Synthesis, characterization, and crystal and molecular structures of caesium N-(carbamoylethyl)iminodiacetatooxoperoxovanadate(V) monohydrate

Abstract

A new monoperoxo complex of vanadium(V) of composition Cs[VO(O₂)(CEIDA)]·H₂O [where H₂CEIDA is N-(carbamoylethyl)iminodiacetic acid] was prepared and characterized by IR, UV-VIS and ⁵¹V NMR spectroscopies. Thermal analysis showed that after crystal water release the anhydrous Cs[VO(O₂)(CEIDA)] is formed, which is stable over a relatively large temperature interval and can be isolated by interruption of the dynamic heating in that interval. The X-ray structure analysis of Cs[VO(O₂)(CEIDA)]·H₂O revealed a mononuclear structure of the complex anion with a typical distorted pentagonal bipyramidal arrangement around vanadium formed by two peroxo oxygens bound in an η²-fashion, two oxygens from the deprotonated carboxylic groups and a nitrogen in the equatorial plane, and an oxo ligand and an oxygen from the carbamoyl group in the apical positions. The heteroligand is thus bound as a tetradentate CEIDA(2-)-N,O,O,O ligand to form one six-membered and two glycinate rings.