated only to one vanadium center. A thermal analysis of the complex confirmed the presence of water molecules in the crystal structure and revealed a considerable stability of the dehydrated complex.

open chemistry

The first transition metal iodato peroxido complex: the synthesis, vibrational spectra and crystal structure from powder diffraction data of K3[V2O2(O2)4(IO3)]·H2O