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Braga, Susana S.
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article
Structural studies of [CpMoL2(CO)2]+ (L = NCMe, L2 = 2,2′-biimidazole) complexes and their inclusion compounds with cyclodextrins
Abstract
<p>Protonation of [CpMo(η<sup>3</sup>-C<sub>3</sub>H<sub>5</sub>)(CO) <sub>2</sub>] followed by addition of acetonitrile or 2,2′-biimidazole (H<sub>2</sub>biim) gave the complexes [CpMo(NCMe)<sub>2</sub>(CO) <sub>2</sub>](BF<sub>4</sub>) (1) and [CpMo(H<sub>2</sub>biim)-(CO) <sub>2</sub>](BF<sub>4</sub>) (2) in good yields. The structures of 1 and 2 were determined by single-crystal X-ray diffraction in the orthorhombic Pbca and triclinic P1 space groups, respectively. Both complexes have similar metal ion coordination environments, which can be envisaged as slightly distorted pseudosquare pyramids, a coordination geometry commonly compared with a four-legged piano stool. The two complexes were immobilised in native and permethylated β-cyclodextrins (β 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), <sup>13</sup>C(<sup>1</sup>H) 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) <sub>3</sub>] (X = Cl, CH<sub>2</sub>CONH<sub>2</sub>), featuring columns in which the macrocycles are arranged along the b axis in a tilted fashion.</p>