A novel pillared-layer framework with a （52.6）（53.63.73.8） Schlaifli symbol, [Mn（H2O）（Htrc）（Hbtc）]n （1）, was prepared by the reaction of 1,2,4-triazole （Htrz）, 1,3,5-benzene- tricarboxylic acid （H3btc）, and MnII salt and structurally and magnetically characterized. It crystallizes in the orthorhombic system, space group P212121 with a = 7.1618（5）, b = 9.0356（6）, c = 10.9740（13） A, V = 1292.54（15） A3, Dc = 1.799 g/cm3, Mr = 350.15, Z = 4, F（000） = 708, p = 1.064 mm-1, and the final R = 0.0177 and wR = 0.0462 for 2273 observed reflections with I〉 2σ（I）. The unique octahedral Mnn ion in 1 is periodically linked into a two-dimensional （2D） magnetic layer by p2-N1, N4-Htrz and syn, anti-COO of doubly deprotonated Hbtc2- anion, which is further supported by the phenyl backbone of Hbtc2- ligand to generate a 3D pillared-layer framework. Magnetically, complex 1 displays an antiferromagnetic ordering below 5.0 K due to the cooperative antiferromagnetic couplings mediated by the mixed heterobridges within the magnetic layer.
