Hydrothermal approach has led to the formation of a three-dimensional metal-organic framework (MOF), [NiCo(μ2-tp)(μ4-tp)(4,4′-bpy)2]n (1) (tp = terephthalic acid and 4,4′-bpy = 4,4′-bipyridine) which was characterized by means of single-crystal X-ray diffraction analysis, powder X-ray diffraction (PXRD), FT-IR spectroscopy, scanning electron microscopy (SEM) and inductive coupled plasma optical emission spectroscopy (ICP-OES). Thermal decomposition of the MOF afforded nanostructured mixed metal oxide, namely NiO/Co3O4. The XRD and SEM analysis confirm the formation of the mixed metal oxide. The nanostructured NiO/Co3O4 demonstrated good catalytic activity and selectivity in the epoxidation of cyclooctene in the presence of tert-butyl hydroperoxide (TBHP) as oxidant.