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Controlled modification of the inorganic and organic bricks in an Al-based MOF by direct and post-synthetic synthesis routes

Ahnfeldt, Tim, Gunzelmann, Daniel, Wack, Julia, Senker, Jurgen and Stock, Norbert 2012, Controlled modification of the inorganic and organic bricks in an Al-based MOF by direct and post-synthetic synthesis routes, CrystEngComm, vol. 14, pp. 4126-4136.

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Title Controlled modification of the inorganic and organic bricks in an Al-based MOF by direct and post-synthetic synthesis routes
Author(s) Ahnfeldt, Tim
Gunzelmann, Daniel
Wack, Julia
Senker, Jurgen
Stock, Norbert
Journal name CrystEngComm
Volume number 14
Start page 4126
End page 4136
Total pages 11
Publisher Royal Society of Chemistry
Place of publication London, Eng.
Publication date 2012
ISSN 1466-8033
Summary Four new porous CAU-1 derivatives CAU-1–NH2 ([Al4(OH)2(OCH3)4(BDC–NH2)3]·xH2O, BDC–NH22− = aminoterephthalate), CAU-1–NH2(OH) ([Al4(OH)6(BDC–NH2)3]·xH2O), CAU-1–NHCH3 ([Al4(OH)2(OCH3)4(BDC–NHCH3)3]·xH2O) and CAU-1–NHCOCH3 ([Al4(OH)2(OCH3)4(BDC–NHCOCH3)3]·xH2O) all containing an octameric [Al8(OH)4+y(OCH3)8−y]12+ cluster, with y = 0–8, have been obtained by MW-assisted synthesis and post-synthetic modification. The inorganic as well as the organic unit can be modified. Heteronuclear 1H–15N, 1H–13C and homonuclear 1H–1H connectivities determined by solid-state NMR spectroscopy prove the methylation of the NH2 groups when conventional heating is used. Varying reaction times and temperatures allow controlling the degree of methylation of the amino groups. Short reaction times lead to non-methylated CAU-1 (CAU-1–NH2), while longer reaction times result in CAU-1–NHCH3. CAU-1–NH2 can be modified chemically by using acetic anhydride, and the acetamide derivative CAU-1–NHCOCH3 is obtained. Thermal treatment permits us to change the composition of the Al-containing unit. Methoxy groups are gradually exchanged by hydroxy groups at 190 °C in air. Solid-state NMR spectra unequivocally demonstrate the presence of the amino groups, as well as the successful post-synthetic modification. Furthermore 1H–1H correlation spectra using homonuclear decoupling allow the orientation of the NHCOCH3 groups within the pores to be unravelled. The influence of time and temperature on the synthesis of CAU-1 was studied by X-ray powder diffraction, elemental analyses, and 1H liquid-state NMR and IR spectroscopy.
Language eng
Field of Research 039999 Chemical Sciences not elsewhere classified
Socio Economic Objective 970103 Expanding Knowledge in the Chemical Sciences
HERDC Research category C1.1 Refereed article in a scholarly journal
Copyright notice ©2012, Royal Society of Chemistry
Persistent URL http://hdl.handle.net/10536/DRO/DU:30064423

Document type: Journal Article
Collections: Population Health
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