A new ordered mesoporous organosilica has been synthesized through co-condensation of 1,1′-bis[2-(triethoxylsilyl)ethyl]ferrocene and tetraethyl orthosilicate under basic conditions using supramolecular templates of cetyltrimethylammonium bromide as structure directing agents. The templates were removed through solvent extraction to yield the ferrocene-containing ordered mesoporous organosilicas. The pore diameter, BET surface area, and pore volume of the extracted material were 2.2 nm, 1,085 m2/g and 0.67 cm3/g, respectively. The material also has been characterized by XRD, TEM, FT-IR, UV–Vis DRS, solid state 29Si MAS NMR and 13C CP-MAS NMR etc. In the reaction of benzene hydroxylation to phenol, the ferrocene-containing ordered mesoporous materials show a comparable activity with the homogeneous ferrocene catalyst, giving 20.2% of yield and 65.3% of selectivity for phenol.