Journal
JOURNAL OF INCLUSION PHENOMENA AND MACROCYCLIC CHEMISTRY
Volume 60, Issue 3-4, Pages 263-270Publisher
SPRINGER
DOI: 10.1007/s10847-007-9374-4
Keywords
cyclodextrin; niobocene; inclusion complex; PXRD; C-13 CP-MAS
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The possible inclusion complexes of Cp2NbCl2 into alpha-, beta-, and gamma-CD hosts have been investigated. The existence of a true inclusion complex in the solid state was confirmed by a combination of thermogravimetric analysis, FTIR, PXRD, and C-13 CP-MAS NMR spectroscopies. The solid-state results demonstrated that alpha-cyclodextrin does not form inclusion complexes with Cp2NbCl2 whereas beta- and gamma-cyclodextrins do form such complexes. PXRD, NMR, and thermal analysis showed that the organometallic molecules of Cp2NbCl2OH are included in the cavities of beta- and gamma-cyclodextrins, possibly adopting a symmetrical conformation in the complex, with each glucose unit in a similar environment. In solution, H-1 NMR experiments suggest that niobocene has a shallow penetration on the beta-CD leading to upfield shift on H-3 signal with a minor perturbation on the H-5 proton while for gamma-CD, both H-3 and H-5 are shifted upfield substantially. This suggests that niobocene penetrates deeper into the gamma-CD cavity than in the beta-CD cavity, as a result of the cavity size.
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