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Anomalous small-angle X-ray scattering was employed to monitor in situ the formation of colloidal Pt particles by the reaction of Pt(acac)2 and Al(CH3)3 in solution. An intermediate complex molecule was found to decompose to form stable Pt particles of 1.2 nm diameter with a monomodal particle size distribution. A network like correlation in the particle positions tends to build up by organic spacer molecules between stabilizing aluminum-organic shells.