Spirohomofullerenes were synthesized by cycloaddition of cage and polycyclic diazoalkanes generated in situ by oxidation of hydrazones of camphor, 2-adamantanone, and cholestane-3-one to C-60 fullerene in the presence of the Pd(acac)(2)-2PPh(3)-4Et(3)Al three-component catalyst. It was found that the spiro-homofullerenes obtained from hydrazones of 2-adamantanone and cholestane-3-one and C-60 fullerene do not undergo thermal isomerization to the corresponding spiro-methanofullerenes.