Abstract: | The title compound, tetramethylammonium 4,4′,6,6′‐tetrahydroxy‐2,2′‐spirobi(cyclotriboroxane) 0.25‐hydrate, C4H12N+·B5H4O10−·0.25H2O, was synthesized under mild solvothermal conditions. The B5O6(OH)4− clusters are connected by strong hydrogen‐bonding interactions into a three‐dimensional structure containing rectangular channels along the a axis, in which the C4H12N+ ions and water molecules are located. |