Journal
JOURNAL OF ORGANOMETALLIC CHEMISTRY
Volume 693, Issue 18, Pages 3021-3028Publisher
ELSEVIER SCIENCE SA
DOI: 10.1016/j.jorganchem.2008.06.023
Keywords
cyclodextrins; inclusion compounds; ruthenium complexes; powder X-ray diffraction
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The complex [Ru([9]aneS(3))(bpy)Cl]Cl (bpy = 2,2'-bipyridine) was immobilised in plain beta-cyclodextrin (beta-CD) and permethylated beta-CD (TRIMEB) to yield two adducts with a 1: 1 host: guest stoichiometry. The adducts were studied by powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), (13)C{(1)H} CP/MAS NMR and vibrational spectroscopy (FT-IR and Raman). Results support the formation of stable supramolecular adducts with a proposed geometry in which the coordinated bypiridine fragment of the guest is partially included in the host cavities, and the bulky [9] aneS(3) fragment protrudes out to the interstitial spaces. A packing mode is proposed for [Ru([9]aneS(3))(bpy)Cl]Cl. TRIMEB, obtained by Monte Carlo optimisation of the XRD data. TRIMEB molecules are stacked in tilted channels, with the voluminous part of the guest molecules in the inter-channel space. The behaviour of [Ru([9]aneS(3))(bpy)Cl] Cl upon CD encapsulation and the chloride ligand hydrolysis process in solution for all compounds were studied in detail by Raman spectroscopy. (C) 2008 Elsevier B. V. All rights reserved.
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