A wide range of pore widths and V/Si ratios in the vanadium-containing mesoporous molecular sieve [V]-MCM-41 was synthesized with surfactants of different chain length and variation of the TEAOH and vanadium contents in the synthesis gel. An increase in the content of alkali chlorides (NaCl and KCl) resulted in a decrease of the repeat distance, a 0 , comparable to that produced with a decrease in the template chain length of two carbon atoms. The vanadium content of [V]-MCM-41 was found to be dependent not only on the amount of VOSO 4 .5H 2 O, but also on the sequence of addition of the gel components and the presence of alkali metal chlorides (NaCl and KCl).