砷(Ⅲ)、锑(Ⅲ)配合物的固相合成

Synthesis of Arsenic(Ⅲ) and Antimony(Ⅲ)Complexes by Solid Phase Reaction

用固相反应法合成了碘化砷、氯化锑与硫脲 (Tu)和半胱氨酸 (Cys)的配合物 ,用元素分析、IR及X射线粉末衍射进行了表征。配合物组成为 :ML3X3(M=As、Sb,L=Cys、Tu,X=I、Cl) ,它们在空气中稳定 ,不吸湿 ,微溶于水。几种配合物晶体结构均属单斜晶系 ,配合物 As(Cys) 3I3的晶胞参数为 :a=1 .1 743 nm,b=0 .6945 nm,c=1 .682 2 nm,β=95 .2 8°;As(Tu) 3I3的晶胞参数为 :a=1 .1 1 1 9nm,b=1 .90 3 0 nm,c=1 .5 41 0 nm,β=94.77°;Sb(Cys) 3Cl3晶胞参数为 :a=1 .2 0 5 1 nm,b=0 .6792 nm,c=1 .685 0 nm,β=95 .79°;Sb(Tu) 3Cl3的晶胞参数为 :a=1 .2 3 43 nm,b=1 .65 85 nm,c=1 .92 5 2 nm,β=96.

The cysteine(Cys) and thiourea(Tu) complexes with antimony and arsenic trihalide have been synthesized by solid phase reaction. The compositions and structures of the complexes have been characterized by elemental analysis, infrared spectra and X ray powder diffraction. The complexes have compositions of ML 3X 3(M=As,Sb; L=Cys,Tu; X=I,Cl). They are stable at room temperature, nonhygroscopic and slightly soluble in water. The results indicate that the sulphur in cysteine, nitrogen in thiourea and chlorine or iodine atoms are coordinated with trivalent arsenic or antimony ion. The coordination numbers of arsenic and antimony ion in the complexes are six. The crystal of the complexes belongs to monoclinic system with a =1 174 3 nm, b =0 694 5 nm, c =1 682 2 nm, β = 95 28° for As(Cys) 3I 3; a =1 111 9 nm, b =1 903 0 nm, c =1 541 0 nm, β =94 77° for As(Tu) 3I 3; a =1 205 1 nm, b =0 679 2 nm, c =1 685 0 nm, β =95 79° for Sb(Cys) 3Cl 3; and a = 1 234 3 nm , b =1 658 5 nm, c =1 925 2 nm, β =96 46° for Sb(Tu) 3Cl 3, respectively.