Bifunctional periodic mesoporous organosilicas (BPMOs) with thiopliene-and isocyanurate-bridging groups were prepared by one-pot co-condensation of 2,5-bis(triethoxysilyl)thiophene and tris[3-(trimethoxysilyl)propyl]isocyanurate precursors in the presence of a poly(ethylene oxide)- poly(DL-lactic acid-co-glycolic acid)-poly(ethylene oxide) (PEO-PLGA-PEO) triblock copolymer under acidic conditions. The resulting BPMOs exhibited 2D hexagonal ordering (p6mm), large mesopores of similar to 7.7 nm, and high BET surface area (similar to 600-700 m(2)/g). C-13 CP-MAS and Si-29 MAS NMR studies confirmed the presence of thiophene and isocyanurate bridging groups inside the framework of pore walls with the relative content reflecting the synthesis gel composition. Additional quantitative estimation was provided by N and S elemental analysis. Thermogravimetric analysis showed the thiophene-isocyanurate BPMOs are stable up to 250 degrees C in flowing air and up to 400 degrees C in flowing nitrogen.