A novel coordination polymer, [Co3 （bta）2（dib）2]·4H2O （1, H3bta=benzene-1,3,5-triacetic acid, and dib=1,4-di（1H-imidazol-1-yl）benzene）, has been hydrothermally prepared and characterized by IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The crystal is of triclinic system, space group Pī, with a=9.141（2）, b=9.667（2）, c=13.855（2）, α=100.83（3）, β=90.81（3）, γ=100.94（3）°, V=1179.0（4）3 , C48H46N8O16Co3 , Mr=1167.72, Dc=1.645 g/cm 3 , F（000）=599, μ=1.127 mm-1 and Z=1. The final R=0.0634 and wR=0.1703 for 4291 observed reflections （I 〉 2σ（I））. In the title complex, the bta ligand acts as a four-dentate bridging ligand to link up cobalt atoms into a lamellar framework, which are further interlinked by the dib ligands to generate a binodal （3,8）-connected tfz-d net.
