resumo
Protonation of [CpMo(eta(3)-C3H5)(CO)(2)] followed by addition of acetonitrile or 2,2'-biimidazole (H(2)biim) gave the complexes [CpMo(NCMe)(2)(CO)(2)](BF4) (1) and [CpMo(H(2)biim)(CO)(2)](BF4) (2) in good yields. The structures of 1 and 2 were determined by single-crystal X-ray diffraction in the orthorhombic Pbca and triclinic P (1) over bar space groups, respectively. Both complexes have similar metal ion coordination environments, which can be envisaged as slightly distorted pseudo-square pyramids, a coordination geometry commonly compared with a four-legged piano stool. The two complexes were immobilised in native and permethylated beta-cyclodextrins (beta CD and TRIMEB) by methods tailored according to the stabilities and solubilities of the individual components and this gave four adducts with a 1:1 host/guest stoichiometry. The formation of true inclusion compounds was supported by powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), C-13{H-1} CP/MAS NMR and FTIR spectroscopy. In the case of the TRIMEB adduct containing complex 1, the crystal packing arrangement is markedly similar to that previously reported for the corresponding 1:1 TRIMEB adducts of the neutral guests [CPMoX(CO)(3)] (X = Cl, CH2CONH2), featuring columns in which the macrocycles are arranged along the b axis in a tilted fashion. ((c) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006).
palavras-chave
HALF-SANDWICH COMPLEXES; C-13 CHEMICAL-SHIFTS; X-RAY-DIFFRACTION; BETA-CYCLODEXTRIN; BIOORGANOMETALLIC CHEMISTRY; CARBONYL-COMPLEXES; ORGANOMETALLIC COMPLEXES; CRYSTAL-STRUCTURE; SOLID-STATE; PHARMACEUTICAL APPLICATIONS
categoria
Chemistry
autores
Pereira, CCL; Braga, SS; Paz, FAA; Pillinger, M; Klinowski, J; Goncalves, IS
nossos autores
Filipe Alexandre Almeida Paz
Investigador Principal
Isabel Maria de Sousa Gonçalves
Professor associado