The novel zirconatetraferrocenylcyclotrisiloxane Cp2Zr(OSiFc2)2O (6), dizirconatetraferrocenylcyclotetrasiloxane [Cp2Zr(OSiFc2)O]2 (7), boratetraferrocenylcyclotrisiloxane (C6H5)B(OSiFc2)2O (8), and diboratetraferrocenylcyclotetrasiloxane [(C6H5)B(OSiFc2)O]2 (9) with ferrocenyl (Fc = Fe(η-C5H4)(η-C5H5)) substituents at silicon have been prepared from the reactions of Cp2Zr(NMe2)2 and PhBCl2 with diferrocenylsilanediol Fc2Si(OH)2 (3) and tetraferrocenyldisiloxanediol [Fc2SiOH]2O (5). The compounds were characterized by mass spectrometry, elemental analysis, UVvis, IR, Raman, and multinuclear NMR spectroscopy, as well as single crystal X-ray diffraction. Thermogravimetric analysis and differential scanning calorimetry investigation of 69 showed that the cycles decompose before they can undergo any thermal ring-opening polymerization. In addition, no polymerization was detected in the presence of either KOSiMe3 or HOTf. The bulky ferrocenyl substituents on the Si atoms are likely to be at least partially responsible for the inability of these heterocycles to undergo ring-opening polymerization. Key words: heterocyclosiloxanes, ferrocenyl.