Presented herein is the synthesis and characterization of a new Fe(III)Zn(II) complex containing a Fe(III)-bound phenolate with a carbonyl functional group, which was anchored to 3-aminopropyl-functionalized silica as the solid support. The catalytic efficiency of the immobilized catalyst in the hydrolysis of 2,4-bis(dinitrophenyl)phosphate is comparable to the homogeneous reaction, and the supported catalyst can be reused for subsequent diester hydrolysis reactions.