糖精锌水合物[Zn(C_7H_4NO_3S)_2(H_2O)_4]·2H_2O的合成及晶体结构

Synthesis and Crystal Structure of a Hydrate of the Zinc Salt of Ortho-benzoic Sulfimide Compound [Zn(C_7H_4NO_3S)_2(H_2O)_4]·2H_2O

以糖精和氧化锌或碳酸锌为原料进行反应生成糖精锌,结晶或重结晶后得到糖精锌晶体,并通过X-射线衍射对晶体结构进行了测定,证明该晶体属单斜晶系,空间群为P21/a,晶胞参数为:a=0.784 9(6)nm,b=1.625 2(4)nm,c=0.800 5(2)nm,α=90°,β=100.21(5)°,V=1.004 97 nm3,Z=2,Dc=1.777 g/cm3,F(000)=552.00,μ=14.98 cm-1.最终的偏离因子R=0.066,Rw=0.097.结构分析表明,在该化合物的基本单元中,中心Zn原子处于四角双锥八面体配位环境中,4个水分子在赤道平面上与Zn配位,晶胞中还包含有2个游离的结晶水,形成了含6个水分子的结晶物,证明该化合物与美国专利(US 5358816)所记载的化合物形态有所不同.晶胞中含有2个游离结晶水的糖精锌具有对热不太稳定的性质,该性质也可以从其晶体表面风化变得粗糙而得到证实.

Zinc salt of ortho-benzoic sulfimide compound is synthesized by reaction of benzosulfimide with zinc oxide or zinc corhonate and characterized by single-crystal X-ray diffraction analysis with the following crystal data： monoclinic, space group P21/a,a=0.7849（6）nm,b=1.6252（4）nm,c=0.8005（2）nm,a=90°,β=100.21（5）°,y=1.00497nm^3,Z=2,Dc=1.777g/cm^3,F（000）=552.00,μ=14.98cm^-1. The result of single-crystal X-ray diffraction reveals that the center Zn atom is located in the four-corner hipyramid coordination environment of the basic unit of the compound, four H2O molecules coordinate to Zn above the equatorial plane, and the crystal cell contains two free crystal water molecules, so it forms the six-water crystal compound. It proves that the compound＇s form differs from what＇s recorded in the US patent （US 5358816）. It can he inferred that the gluside zinc which contains two free crystal water molecules in the crystal cell isn＇t very stable to the heat. It can also he proved from the fact that the surface of the crystal becomes rough for the effloresce.