【摘要】 在苯并-1,3-噻唑-2-硫酮（Hbztzt,HL）和三苯膦（PPh₃）的乙腈溶液中,用牺牲铜阳极的电化学方法一步合成了Cu（Ⅰ）的相应配合物,电化学效率（E_f）、元素分析和IR光谱表明:产物为同时含有硫醇阴离子（L）和中性硫酮（HL）两种配体及三苯膦的多元混合配体配合物[Cu（L）（HL）（PPh₃）₂].配合物在CS₂中重结晶得淡黄色晶体,X射线单晶衍射法测定其结构为[Cu（L）（HL）（PPh₃）₂]·CS₂.晶体属三斜晶系,空间群:P1.a=1.0159（2）nm,b=1.4200（2）nm,c=1.8072（3）nm,α=78.12（1）°,β=86.56（1）°,γ=67.65（1）°,Z=2,V=2.3929（6）nm³,D_c=1.41g·cm^-3,R=0.0348,R_w=0.0316.Cu原子以变形四面体与两个PPh₃的两个P原子、被氢键（N—H…N）平均化的硫醇阴离子（L）和中性硫酮分子（HL）上的两个环外S原子配位（两个Cu—S键的键长为0.2372nm和0.2410nm）.更多还原

【Abstract】 Complex [Cu(bztzt) (Hbztzt) (PPh3 )2 ] was synthesized by electrochemical oxidation of copper in an acetonitrile solution of benzo -1,3- thiozoline - 2 - thione (Hbztzt) and triphenylphosphine(PPh3 ) , and characterized by elemental analysis and IR spectrum. The complex was dissolved in CS2, from which yellow crystal formed. The structure of the crystal was shown to be [ Cu( bztzt) ( Hbztzt) ( PPh3 )2 ]·CS2 by an X - ray structure determination. Crystal is triclinic, space group P1 ,with a = 1.0159(2)nm, b = 1.4200(2)nm, c = 1.8072(3)nm, α =78.12(1)°, β = 86.56(1)°, γ = 67.65(1)°, Z = 2. The structure was refined to R = 0.0348 and ,RW =0.0316 for 4869 reflections. The copper atom is pseudotetrahedrally coordinated by two P atoms from PPh3 and two exocyclic S atoms from bztzt- and Hbztzt ligands respectively. The ligands of bztzt-and Hbztzt were "averaged" by the presence of hydrogen bond (N-H…N) between them. The bond distances of two Cu-S are 0.2372nm and 0.2410nm.更多还原