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1.
Artículo en Inglés | MEDLINE | ID: mdl-25989615

RESUMEN

The main target of this paper is to get an interesting data for the preparation and characterizations of metal oxide (MO) nanoparticles using H2L Schiff base complexes as precursors through the thermal decomposition procedure. Five Schiff base complexes of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) metal ions were synthesized from 2-[(2-hydroxy-naphthalen-1-ylmethylene)-amino]-benzoic acid new adduct (H2L). Theses complexes were characterized using infrared, electronic, mass and (1)H NMR spectroscopic techniques. The elemental analysis data was confirmed that the stoichiometry of (metal:H2L) is 1:1 molar ratio. The molar conductance indicates that all of complexes are non electrolytic. The general chemical formulas of these complexes is [M(L)(NH3)]·nH2O. All complexes are tetrahedral geometry. The thermal decomposition behavior of H2L hydrated and anhydrous complexes has been discussed using thermogravimetric analysis (TG/DTG) and differential thermal analyses (DTA) under nitrogen atmosphere. The crystalline phases of the reaction products were checked using X-ray diffractometer (XRD) and scanning electron microscopy (SEM).


Asunto(s)
Complejos de Coordinación/síntesis química , Complejos de Coordinación/farmacología , Bases de Schiff/síntesis química , Bases de Schiff/farmacología , Espectrometría Raman , Elementos de Transición/química , Elementos de Transición/farmacología , Complejos de Coordinación/química , Análisis Diferencial Térmico , Conductividad Eléctrica , Espectroscopía de Resonancia por Spin del Electrón , Electrones , Cinética , Ligandos , Fenómenos Magnéticos , Espectrometría de Masas , Microscopía Electrónica de Rastreo , Espectroscopía de Protones por Resonancia Magnética , Bases de Schiff/química , Espectrofotometría Infrarroja , Termodinámica , Termogravimetría , Difracción de Rayos X
2.
Artículo en Inglés | MEDLINE | ID: mdl-23036937

RESUMEN

A novel method to synthesize some mononuclear ternary palladium(II) complexes of the general formula [Pd(L(n))L] (where LH=diketone=acetylacetone, HL(n)=azorhodanine) has been synthesize. The structure of the new mononuclear ternary palladium(II) complexes was characterized using elemental analysis, spectral (electronic, infrared and (1)H &(13)C NMR) studies, magnetic susceptibility measurements and thermal studies. The IR showed that the ligands (HL(n) & LH) act as monobasic bidentate through the azodye nitrogen, oxygen keto moiety and two enolato oxygen atoms. The molar conductivities show that all the complexes are non-electrolytes. Bidentate chelating nature of ß-diketone and azorhodanine anions in the complexes was characterized by (electronic, infrared and (1)H &(13)C NMR) spectra. Square planar geometry around palladium has been assigned in all complexes. Various ligand and nephelouxetic parameter have been calculated for the complexes. The thermal decomposition for complexes was studied.


Asunto(s)
Compuestos Azo/química , Complejos de Coordinación/química , Paladio/química , Pentanonas/química , Rodanina/análogos & derivados , Compuestos Azo/síntesis química , Quelantes/síntesis química , Quelantes/química , Complejos de Coordinación/síntesis química , Ligandos , Espectroscopía de Resonancia Magnética , Pentanonas/síntesis química , Rodanina/síntesis química , Espectrofotometría Infrarroja
3.
Artículo en Inglés | MEDLINE | ID: mdl-22580139

