Layered semicrystalline silico-alumino-titanate (Si-t&Ti) mixed oxides were synthesized by a modified sol-gel method with hydrothermal synthesis temperatures less than 200"C and autogenic pressure. The solid products are semicrystalline materials with a surface area of 136-367 m2/g and a monomodal pore size distribution with an average pore diameter of 3.6-4.7 nrn. The catalytic activity for pyrene hydrogenation in a batch reactor at 300"C and 500 psig was determined for sulfided Ni-Mo supported on the Si-Al-Ti mixed oxide. The activity was a fiction of the support composition the heat treatment before and after loading the active metals, the addition of organic templates, and difl?erentmethods of metal loading. The most active sulfided Ni-Mo/Si-Al-Ti catalyst has an activity in the same range as the commercial catalyst, Shell 324, but the metal loading is 37% less than the commercial catalyst.