NDLI: Solid-State NMR Characterization of Wilkinson’s Catalyst Immobilized in Mesoporous SBA-3 Silica

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Solid-State NMR Characterization of Wilkinson’s Catalyst Immobilized in Mesoporous SBA-3 Silica

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Yeping, Xu Buntkowsky, Gerd Grünberg, Anna Breitzke, Hergen
Description	Author Affiliation: Grünberg A ( Eduard-Zintl-Institut für Anorganische und Physikalische Chemie, Technische Universität Darmstadt, Petersenstr. 20, 64287 Darmstadt, Germany.)
Abstract	The Wilkinson’s catalyst $[RhCl(PPh_{3})_{3}]$ has been immobilized inside the pores of amine functionalized mesoporous silica material SBA-3 and The structure of the modified silica surface and the immobilized rhodium complex was determined by a combination of different solid-state NMR methods. The successful modification of the silica surface was confirmed by $^{29}Si$ CP-MAS NMR experiments. The presence of the $T_{n}$ peaks confirms the successful functionalization of the support and shows the way of binding the organic groups to the surface of the mesopores. $^{31}P-^{31}P$ J-resolved 2D MAS NMR experiments were conducted in order to characterize the binding of the immobilized catalyst to the amine groups of the linkers attached to the silica surface. The pure catalyst exhibits a considerable $^{31}P-^{31}P$ J-coupling, well resolvable in 2D MAS NMR experiments. This J-coupling was utilized to determine the binding mode of the catalyst to the linkers on the silica surface and the number of triphenylphosphine ligands that are replaced by coordination bonds to the amine groups. From the absence of any resolvable $^{31}P-^{31}P$ J-coupling in off-magic-angle-spinning experiments, as well as slow-spinning MAS experiments, it is concluded, that two triphenylphosphine ligands are replaced and that the catalyst is bonded to the silica surface through two linker molecules.
ISSN	09476539
e-ISSN	15213765
Journal	Chemistry - A European Journal
Issue Number	23
Volume Number	16
Language	English
Publisher	Wiley-VCH;ChemPubSoc Europe
Publisher Date	2010-06-18
Publisher Place	Germany
Access Restriction	Open
Subject Keyword	Magnetic Resonance Spectroscopy Chemistry Organometallic Compounds Rhodium Silicon Dioxide Catalysis Ligands Molecular Structure Research Support, Non-U.S. Gov't
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Catalysis

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