Four lanthanide coordination polymers, {[Ln(HPDA)(PDA)(H 2 O) 2 ]Á4H 2 O} n (Ln = Sm (1), Eu (2), Tb (3)) and {[Sm 3 (H 2 PDA) 2 (HPDA) 2 (PDA) (OH) 5 (H 2 O) 3 ]Á 2dtaÁ4H 2 O} n (4) (H 2 PDA = pyridine-2,6-dicarboxylic acid, dta = diethyl amine), have been synthesized under hydrothermal conditions and were characterized by elemental analysis, IR spectrometer, and single-crystal X-ray crystallography. In the complexes 1-3, the 1D chains are assembled into 2D layer by hydrogen bonds formed between the carboxyl groups, and were further assembled into 3D framework by hydrogen bonds and p-p stacking interactions. In complex 4, each Sm 3? ion connected to the neighboring Sm 3? ion through bridging carboxyl oxygen atoms, and then give rise to a new 2D layered open-framework structure. The 3D supramolecular structure of 4 is constructed through hydrogen-bonding and p-p stacking interactions between adjacent metal-organic polymeric coordination chains. Complexes 1-3 were dispersed in mesoporous materials SBA-15 in DMF solution (denoted as ML-SBA-15, ML = 1, 2, 3), which were characterized by XRD, IR, and fluorescence spectra. Compared to the complexes 1-3, the photoluminescence efficiency of hybrid material was improved by the energy transition between mesoporous materials and the complexes. The complexes encapsulated in mesoporous materials SBA-15 exhibited stronger luminescence intensity and longer fluorescence lifetime.