Optimum conditions for the formation of stable dispersions of Na,TaS, in N-methylformamide-water mixtures have been determined. Under appropriate conditions, the addition of large guest cations to these dispersions results in instantaneous flocculation and the formation of ordered intercalation compounds. The method has been used to prepare intercalation compounds with cobaltocenium cations, A1 and Ga polyoxycations, and a large iron-sulfur cluster cation. Powder X-ray diffraction data from oriented films of the samples were used to obtain one-dimensional projr, actions of the electron density perpendicular to the layers. These electron-density maps provided information on the orientation of the guest species in the interlamellar space.