双缩二氨基硫脲类化合物的合成与结构

Synthesis and Crystal Structure of Some Dithiocarbohydrazones

合成了 1,5 二 (4 甲氧基苯甲醛 )双缩二氨基硫脲 (1) ,1,5 二 (对二甲基氨基苯甲醛 )双缩二氨基硫脲 (2 ) ,1,5 二 (2 呋喃甲醛 )双缩二氨基硫脲 (3)三个化合物 ,并通过元素分析、红外光谱、核磁共振、质谱进行了结构表征 .首次报道了双缩二氨基硫脲类化合物的13CNMR数据 ,并发现在溶液中由于构象异构体或二聚体的存在 ,该类化合物的部分13CNMR谱峰出现矮而宽、不易检测的特征 .配体 1形成的晶体为单斜晶系 ,具有P2 1/c空间群 ,a =1 4363(3)nm ,b =1 2 62 2 (2 )nm ,c =1 0 970 (2 )nm ,β =10 1 730 (10 )° ,V =1 9472 (6)nm3,Z =4,Dc=1 318g/cm3,μ =0 193mm-1,F(0 0 0 ) =816,R1=0 0 5 60 ,wR2 =0 14 96.由于分子间弱氢键力的作用 。

Novel 1,5-bis(4-methoxybenzaldehyde)-dithiocarbohydrazone (1), 1,5-bis(p-dimethylaminobenzaldehyde)dithiocarbohydrazone ( 2) and 1, 5-bis ( 2-furaldehyde) -dithiocarbohydrazone ( 3) have been synthesized and characterized by elemental analysis, IR, NMR and MS spectra. The C-13 NMR data of the dithiocarbohydrazones was initially reported. It was found that the partial 13C NMR signals of the title compounds presented small and broad, and were difficult to be detected as the result of different conformers or diners formed in solution. The crystal structure of compound 1 was determined by X-ray single crystal diffraction analysis. Crystal structure of compound 1 belongs to monoclinic system with space P2(1)/c. The unit cell parameters are a = 1.4363(3) nm, b = 1.2622(2) nm, c = 1.0970(2) nm, beta=101.730(10), V=1.9472(6) nm(3), Z = 4, D-c = 1.318 g/cm(3), mu = 0.193 mm(-1), F(000) = 816, R-1 = 0.0560, wR(2) = 0.1496.