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As part of our studies on the synthesis, structure and properties of crystalline metallaorganosiloxanes we present our investigations on the influences of electron donors on the structure of polyhedral organosiloxanes containing copper and alkali metal ions. Specifically, we report the synthesis of various organosiloxanes based on copper ions, a matrix, which are considered to be potential molecular magnets. The present work is devoted to the rebuilding of {M4[PhSi(O)O]12Cu4}·L (M = Na, K) under the influence of DMF and THF. It has been found that Cu/M-phenylsiloxanes consisting of one stereoregular organosiloxanolate ring [ RSi(O)O ]12 fixed on a metal-ion matrix are reorganized under the influence of strong electron donors. Phenylsiloxane complexes form a sandwich like molecular structure containing copper and Na or K (or only copper (II) ions) depending on the solvent, ligands and reaction conditions.