In the present book , the work has been focused on EXAFS data analysis using IFEFFIT method of copper (II) complexes. The coordination chemistry of Schiff base ligands is a fascinating area of research. The production of novel 1-(4,5-dimethoxy-2-nitrobenzylidene) thiosemicarbazide, were synthesized by chemical root method. The copper (II) complexes were characterized by X-ray absorption spectroscopy (XAS) techniques. X-ray absorption spectroscopy (XAS) is a widely-used technique for determining the local geometric and/or electronic structure of matter. The XAS experiment has been performed at synchrotron radiation sources (SRS), at the recently developed BL-8 Dispersive EXAFS (DEXAFS) beamline at 2·5 GeV Indus-2 synchrotron source at Raja Ramanna Centre for Advanced Technology (RRCAT), Indore, India which provides intense and tuneable X-ray beams.