Synthesis and Crystal Structure of 3,6-Bis(4-methyl-1,2,3-thiadiazol-5-yl)-1,2,4-triazolo[3,4-b][1,3,4]thiadiazole  

作　　者：杨知昆 范志金 左翔 郑琴香 宋海斌 尤进茂 NATALIA P.Belskaia VASILIY A.Bakulev 

机构地区：[1]State Key Laboratory of Elemento Organic Chemistry,Nankai University [2]Department of Chemistry,Qufu Normal University [3]TOSLab,The Urals State Technical University

出　　处：《Chinese Journal of Structural Chemistry》2010年第1期13-16,共4页结构化学（英文）

基　　金：supported by the National Natural Science Foundation of China (Nos 20672062 and 20872071);the Natural Science Foundation of Tianjin (No 07JCYBJC01200);the International Collaboration Program of the National Natural Science Foundation of China (No 20911120069);International Collaboration Program of Tianjin on Science and Technology (No 07ZCGHHZ01400)

摘　　要：The compound 3,6-bis（4-methyl-1,2,3-thiadiazol-5-yl）-1,2,4-triazolo[3,4-b][1,3,4] thiadiazole（C9H6N8S3,Mr = 322.40） has been synthesized by the reaction of 4-amino-3-（4-methyl-1,2,3-thiadiazolyl）-5-mercapto-1,2,4-triazole with 4-methyl-1,2,3-thiadiazol-5-carboxylic acid and phosphorus oxychloride,and its structure was characterized by IR,1H NMR,EI-MS,elemental analysis and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic,space group C2/c with a = 2.0053（4）,b = 1.3081（3）, c = 1.0556（2） nm, β = 112.69（3）°,Z = 4, V= 2.5548（9） nm^3, Dc = 1.676 g/cm^3, μ= 0.582 mm^-1, F（000） = 1312, R = 0.0546 and wR = 0.1523. X-ray analysis indicates that all rings are essentially planar in this molecule, and an intermolecular hydrogen bond C（9）-H（9）…N（2） and weak intramolecular interactions between S（1）…N（7）, S（3）…N（1） and S（2）…N（4） are observed.The compound 3,6-bis（4-methyl-1,2,3-thiadiazol-5-yl）-1,2,4-triazolo[3,4-b][1,3,4] thiadiazole（C9H6N8S3,Mr = 322.40） has been synthesized by the reaction of 4-amino-3-（4-methyl-1,2,3-thiadiazolyl）-5-mercapto-1,2,4-triazole with 4-methyl-1,2,3-thiadiazol-5-carboxylic acid and phosphorus oxychloride,and its structure was characterized by IR,1H NMR,EI-MS,elemental analysis and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic,space group C2/c with a = 2.0053（4）,b = 1.3081（3）, c = 1.0556（2） nm, β = 112.69（3）°,Z = 4, V= 2.5548（9） nm^3, Dc = 1.676 g/cm^3, μ= 0.582 mm^-1, F（000） = 1312, R = 0.0546 and wR = 0.1523. X-ray analysis indicates that all rings are essentially planar in this molecule, and an intermolecular hydrogen bond C（9）-H（9）…N（2） and weak intramolecular interactions between S（1）…N（7）, S（3）…N（1） and S（2）…N（4） are observed.

关 键 词：X-ray diffraction crystal structure synthesis 1 2 3-thiadiazole 

分 类 号：O621.25[理学—有机化学]