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Ion pairing of trinuclear macrocation cluster (known as basic carboxylate), [\(\hbox {M}_{3}(\upmu _{3}\)-O)\((\hbox {ClCH}_{2}\hbox {COO})_{6}(\hbox {H}_{2}\hbox {O})_{3}]^{1+}\) and a Keggin type polyoxometalate cluster anion \([\hbox {SiW}_{12}\hbox {O}_{40}]^{4-}\) is stabilized with a number of crystal water molecules in composite type compounds [\(\hbox {M}_{3}(\upmu _{3}\)-O)\((\hbox {ClCH}_{2}\hbox {COO})_{6}(\hbox {H}_{2}\hbox {O})_{3}] _{4}\) [\(\hbox {SiW}_{12}\hbox {O}_{40}\)] \(\cdot \hbox {xH}_{2}\hbox {O}\, \cdot \hbox {2ClCH}_{2}\hbox {COOH}\) [\(\hbox {M}=\hbox {Fe}^{3+}, \,\,\hbox {x} = 18 (\mathbf{1}); \,\,\hbox {M} = \hbox {Cr}^{3+} \,\,\hbox {x} = 14 (\mathbf{2})\)]. When the crystals of 1 are heated at 85\({^{\circ }}\)C and 135\({^{\circ }}\)C for 3.5 hours in an open atmospheric condition, it goes to [\(\hbox {Fe}_{3}(\upmu _{3}\)-O)\((\hbox {ClCH}_{2}\hbox {COO})_{6}(\hbox {H}_{2}\hbox {O}) _{3}]_{4}\)[\(\hbox {SiW}_{12}\hbox {O}_{40}\)] \(\cdot 10\hbox {H}_{2}\)O \(\cdot \hbox {2ClCH}_{2}\)COOH (dehydrated 1-\({\mathbf{85}}^{\mathbf{o}}\equiv \) \(\mathbf{1}^{\prime }\)), and [\(\hbox {Fe}_{3}(\upmu _{3}\)-O)(\(\hbox {ClCH}_{2}\hbox {COO})_{6}\)(\(\hbox {H}_{2}\hbox {O}) _{3}]_{4}\)[\(\hbox {SiW}_{12}\hbox {O}_{40}\)] \(\cdot \,\, 8\hbox {H}_{2}\)O \(\cdot \,\,2\hbox {ClCH}_{2}\)COOH (dehydrated 1-\(\mathbf{135}^{\mathbf{o}}\equiv \) \(\mathbf{1}^{\prime \prime }\)) respectively with the loss of considerable amount of lattice water molecules retaining their single crystallinity. On the other hand, the single crystals of compound 2, upon heating at 85\({^{\circ }}\)C or 135\({^{\circ }}\)C for 3.5 hours, undergo ‘crystal-to-crystal transformation’ to the single crystals of [\(\hbox {Cr}_{3}(\upmu _{3}\)-O)(\(\hbox {ClCH}_{2}\hbox {COO})_{6} (\hbox {H}_{2}\hbox {O})_{3}]_{4}\)[\(\hbox {SiW}_{12}\hbox {O}_{40}\)]\(\cdot 8\hbox {H}_{2}\hbox {O}\cdot 2\hbox {ClCH}_{2}\)COOH (\(\mathbf{dehydrated\, 2}\equiv \mathbf{2}^{\prime }\)). Crystal structure analyses show that the parent compounds 1 and 2 undergo molecular rearrangement (molecular motion in the solid state) in respective dehydrated compounds. Remarkably, these dehydrated crystals (\(\mathbf{1}^{\prime }, \mathbf{1}^{\prime \prime }\) and \(\mathbf{2}^{\prime }\)), upon exposure to water vapor at an ambient condition, regenerate the crystals of parent compounds 1 and 2, respectively.

journal of chemical sciences

‘Ionic crystals’ consisting of trinuclear macrocations and polyoxometalate anions exhibiting single crystal to single crystal transformation: breathing of crystals