The complexes of formulas [Ln 2 (pydc) 2 (Hpydc) 2 (H 2 O) 4 ]•2H 2 O [Ln=Ce (1), Pr (2), H 2 pydc=pyridine-2,5-dicarboxylic acid] have been hydrothermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The structure analyses for 1 and 2 indicate that one-dimensional metal helical chains are linked through carboxylate groups, and the helical chains are connected with the bridging pydc 2anion, forming two-dimensional layered polymeric structures. The luminescent properties of complexes were also discussed.