| In the paper, on the basis of molecular design and assembly, adopting simple materials or classical heteropolymolybdate precursor, under the conventional aqueous or hydrothermal conditions methods, two kinds of novel Polyoxometalate derivatives based on alkaline-earth or rare-earth metal ions were obtained. These complexes were charactered by X-ray crystallography, IR, UV, thermal properties, magnetic analyses or photocatalytic analysis.(1) Two kinds of polyoxometalate alkaline-earth derivatives have been successfully isolated and characterized by X-ray crystallography. Interestingly, the phenomenon that the two novel heteropolyoxoanion can be mutually transformed when the pH of solution is adjusted to ca. 4.50 in aqueous solution has been observed.(2) Through hydrothermal synthesis method, three polyoxotungstate-based 3D metalAorganic polymers were sysnthesized by introducing macromolecular ligands which has never been introduced in the heteropolymolybdate realm, by reaction of the Keggin type precursor, lanthanide cations and 2,5-Pyridinedicarboxylic acid. They represent the first 3D polyoxometalate-organic lanthanide derivatives consisting of monolacunary polyoxotungstates fragments.The crystal data are as follows:1. (NH4)4Na8{[Ca(H2O)]6[P4Mo6O34]2}A36H2O: monoclinic, space group P-1, a = 13.427(2) A, b = 13.814(2) A, c = 16.790(2) A,α= 76.641(2) o,β= 66.753(2)°,γ= 62.278(2)°, V = 2528.7(6) A3, Z = 1, R1 = 0.0321, wR 2 = 0.0891;2. K11H{[Ca(H2O)]6[P4Mo6O34]2}A22H2O: triclinic, space group P-1, a = 12.8983(13) A, b = 13.4856(14) A, c = 16.2197(17) A,α= 113.259(2) o,β= 91.930(2)°,γ= 115.2250(10)°, V = 2274.5(4) A3, Z = 2, R1 = 0.0404, wR2 = 0.0977; 3. Na10.5H1.5{[Ca(H2O)]6[P4Mo6O34]2}.25H2O: triclinic, space group P-1, a = 13.2214(7) A, b = 17.7655(10) A, c = 20.7275(11) A,α= 81.8640(10) o,β= 81.1400(10)°,γ= 79.1260(10)°, V = 4692.3(4) A3, Z = 2, R1 = 0.0133, wR2 = 0.0249;4. [K3Ca(H2O)4(HP2Mo5O23)]·6H2O: monoclinic, space group P21/c, a = 10.392(4) A, b = 18.931(7) A, c = 16.180(6) A,β= 105.632(5) o, V = 3065.4(18) A3, Z = 4, R1 = 0.0217, wR2 = 0.0634;5. [La(HL)(L)(H2O)6{La(H2L)0.5(α-PW11O39H)La(H2O)4}]2·8H2O: triclinic, space group P-1, a = 12.3807(11) A, b = 14.6888(12) A, c = 21.2276(18) A,α= 72.558(2) o,β= 77.1550(10) o,γ= 67.9110(10) o, V = 3386.3(5) A3, Z = 1, R1= 0.0618, wR2 = 0.1062;6. [Ce(HL)(L)(H2O)6{Ce(H2L)0.5(α-PW11O39H)Ce(H2O)4}]2·12H2O: triclinic, space group P-1, a = 12.4306(9) A, b = 14.7656(11) A, c = 21.2760(16) A,α= 72.5620(10) o,β= 77.7990(10) o,γ= 67.6590(10) o, V = 3424.9(4) A3, Z = 1, R1 = 0.0279, wR2 = 0.0646;7. [Pr(HL)(L)(H2O)4{Pr(H2L)0.5(α-PW11O39H)Pr(H2O)4}]2·8H2O: triclinic, space group P-1, a = 12.2350(19) A, b = 14.546(2) A, c = 19.853(3) A,α= 109.711(2) o,β= 91.443(2) o,γ= 112.699(2) o, V = 3019.2(8) A3, Z = 1, R1 = 0.0612, wR2 = 0.1216.
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