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A new heterobimetallic nitrilotriacetatoperoxotitanate complex with the formula of [Mn(H2O)5]2[Ti(O2)2O(nta)2]·7H2O(1,C6H6O6N = H3nta)has been isolated in pure crystals.It was characterized by elemental analyses,IR,thermal analysis(TGA)and single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinie,space group C2/c with a = 15.088(3),b = 13.311(3),c =17.741(4)(A),β= 100.92(3)°,Z = 4,V = 3498.6(12)(A)3,Mr = 968.19,Dc = 1.838 g/cm3,μ = 1.266 mm-1,F(000)= 1992,R = 0.0337 and wR = 0.0819.Single-crystal X-ray analysis reveals that the titanium atom is N,O,O,O"-ehelated by the nitrilotriacetate and O,O-chelated by the peroxo group,and is coordinated to the bridging O atom in an overall pentagonal-bipyramidal geometry.The manganese ions in the compound are both 6-coordinated by five water molecules and one bridged carboxylato oxygen atom.A decameric water cluster consisting of a cyclic water hexamer in a boat fashion is also found in complex 1.The TGA and XRD results prove that 1 undergoes facile thermal decomposition to form the mixture of Mu2O3 and TiO2 at 600～800 ℃,and pure MnTiO3 at 900 ℃.