The preparation and crystal structure of a dioxouranium(VI) and of an oxo-vanadium(IV) complex with a hexadentate, compartmental schiff base ligand

Abstract

The title compounds were prepared by reacting the compartmental Schiff base ligand, H 4-aapen, obtained by condensation of o-acetoacetylphenol and ethylenediamine, and oxovanadium(IV) or dioxouranium(VI) salts in alcoholic media and their crystal structures were determined by X-ray crystallography, VO(H 2-aapen), 0.5 CHCl 3, 0.5H 2O is monoclinic P2 1/ a, a = 15.04(3), b =14.37(3), c = 11.20(2) Å, and β = 96.43(3)°; D c = 1.42 g cm −3 for Z = 4. UO 2(H 2-aapen)(dmf) is monoclinic, P2 1/n, a = 22.20(3), b = 8.70(1), c = 13.86(2) Å and β = 97.90(3)°; D c = 1.80 g cm −3 for Z = 4. The oxovanadium(IV) and dioxouranium(VI) units occupy the outer (O 2O 2) compartment of the potentially binucleating ligand. Relevant distances are: VO (ligand), 1.916–1.992 Å; VO (oxovanadium), 1.585 Å; UO (ligand), 2.28–2.47 Å; UO (dmf), 2.45 Å; UO (dioxouranium), 1.66 Å (mean).