The new mixed-ligad complex of [Tl(Ph2phen)Cl3(DMSO)] (1) was obtained from the reaction of TlCl3.4H2O with 4,7-diphenyl-1,10-phenanthroline (Ph2phen) in methanol solution. Suitable crystals of 1 were obtained for X-ray diffraction measurement by methanol diffusion into a DMSO solution. This complex was characterized by spectral methods (IR, UV-Vis, 1H NMR and luminescence), elemental analysis, thermal analysis (TG, DTA) and single crystal X-ray diffraction.