Abstract

A novel ligand, (Z)-1,5-dimethyl-4-(2-(3-methyl-5-oxo-1-phenyl-1H-pyrazol-4(5H)-ylidene)hydrazinyl)-2-phenyl-1,2-dihydropyrazol-3-one] and its metal(II)azo complexes were synthesized and characterized using elemental analyses, proton NMR, electrospray ionization mass spectrometry, FT-IR and UVvisible absorption. Smooth thin films of the metal(II)azo complexes were prepared using spin-coating, and the absorption spectra of the films were measured. The thermal properties of the metal()azo complexes were investigated using TGA and DSC. The optical constants (complex refractive index N = n + ik) of the films on single-crystal silicon were determined using variable-angle scanning ellipsometry from which the complex dielectric function () and absorption coefficient () were calculated. The photostabilities of the metal(II)azo complex films were also investigated.

Article Outline

o o o

1. Introduction 2. Experimental

2.1. Materials 2.2. Synthesis of the ligand (HL) and its metal()azo complexes

2.2.1. Diazotization 2.2.2. Coupling 2.2.3. Metallization

o o o o o o o o

2.2.3.1. NiL2 complex 2.2.3.2. CoL2 complex 2.2.3.3. CuL2 complex 2.2.3.4. ZnL2 complex 2.3. Preparation of the spin-coated thin films 2.4. Instrument and methods

3. Results and discussion

3.1. Synthesis and characterization 3.2. FT-IR spectra of the ligand and its metal()azo complexes 3.3. UVvis electronic absorption spectra of the ligand and its metal(II)azo complexes 3.4. Thermal properties of the metal(II)azo complexes 3.5. The optical properties of the metal(II)azo complex films 3.6. The photostabilities of the metal(II)azo complex films 4. Conclusions Acknowledgements References

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Synthesis, characterization and thermal studies on metal complexes of new azo compounds derived from sulfa drugs Original Research Article Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, Volume 68, Issue 5, 31 December 2007, Pages 1382-1387 Gehad G. Mohamed, Mohamed A.M. Gad-Elkareem

abstract
Four new azo ligands, L1 and HL24, of sulfa drugs have been prepared and characterized. [MX2(L1)(H2O)m]nH2O; [(MX2)2(HL2 or HL3)(H2O)m]nH2O and [M2X3(L4)(H2O)]nH2O; M = Co(II), Ni(II) and Cu(II) (X = Cl) and Zn(II) (X = AcO); m = 04 and n = 03, complexes were prepared. Elemental and thermal analyses (TGA and DTA), IR, solid reflectance spectra, magnetic moment and molar conductance measurements have accomplished characterization of the complexes. The IR data reveal that HL1 and HL23 ligands behave as a bidentate neutral ligands while HL4 ligand behaves as a bidentate monoionic ligand. They coordinated to the metal ions via the carbonyl O, enolic sulfonamide S(O)OH, pyrazole or thiazole N and azo N groups. The molar conductance data reveal that the chelates are non-electrolytes. From the solid reflectance spectra and magnetic moment data, the complexes were found to have octahedral, tetrahedral and square planar geometrical structures. The thermal behaviour of these chelates shows that the water molecules (hydrated and coordinated) and the anions are removed in a successive two steps followed immediately by decomposition of the ligand in the subsequent steps. The activation thermodynamic parameters, such as, E*, H*, S* and G* are calculated from the TG curves applying CoatsRedfern method.

Article Outline

o o o o o o o o o

1. Introduction 2. Experimental

2.1. Preparation of the azo ligands (L1 and HL24) 2.2. Preparation of solid complexes 3. Results and discussion

3.1. Preparation and characterization of the ligands 3.2. Infrared spectra and mode of bonding 3.3. Molar conductance data 3.4. Solid reflectance spectra and magnetic susceptibility measurements 3.5. Thermal analysis data 3.6. Kinetic analysis 3.7. Structural interpretation Supplemental information Appendix B. Supplementary data References

Abstract
A novel ligand, (Z)-1,5-dimethyl-4-(2-(3-methyl-5-oxo-1-phenyl-1H-pyrazol-4(5H)-ylidene)hydrazinyl)-2-phenyl-1,2-dihydropyrazol-3-one] and its metal(II)azo complexes were synthesized and characterized using elemental analyses, proton NMR, electrospray ionization mass spectrometry, FT-IR and UVvisible absorption. Smooth thin films of the metal(II)azo complexes were prepared using spin-coating, and the absorption spectra of the films were measured. The thermal properties of the metal()azo complexes were investigated using TGA and DSC. The optical constants (complex refractive index N = n + ik) of the films on single-crystal silicon were determined using variable-angle scanning ellipsometry from which the complex dielectric function () and absorption coefficient () were calculated. The photostabilities of the metal(II)azo complex films were also investigated.

Article Outline

o o o

1. Introduction 2. Experimental

2.1. Materials 2.2. Synthesis of the ligand (HL) and its metal()azo complexes

2.2.1. Diazotization 2.2.2. Coupling 2.2.3. Metallization

o o o o o o o o

2.2.3.1. NiL2 complex 2.2.3.2. CoL2 complex 2.2.3.3. CuL2 complex 2.2.3.4. ZnL2 complex 2.3. Preparation of the spin-coated thin films 2.4. Instrument and methods

3. Results and discussion

3.1. Synthesis and characterization 3.2. FT-IR spectra of the ligand and its metal()azo complexes 3.3. UVvis electronic absorption spectra of the ligand and its metal(II)azo complexes 3.4. Thermal properties of the metal(II)azo complexes 3.5. The optical properties of the metal(II)azo complex films 3.6. The photostabilities of the metal(II)azo complex films 4. Conclusions Acknowledgements References