Synthesis and Crystal Structure of an Octa-nuclear V-Cu-S Cluster:[VS_3O(CuPBu_3)_2(CuSPBu_3)]_2
Synthesis and Crystal Structure of an Octa-nuclear V-Cu-S Cluster:[VS_3O(CuPBu_3)_2(CuSPBu_3)]_2作者机构:中科院福建物质结构所 结构化学国家重点实验室 福建 福州
出 版 物:《Chinese Journal of Structural Chemistry》 (结构化学(英文))
年 卷 期:1997年第16卷第5期
页 面:365-370页
核心收录:
学科分类:07[理学] 070205[理学-凝聚态物理] 08[工学] 080501[工学-材料物理与化学] 0805[工学-材料科学与工程(可授工学、理学学位)] 0703[理学-化学] 0702[理学-物理学]
主 题:synthesis crystal structure vanadium cluster copper cluster
摘 要:The title compound has been synthesized by reaction of (NH4)3VS4,CuCl, and PBu3 in CH2Cl2 and its structure was determined by single crystal X-raydiffraction. Crystallographic data: C72 H162 Cu6O2P6S8V2, Mr= 1985. 57, monoclinicspace group C2/c, a= 17. 864(3), b= 25. 946(8), c= 24.071 (7),β= 112. 79(2)°,V = 10285. 9, Z= 4, Dc= 1. 28 g/cm3, F(000) = 4192, μ(MoKa) = 16. 7 cm-1,the final R=0.065 and Rw =0.074 for 4051 unique reflections with I 3σ(I). Thestructure can be described as a metal-sulfur dodecahedral cage fused by two incompletecubane-like VS3Cu3 units connected by Cu - S bonds. The Cu - S bonds within theasymmetric VS3Cu3 unit are slightly shorter than those linking the two centrosymmetrically related VS3Cu3 units. The six copper and two vanadium atoms display asomewhat distorted cubane array with a μ4-S atom on each face of the metal cubane.