A series of new chainlike polyoxometalate(POM)-based lanthanide (Ln) complexes, Na10[Ln6(H2O)x{As4W44(OH)2(proline)2O151}]·nH2O (Ln = Tb(III), x = 22 and n = 22 for 1; Ln = Dy(III), x = 22 and n = 25 for 2; Ln = Nd(III), x = 26 and n = 31 for 3) were isolated from a one-pot reaction system. In such a reaction system, the initial three discrete solutions, namely K14[As2W19O67(H2O)] precursor in solution A, Ln3+ ion and proline in solution B, and NaCl in solution C, were simultaneously mixed together in one-pot reaction field with pH = 1.5 and heated at 80 °C for 1.5 h, leading to the isolation of crystalline compounds 1–3. The crystal structure of 1–3 contains a crown-type POM-based cluster embedded with four hydrated Ln(III) ions. Moreover, these clusters were further linked by extra two hydrate Ln(III) ions into one-dimensional chains. Photoluminescent properties of compounds 1–3 were also investigated, exhibiting the characteristic emission peaks of relevant Ln(III) ions.
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