Syntheses and structures of 2-acetylpyridine-(2-amino-benzoylhydrazone) and its dioxouranium(VI) complex

Abstract

A síntese e a caracterização da 2-acetilpiridina-(2-aminobenzoilhidrazona) (HL 1 ) e do seu primeiro complexo com dióxido de urânio são descritas neste trabalho. A análise estrutural da hidrazona, HL 1 , por difração de raios X do monocristal, mostra que sua estrutura molecular é quase planar no estado sólido, apresentando ligações de hidrogênio intermoleculares. O complexo [UO 2 (L 1 )(dmf) 2 ](NO 3 ) é formado a partir de uma suspensão em refluxo de HL 1 com nitrato de uranila em metanol, na presença de pequena quantidade de trietilamina. A recristalização em dmf resulta na obtenção de cristais adequados para a difração de raios X. A análise por difração de raios X do complexo mostra uma geometria de coordenação bipiramidal de base pentagonal para o urânio(VI), formada pelos oxigênios da uranila nas posições apicais, uma molécula da hidrazona monodesprotonada e dois átomos de oxigênio das moléculas de dimetilformamida nas posições equatoriais.We describe the synthesis and characterization of 2-acetylpyridine-(2-aminobenzoylhydrazone) (HL 1 ) and its first dioxouranium complex. The single crystal X-ray structural analysis of the hydrazone, HL 1 , reveals an almost planar structure with intermolecular hydrogen bonds. The complex [UO 2 (L 1 )(dmf) 2 ](NO 3 ) is formed by refluxing a suspension of HL 1 with uranyl nitrate in methanol in the presence of a small quantity of triethylamine. Recrystallisation from dmf results in single crystals suitable for X-ray crystallography. The single crystal X-ray study of the complex shows a distorted pentagonal-bipyramidal coordination geometry around the uranium(VI) center, determined by two axial oxo ligands, two nitrogen and one oxygen atoms from a chelating monodeprotonated hydrazone and the oxygen donor atoms of two dimethylformamide molecules.

Recent Developments in Synthesis and Structural Chemistry of Nonaqueous Actinide Complexes

“…Reaction of HSB 3 ( 76) with either [UO 2 (NO 3 ) 2 ]•6H 2 O or [NBu 4 ] 2 [UO 2 Cl 4 ] affords an orange precipitate, which crystallizes from hot DMF solution as [UO 2 (SB 3 )(DMF) 2 ] + (nitrate or chloride balance the charge depending on the identity of the starting material). 105 The SB 3 ligand binds to the uranyl cation through the O atom and two N donor atoms, with O atoms from two DMF solvent molecules completing the distorted pentagonal bipyramidal geometry about the uranium center.…”

“…The SB 2 ligand did not appear to coordinate to lanthanide ions, highlighting the potential application of these ligand types in nuclear fuel cycle separation chemistry. Reaction of HSB 3 ( 76 ) with either [UO 2 (NO 3 ) 2 ]·6H 2 O or [NBu 4 ] 2 [UO 2 Cl 4 ] affords an orange precipitate, which crystallizes from hot DMF solution as [UO 2 (SB 3 )(DMF) 2 ] + (nitrate or chloride balance the charge depending on the identity of the starting material) …”

Oxidovanadium(v) complexes of aroylhydrazones incorporating heterocycles: synthesis, characterization and study of DNA binding, photo-induced DNA cleavage and cytotoxic activities

“…74 The analogous ligand where the phenyl group has been substituted for a methyl group has been characterized in two crystal structures, i.e. mononuclear cobalt 75 and uranium 76 complexes, each with a nearly planar conformation of the tridentate ligand.…”

Electrochemical Detection of Chloride Ions by Copper (II) Complex with Mixed Ligand of Oxindole Derivative and Dithiocarbamates Moiety

“…Upon increasing the alkyl chain of the corresponding alcohols (ethanol to butanol), the slight blue shift in the peaks (211 and 207, respectively) and red shift in the peaks (295 and 298, respectively) were observed. However, the electronic spectra in isopropanol solution shows a peak at 209 nm and a distinct sharp peak at 297 nm [33].…”