The exploration of organically templated layered transition metal phosphates with novel structures has been driven by their potential for application as redox catalysts,ion-exchangers, adsorbents, molecular sieves, etc. The incorporation of 3d transition metals into these materials offers the possibility of devising new materials with enhanced catalytic, magnetic, and also generates their redox activity. This book describes the room temperature synthesis of 3d- transition metal (TM) ions doped chlorocadmium phosphate crystals by using 1,6-Diamino Hexane as an organic templating molecule. The structural characterization was carried out by using Powder X-ray diffraction studies. The structural stability of crystalline samples is measured from Thermogravimetric studies. Several spectroscopic techniques Optical absorption, EPR and FT-IR Spectrophotometers are used to collect the information about the coordination site symmetry and bonding nature of the doped TM ions. This book is very helpful to the academicians and researchers those who are working in the fields of Spectroscopy of Porous materials, Layered metal phosphates, Heterogeneous catalysis…etc.