Abstract

The aqueous chemistry of vanadium with physiologically relevant ligands constitutes a subject of burgeoning research, extending from bacterial metalloenzymic functions to human-health physiology. Vanadium, in the form of VCl 3 and V 2O 5, reacted expediently with citric acid, in a 1:2 molar ratio in water at pH∼4, and, in the presence of various cations, afforded crystalline materials bearing the general formula (Cat) 2[V 2O 4(C 6H 6O 7) 2]· nH 2O (A) (Cat +=Na +, NH 4 + , n=2; Me 4N +, K +, n=4). Exploration of the reactivity of A toward H 2O 2 yielded the peroxo-containing complexes (Cat) 2[V 2O 2(O 2) 2(C 6H 6O 7) 2]·2H 2O (B) (Cat +=K +, NH 4 + ). Both classes of compounds were characterized analytically and spectroscopically. The X-ray structures of complexes A and B emphasize the exceptional stability of the dimeric rhombic unit V V 2O 2, which is retained upon H 2O 2 reaction, and the preserved mode of coordination of the citrate ligand as a doubly deprotonated moiety. In these complexes, typical six and eight coordination numbers were observed for the Na + and K + counter-ions, respectively. The variety of synthetic approaches leading to A, along with the stepwise and direct assembly and isolation of peroxo-compounds (B), denotes the significance of reaction pathways and intermediates in vanadium(III–V)–citrate synthetic chemistry. Hence, a systematic investigation of reactivity modes in aqueous vanadium–citrate systems emerges as a crucial tool for the establishment of chemical interconnectivity among low MW complex species, potentially participating in the intricate biodistribution of that metal ion in biological fluids.

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