The acid-hydrolysis of a bismethyldiethoxysilylated para-phenylene-bridged derivative, (EtO)(2)MeSi(CH2)(3)NHCONH(C6H4)NHCONH(CH2)(3)SiMe(OEt)(2), with urea groups has been performed in pure aqueous medium. The scanning electron microscopy (SEM) analysis of the resulting insoluble solid revealed plate-like forms. A lamellar structure was determined from the powder X-ray diffraction (PXRD) studies with a sharp peak at 21.1 angstrom. The solid state CP-MAS NMR spectra (Si-29 and C-13) of the bridged siloxane hybrid exhibit a moderately condensed material with complete preservation of the Si-C bonds throughout the hybrid network.