A novel neodymium pentafluoropropionate binuclear complex, Nd(C 2 F 5 COO) 3 Á Phen (Phen: 1,10-phenanthroline), was synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, FT-IR spectra, UV-Vis-NIR absorption, and PL spectra. Singlecrystal data show that the complex bears centrosymmetric dinuclear structure with a planar ligand configuration. Four carboxylato groups act as g 2 -chelate-l 2 -carboxylato-k 1 O: k 1 O 0 -bridge-ligands, the other two occupy the terminal position as monodentate ligands. At the same time, the C-O distances appear averaged which indicate the three atoms of carboxylato forming electron-conjugate system. Hydrogen bond and p-p-stacking link the binuclear to two-dimensional sheet. Optical spectra exhibit the complex possesses typical Nd(III) ion absorption and photoluminescence emission.