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Abstract: Three organic–inorganic hybrid TM–Ln heterometallic phosphotungstates [Cu(dap)2(H2O)][Cu(dap)2]3.5[La(α-HPW11O39)2]·6H2O (1) [Cu(dap)2(H2O)]0.5[Cu(dap)2]4[Nd(α-HPW11O39)2]·4H2O (2) and [Cu(dap)2(H2O)]2[Cu(dap)2]3.5[Eu(α-PW11O39)2]·6H2O (3) (dap=1,2-diaminopropane) have been hydrothermally synthesized and structurally characterized by elemental analyses, IR spectra, optical diffuse reflectance spectra, powder X-ray diffraction (PXRD), thermogravimetric (TG) analyses and single-crystal X-ray diffraction. Their common features are that 1–3 all consist of asymmetric sandwich-type subunits [Ln(α-PW11O39)2]11− and [Cu(dap)2]2+ bridges. Both 1 and 2 display the 2-D (4,4)-topological sheets whereas 3 exhibits the 3-D 5-connected (46·64) topological framework. The magnetic properties of 2 and 3 and the luminescence performance of 3 have been measured. [Copyright &y& Elsevier]