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以 Sm2O3, HClO4, NaOH和α -K8SiW11O39·nH2O等为原料合成了组成为 K3{[Sm(H2O)7]2Na[α-SiW11O39Sm(H2O)4]2}·14H2O 的三维无限伸展结构稀土配合物, 并经 IR, UV 光谱,ICP 原子发射光谱, TG-DTA, 循环伏安, 变温磁化率和 X 射线单晶衍射等分析手段进行了表征.X射线单晶衍射测定表明, 该化合物属于三斜晶系, Pī 空间群, 晶胞参数: a = 1.2462(3), b =1.2652(3), 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. 结 构 分 析 结 果 显 示 , Sm3+(1) 配 离 子 镶 嵌 在 [α-SiW11O39]8? 的 空 缺 位 置 形 成[α -SiW11O39Sm(H2O)4]5?亚单元, 两个[α -SiW11O39Sm(H2O)4]5?亚单元通过两个 Sm(1)-O-W 桥互相连接形成标题化合物的二聚体结构单元[α -SiW11O39Sm(H2O)4]2 , 相邻的二聚体结构单元又10?通过两个Sm3+(2)配离子和一个Na+(1)离子桥连成一维链状结构, 链与链之间通过K+ (1)离子连接成二维网状结构, 网状结构又通过 K+(2)离子构筑成新奇的三维无限伸展结构. TG-DTA 结果表明,标题化合物阴离子骨架分解温度为 554℃. 循环伏安行为测试表明, 标题化合物阴离子在 pH =3.1 的水溶液中存在两步氧化还原过程. 变温磁化率结果表明, 在较高温度(11
The three-dimensional infinitely expanded rare earth complex with the composition of K3 {[Sm (H2O) 7] 2Na [α-SiW11O39Sm (H2O) 4] 2} · 14H2O was synthesized from Sm2O3, HClO4, NaOH and α-K8SiW11O39 · nH2O , And characterized by IR, UV spectroscopy, ICP atomic emission spectroscopy, TG-DTA, cyclic voltammetry, temperature-dependent magnetic susceptibility and single crystal X-ray diffraction analysis.X-ray single crystal diffraction measurement showed that the compound belongs to triclin A = 1.2462 (3), b = 1.2652 (3), 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. The structural analysis showed that the Sm3 + (1) ion was inlaid in [α-SiW11O39] 8? Vacancies to form [α -SiW11O39Sm (H2O) 4] 5 [alpha] -SiW11O39Sm (H2O) 4] 5? Subunits are connected to each other by two Sm (1) -OW bridges to form the dimer structural unit of the title compound [? -SiW11O39Sm (H2O) 4] 2, the adjacent dimeric building blocks and 10? Bridged into one-dimensional chain structure by two Sm3 + (2) ions and one Na + (1) ion, and the chains are connected by K + (1) ions Two-dimensional network structure, mesh The structure was further characterized by a novel three-dimensional infinite extension structure by K + (2) ion.The results of TG-DTA showed that the anion of the title compound decomposed at a temperature of 554 ° C. Cyclic voltammetry tests showed that the anion of the title compound in an aqueous solution of pH = 3.1 There is a two-step redox process.Variable magnetic susceptibility results show that at higher temperatures (11