N,N',N″-三(3-吡啶基)均苯三甲酰胺的合成及晶体结构

Synthesis and Crystal Structure of N,N',N″-Tris(3-pyridyl) trimesic Amide

为确定有机晶体中的分子排列,以均苯三甲酸、氯化亚砜、3-氨基吡啶为原料,采用酰胺缩合反应合成N,N',N″-三(3-吡啶基)均苯三甲酰胺(TPTA),并研究其晶体结构.利用核磁共振氢谱、红外光谱、X射线粉末衍射以及X射线单晶衍射对其进行表征.结果发现:TPTA晶体为三方晶系,空间群为P 3-,晶胞参数a=1.400 48(2)nm,b=1.400 48(2)nm,c=0.848 98(3)nm,α=90°,β=90°,γ=120°,Z=2,V=1.442 05(6)nm3,Dc=1.003 g/cm3,μ=0.07 mm-1,F(000)=450.0,R1=1.101,wR2=0.343,S=1.52.研究结果表明:TPTA分子间通过氢键结合,形成了一种含有孔隙直径约为1.087 nm的有机多孔结构.

To determine the molecular arrangement in organic crystal, N,N’,N"-tris(3-pyridyl) trimesic amide (TPTA) was synthesized by a typical condensation amidation reaction using trimesic acid, thionyl chloride, and 3-aminopyridine. The crystal and molecular structure of TPTA were characterized by 1 H NMR, FT-IR, XRD and single-crystal X-ray diffraction method. It is found that TPTA crystal is trigonal with a space group of P 3-. Crystal data for TPTA are a = 1. 400 48(2)nm, b = 1. 400 48(2)nm, c = 0. 848 98(3)nm, α = 90°, β = 90°, γ = 120°, Z = 2, V = 1. 442 05(6)nm3 , Dc = 1. 003 g / cm3 ,μ =0. 07 mm - 1 , F (000) = 450. 0, R1 = 1. 101, wR2 = 0. 343, and S = 1. 52. Results show that TPTA molecules are connected by intermolecular hydrogen bonds, and an organic porous structure containing pores with a diameter of about 1. 087 nm is generated.