Mohamed Gehad G, Gad-Elkareem Mohamed A M
Chemistry Department, Faculty of Science, Cairo University, Giza, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2007 Dec 31;68(5):1382-7. doi: 10.1016/j.saa.2007.01.034. Epub 2007 Mar 3.
Four new azo ligands, L1 and HL2-4, of sulfa drugs have been prepared and characterized. [MX(2)(L1)(H(2)O)(m)].nH(2)O; [(MX(2))(2)(HL2 or HL3)(H(2)O)(m)].nH(2)O and [M(2)X(3)(L4)(H(2)O)].nH(2)O; M=Co(II), Ni(II) and Cu(II) (X=Cl) and Zn(II) (X=AcO); m=0-4 and n=0-3, 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 HL2-3 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*, DeltaH*, DeltaS* and DeltaG* are calculated from the TG curves applying Coats-Redfern method.
已制备并表征了四种新型磺胺类药物的偶氮配体L1和HL2 - 4。制备了[MX(2)(L1)(H(2)O)(m)].nH(2)O;[(MX(2))(2)(HL2或HL3)(H(2)O)(m)].nH(2)O和[M(2)X(3)(L4)(H(2)O)].nH(2)O;其中M = Co(II)、Ni(II)和Cu(II)(X = Cl)以及Zn(II)(X = AcO);m = 0 - 4且n = 0 - 3的配合物。通过元素分析和热分析(TGA和DTA)、红外光谱、固体反射光谱、磁矩和摩尔电导率测量完成了对配合物的表征。红外数据表明,HL1和HL2 - 3配体表现为双齿中性配体,而HL4配体表现为双齿单离子配体。它们通过羰基O、烯醇式磺酰胺S(O)OH、吡唑或噻唑N以及偶氮N基团与金属离子配位。摩尔电导率数据表明螯合物为非电解质。从固体反射光谱和磁矩数据发现,配合物具有八面体、四面体和平面正方形几何结构。这些螯合物的热行为表明,水分子(水合和配位的)和阴离子在连续的两步中被除去,随后在后续步骤中配体立即分解。应用Coats - Redfern方法从TG曲线计算活化热力学参数,如E*、ΔH*、ΔS和ΔG。