Zn-Al layered double hydroxides (LDHs) intercalated byterephthalate (TPH) and biphenyl-4,4'-dicarboxylate (BPH) anions have beensynthesized by direct co-precipitation from aqueous solution. The Zn/Al ratio inthe final materials was 1.8. The products were characterized by powder X-raydiffraction, thermogravimetric analysis, FTIR and FT Raman spectroscopy, and MASNMR spectroscopy. The basal spacing for the TPH-LDH intercalate was 14.62Å, indicating that the guest anions stack to form a monolayer with thearomatic rings perpendicular to the host layers. For the LDH intercalatecontaining BPH anions, a basal spacing of at least 19.2 Å would beexpected if the anions adopted an arrangement similar to that for the TPHanions. The observed spacing was 18.24 Å, suggesting that the anions aretilted slightly with respect to the host layers.