Abstract: The new novel metal-organic framework (M0Fs) Ni₃(tib)₂(H₂0)₁₂(S0₄)₃n(1) is obtained by hydrothermal reaction of the metal salt NiSO₄·6H₂0 and the three-connecting ligand 1,3,5-tris(1-imidazolyl) benzene (tib). The crystal data and structure are established by single-crystal X-ray diffraction analysis， and characterized by elemental, IR, XRD, et al. and by using SHELXL-97 software for the structure elucidation and Topos40 software for its topology analysis. It shows that complex 1 is a 2D network honeycomb networks with (6,3) topology， which is further linked to three-dimensional (3D) frameworks by the spatial additive effect of π-π and interaction of hydrogen bonds. Dielectric constant studies show that the ε_max of complex 1 reaches a value of about 10.08 at 138 ℃ ,which is the typical dielectric material. This material has good thermal stability indicated by thermogravimetric,which provides a reference and guidance for the development of the novel multidimensional M0FS and dielectric properties of new materials.