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采用水热法合成一个新的K/Pd/Se四金属硒化物.K4Pd12Se20(Ⅰ)通过K2PdCl4,K2Se2以及六次甲基四胺(HMT)在110℃以1∶4∶2摩尔比水热反应制得.黑色晶体(Ⅰ)不溶于水和多数有机溶剂.化合物属正交空间群Pbca,晶胞参数a=10.840(1),b=25.735(2),c=30.554(2),V=8523.4(9)3,Z=8.K4Pd12Se20有一个新型簇状阴离子[Pd12Se8(Se2)6]4-和四个抗衡K+阳离子组成.[Pd12Se8(Se2)6]4-阴离子簇是第一个结构全新的多核Pd多硒化物簇.所有12个Pd(Ⅱ)金属离子都是平面几何构型由八个(Se2-)和6个(Se22-)离子配体连接形成大球形[Pd12Se8(Se2)6]4-阴离子簇.值得注意的是,4个K+中的一个是位于[Pd12Se8(Se2)6]4-离子簇中间的空穴位置的.
A new K / Pd / Se quaternary metal selenide was synthesized by hydrothermal method.K4Pd12Se20 (Ⅰ) was hydrothermally reacted with K2PdCl4, K2Se2 and hexamethylenetetramine (HMT) at 110 ℃ in a 1: 4: 2 molar ratio The black crystals (I) are insoluble in water and in most organic solvents.The compounds belong to orthorhombic space group Pbca with unit cell parameters of a = 10.840 (1), b = 25.735 (2), c = 30.554 8523.4 (9) 3, Z = 8.K4Pd12Se20 has a new cluster-like anion [Pd12Se8 (Se2) 6] 4- and four counter- K + cations. [Pd12Se8 (Se2) 6] All of the 12 Pd (Ⅱ) metal ions are planar geometric configurations consisting of eight (Se2-) and six (Se22-) ionic ligands connected to form a large sphere [Pd12Se8 (Se2) 6] 4-Anion Clusters. It is noteworthy that one of the 4 K + is located at the hole site in the middle of the [Pd12Se8 (Se2) 6] 4- ion cluster.