RESUMEN

An interesting series of heterocyclic mixed ligand of oxovanadium(IV) complexes have been synthesized by the reaction of vanadium(IV) sulfate with rhodanine azo (HL(n)) in the presence of ß-diketon (LH). The elemental analysis, magnetic moments, spectral (UV-Vis, IR, (1)HNMR and ESR) with thermal studies were used to characterize the isolated complexes. The IR showed that the ligands (HL(n) and LH) act as a monobasic bidentate through the (NN), oxygen keto moiety and oxygen atom of the two enolate groups thereby forming a six-membered. The molar conductivities show that all the complexes are non-electrolytes. The ESR spectra indicate that the free electron is in d(xy) orbital. The calculated bonding parameter indicates that in-plane σ-bonding is more covalent than in-plane π-bonding. The coordination geometry around oxovanadium(IV) in all complexes is a hex-coordinated trans octahedral, with one bidentate ligand (L(n)), and one bidentate ligand (L). Electronic and magnetic data proposed the octahedral structure for all complexes under investigation. ESR spectra of VO(2+) reveal data that confirmed the proposed structure. The value of covalency factor (ß(1)(∗))(2) and orbital reduction factor K accounts for the covalent nature of the complexes. All electronic transitions were assigned. The Hammett's constant is also discussed.


Asunto(s)
Química Bioinorgánica , Química Farmacéutica , Complejos de Coordinación/química , Vanadatos/química , Conductividad Eléctrica , Espectroscopía de Resonancia por Spin del Electrón , Electrones , Cinética , Ligandos , Espectroscopía de Resonancia Magnética , Magnetismo , Rodanina/química , Espectrofotometría Infrarroja , Termogravimetría
4.
Spectrochim Acta A Mol Biomol Spectrosc ; 78(3): 1119-25, 2011 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-21227746

RESUMEN

Oxovanadium(IV) polymer complexes of formulation {[(VO)L](2)}(n) (1) and [(VO)LB](n) (2-4), where H(2)L is tridentate and dianionic ligand (allylazorhodanine) and B is planar heterocyclic and aliphatic base have been prepared and characterized by elemental analyses, IR, (1)H NMR, electronic spin resonance spectra, magnetic susceptibility measurements, molar conductance and thermal studies. The molecular structure shows the presence of a vanadyl group in six-coordinate VNO(3)/VN(3)O(3) coordination geometry. The N,N-donor heterocyclic and aliphatic bas displays a chelating mode of binding with an N-donor site trans to the vanadyl oxo-group. In all polymeric complexes (1-4) the ligand coordinates through oxygen of phenolic/enolic and azodye nitrogen. The molar conductivity data show them to be non-electrolytes. All the polymer complexes are ESR active due to the presence of an unpaired electron. The calculated bonding parameters indicate that in-plane σ bonding is more covalent than in-plane π bonding. From the electronic, magnetic and ESR spectral data suggest that all the oxovanadium(IV) polymer complexes have distorted octahedral geometry. The thermal decomposition process of the polymeric complexes involves three decomposition steps.


Asunto(s)
Quelantes/química , Polímeros/química , Vanadio/química , Espectroscopía de Resonancia por Spin del Electrón , Estructura Molecular , Análisis Espectral/métodos
5.
Artículo en Inglés | MEDLINE | ID: mdl-15036110

RESUMEN

New polymeric complexes of Cu(II), Co(II), Ni(II) and UO2(II) with 5-(2(1)-carboxyphenylazo)-8-hydroxyquinoline (LH2) have been prepared and characterized on the basis of analytical, magnetic, 1H NMR, EPR and electronic spectral studies. Tentative structures for the polymeric complexes are proposed. The important infrared (IR) bands and the main 1H NMR signals are assigned and discussed relative to the molecular structure. EPR spectrum of copper(II) complex has been studied with a view to assigning their stereochemistries. Various EPR parameters have been calculated. Each metal has six-coordinates in an octahedral environment. The ligand acts as a dibasic (bis-bidentate chelating agent coordinating through CN, N=N, COOH and OH groups by replacement of a proton from the two latter groups. Considerable interest has also been focused on the synthesis of the azo compounds and its polymeric metal complex due to its wide potential applications. The thermal decomposition behavior of the complexes is also discussed.


Asunto(s)
Compuestos Heterocíclicos/química , Nitrógeno/química , Polímeros/química , Espectroscopía de Resonancia por Spin del Electrón , Electrones , Ligandos , Espectroscopía de Resonancia Magnética , Metales , Modelos Químicos , Estructura Molecular , Protones , Espectrofotometría , Espectrofotometría Infrarroja , Estereoisomerismo , Temperatura
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