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Abstract The present thesis comprises three main chapters in addition to Arabic and English summaries as well as relevant references. The data in this thesis are collected in (17 Tables), (36 Figures), (15 Schemes). And list of references is given and containing 151 references. The First Chapter: Introduction The chapter is concerned with a scientific literature survey related to pyrazolopyridine, uracil, azo compounds and their metal complexes especially from their biological activity and structural viewpoints. The Second Chapter: Experimental This part describes the preparation of ligands; 4,6-dimethyl-1H-pyrazolo[3,4-b]pyridine-3-amine and 5-((4,6-dimethyl -1H-pyrazolo [3,4-b] pyridin-3-yl) diazenyl) pyrimidine -2,4 (1H,3H)-dione, and their metal complexes (Mn(II), Pd(II), Fe(III), Cr(III), Ru(III), Zr(IV), Hf(IV) and UO2(II) ) and (Cu(II), Co(II), Ni(II), Cr(III) and Ru(III)), respectively. Different instrumental methods are used to investigate the structure of all these systems as elemental analyses, spectral techniques (IR, UV–Vis, 1H NMR and mass spectra for the ligands), magnetic susceptibility, molar conductance of complexes and thermogravimetric studies. Finally, the biological activity (antitumor and antimicrobial) of the prepared ligands and some of their metal complexes are evaluated. The Third Chapter: Results and Discussion This chapter is divided into two parts: Part I An extraordinary range of properties for HL1 ligand are exhibited by the prepared complexes. The analytical and spectral data depict that: 1- The 1:2 (M:L) molar ratio reaction of chloride salts (Mn(II), Pd(II), Fe(III), Cr(III), Ru(III), Hf(IV) and Zr(IV)) and UO2(II) nitrate with the (HL1) ligand produced complexes with 1:2 and 1:3 (M:L) molar ratios. 2- All complexes are non-electrolyte and they have octahedral structure, except Pd( |