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Abstract: The hexamolybdate cluster has been functionalized with fluorine-containing aromatic amine by the DCC (N,N′-dicyclohexylcarbodiimide) dehydrating protocol and two novel mono-functionalized arylimido derivatives of hexamolybdates bearing the electron-withdrawing trifluoromethyl group and trifluoromethoxy group, (Bu4N)2[Mo6O18(≡NAr)] (Ar= o-CF3C6H4) 1 and (Bu4N)2[Mo6O18(≡NAr)] (Ar= p-OCF3C6H4) 2 have been synthesized by improved method. Complete assignments were achieved for the title compounds by elemental analysis, IR, 1H NMR, UV/visible and single-crystal X-ray diffraction analyses. The preliminary herbicidal activity test indicated that they have some herbicidal activities. [Copyright &y& Elsevier]