A series of layered titanates containing in the interlayer space tris(2,2'-bipyndyl)ruthenium(II) [Ru(bpy)(3)(2 center dot center dot center dot)] or methyl viologen (MV2 center dot) or both has been prepared and characterized by elemental analyses. XRD, and optical and vibrational spectroscopy Incorporation of Ru(bpy)(3)(2+) and MV2+ is confirmed by the increase of the distance between the titanate layers. The presence of Ru(bpy)(3)(2 center dot) in the material is also revealed in optical spectroscopy where the ligand to metal charge transfer band appearing at 460 nm is observed Also incorporation of MV2+ leads to the observation of the charge transfer complex band with the titanate host from 350 to 650 nm. These solids are active for the photocatalytic hydrogen generation from water when colloidal platinum as catalyst and EDTA as sacrificial electron donor are present in the solution The maximum efficiency was obtained for a solid consisting of layered titanate containing a 102 wt % loading of Ru(bpy)(3)(2-) incorporated in the titanate layers and MV2+ and Pt nanoparticles in the aqueous solution. This heterogeneous system produced about one-half the hydrogen generated for the conventional homogeneous system where all the components [RLi(bpy)(3)(2+), MV2+, Pt, and EDTA] are in solution, with the advantage that it can be used as film or recovered by filtration from the aqueous medium (C) 2010 Elsevier Inc. All rights reserved