A new complex [Cd(btca) 0.5 (H 2 O) 3 ] (1) (H 4 btca: 1,2,4,5-benzenetetracarboxlyic acid) has been synthesized and characterized by single crystal X-ray diffraction studies, elemental analysis and FT-IR. In compound 1, Cd(II) center atoms coordinate to three ligand btca 4-anions and three water molecules with a six-coordinated distorted octahedral geometry. Four carboxyl groups of btca 4-adopt μ 2 -η 2 :η 0 and μ 1 -η 1 :η 0 two different coordination modes. The whole anion btca 4-acts as a hexadentate bridge to connect adjacent Cd(II) atoms, resulting in 2D layer structure. Further, these two-dimensional layers are linked together by O-H···O to give rise to three-dimensional structure. Thermal stability and luminescent property of 1 are investigated. CdO micro-crystalline particles are then produced by calcination of compound 1 at 580 o C. The obtained CdO is characterized by XRD and SEM analyses.