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Two 3d-4f heterometallic monovacant Keggin phosphotungstate derivatives [Cu(dap) (H 2 O) 2 ] 0.5 [Cu(dap) 2 ] 4 H 2 [Pr(-PW 11 O 39 ) 2 ] Á 3H 2 O (1) and [Cu(en) 2 (H 2 O)] 2 [Cu(en) 2 ] 1.5 H 4 [Pr(-PW 11 O 39 ) 2 ] Á 10H 2 O (2) (dap ¼ 1,2-diaminopropane, en ¼ ethylenediamine) have been hydrothermally synthesized by reaction of the trivacant Keggin phosphotungstate precursor Na 9 [A--PW 9 O 34 ] Á 7H 2 O with CuCl 2 Á 2H 2 O and PrCl 3 in the presence of dap or en and structurally characterized by elemental analyses, IR spectra, X-ray single-crystal diffraction, and thermogravimetric analyses. Compound 1 crystallizes in the triclinic space group P 1 with a ¼ 17.325(3), b ¼ 18.917(3), c ¼ 19.938(3) Å , ¼ 104.481(2), ¼ 98.968(3), ¼ 91.306(3) , V ¼ 6236.4(18) Å 3 , Z ¼ 2, GOOF ¼ 1.000, R 1 ¼ 0.0806, wR 2 ¼ 0.2016. Compound 2 also belongs to the triclinic space group P 1 with a ¼ 16.005(4), b ¼ 18.053(4), c ¼ 21.127(5) Å , ¼ 113.894(3), ¼ 90.745(4), ¼ 94.255(4) , V ¼ 5560(2) Å 3 , Z ¼ 2, GOOF ¼ 0.999, R 1 ¼ 0.0686, wR 2 ¼ 0.1885. Both 1 and 2 display organic-inorganic hybrid 2-D sheet architectures built by classic monoPr III sandwiched dimeric moieties [Pr(-PW 11 O 39 ) 2 ] 11À through [Cu(L) 2 ] 2þ bridges (L ¼ dap, en), which represent rare organic-inorganic hybrid 2-D 3d-4f heterometallic monovacant Keggin polyoxometalates.

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