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Issue 33, 2014
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Immobilization of Co-containing polyoxometalates in MIL-101(Cr): structural integrity versus chemical transformation

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Abstract

The encapsulation of three different cobalt substituted polyoxometalates (POMs) within the mesoporous chromium(III) terephthalate MIL-101(Cr) metal–organic framework (MOF) was studied by a simple and green impregnation method using water. The POM@MIL composite materials were fully characterized by EDX, XRPD, IR, MAS NMR and N2 porosimetry measurements. The encapsulated POMs were then extracted by an exchange procedure using a LiCl solution. 31P NMR spectroscopy is the key experiment which indicates that the monosubstituted Keggin anion [PW11CoO39(H2O)]5− (PW11Co) and the sandwich-type anion [(PW9O34)2Co4(H2O)2]10− (P2W18Co4) can be encapsulated and extracted without degradation, neither of the POM nor of the MOF, while the hybrid sandwich-type POM [(PW9O34)2Co7(OH)2(H2O)4(O3PC(O)(C3H6NH3)PO3)2]14− (Co7-Ale) evolves into P2W18Co4 inside the cavities of the mesoporous material. The PW11Co Keggin anion is the most quantitatively uploaded and the most easily extracted anion. 31P MAS-NMR spectroscopy further suggests that this anion is more mobile inside the cavities of the MOF than the P2W18Co4 POM.

Graphical abstract: Immobilization of Co-containing polyoxometalates in MIL-101(Cr): structural integrity versus chemical transformation

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Publication details

The article was received on 30 Apr 2014, accepted on 21 Jun 2014 and first published on 24 Jun 2014


Article type: Paper
DOI: 10.1039/C4DT01286K
Citation: Dalton Trans., 2014,43, 12698-12705
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    Immobilization of Co-containing polyoxometalates in MIL-101(Cr): structural integrity versus chemical transformation

    W. Salomon, F. Yazigi, C. Roch-Marchal, P. Mialane, P. Horcajada, C. Serre, M. Haouas, F. Taulelle and A. Dolbecq, Dalton Trans., 2014, 43, 12698
    DOI: 10.1039/C4DT01286K

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