We are interested in making layered metal halide inorganic-organic perovskite hybrids. They make up an interesting class of compounds to study due to their unique optical and electronic properties. The inter-layer spacing of these materials can be changed by varying the organic component, which is either an alkyl or aryl ammonium cation. (See figure below, structure from Cambridge Structural Database Refcode BEDYEP) Currently, we are investigating the ability to intercalate small organic guest molecules into the solid host framework by sonication. The intercalation of guest molecules depending on the nature of the organic substitute (alkyl vs aryl) will be discussed. The products are mainly characterized by thermal analysis (TGA & DSC), X-ray diffraction (XRD & PXRD) and surface analysis (TEM & SEM).