Influence of polymorphism on N-thiophosphorylated thiourea 4-Me₂NC₆H₄NHC(S)NHP(S)(OiPr)₂ crystal design

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• 作者：Maria G. Babashkina ; ^{maria.babashkina@ksu.ru} ; Damir A. Safin ; Koen Robeyns ; Yann Garcia
• 关键词：N-thiophosphoryl thiourea ; Crystal structure ; H-bond networks ; Polymorphism ; IR spectroscopy ; NMR spectroscopy
• 刊名：Inorganic Chemistry Communications
• 出版年：2012
• 期刊代码：39_13877003
• 类别：ch
• 出版时间：April, 2012
• 卷：18
• 期：Complete
• 页码：34-37
• 文件大小：511 K

摘要

The reaction between 4-(dimethylamino)aniline and O,O鈥?diisopropyl-isothiocyanatothiophosphoric acid (iPrO)₂P(S)NCS gives the N-thiophosphorylated thiourea 4-Me₂NC₆H₄NHC(S)NHP(S)(OiPr)₂ (L). The structure of this compound was investigated by IR, ¹H, ³¹P{¹H} NMR spectroscopy; its composition was examined by microanalysis. Recrystallization of L from an acetone/n-hexane mixture leads to the formation of the triclinic polymorph L1 with cell parameters a = 7.6486(2), b = 9.8087(13), c = 13.7522(14) 脜, 伪 = 79.685(10), 尾 = 84.090(7), 纬 = 70.463(8)掳, V = 955.58(17) 脜³, and Z = 2. Recrystallization of L from a CH₂Cl₂/n-hexane mixture leads to the formation of the triclinic polymorph L2 with cell parameters a = 10.2581(6), b = 13.1606(7), c = 14.9343(8) 脜, 伪 = 90.718(3), 尾 = 107.751(3), 纬 = 93.285(2)掳, V = 1916.07(18) 脜³, and Z = 4.