Nanoscale microreactor containing (5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-4,11-diene) nickel(II) were successfully have been prepared by the template condensation of tris(ethylenediamine)nickel(II) complex with acetone within the nanodimensional pores of zeolite Y. This complex were entrapped in the supercage of zeolite Y by a two-step process in the liquid phase (i) inclusion of a nickel(11) precursor complex [Ni(en)(3)](2+)-NaY and (ii) in situ template reaction of the nickel(II) precursor complex with the acetone. The new material [Ni(Me-6[14]ane N-4](2+)-NaY characterized by several techniques: chemical analysis and spectroscopic methods(FT-IR, UV-vis, XPS, XRD, BET, DRS). Analysis of the data indicates that the nickel(II) complex are encapsulated in the nanodimensional pores zeolite and exhibit different from the free this of complex, which can arise from distortions caused steric effects due to the presence of sodium cations, or from interactions with the zeolite matrix. The host-guest nanoscale tetraaza macrocycle was found catalytic activity. Cyclohexene was catalytically oxidized in the presence of molecular oxygen and [Ni(Me-6[14]ane N-4)](2+)-NaY in the absence of solvent at 70degreesC, affording 2-cyclohexene-1-ol and 2-cyclohexene-1-one. The effect of temperature, and the amount of [Ni(Me-6[14]ane N-4)](2+)-NaY used on the catalytic activity and product selectivity were discussed. (C) 2004 Elsevier B.V. All rights reserved.