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以N,N′-二(2-吡啶甲酰)肼为配体(H2L),水热法合成了1个新的双核钴(Ⅲ)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=1.636 40(11)nm,α=48.52°,V=2.255 6(3)nm3,Z=2,R1=0.062。每个钴(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0.349 7(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(1.8~375 K)。
A novel dinuclear cobalt (Ⅲ) complex [Co2L3] · 8H2O (1) was synthesized by hydrothermal method using N, N’-bis (picolinoyl) hydrazine as a ligand UV, IR, ESI-MS, TG, elemental analysis and single crystal structure characterization. Single crystal structure analysis shows that 1 belongs to the triclinic system with space group R3c, a = 1.636 40 (11) nm, α = 48.52 °, V = 2.255 6 (3) nm3, Z = 2 and R1 = 0.062. Each cobalt (III) ion is in octahedral [CoN6], with each L2-ligand bridging two cobalt (III) ions through N-N and binuclear cobalt with a distance of 0.349 7 (2) nm. One-dimensional long chain is formed between hydrogen bonds of the carbonyl group and the pyridine ring through the intermolecular complexes, and the three-dimensional supramolecular structure is formed by the crystal lattice water connection between the chains. Thermogravimetry showed that 1 lost crystalline water at 90 ℃ and decomposed above 500 ℃. Variable temperature magnetic susceptibility shows that 1 is diamagnetic (1.8 ~ 375 K).