This book deals with some modern methods used in the synthesis and characterization of transition metal complexes. It is written primarily to stimulate the interest of students in metallo-organic chemistry and spectroscopy as well. The book is contained much useful spectral data in the form of tables and spectra. It contains a number of electronic, IR and EPR spectra, so the reader who is not familiar with these techniques can see how the spectra actually appear. It begins with a general introduction of applications of transition metal complexes in different fields. In subsequent chapters the detailed study regarding the synthesis and physicochemical characterization of bivalent transition metal ions [Cr(III), Mn(II), Co(II), Ni(II) and Cu(II)] complexes derived from 2-methylcyclohexanone semicarbazone and thiosemicarbazone using modern techniques like elemental analysis, magnetic moments and conductance measurements and spectroscopic (Electronic, IR, EPR ) studies is discussed. The geometry of synthesized complexes is emphasized. The book is intended to be useful to new metallo-organic researchers.