Synthesis and characterization of the inclusion compound of a ferrocenyldiimine dioxomolybdenum complex with heptakis-2,3,6-tri-O-methyl-beta-cyclodextrin
authors Petrovski, Z; Braga, SS; Santos, AM; Rodrigues, SS; Goncalves, IS; Pillinger, M; Kuhn, FE; Romao, CC
nationality International
journal INORGANICA CHIMICA ACTA
author keywords molybdenum; ferrocene derivatives; diimine ligands; permethylated beta-cyclodextrin; inclusion compounds; oletin epoxidation
keywords LEWIS-BASE ADDUCTS; MOLYBDENUM-CATALYZED EPOXIDATION; TRANSITION-METAL-COMPLEXES; MAIN-GROUP ELEMENTS; OLEFIN EPOXIDATION; BETA-CYCLODEXTRIN; EFFICIENT EPOXIDATION; HYDROGEN-PEROXIDE; CRYSTAL-STRUCTURE; MULTIPLE BONDS
abstract A dioxomolybdenum(VI) complex bearing the diimine ligand NN'-bis(ferrocenylmethylene)ethylenediamine (FcNN) has been prepared in good yield by the reaction of FcNN with MoO(2)Cl(2)(THF)(2)- One isomeric form was identified by (1)H NMR (including NOE experiments), corresponding to the cis,cis geometry with respect to the C=N bonds of the free ligand. The polynuclear complex was immobilized in permethylated beta-cyclodextrin (TRIMEB) by addition of the guest to a solution of TRIMEB in a mixture of dichloromethane and nitromethane. Removal of the solvent led to the isolation of an inclusion compound with a 2:1 host:guest stoichiometry. For comparison, an inclusion compound containing just the ligand FcNN and TRIMEB was prepared using a similar method. The products were characterized in the solid state by powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), FT-IR and (13)C CP MAS NMR spectroscopy. UV-Vis measurements were also carried out in solution. Both the complex MoO(2)Cl(2)(FcNN) and its inclusion compound with TRIMEB catalyze with high selectivity the liquid phase epoxidation of cyclooctene using tert-butyl hydroperoxide (TBHP) as the oxidant. In general, the catalytic behavior of the Mo(VI) complex was not markedly affected by encapsulation in TRIMEB, although observed activities were slightly lower. (c) 2004 Elsevier B.V. All rights reserved.
publisher ELSEVIER SCIENCE SA
issn 0020-1693
year published 2005
volume 358
issue 4
beginning page 981
ending page 988
digital object identifier (doi) 10.1016/j.ica.2004.11.032
web of science category Chemistry, Inorganic & Nuclear
subject category Chemistry
unique article identifier WOS:000227507800016
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journal impact factor 2.304
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