Solvothermal reaction of [Ni(tppz) 2 ](NO 3 ) 2 with Ln(NO 3 ) 3 • 6H 2 O afforded a 3d-4f heterometallic coordination complexes [Ni-(tppz) 2 ][Ln(NO 3 ) 5 ] ((where tppz = 2,3,5,6-tetra(2-pyridyl) pyrazine and Ln(III) = Nd (1), Eu (2), Gd (3), Tb (4), Dy (5), Er ( 6)). The complexes were characterized by elemental analysis, infrared spectroscopy, single-crystal X-ray diffraction, and powder X-ray diffraction. Moreover, UV-Vis absorption properties of 1-6 and solid-state luminescence properties of 2 and 4 are also discussed.[a] X.