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Investigations to elucidate the structures of the cobalt(III) and manganese(III) complexes of tetra(p-sulfonatophenyl)porphinate anions (M(III)TSPP; M = Co and Mn), intercalated in Mg-Fe/Cl and Mg-Al/Cl layered double hydroxides (LDHs) have been carried out. Powder X-ray diffraction analysis, IR and UV-vis diffuse reflectance spectroscopy of Co(III)TSPP and Mn(III)TSPP intercalated into the interlayer spaces of LDH resulted in their perpendicular alignment against the host layers in the plane of the hybrid. [ABSTRACT FROM AUTHOR]