[Cd<sub>3</sub>(H<sub>2</sub>O)<sub>3</sub>((O<sub>3</sub>PCH<sub>2</sub>)<sub>2</sub>NH−CH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>−COOH)<sub>2</sub>]·11H<sub>2</sub>O: A Layered Cadmium Phosphonate with Reversible Dehydration/Hydration Properties
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In a recent systematic study on the influence of the reaction temperature on the structure formation in the system CdCl2/H(HO3PCH2)2NH−CH2C6H4−COOH (H5L) /NaOH, [Cd3(H2O)3((O3PCH2)2NH−CH2C6H4−COOH)2]·11H2O was obtained as a microcrystalline compound. We have now been able to elucidate the structure from single-crystal data: triclinic, P1̄; a = 5.4503(9), b = 12.880(2), and c = 16.417(3) Å; α = 67.841(6)°, β = 80.633(6)°, γ = 87.688(8)°, V = 1052.9(3) Å3; Z = 1; R1 = 0.1143, R2 = 0.2108 (all data); 0.0705, 0.1823 ((I > 2σ(I))). The structure of [Cd3(H2O)3((O3PCH2)2NH−CH2C6H4−COOH)2]·11H2O is built up of cadmium phosphonate layers connected by water-mediated hydrogen bonds between aryl-carboxylic acid groups and water molecules coordinated to Cd2+ ions of adjacent layers (C−OH···H2O···H2O−Cd2+). The title compound was characterized by IR spectroscopy and energy dispersive X-ray, elemental, and thermogravimetric analyses. Furthermore, temperature-dependent X-ray diffraction data are presented. [Cd3(H2O)3((O3PCH2)2NH−CH2C6H4−COOH)2]·11H2O can be reversibly dehydrated, and mechanical stress and grinding in the presence of water leads to the intercalation of additional water molecules.
