A method for producing oriented periodic mesoporous organosilica filaments within the confined channels of anodic alumina membranes is presented. Deposition of the mesoporous filaments were performed under a variety of conditions, which favoured the evaporation induced self-assembly of the mesoporous material. The experimental conditions examined included different drying rates, over a range of humidity values, and sol compositions, e.g. varying the amount of the organosilica component. The deposition process was followed in situ by time resolved small angle X-ray scattering which was essential for evaluating the formation mechanism of the mesophase structures. Through careful control of the deposition environment, the structure and orientation of the mesoporous filaments could readily be varied. (C) 2009 Elsevier Inc. All rights reserved.