Recently there has been much interest in reacting vanadium oxides hydrothermally with cationic surfactants to form novel layered compounds. A series of new transition metal oxides, however, has also been formed at or near room temperature in open containers. Synthesis, characterization, and proposed mechanisms of formation are the focus of this work. Low temperature reactions of vanadium pentoxide and ammonium (DTA) transition metal oxides with long chain amine surfactants, such as dodecyltrimethylammonium bromide yielded interesting new products many of which are layered phases. DTA4H2V10O28•8H2O, a layered highly crystalline phase, is the first such phase for which a single crystal X-ray structure has been determined. The unit cell for this material was found to be triclinic with space group P 1 and dimensions a=9.895(1)Å, b=11.596(1)Å, c=21.924(1)Å, α=95.153(2)°, β=93.778(1)°, and γ= 101.360(1)°. Additionally, we synthesized a dichromate phase and a manganese chloride layered phase, with interlayer spacings of 26.8Å, and 28.7Å respectively. The structure, composition, and synthesis of the vanadium compound are described, as well as the synthesis and preliminary characterization of the new chromium and manganese materials.