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A series of Ni II and Pd II complexes with pyrene-based thiosemicarbazones were conveniently prepared. The crystal structures of Ni(L 2 ) 2 , Pd(L 1 ) 2 , and Pd(L 2 ) 2 were determined. X-ray crystallographic analysis reveals that the complexes are of mononuclear struc-* Dr. T.-H. Dinh 113 ture with two pyrenyl rings cofacially aligned. The photoluminescence spectra of the complexes exhibit moderate characteristic excimeric emissions arising from intramolecular π-π stacking between pyrenyl rings.