加合物C_(29)H_(25)N_5O_6S的合成及晶体结构研究  

Synthesis and Crystal Structures of C_(29)H_(25)N_5O_6S of Adduct

作　　者：马亚娟[1] 鲜亮[1,2] 苏碧泉[1] 

机构地区：[1]兰州交通大学化学与生物工程学院,甘肃兰州730070 [2]西北民族大学化工学院,甘肃兰州730124

出　　处：《兰州交通大学学报》2013年第1期193-197,共5页Journal of Lanzhou Jiaotong University

基　　金：甘肃省自然科学基金(096RJZA111);中央高校基本科研业务费专项资金(ZYZ2012066);留学人员科技活动资助(2012258)

摘　　要：介绍了有机加合物N-(2-硝基苯基)-2-苯乙酰胺并N-乙氧羰基-N'-o-硝基苯乙酰基硫脲的合成及结构研究,其分子式为C29H25N5O6S,分子量为571.60.采用溶剂挥发培养出了0.30mm×0.26mm×0.24mm尺寸的加合物单晶,该加合物通过FT-IR、1 HNMR和X-射线单晶衍射分析方法进行了表征.该化合物属于单斜晶系,P21/c空间群,晶胞参数:a=12.796 5(11),b=13.502(3),c=11.261(3),α=90°,β=102.329°(3),γ=90°,Z=4,V=2 726.6(10)3,D=1.329mg/m3,F(000)=1 192,GOF=1.035.结构由直接法解出,最终偏离因子为R1=0.080 6,wR2=0.135 6.X-射线单晶衍射分析显示,晶体中分子主要通过分子间N-H…O氢键(N1-H1A…O4键长为3.005,键角为170.23°)和C-S键(C23-S1键长为3.847)相互连接,在晶体中形成了一维链状结构.对该加合物的合成及其分子的微观晶体结构进行了研究.An organic adduct, N-（2-nitrophenyl）-2-phenylethylamide and N-ethoxycarbonyl- N＇-O-nitrophenyl acetylthiourea,was synthesized and the crystal structure was measured. Its molecular formular is C-9 HzsNsO6S and its molecular weight is 571.60. A large single crystal with dimensions of 0. 30 mm X 0. 26 mm X 0. 24 mm was obtained by slow evaporation at room temperature. The adduct was analyzed by FT- IR, 1H NMR and X-ray diffraction. The crystal is monoclinic, space group P21/c, with cell dimensions a= 12. 7965（11）,b=13. 502（3）,c=11. 261（3）,a=90°,/3=102. 329°（3）,＇y=90＊,Z=4,V=2726. 6（10） A3,D = 1. 329 mg/m3,F（000） = 1192, GOF= 1. 035. Its structure is worked out by direct method, and its ultimately deviation factor is RI=0. 0546 ,wR2=0. 123. The X-ray diffraction analysis showed that the crystal mainly depends on the molecular hydrogAen bonds N-H＇＂O（N,-Hx AO4 bond length 3. 005A, bond angle 170. 23°）and the bond C-S（C23-S1 band length 3. 847A） between the mole-cules connected in the crystal constitutes one-dimensional chain structure. The synthesis of the adduct and its crystal structure of the microlements are discussed.

关 键 词：合成 氢键 加合物 晶体结构 

分 类 号：O625.72[理学—有机化学]