Host–guest interactions between niobocene dichloride and α-, β-, and γ-cyclodextrins: preparation and characterization

  • Alexis Morales
  • Jochem Struppe
  • Enrique Meléndez
Original Article

Abstract

The possible inclusion complexes of Cp2NbCl2 into α-, β-, and γ-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 13C CP-MAS NMR spectroscopies. The solid-state results demonstrated that α-cyclodextrin does not form inclusion complexes with Cp2NbCl2 whereas β- and γ-cyclodextrins do form such complexes. PXRD, NMR, and thermal analysis showed that the organometallic molecules of Cp2NbCl2OH are included in the cavities of β- and γ-cyclodextrins, possibly adopting a symmetrical conformation in the complex, with each glucose unit in a similar environment. In solution, 1H NMR experiments suggest that niobocene has a shallow penetration on the β-CD leading to upfield shift on H-3 signal with a minor perturbation on the H-5 proton while for γ-CD, both H-3 and H-5 are shifted upfield substantially. This suggests that niobocene penetrates deeper into the γ-CD cavity than in the β-CD cavity, as a result of the cavity size.

Keywords

Cyclodextrin Niobocene Inclusion complex PXRD 13C CP-MAS 

Supplementary material

10847_2007_9374_MOESM1_ESM.doc (871 kb)
(DOC 871 kb)

Copyright information

© Springer Science+Business Media B.V. 2007

Authors and Affiliations

  • Alexis Morales
    • 1
  • Jochem Struppe
    • 2
  • Enrique Meléndez
    • 1
  1. 1.Department of ChemistryUniversity of Puerto RicoMayaguezUSA
  2. 2.Brucker Biospin CorporationBillericaUSA

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