RESUMEN
A series of thiouracil complexes was prepared, all the prepared compounds are investigated by all possible tools. The ligand coordinates towards two central atoms as a neutral hexadentate mode. The octahedral structure was proposed with Ni(II), Pt(IV) and UO2(II) complexes. Square-pyramidal and square planar with VO(II) and Pd(II) complexes, respectively. VO(II) complex was irradiated by using Gamma radiation to through a light on the probability of geometry changes with the effect of radiation. The parameters calculated from ESR spectra before and after γ-irradiation reflect the rigidity of the complex towards the effect. Such may discuss the unaffected biological behavior before and after irradiation. XRD patterns were carried out to emphasis on the nature of the particles and the purity of products. The ligand, Pt(IV) and Pd(II) are found in nanometer range. TEM is a sensitive tool used to justify on the microstructure and surface morphology. All the investigated compounds are in nanorange. TG curves reflect a lower thermal stability of all investigated complexes due to the presence of water of crystallization. Finally, a toxic effect was observed with all investigated complexes towards Gram positive bacterium as well as a resistant behavior was observed with Gram negative bacteria.
Asunto(s)
Complejos de Coordinación/farmacología , Complejos de Coordinación/efectos de la radiación , Rayos gamma , Microscopía Electrónica de Transmisión , Pirimidinas/química , Antibacterianos/farmacología , Bacterias/efectos de los fármacos , Complejos de Coordinación/química , Espectroscopía de Resonancia por Spin del Electrón , Electrones , Iones , Ligandos , Fenómenos Magnéticos , Pruebas de Sensibilidad Microbiana , Modelos Moleculares , Espectrofotometría Infrarroja , Termogravimetría , Difracción de Rayos XRESUMEN
The ligational behavior of 2-hydroxybenzophenone and 2-hydroxy-4-methoxybenzophenone N-substituted thiosemicarbazones towards Ni(II) and Cu(II) ions has been investigated. The isolated complexes were identified by elemental analyses, molar conductance, magnetic moment, IR, UV-vis and ESR spectral studies. The IR spectra indicated that the investigated thiosemicarbazones lost the N(2) proton or the N(2) and OH protons and act as mononegative or binegative tridentate ligands. The ligands containing methoxy group facilitate the deprotonation of OH by resonance more than the SH. Most of the Ni(II) complexes measured subnormal magnetic moments due to square-planar+tetrahedral configuration and supported by the electronic spectra. The percentage of square-planar to tetrahedral was calculated and found in agreement with the ligand splitting energy (10Dq). Also, Cu(II) complexes measured subnormal values due to the interaction between copper centers; the lower the value the higher the interaction. It was found that the substitutent has a noticeable effect on the distortion of the complex. The ESR spectra of some solid Cu(II) complexes at room temperature exhibit g(parallel)>g( perpendicular)>2.0023 confirming a square-planar structure.
Asunto(s)
Benzofenonas/química , Cobre/metabolismo , Níquel/metabolismo , Tiosemicarbazonas/química , Tiosemicarbazonas/síntesis química , Cobre/química , Espectroscopía de Resonancia por Spin del Electrón , Ligandos , Sustancias Macromoleculares/síntesis química , Sustancias Macromoleculares/química , Sustancias Macromoleculares/metabolismo , Espectroscopía de Resonancia Magnética , Modelos Biológicos , Níquel/química , Espectrofotometría Infrarroja , Tiosemicarbazonas/metabolismoRESUMEN
Both osteryoung square wave voltammetry and cyclic voltammetry have been utilized to elucidate and confirm the possible complexation reaction that occur between the various cephalosporin antibiotics and either the toxic, non-essential metal ion, viz. Cd (II), or the essential but toxic (when their concentration exceeds certain level in serum) metal ions, viz. Cu (II) and Zn (II). Voltammetric measurements indicated the existence of 1:1 metal-to-ligand ratio (as in cephalexin and cephapirin complexes), 1:2 ratio (such as in cefamandole, cefuroxime and cefotaxime complexes) and 2:1 ratio in case of ceftazidime complexes. Adsorption behavior was evidenced for Cu (II)-cefuroxime or ceftazidime complexes as well as for those for Zn (II)-cephalexin or cephapirin. This phenomenon could be used for the determination of either the antibiotic or the metal ion using adsorptive stripping voltammetry. Detection limits down to 7x10(-10) M have been easily achieved.
Asunto(s)
Cefalosporinas/química , Electroquímica , Compuestos Organometálicos/química , Elementos de Transición/química , Cadmio/química , Cobre/química , Ligandos , Zinc/químicaRESUMEN
Several complexes of thiosemicarbazone derivatives with Ni(II) have been prepared. Structural investigation of the ligands and their complexes has been made based on elemental analysis, magnetic moment, spectral (UV-Vis, i.r., (1)H NMR, ms), and thermal studies. The i.r. spectra suggest the bidentate mononegative and tridentate (neutral, mono-, and binegative) behavior of the ligands. Different stereochemistries were suggested for the isolated complexes. The thermogravimetry (TG) and derivative thermogravimetry (DTG) have been used to study the thermal decomposition and kinetic parameters of some ligands and complexes using the Coats-Redfern and Horowitz-Metzger equations. The redox properties and stability of the complexes toward oxidation waves explored by cyclic voltammetry are related to the electron withdrawing or releasing ability of the substituent of thiosemicarbazone moiety. The samples displayed Ni(II)/Ni(I) couples irreversible waves associated with Ni(III)/Ni(II) process.