Two one-dimensional coordination polymers were synthesized using rigid organic compound 2-carboxylic acid-4-nitropyridine-1-oxide(POA) as ligand, reacting with rare earth La(III) and Pr(III). The single crystal X-ray diffraction results show that the molecular formula of complex 1 is {［La(POA)3H2O］·CH3OH}n, which belongs to monoclinic system, and the space group is P21/c; with a=1.756 8 nm, b=0.663 6 nm, c=2.048 6 nm, α=90°, β=96.96°, γ=90°, V=2.370 7 nm3, Mr=738.28. The molecular formula of complex 2 is {［Pr(POA)3H2O］·H2O}n, which belongs to monoclinic system, and the space group is P21/c. The cell parameters are a=1.757 8 nm, b=0.656 9 nm, c=2.046 7 nm, α=90°, β=97.20°, γ=90°, V=2.344 8 nm3, Mr=726.25. The composition and structure of coordination units of two complexes are similar, and the central Ln(III) ion is in the coordination environment of a slightly modified tricapped trigonal prism configuration. The properties of two complexes were characterized by infrared, ultraviolet, thermogravimetric analyzer and fluorescence spectrometer. Fluorescence analysis shows that both ligand and complexes have strong fluorescence properties.