Two novel metal-organic frameworks, {[Eu(phen)(NDA)1.5(H2O)]}n ((1); NDA = 2,6-naphthalenedicarboxylate ions, phen = 1,10-phenanthroline) and {[Gd(phen)(NDA)1.5]·0.5H2NDA}n (2), have been synthesized under hydrothermal conditions. The structure analyses of 1 and 2 reveal that the two compounds belong to the triclinic system with space group P-1. Compound 1 features a 2D lattice structure while compound 2 displays a novel 3D architecture. The two frameworks were further characterized by elemental analyses, luminescent spectrua, and variable-temperature magnetic susceptibilities. The investigation of lumi-nescent property reveals that 1 exhibits characteristic red emission of Eu3+. Magnetic investigation suggests that the ferromagnetic coupling exists between adjacent Gd3+ in compound 2.