A chiral molecule-based magnet [Mn (-pnH) (HO)][Mn(CN)]·HO (-pn = -1,2-diaminopropane), ·2HO (222), has been obtained, which has a two-dimensional (2D) square network of cyanide-bridged Mn-Mn ions. The crystallographic research on this coordination polymer indicates that it is robust enough to transform the single-crystal structure upon dehydration as well as rehydration. Meanwhile, the magnetic property changes are reversibly associated with the structural phase transitions. The complete reversibility upon dehydration/rehydration was demonstrated using in situ X-ray diffraction from the as-prepared ·2HO to the dehydrated [Mn (-pnH)][Mn(CN)], , then rehydrated to [Mn (-pnH) (HO)][Mn(CN)]·HO, , and dehydrated again to [Mn (-pnH)][Mn(CN)], . Neither the space groups nor the crystal axes changed during the dehydration/rehydration process. The dehydration is considered to be associated with a change in the coordination of the -pnH from one 2D layer to the neighboring one involving a proton transfer and is accompanied by new cyanide bridging of Mn and Mn ions formed between the 2D sheet. Corresponding to the 2D to three-dimensional (3D) structural transition, the study of magnetic properties reveals that the Curie temperature of long-range magnetic ordering for ( = 45 K) is more than double that for ·2HO ( = 21 K).
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