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在苯并-1,3-噻唑-2-硫酮(Hbztzt,HL)和三苯膦(PPh_3)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)(PPh_3)_2].配合物在CS_2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)(PPh_3)_2]·CS_2.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)nm~3,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PPh_3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).
The corresponding complexes of Cu (Ⅰ) were synthesized in one step by the electrochemical method of sacrificial copper anode in acetonitrile solution of benzo-1,3-thiazole-2-thione (Hbztzt, HL) and triphenylphosphine (PPh_3) , Electrochemical efficiency (E_f), elemental analysis and IR spectra indicated that the product was a complex mixed ligand complex containing two ligands of mercaptan anion (L) and neutral thione (HL) and triphenylphosphine [Cu (L) (HL) (PPh_3) _2]. The complex was recrystallized from light yellow crystals in CS_2. The structure of [Cu (L) (HL) (PPh_3) _2] · CS_2 was determined by X-ray single crystal diffraction. The crystal belongs to the triclinic system with space group: P1.a = 1.0159 (2) nm, b = 1.4200 (2) nm, c = 1.8072 (3) nm, °, γ = 67.65 (1) °, Z = 2, V = 2.3929 (6) nm ~ 3, D_c = 1.41g · cm -3, R = 0.0348 and R_w = 0.0316. With the two P atoms of the two PPh_3, the two exocyclic S atoms on the thiol anion (L) and the neutral thiol molecule (HL) averaged by the hydrogen bonding (N-H ... N) A Cu-S bond length of 0.2372nm and 0.2410nm).