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Fax: + 7 (095) 932 8846Copper-and (copper,aluminum)-containing organosiloxanes were studied by spectroscopic methods. It was found that in organometallosiloxanes (OMS) with an increased content of copper (Si/Cu = 1 : 1), Cu atoms are rather uniformly distributed in the siloxane matrix. All compounds under study are complexes characterized by d--d-transitions in copper ions with a constant coordination number of the metal atom. The intensity of the d--d-transition band increases as the copper content increases. ESR studies demonstrated that in the compounds under consideration, a change from mononuclear paranaagnetic centers to clusters, in which copper ions are linked by strong spin-exchange interactions, occurs as the copper content increases. The catalytic activity of the above-mentioned compounds in isomerization reactions of 3,4-dichlorobutene-I was studied. It was found that copper atoms serve as catalytic centers.