Micro and nano-structures of a new Ce(III) Coordination supramolecular compound, [Ce (1,5-NDS)1.5(H2O)5]n,1, (1,5-Naphthalenedisulfonic acid), were prepared using hydrothermal and sonochemical approaches, respectively. These new micro and nano structures were characterized by elemental analysis, IR spectra, thermal gravimetric analysis (TGA), scanning electron microscopy (SEM), and powder X-ray diffraction. The X-ray single crystal structure determination of 1 shows that it features a neutral 2D framework based on the [Ce2H20O16S2] clusters as a secondary building unit (SBU) which shows a sql/Shubnikov tetragonal plane net. Moreover by considering the H-bonds, the final structure can be considered as 3D supramolecular network. The influence of ultrasound irradiation time on the morphology and size of the nanostructure 1 was investigated. The results indicated that by increasing the time of ultrasonic radiation, smaller nanostructures form and morphological changes occur. Fluorescent properties of the nanoparticles of 1 were also investigated. Coordination polymer 1 shows high fluorescence intensity and good tendency to copper ion that can be used as an optical sensor for selective and sensitive determination of Cu2+ in aqueous media with detection limit of 3.0μM.