This book explained the preparation and characterization of ligand metal complexes. The structural elucidation of these metal complexes carried out by their effective magnetic moment value, ESI mass, UV/Visible, IR and 1HNMR spectroscopic techniques and thermo-gravimetric analysis. Magnetic moment value of Cu (II) and Co(II) complexes suggested octahedral geometry. Electronic transitions of metal complexes also supported their geometry. IR spectra indicated the complex formation by the shifting of IR frequency of azomethine group to lower wave number. Distortion and absence of OH proton of the 1HNMR metal complexes supported the formation of metal complexes. TGA of complexes clearly showed absence of coordinated water molecule. Complexes found non electrolytes.