N,N'-双(苯甲酰丙酮)-1,4-丁二胺席夫碱银(I)配合物的合成及其晶体结构

Synthesis and Crystal Structure of the Schiff Base Ag(Ⅰ)Complex of N,N'-bis(benzoylacetone)-1,4-butanediamine

以苯甲酰丙酮与1,4-丁二胺经缩合反应制得一个新的席夫碱配体——N,N'-双(苯甲酰丙酮)-1,4-丁二胺(L);L与硝酸银经配位反应合成了配合物[Ag_2(L)(NO_3)_2]_n(1),其结构经1H NMR,13C NMR,FT-IR,元素分析和X-射线单晶衍射表征。晶体结构解析表明:1(CCDC∶1 434 692)属单斜晶系,空间群P21/c,晶胞参数a=0.997 81(5)nm,b=0.778 36(4)nm,c=1.704 13(8)nm,β=106.637 0(10),V=1.261 85(11)nm3,Z=2,Dc=1.884 g·cm^(-3),R1=0.020 8,wR_2=0.054 4。1中每个银离子为扭曲四面体的配位构型,分别和相邻配体的γ-碳原子,氧原子及两个NO_3^-的氧原子配位;每个配体作为四齿配体,分别用两端的γ-碳原子,氧原子和四个银离子配位形成1D链结构,1D通过NO_3^-与银离子配位扩展形成3D网状结构。热稳定性研究结果表明:L和1的初始分解温度分别为300℃和200℃。

A novel Schiff base ligand, N, N＇-dibenzoylacetone-1,4-diaminobutane （ L）, was obtained by condensation reaction of 1,4-diaminobutane with benzoylaeetone. The Schiff base Ag（I） coordina- tion complex, [ Ag2 （L） （ NO3 ） 2 ] n （ 1 ）, was synthesized by coordination of L with silver nitrate. The structure was characterized by t H NMR, 13C NMR, FT-IR, elemental analysis and X-ray single-crystal diffraction. 1 （CCDC： 1 434 692） belongs to monoclinic system, space group P21/c with a = 0.997 81 （5） nm, b =0.778 36（4） nm, c=1.704 13（8） nm,/3=106.6370（10）, V=1.261 85（11） nm3, Z =2, Dc =1.884 g · cm-3, RI =0.020 8, wR2 =0.054 4. Each Ag（I） has a distorted tetrahedral coordination geometry, and coordinates with the T-C and O of the adjacent ligand and two O atoms of NO3-. Each ligand is observed to be tetradentate. The T-C and O at the two ends of L coordinate with four Ag（I） and form a 1 D chain framework. These 1 D chains further expand to form a 3 D retieulated structure through NO3- and Ag（I） coordination. The initial decomposition temperature of L and 1 were 300 ℃ and 200 ℃, respectively.