4-(1,2,4-三唑-5-酮-4-基)-3-硫代脲酸乙酯的合成、晶体结构及理论计算

4-氨基-1,2,4-三唑-5-酮(ATO)与硫氰酸钾、氯甲酸乙酯在乙酸乙酯中反应, 合成了4-(1,2,4-三唑-5-酮-4-基)-3-硫代脲酸乙酯, 在室温下采用缓慢蒸发溶剂二甲基甲酰胺得到合适的可用于X射线衍射的单晶. 晶体属六方系, 空间群为R-3, 晶体结构参数为a＝2.60524(7) nm, b＝2.60524(7) nm, c＝0.82579(6) nm, γ＝120°, V＝4.8540(4) nm³, D_c＝1.442 g/cm³, μ＝0.300 mm^－1, F(000)＝2190, Z＝18, R₁＝0.0569, wR₂＝0.1424. 选取标题化合物的一个结构单元作为初始模型, 运用Gaussian 03程序对化合物进行了HF/6-311G, MP2/6-311G和B3LYP/6-311G水平的几何全优化，并对其原子电荷及自然键轨道(NBO)进行了分析.

Synthesis, Crystal Structure and Theoretical Calculation of 4-(1,2,4-Triazole-5-one-4-yl)-3-thiourea Carboxylic Acid Ethyl Ester

4-(1,2,4-Triazole-5-one-4-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by mixing 4-amino-1,2,4-triazole-5-one (ATO), potassium thiocyanate and ethyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by slow evaporation of the solvent dimethylformamide at room temperature. The crystal belongs to rhombohedral symmetry with space group R-3 and crystal parameters of a＝2.60524(7) nm, b＝2.60524(7) nm, c＝0.82579(6) nm, γ＝120°, V＝4.8540(4) nm³, D_c＝1.442 g/cm³, μ＝0.300 mm^－1, F(000)＝2190, Z＝18, R₁＝0.0569, wR₂＝0.1424. A crystal unit of the title compound was selected as the initial structure, and it was fully optimized by HF/6-311G, MP2/6-311G and B3LYP/6-311G methods in Gaussian 03 package, and the atomic charges and natural bond orbital (NBO) analysis were also discussed.