希夫氏碱2-(1-亚异丙基)硫代氨基脲的合成、晶体结构

Synthesis and Crystal Structure of Schiff Base 2-(1-methylethylidene)-hydrazinecarbothioamide

关键词:  2-(1-亚异丙基)硫代氨基脲  合成  晶体结构

Key words:  2-(1-methylethylidene)-hydrazinecarbothioamide  synthesis  crystal structure

摘要:

由丙酮与硫代氨基脲在乙醇中反应得到2-(1-亚异丙基)硫代氨基脲,并培养得到无色单晶。用X-射线衍射法测定了化合物的单晶结构。晶体属于三斜晶系,空间群P1,晶胞参数:a=6.2100(10)Å,b=7.8530(10)Å,c=7.9660(10)Å,U=85.300(10)°,V=68.560(10)°,γ=70.240(10)°,V=339.92(8)ų,Z=2,Mr=131.20,Dc=1.282mg/m³,_=0.378mm^-1,F(000)=140,在5.50°≤2θ≤57.98°范围内用ω-2θ扫描方式进行扫描共收集到2032个衍射点,其中1458个(F₀>4σ(F₀))可观察点用于结构解析和修改。R=0.0303,wR=0.0876(Δ/σ)max=-0.002,W=1/[σ²(F₀²)]+(0.0620P)²,P=(max(F₀²,0)+2F_c²)/3,S=1.009。

Abstract:

Schiff base 2-(1-methylethylidene) hydrazinecarbothioamide was synthesized from the reaction of acetone with hydrazine carbothioamide in ethanol and its colorless single crystals were obtained. The crystal structure was determined by X-ray diffration method.The crystal is included in the tricilinic system.space group is P1,unit cell data:a=6.2100(10) Å, b=7.8530(10) Å, c=7.9660(10) Å, T=85.300(10)°, U=68.560(10)°, V=70.240(10)°, V=339.92(8) ų, Z=2, Mr=131.20, Dc=1.282 mg/m³, _=0.378 mm^-1, F(000)=140, In the range of 5.50° ≤ 2θ ≤ 57.98°,using ω-2θ scanning mode,a total of 2032 reflections are collected,in which 1.458 independent observed reflections(F₀ >4σ(F₀)) are used for structure analysis and modification.Final R=0.0303,wR=0.0876,(Δ/σ) max=-0.002, W=1/[^e2(F₀²)]+(0.0620P) ²,P=(max(F₀²,0) +2F_c²)/3,S=1.009。