摘要
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 monoclinic, space group C2/c with a = 15.088（3）, b = 13.311（3）, c = 17.741（4） , β = 100.92（3）°, Z = 4, V = 3498.6（12） 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＇＇-chelated 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 Mn2O3 and TiO2 at 600～800 ℃, and pure MnTiO3 at 900 ℃.
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 monoclinic, space group C2/c with a = 15.088（3）, b = 13.311（3）, c = 17.741（4） , β = 100.92（3）°, Z = 4, V = 3498.6（12） 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＇＇-chelated 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 Mn2O3 and TiO2 at 600～800 ℃, and pure MnTiO3 at 900 ℃.
基金
supported by the Fundamental Research Funds for the Central Universities, SCUT (No. 2009ZM0313)
the National Natural Science Foundation of China (B5080320)
