An efficient method for the deposition of ionic platinum species PtO x onto a TiO 2 surface was developed on the basis of light-induced activation of the [Pt(NO 3 ) 6 ] 2− anion. The deposited PtO x species with an effective Pt oxidation state between +4 and +2 have an oxygen-made environment and include single ion centers {PtO n } and polyatomic ensembles {Pt n O m } connected to a TiO 2 surface with Pt−O−Ti bonds. The resulting PtO x /TiO 2 materials were tested as photocatalysts for the hydrogen evolution reaction (HER) from a water ethanol mixture and have shown uniquely high activity with the rate of H 2 evolution achieving 11 mol h −1 per gram of Pt, which is the highest result for such materials reported to date. A combination of spectral methods shows that, under HER conditions, reduction of the supported PtO x species leads to the formation of well-dispersed nanoparticles of metallic platinum attached on the surface of TiO 2 by Ti−O−Pt bonds. The high activity of the PtO x /TiO 2 materials is believed to result from a combination of uniform distribution of small platinum nanoparticles over the titania surface and their close interaction with TiO 2 .