A new polyoxomolybdate complex HNaT[Mo36O112（H2O）16]·47H2O 1 has been prepared in the beaker solution and characterized by single-crystal X-ray diffraction and elemental analyses. Crystal data： H127Mo36Na7O175, Mr = 6542.79, monoclinic, C2/c, a = 40.891（6）, b = 17.900（3）, c = 25.580（4）A, β = 125.673（2）°, V = 15210（4）A3, Z = 4, Dc = 2.857 g/cm^3, F（000） = 12464,μ = 3.013 mm^-1, R = 0.0633 and wR = 0.1654 （I 〉 20（I））. With the bridging sodium cations, the [Mo36Ou2（H2O）16]^8- units in compound 1 are linked to form a one-dimensional structure, on the basis of which a three-dimensional architecture is further constructed via other sodium cations and complicated hydrogen bonds.
LIU Ying DOU Jian-Min WANG Da-Qi ZHANG Xian-Xi LI Da-Cheng JIA Ying-Chun
One novel polyoxometalate compound connected via trivalent cerium cation as bridge H2{ [K（H2O）212[Ce（H2O）5]2（H2Mo1.16W10.84O42）}.8H2O 1 was designed and synthesized in aqueous solution. X-ray diffraction analysis reveals that the structure of 1 is a three-dimensional framework assembled from the arrangement of H2Mo1.16W10.84O42 （named paradodecmetalate-B） and Ce（H2O）5^3＋ containing two planes, which are constructed through the unification of H2Mo1.16W10.84O42^10- and Ce（H2O）5^3＋ along the [100] and [001] directions. Crystal data： H96Ce4KaMo2.32O128W21.68, Mr = 7074.89, monoclinic, P21/n, a = 12.5037（17）, b = 17.002（2）, c = 12.7473（17）A, β = 105.966（2）°, V = 2605.4（6）A^3, Z = 1, Dc = 4.509 g/cm^3, F（000） = 3132,μ = 26.098 mm^-1, R = 0.0377 and wR = 0.0789 （I 〉 2σ（I））.
A novel vanadium-phosphate compound [PV2.5O8.5]·3.83{H2O} （1） was obtained from the hydrothermal reaction and structurally characterized by elemental analysis and single-crystal X-ray diffraction, which exhibited that the title complex crystallized in cubic space group I-43m with crystal data： a= 1.6115（1） nm, V=4.1848（1） nm^3, Z=12, Dc=1.783 g/cm^3, F（000）=2278, R1=0.0528, and wR2=0.1329 [1〉2σ（I）] （all data）. The basic unit of {PV2.5O8.5} symmetrically extended to closed sphere-like structure of {P4V10O34}, WhiCh was further linked to interleaving three-dimensional network via sharing four phosphate through μ3-oxygen atoms around the closed sphere-like structures.
One new polyoxometalate compound connected via nickel/potassium cations, H8K{[Ni（H2O）5]2（H2Mo1.80W10.20O42）}Cl3·16H2O 1, was prepared and characterized by elemental analysis and IR spectroscopy. Single-crystal X-ray diffraction analysis results reveal that clusters of [Ni（H2O）5]2（H2Mo1.80W10.20O42）}^6-in compound 1 are linked by potassium cations to form one- dimiensional chains, based on which a three-dimensional network is further constructed via the hydrogen bonds of O…O and O…Cl. Magnetic measurements show that compound 1 has paramagnetic properties. Crystal data： H62Cl3KMo1.80Ni2O68W10.20, Mr = 3461.33, monoclinic, space group C2/c, a = 18.9291（19）, b = 16.6758（17）, c = 19.1064（19）A, β = 106.6880（10）°, V = 5777.1（10）A^3, Z = 4, Dc = 3.980 g/cm^3, F（000） = 6250, μ = 21.574 mm^-1, R = 0.0579 and wR = 0.1623 （Ⅰ 〉 2σ（Ⅰ））.
LIU Ying DOU Jian-Min WANG Da-Qi ZHANG Xian-Xi LI Da-Cheng XU Feng ZHOU Lei
One new polyoxotungstate complex H6Na2K4（H2W12O42）Cl2·14H2O 1 has been prepared in the beaker solution and characterized by elemental analysis and IR spectroscopy. Crystal data： H36Cl2K4W12Na2O56, Mr = 3411.77, monoclinic, space group P21/c, a = 11.5734（16）, b = 14.3136（19）, c = 15.459（2）A, β = 105.601（2）°, V = 2466.5（6）A^3, Z = 2, Dc = 4.594 g/cm^3, F（000） = 3008, μ = 28.447 mm^-1, R = 0.0574 and wR = 0.1239 （Ⅰ〉 2σ（Ⅰ））. Single-crystal X-ray diffraction analysis results reveal that a three-dimensional architecture in the title compound is constructed from the H2W12O42^10- units linked by potassium.
