Under solvothermal conditions with the mixed solvents of C₂H₅OH and H₂O, a new heterometallic lanthanide-titanium-organic compound, [TbTi(μ₃-O)(L₃)(H₂O)₄]·H₃O (1, H₂L = diphenylglycolic acid), has been synthesized. Compound 1 exhibits a 3D supramolecular framework by incorporating the tetra-nuclear [Tb₂Ti₂(μ₃-O)₂] unit and L^2- ligand. Compound 1 shows intense green luminescence. Furthermore, the PXRD, TGA and IR spectra were also studied.