Hydrothermal synthesis and characterization of the tri-capped and mono-supported pseudo-Keggin-type tungstovanadophosphate: {PW4W5V3O40(VO)3[Cu(en)2]} |
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| Authors: | Jian Liu Jia-Ning Xu Ya-Bing Liu Yu-Kun Lu Jiang-Feng Song Xiao Zhang Xiao-Bing Cui Ji-Qing Xu Tie-Gang Wang |
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| Affiliation: | aCollege of Chemistry and State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Jilin Province, Changchun 130021, PR China |
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| Abstract: | A novel polyoxometalate [Cu(phen)2]3{PW4VIW5VV3IVO40(VIVO)3[Cu(en)2]} 4H2O 1 (en=ethylenediamine, phen=1,10-phenanthroline) has been synthesized hydrothermally and characterized by elemental analysis, IR, XPS, TG, EPR and single-crystal X-ray diffraction analysis. The crystal structure analysis shows that compound 1 contains a novel highly reduced tri-capped and mono-supported pseudo-Keggin-type heteropolyanion, {PW4VIW5VV3IVO40(VIVO)3[Cu(en)2]}6−, three [Cu(phen)2]2+ cations and four lattice water molecules. They are further linked to form three-dimensional supramolecular networks through extensive hydrogen bonding and π–π stacking interactions. Interestingly, the water dimer and terminal oxygen of the cluster polyanion constitute a beautiful supramolecular helix chain. The heteropolyanion is the first example of tri-capped and mono-supported pseudo-Keggin-type tungstovanadophosphate and the pH value is crucial for obtaining compound 1 in synthetic procedure. |
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| Keywords: | POMs Hydrothermal synthesis Tri-capped Keggin structure Tungstovanadophosphate Crystal structure |
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