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Three new rare earth coordination compounds [REL3Ph]2(RE = Pr(1), Sm(2)); [ErL3Ph]2·4C2H5OH(3); (L = 2,6-dimethylbenzoate, Ph = o-phenanthroline) were synthesized. The crystal structures of the three compounds were measured by X-ray single-crystal diffraction. From the results, we made out that compounds 1–3 were binuclear structures, and 1D chain-like structures could be formed by hydrogen bonding. The thermal degradation data of the compounds and the three-dimentional infrared cumulative spectra of the gaseous decomposed products were obtained by TG/DSC-FTIR technique, and the thermal degradation patterns were explained. The isobaric molar heat capacity of compounds 1 and 2 in the low-temperature region was obtained by the DSC technique and the thermodynamic parameters were derived. The fluorescence spectrum of compound 2 was determined, showing that it had potential application value in the orange-red luminescence region.