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通过4,4’-二氨基二苯醚与硫氰酸钾、氯甲酸乙酯在乙酸乙酯中反应,合成了4-[(3-乙氧酰基-2-硫代)硫脲]-4’-[(3-乙氧酰基-2-硫代)硫脲]二苯醚,用缓慢蒸发溶剂培养了标题化合物的单晶.并用X射线单晶衍射法测定其晶体结构,晶体属三斜系,空间群P-1,晶胞参数为:a=0.8589(5)nm,b=1.0519(6)nm,c=1.2876(12)nm,α=99.391(10)°,β=91.689(11)°,γ=95.756(11)°,V=1.1407(11)nm3,Z=2,Dc=1.347g·cm-3,F(000)=484,μ=0.272cm-1,R1=0.0490,wR2=0.1032.运用Gaussian03程序,采用HF/6-311G和B3LYP/6-311G两种计算方法对标题化合物进行了几何全优化和自然电荷计算,对其成键情况及自然键轨道(NBO)进行了分析.对化合物进行了热重分析和比热测定,计算了热力学函数,证明该化合物有良好的热稳定性.
Through the reaction of 4,4’-diaminodiphenyl ether with potassium thiocyanate and ethyl chloroformate in ethyl acetate, 4 - [(3-ethoxycarbonyl-2-thio) thiourea] ’- [(3-ethoxycarbonyl-2-thio) thiourea] diphenyl ether and the single crystal of the title compound was prepared by slowly evaporating the solvent. The crystal structure of the title compound was determined by X-ray single crystal diffraction. A = 0.8589 (5) nm, b = 1.0519 (6) nm, c = 1.2876 (12) nm, α = 99.391 (10) °, β = 91.689 (11) ) = Γ = 95.756 (11) ° V = 1.1407 (11) nm3 Z = 2 Dc = 1.347 g · cm -3 F (000) = 484 μ = 0.272 cm -1 R1 = 0.0490, wR2 = 0.1032. By using the Gaussian03 program, the geometrical optimization and natural charge calculation of the title compounds were carried out by using the two methods of calculation of HF / 6-311G and B3LYP / 6-311G. The bonding and the natural bond orbital (NBO) The thermogravimetric analysis and specific heat measurement of the compounds were carried out and the thermodynamic functions were calculated to prove that the compounds have good thermal stability.