RESUMO
New complexes of Pd(II) with N-substituted thiosemicarbazone (1)-(3) have been synthesised and characterised by elemental analyses, IR, electronic, (1)H NMR spectroscopies. The electrochemical behaviour of the complexes has been tested by using cyclic voltammetry. The crystal structures of the complexes have been determined by single crystal X-ray diffraction technique. In all the complexes the thiosemicarbazone ligand is coordinated to palladium through ONS mode. The complex 1 crystallises in the monoclinic space group P2(1)/c with two molecules per unit cell, has the dimensions of a=9.4390(19)A, b=10.645(2)A, c=13.668(3)A, alpha=90 degrees , beta=91.43 degrees and gamma=90 degrees . The complex 3 crystallises in the monoclinic space group P2(1)/c with four molecules per unit cell, has the dimensions of a=14.119(3)A, b=11.155(2)A, c=18.503(4)A, alpha=90 degrees , beta=112.02 degrees and gamma=90 degrees . The new complexes have been tested for their antibacterial activity against various pathogenic bacteria. From this study, it was found out that the activity of the complex 2 almost reaches the effectiveness of the conventional bacteriocide Streptomycin.
Assuntos
Paládio/química , Paládio/farmacologia , Tiossemicarbazonas/química , Tiossemicarbazonas/farmacologia , Antibacterianos/química , Antibacterianos/farmacologia , Cristalografia por Raios X , Eletroquímica , Espectroscopia de Ressonância Magnética , Modelos Moleculares , Estrutura Molecular , Espectrofotometria Ultravioleta , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
Mesitylcopper reacts with flavonol (flaH) in the presence of 1,3-bis(2-pyridylimino)isoindoline (indH) to yield the diamagnetic complex CuI(fla)(indH), which on reaction with molecular oxygen undergoes oxidative splitting of the C2-C3 bond of the pyranone ring of the flavonolate ligand to give CuI(indH)(O-bs) (O-bs = O-benzoylsalicylate) (orthorhombic, P1, a = 8.048(7) A, b = 8.969(9) A, c = 19.240(2) A, alpha = 85.69 degrees, beta = 80.24(7) degrees, gamma = 77.87(7) degrees, V = 1337(2) A3, Z = 2) and carbon monoxide. The reaction of [CuI(CH3CN)4]ClO4, flaH, and indH with dioxygen at room temperature affords the paramagnetic complex [CuII(fla)(indH)]ClO4 (mu = 2.10 mu B), and after elimination of HClO4, CuII(fla)(ind) (orthorhombic, Pbca, a = 8.888(2) A, b = 19.169(7) A, c = 33.614(10) A, alpha = beta = gamma = 90 degrees, V = 5727(3) A3, Z = 8) with mu = 1.86 mu B is formed. The latter undergoes cleavage of the pyranone ring on oxygenation at 80 degrees C to give CuII(ind)(O-bs) (mu = 1.87 mu B, nu(CO) = 1742 cm-1, and nu(CO2) = 1581, 1387 cm-1) and carbon monoxide. CuII(fla)(ind) and [CuII(fla)(indH)]ClO4 serve as good catalysts for the oxygenation of flavonol to O-benzoylsalicyclic acid.