摘要
以N,N’-二(2-吡啶甲酰)肼为配体(H2L),水热法合成了1个新的双核钻㈣配合物[Co2L3]·8H2O(1),对其进行了紫外、红外、电喷雾质谱、热重、元素分析和单晶结构表征。单晶结构分析表明1属于三方晶系,空间群R3c,a=1.63640(11)nm,α=48.52°,V=2.2556(3)nm3,Z=2,R1=0.062。每个钻(Ⅲ)离子处于八面体[CoN6]中,每个L2-配体通过N-N桥连2个钴(Ⅲ)离子,双核钴的距离为0.3497(2)nm。配合物分子间通过羰基和吡啶环间的氢键形成一维长链,链之间由晶格水连接形成三维超分子结构。热重表明1在90℃失去结晶水,500℃以上分解。变温磁化率显示1为抗磁性(1.8~375K)。
A new dinuclear cobalt(Ⅲ) complex, [Co2L3] ·8H2O (1), (H2L=N,N'-bis(2-picolinoyl)hydrazine), was synthesized by a hydrothermal method and characterized by UV, FT-IR, ESI-MS, TGA, EA and single crystal X- ray crystallography. The complex crystallizes in trigonal system with space group R3c, a=1.636 40(11) nm, α= 48.52°, V=2.255 6 (3) nm3, Z=2, and final R=0.062. Each Co(Ⅲ) has an octahedral [CON6] core. Each L2- ligand binds simultaneously to two Co(Ⅲ) cations in a bis(N,N')-bridging coordination mode with a Co…Co distance of 0.349 7(2) nm. The hydrogen bonding interactions between carbonyl group and pyridyl ring link the molecules of 1 into a 1D chain which was further connected by the lattice water to form a 3D supramolecular framework. The TG analysis shows that 1 loses lattice water at 90 ℃ and is stable below 500℃. Magnetic measurement reveals that 1 is a low-spin species in the range of 1.8-375 K. CCDC: 744616.
出处
《无机化学学报》
SCIE
CAS
CSCD
北大核心
2014年第1期163-168,共6页
Chinese Journal of Inorganic Chemistry
基金
国家自然科学基金(No.20771059,21171093)
南京工业大学材料化学工程国家重点实验室开放课题基金(KL11-03)资助项目