The novel three-dimension edta-linked (edta=ethylenediamine-N,N,N′,N′-tetraacetate) heterometallic complex [Sb 2 (edta) 2 -µ 4 -Co(H 2 O) 2 ]•5.15H 2 O has been synthesized and characterized by elemental analyses, FT-IR spectrum, X-ray diffraction analyses and thermogravimetry-differential scanning calorimetry (TG-DSC). The complex crystallizes in the monoclinic system, space group P2 1 /n, lattice parameters: a=0.69969 (2) the Sb(III) ion is six coordinated by two nitrogen and four oxygen from edta ions, together with a lone electron pair at the equatorial position. In the complex, the coordination number of Co(II) ion is six and its coordination environment is composed of four carboxylic oxygen atoms from four different edta ions and two oxygen atoms from two H 2 O molecules. The degradation of the sample proceeds in several steps and the water molecules and ligands are successively emited.