The first part of the thesis includes examining inorganic/organic hybird layered solids, also termed “clay mimics.” Transmission and scanning electron microscopy techniques were used to characterize particles before and after intercalation of pyridine based groups. The particle sizes, shape, and surface morphology were studied for a control and five intercalated species, and evidence for change in particle size and shape was found. The second part of the thesis involves a study in the area of inorganic-organic perovskite networks. Variations in the nature of the cationic organic portion as well as the divalent metal halides have been used to try to better predict the type of network formed. In the work reported here, metal halide and ortho-substituted anilines are combined to relate metal halide network dimensionalities to the steric demands of the ortho- substituents on aniline species. The study involved divalent d10 metal halides, and the halides used were: chloride, iodide, and bromide. The anilines used had varied substituents ortho- to the ammonium group, in order to encompass a wide range of substituents. The goal of the study was to determine if the nature of the ortho-substituent caused consistent effects on the resulting crystal structure. Crystals were grown using slow evaporation techniques and viable crystals were characterized using single crystal X-ray diffraction.