A porous crytalline metal-organic framework Fe₃O(BPDC)₃ was synthesized, and its properties were characterized by various techniques, including X-ray powder diffraction (PXRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and nitrogen physisorption measurements. The Fe₃O(BPDC)₃ was used as an efficient catalyst for the oxidative coupling reaction of benzaldehyde and (E)-1-phenylethan-1-one O-acetyl oxime to form 2,4,6-triphenylpyridine as desired product. The reaction could proceed readily, with more than 83 % reaction yield being achieved after 360 min at 140 ^oC in the presence of 10 mol% Fe₃O(BPDC)₃) catalyst and Di-tert-butyl peroxide as an oxidant. This Fe-MOF exhibited higher activity than other MOFs and traditional homogeneous catalysts in the oxidative coupling reaction. The transformation could only proceed to obtain main product in the presence of Fe₃O(BPDC)₃.