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, including adsorbate-induced changes to the framework.A family of nanoclusters, [Ln33(EDTA)12(OAc)2(CO3)4(μ3-OH)36(μ5-OH)4(H2O)38]·OAc·xH2O (x ≈ 50, Ln = Sm for 1; x ≈ 70, Ln = Eu for 2) and [Gd32(EDTA)12(OAc)2(C2O4)(CO3)2(μ3-OH)36(μ5-OH)4(H2O)36]·H2O) (x ≈ 70 for 3; H4EDTA = ethylene diamine tetraacetic acid), was prepared through the assembly of repeating subunits under the action of an anion template. The analysis of the structures showed that compounds 1 and 2 containing 33 Ln3+ ions were isostructural, which were constructed