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The phase transition of a new coordination polymer, [Zn(HBT C)(BPE)0.5(H2O)]n·nH2O, HBTC2-=dianion of trimesic acid, DPE = 1,2-bis-(4-pyridyl)ethane, during dehydration and rehydration processes has been monitored by in-situ synchrotron powder X-ray diffractometry. The complex with an extended 1D ladderlike metalorganic framework (MOF) has been synthesized and structural characterized by single-crystal X-ray diffraction method. Structural determination reveals that the Zn(II) ion is four-coordinated in a distorted tetrahedral geometry, bonded to one nitrogen atom from one BPE ligand, and three oxygen atoms from two monodentate carboxylate groups of two HBTC2ligands and one coordinated water molecule. The 1D ladderlike MOF 1 dehydrates up heating of the solid to 180oC to form a new 2D MOF, [Zn(HBTC)(DPE)0.5]n (2). The reversible solid-state structural transformation between crystalline 1 with 1D ladderlike framework and its dehydrated powder 2 with 2D framework via the displacement of coordinated water molecule to HBTC2ligand, by thermal de/rehydrated processes has been monitoring by in situ PXRD measurements. In the crystal lattice, during heating process, one oxygen atom of the uncoordinated carboxylate group of HBTC2ligand moves toward the neighboring Zn(II) ion, with concomitant removal of the water molecule, and form a new Zn-O bond without expanding the coordination geometry of metal center. The dehydrated structure for 2 at 180oC was determined from the powder diffraction data with program DASH. Powder pattern was indexed with Dicvol and Treor programs. The structure factors of the powder patterns were extracted with Pawley’s method, and simulated annealing method was employed to determine the crystal structure. The final refinement with the Rietveld method was performed using GSAS-EXPGUI program.

Reversible phase transition of metal–organic framework by de/rehydration