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A new heterometallic 3d–4f tungstoantimonite, KNa5{K2Dy2Cu2(H2O)8(SbW9O33)2}·17H2O (1) was designed and synthesized by decomposition of preformed large cluster, resulting in a ring-like 3d–4f–4p cluster {K2Dy2Cu2(H2O)8}-containing polyoxotungstate.

Reactions of lacunary polyoxometalate (POM), transitionmetal (TM), and lanthanide-metal (Ln) cations with the assistance of additional small organic molecules under hydrothermal conditions led to the formation of a group of metal-POM frameworks (MPFs) with nanospaces: [Cu(enMe) 2 ] 13 -{Ln(SiW 11 O 39 ) 2 } 2 ·xH 2 O [Ln = Ho 3+ (compound 1), Dy 3+ (compound 2), Eu 3+ (compound 3), Er 3+ (compound 4), Sm 3+ (compound 5), Pr 3+ (compound 6); x = 18 for 1, 5, 6; x = 20 for 2, 3, 4; enMe = 1,2-diaminopropane). Single-crystal X-ray dif-[a] School

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