Synthesis and structural characterization of a new supermolecular compound: H3PW12O40·6C14H20O5·16H2O (C14H20O5=benzo-15-crown-5)

Abstract

The new supermolecular compound, H3PW12O40·6C40H20O5·16H2O (C14H20O5=benzo-15-crown-5), was synthesized in methanol solution and structurally characterized by elemental analysis, IR, 1H NMR and single crystal X-ray diffraction. It was shown that PW12O403− anions possess α-Keggin structure with crystallographic disorder. The disorder averages the W–W distances and W–Ob/c–W angles, but the vibrational ellipsoids of oxygen atoms are not elongated obviously. In the compound, water blocks are formed, which are hydrogen-bonded to crown ether molecules. Since crown ether molecules fetter the movement of water molecules and oxonium ions, the conductivity is lower (ρr.t.<10−7Scm−1). The compound crystallizes in the triclinic space group P1̄ with a=14.154(3), b=15.598(3), c=18.023(3)Å,α=67.17(3), β=89.83(3), γ=83.27(3)°, V=3638.1(13)Å3,Z=1 and R1(wR2)=0.0655(0.1701).