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The hybrid compound [Cu(cyclam)(H 2 O) 2 ] 0.5 [{Cu(cyclam)} 1.5 { B -H 2 As 2 Mo 6 O 26 (H 2 O)}]·9H 2 O ( 1 ) (cyclam = 1,4,8,11-tetraazacyclotetradecane) was synthesized in aqueous solution by reacting the {Cu(cyclam)} 2+ complex with a mixture of heptamolybdate and an arsenate(V) source. Crystal packing of 1 exhibits a supramolecular open-framework built of discrete covalent molybdoarsenate/metalorganic units and additional [Cu(cyclam)(H 2 O) 2 ] 2+ cations, the stacking of which generates squarelike channels parallel to the z axis with an approximate cross section of 10 × 11 Å 2 where all the hydration water molecules are hosted. Thermal evacuation of solvent molecules yields a new anhydrous crystalline phase, but compound 1 does not preserve its single-crystalline nature upon heating. However, when crystals are dehydrated under vacuum, they undergo a structural transformation that proceeds via a single-crystal-to-single-crystal pathway, leading to the anhydrous phase [{Cu(cyclam)} 2 ( A -H 2 As 2 Mo 6 O 26 )] ( 2 ). Total dehydration results in important modifications within the inorganic cluster skeleton which reveals an unprecedented solid-state B to A isomerization of the polyoxoanion. This transition also involves changes in the Cu II bonding scheme that lead to covalent cluster/metalorganic layers by retaining the open-framework nature of 1 . Compound 2 adsorbs ambient moisture upon air exposure, but it does not revert back to 1 , and the hydrated phase [{Cu(cyclam)} 2 ( A -H 2 As 2 Mo 6 O 26 )]·6H 2 O ( 2h ) is obtained instead. Structural variations between 1 and 2 are reflected in electron paramagnetic resonance spectroscopy measurements, and the permanent microporosity of 2 provides interesting functionalities to the system such as the selective adsorption of gaseous CO 2 over N 2 .

Single-Crystal-to-Single-Crystal Cluster Transformation in a Microporous Molybdoarsenate(V)-Metalorganic Framework