Mg-Al layered double hydroxide (LDH) intercalated with glycinate anions was synthesized through co-precipitation and exfoliated in formamide and the single-layer suspension was reacted with an aqueous iron porphyrin (FeTDFSPP) solution. The new composite was characterized by powder X-ray diffraction, UV-vis, FTIR, and electron paramagnetic spectroscopies and thermal analyses (simultaneous TG/DSC). The analyses demonstrated that glycinate anions continue to be intercalated and the anionic iron porphyrin is adsorbed at the surface of the layered double hydroxide crystals. (C) 2003 Elsevier Inc. All rights reserved.