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Structural Studies of β‐Cyclodextrin and Permethylated β‐Cyclodextrin Inclusion Compounds of Cyclopentadienyl Metal Carbonyl Complexes

2006; Wiley; Volume: 2006; Issue: 8 Linguagem: Inglês

10.1002/ejic.200501006

1099-0682

Susana S. Braga, Filipe A. Almeida Paz, Martyn Pillinger, João Seixas, Carlos C. Romão, Isabel S. Gonçalves,

Crystallization and Solubility Studies

Abstract [CpM(CO) n Cl] complexes with M = Fe ( n = 2) and Mo ( n = 3) have been immobilised in plain β‐cyclodextrin (β‐CD) and permethylated β‐CD (TRIMEB) by methods tailored according to the stabilities and solubilities of the individual components. Four adducts were obtained with a 1:1 host/guest stoichiometry. The compounds were studied by powder X‐ray diffraction (XRD), thermogravimetric analysis (TGA), 13 C{ 1 H} CP/MAS NMR and FTIR spectroscopy. A comparison of the experimental powder XRD data for the TRIMEB/[CpMo(CO) 3 Cl] inclusion compound with reference patterns revealed that the crystal packing is very similar to that reported previously for a TRIMEB/ethyl laurate inclusion compound. The unit‐cell parameters refined to a = 14.731, b = 22.476, c = 27.714 Å (volume = 9176.3 Å 3 ), and the space group was confirmed as P 2 1 2 1 2 1 . A hypothetical structural model of the inclusion compound was subsequently obtained by global optimisation using simulated annealing. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006)