The reaction of methylviologen iodide with crystalline V
2O
5 in the molar ratio of 1 to 3.8 at 100
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C in water led to the formation of (MV)
0.25V
2O
5 in quantitative yield. The structure of this organic-inorganic multilayered hybrid compound was determined by single-crystal X-ray crystallography. Strong van der Waals interactions were found between the electron-deficient aromatic organic molecules and the inorganic layers. In the solid state, the compound is a semiconductor due to small polaron hopping and shows novel reversible alkali-ion intercalation/deintercalation via electrochemistry.