Folded sheet mesoporous material FSM-16 has been synthesized and loaded with 3, 6 & 9 wt% of iron, copper or silver. The powder X-ray diffraction and N₂ sorption characterizations show that the parent FSM-16 and the prepared nine catalysts have well-order hexagonal meso-structures. However, partial loss of crystallinity is only observed in catalysts containing 6 and 9 wt % iron. BET surface area, pore volume and pore diameter, d (100) spacing and average crystal size values decreased for all the catalysts containing 3 wt % metal, the decrease is in the order Fe< Cu< Ag. According to temperature programmed reduction, different metal phases are detected. In infrared spectra, bands at 1637, 955, 800 and 620 cm^-1 are greatly affected by metal loading and a new band is only observed at 1385 Cm^-1in the metal/FSM-16 catalysts.