1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲的另一个手性对映体晶体结构

Another Chiral Crystal Structure of 1-[4-(Dimethylamino)-benzylidene]-4-phenylthiosemicarbazide

对-二甲氨基苯甲醛和苯基氨基硫脲缩合反应生成1-[4-(二甲氨基)苯亚甲基氨基]-4-苯基硫脲(DMB),产物能从溶液中析出单一手性对映体晶体.用单晶X射线衍射技术测定了它的绝对构型,晶体属正交晶系,P212121空间群,a=0.7870(2)nm,b=1.1560(2)nm,c=1.6668(3)nm,V=1.5164(5)nm3,Z=4,Dc=1.307g/cm3,F(000)=632,μ=0.213mm-1,2557个可观测点[I>2σ(I)]精修的最终残差因子:R=0.0409,wR=0.1061,Flack参数为0.00(9),能够确定绝对构型.化合物的晶体结构和大宗粉末样品的固体圆二色谱表明化合物在结晶过程中发生单一对映体的手性堆积.

Another chiral crystal of 1-[4-（dimethylamino）benzylidene]-4-phenylthiosemicarbazide （DMB） was obtained, and its absolute structure was determined by X-ray single crystal diffraction and the solid circular dichroism （CD） spectrum. The crystal belongs to orthorhombic system with space group P212121 and a=0.7870（2）, b=1.1560（2）, c=1.6668（3） nm, V=1.5164（5） nm^3, Z=4, Dc=1.307 g/cm^3, F（000）=632, μ=0.213 mm^- 1, the final R=0.0409 and wR = 0.1061 for 2577 observed reflections [I〉 2σ（I）]. The absolute structure can be determined well with the Flack parameter 0.00（9）. The crystal structure and CD spectrum show that an enantiomer of the compound packs into the chiral crystal.