通过含2-噁唑啉基三角架配体1,3,5-三(2-噁唑啉基)苯(L)与三氟醋酸银反应合成了配合物[Ag4(L)2(CH3CN)2-(CF3CO2)4]n(1),并利用元素分析、电喷雾质谱、X射线单晶衍射等方法对其进行了表征.晶体结构解析结果显示配合物1属三斜晶系,空间群P-1,a=0.83731(6)nm,b=1.22828(9)nm,c=1.33997(10)nm,α=102.9760(10)°,β=107.3050(10)°,γ=93.8600(10)°,Z=1,R=0.0365,wR2=0.0929.该配合物是由[Ag4(L)2(CF3CO2)2]^2+笼状结构单元通过另外两个三氟醋酸根双桥连形成的一维链状结构.相邻的链间通过C-H…O氢键进一步扩展为二维网状结构.电喷雾质谱研究结果显示在实验条件下,溶液中配合物1是以聚合状态存在的.
A new Ag(Ⅰ) complex [Ag4(L)2(CH3CN)2-(CF3CO2)4]n (1) was synthesized by the reaction of a 2-oxazolinyl-containing tripodal ligand 1,3,5-tris(2-oxazolinyl)benzene (L) with a silver(Ⅰ) trifluoroacetate and characterized by means of elemental analysis, electrospray mass (ES-MS) spectroscopy and single crystal X-ray diffraction. The results of the crystallographic analysis showed that the complex 1 is triclinic, with space group P-1, a=0.83731(6)nm,b=1.22828(9)nm,c=1.33997(10)nm,α=102.9760(10)°,β=107.3050(10)°,γ=93.8600(10)°,Z=1,R=0.0365,wR2=0.0929. The complex consists of [Ag4(L)2(CF3CO2)2]^2+ cage-like subunits, which are further connected into 1D infinite chain by two bridging CF3COO^- anions. The 1D chains are further linked by C-H…O hydrogen bonds to form 2D network structure. The results of the ES-MS measurements suggested the polymeric structure of the complex in solution under the ES mass spectroscopy experimental conditions.