Polyoxometallates are known to form a plethora of large polyanions, the number of which even grows with the introduction of heteroatoms. They are frequently synthesized under solvothermal conditions, but with suitable precursors even at room temperature reactions can be carried out. Under such conditions the growth of single crystals is not always possible and structure solution from powder diffraction data remains the only way to determine the crystal structure. Herein, the challenging case of the arsenato polyoxovanadate [Ni(en)3]2[V12As8O40(H2O)]x4H2O is presented, where both lab and synchrotron based powder diffraction data were employed for structure solution and refinement.
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