A new tin complex, [l-(4-bpdb){Me 2 Sn(cupf) 2 } 2 ] (1), was prepared by reacting dimethyltin(IV) dichloride, with 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene (4-bpdb) and cupferron in a fast and facile process. The complex was fully characterized based on its 1 H and 13 C NMR, IR, and UV spectra and elemental analysis. The nanostructure of the prepared compound was synthesized by the sonochemical method. The new nanostructure was characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), IR spectroscopy and elemental analysis. Thermal stability of single crystalline and nanosize samples of the prepared compound was studied by thermal gravimetric and differential thermal analysis. The prepared complexes, as bulk and as nanoparticles, were utilized as a precursor for preparation of SnO 2 nanoparticles by direct thermal decomposition at 600°C in air. The morphology and size of the SnO 2 nanoparticles were determined by scanning electron microscopy, XRD and IR spectroscopy and the results showed that particle size of the SnO 2 nanoparticle depend on the initial particles size of 1. Photoluminescence properties of the nanostructured and crystalline bulk of the prepared complex and SnO 2 nanoparticles core of them were investigated.