Rigid meta-phosphonobenzoic acid 2 possesses two functional groups (phosphonic acid and carboxylic acid) both having the aptitude to associate with a metallic precursor to form hybrid materials. The hydrothermal reactions of compound 2 with MnCl 2 ·4H 2 O or Co(NO 3 ) 2 ·6H 2 O produce, respectively, the isostructural layered materials M(H 2 O)-(PO 3 C 6 H 4 CO 2 H) (3, M = Mn; 4, M = Co) characterized by the presence of the free carboxylic acid groups in the interlayer space (space group P2 1 /n). The reaction of Zn(CH 3 COO) 2 · 2H 2 O with 2 produces two different materials depending on the pH of the reaction media. At low pH (pH Ͻ 4.1), the iso-
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