Abstract: | ![]() The title compound, tetrakis(ethylenediammonium) tetra‐μ‐hydrogenphosphato‐di‐μ‐hydroxo‐ tetra‐μ‐phosphato‐bis(aquacobalt)hexakis(oxovanadium) trihydrate, was synthesized hydrothermally at moderate temperature. The structure consists of diprotonated ethylenediammonium cations and layers of the polyanions. The polyanion contains four PO4 tetrahedra and three VO5 square pyramids that are linked through corner‐sharing by alternating P—O—V, which gives rise to a chain. The chains, connected by CoO4(H2O)2 octahedra, form layers, resulting in a two‐dimensional layered structure. The Co—O distances are in the range 1.984 (3)–2.038 (4) Å, the P—O distances 1.508 (3)–1.575 (3) Å and the V—O distances 1.585 (3)–2.010 (3) Å. |