The inclusion of water oxidation active polyoxometalates (POMs) inside layered materials is a promising strategy to increase their catalytic efficiency while overcoming their fragility under homogeneous conditions. In this sense, intercalation of POMs in the interlaminar space of layered double hydroxides (LDHs), formed by positively charged brucite-type inorganic layers, is a very interesting strategy that is gaining attention in the field. Despite their huge potential, there is a lack of accurate characterization of the materials, especially after their use as water oxidation catalysts under pH conditions in which the POM counterpart has been demonstrated to be unstable (strong alkali media). For this reason and as a proof of concept, we have intercalated the well-known [Co