Metal(II) p-dimetilaminobenzoatların izonikotinamid komplekslerinin sentezi, spektroskopik ve termal karakterizasyonu

Synthesis, spectroscopic and thermal characterization of isonicotinamide complexes of metal(II) p-dimethylaminobenzoates.

Özet

Bu çalışmada Mn(II), Co(II), Ni(II), Cu(II), Zn(II) ve Cd(II) metallerinin p-dimetilaminobenzoik asit (DMABA) ve izonikotinamid (İNA) ile 6 adet karışık ligand kompleksi sentezlendi: [Mn(DMAB)2(İNA)(H2O)2] 1, [Co(DMAB)2(İNA)(H2O)2] 2, [Ni(DMAB)2(İNA)(H2O)2] 3, Cu2(DMAB)4(İNA)2] 4, [Zn(DMAB)2(İNA)(H2O)2] 5, [Cd(DMAB)2(İNA)(H2O)2] 6. Komplekslerin yapıları elementel analiz, kütle analizi, termik analiz, IR, UV, 1H-NMR, 13C-NMR ve ESR spektroskopi verileri ile karakterize edilmiştir. Neticede Cu(II) kompleksinin kare piramidal, diğer komplekslerin ise oktahedral geometriye sahip oldukları belirlenmistir. Kompekslerin bozunması 1. veya 2. basamakta termal su kaybı ile başlamakta, daha sonra organik ligandlar bozunmaktadır. İncelenen komplekslerin termal dayanıklılığı ve ayrışma mekanizması aydınlatılarak son bozunma ürünü olarak metal oksit kaldığı belirlenmiştir.

Abstract

In this study, the 6 new mixed complexes of Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) with pdimethylaminobenzoic [Mn(DMAB)2(İNA)(H2O)2] 1, [Co(DMAB)2(İNA)(H2O)2] 2, [Ni(DMAB)2(İNA)(H2O)2] 3, Cu2(DMAB)4(İNA)2] 4, [Zn(DMAB)2(İNA)(H2O)2] 5, [Cd(DMAB)2(İNA)(H2O)2] 6. The complexes were characterized by elemental analysis, direct injection probe mass, IR, 1H-NMR, 13C-NMR, UV-vis, ESR spectroscopy, thermogravimetry measurements. Concequently, it has been determined that Complex 4 have square-pyramidal and the others complexes have octahedral geometries. The decomposition of each complex starts with dehydration and follows by decomposition organic part, respectively.The thermal dehydration of complexes takes place in steps from one to two. The decomposition mechanism and termal stability of the investigated complexes are interpreted in terms of their structures.The final decomposition products are found to be the respective metal oxides.