Synthesis, structural characterization and properties of a 3D infinitely extended structural rare earth coordination compound of K3{[Sm(H2O)7]2Na[α-SiW11O39Sm(H2O)4]2} · 14 H2O· 14 H2O |
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| Authors: | Jingping Wang Junwei Zhao and Jingyang Niu |
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| Institution: | (1) Institute of Molecule and Crystal Engineering, School of Chemistry and Chemical Engineering, Henan University, 475001 Kaifeng, China |
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| Abstract: | A 3D infinitely extended structural rare earth coordination compound with a formula of K3{Sm(H2O)7]2Naα-SiW11O39Sm(H2O)4]2}·14H2O has been synthesized by reaction of Sm2O3, HClO4, NaOH with α-K8SiW11O39·nH2O, and characterized by IR, UV spectra, ICP, TG-DTA, cyclic voltammetry, variable-temperature magnetic susceptibility and
X-ray single-crystal diffraction. X-ray single-crystal diffraction indicates that the title compound crystallizes in a triclinic
lattice, Pī space group, with a = 1.2462(3) nm, b = 1.2652(3) nm, c = 1.8420(4) nm, α = 87.45(3)°, β = 79.91(3)°, γ= 82.57(3)°, Z = 1, R1 = 0.0778, wR2 = 0.1610. Structural analysis reveals that Sm3+(1) coordination cation has incorporated into the vacant site of α-SiW11O39]8− entity, forming the α- SiW11O39Sm(H2O)4]5− subunit. The two adjacent α-SiW11O39Sm(H2O)4]5− subunits are combined with each other through two Sm(1)-O-W bridges accompanying the formation of dimmer structural unit
α-SiW11O39Sm(H2O)4]2
10− of the title compound. The neighboring dimmer structural units α-SiW11O39Sm(H2O)4]2
10− are linked to form the 1D chainlike structure by means of two Sm3+(2) and a Na+(1) coordination cations. The K+(1) cations connect the 1D packing chains constructing the 2D netlike structure, and adjacent netlike layers are also grafted
by K+(2) cations to build the novel 3D infinitely extended structure. The result of TG-DTA curves manifests that the decomposition
temperature of the title polyanionic framework is 554°C. The cyclic voltammetry measurements show that the title polyanion
has the two-step redox processes in aqueous solution with pH = 3.1. Variable temperature magnetic susceptibility indicates
the title compound obeys the Cruie-Weiss Law in the higher temperature range from 110 to 300 K, while in the lower temperature
range from 2 to 110 K the comparatively strong antiferromagnetism interactions can be observed. |
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| Keywords: | silicotungstic acid Keggin structure crystal structure polyoxometalates rare earth metal |
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