A new metal-organic polymer Mn3（BTC）2(H2O)9·(H2O) was synthesized by reaction of the metal ions Mn（Ⅱ） with 1,3,5-benzenetricarboxylic acid(H3BTC) in a mixed solution of DMF/C2H5OH/(H2O) and crystallized.The crystal belongs to monoclinic system,space group C2/c with a=1.901 4（4） nm,b=0.740 23（15） nm,c=2.044 9（4） nm,β=97.18（3）°,V=2.855 5（10） nm3,Z=4,Dc=1.766（g/cm3）,μ（Mo Kα）=1.401 mm-1,R[I>2σ（I）]=0.072 7,wR=0.235 1 for 2 419 independent reflections with goodness-of-fit 1.046. Its structure possesses bilayer architectures constructed from Mn ions linked infinite Mn（BTC） chains which were build up from BTC ligand as the "T-shape" module and Mn as the linear module.The hydrogen-bond and π-π stacking interactions between bilayers make them three-dimensional channel-like interpenetrated frameworks.
