配合物VO[(C_(15)H_(12)N_2O_4)(OC_2H_5)]的合成晶体结构和氧化还原性质

Synthesis,crystal structure and redox property ofoxovanadium(Ⅴ)

含有ONO给体原子的N-邻甲氧基苯甲酰基水杨酰肼配体与[VO(acac)2]在乙醇中反应得到钒(V)酰配合物VO[(C15H12N2O4)(OC2H5)].标题化合物晶体属三斜晶系,空间群P墿,晶胞参数:a=0.89411(5)nm,b=1.0063(2)nm,c=1.0392(2)nm,α=110.171(7)°,β=95.219(3)°,γ=93.822(2)°;V=0.8692(2)nm3,Z=2,R1=0.0513,wR=0.1532.研究结果表明:钒原子具有扭曲的四方锥配位构型,钒酰氧原子处在锥顶位置,配体的3个给体原子与溶剂分子形成锥底平面.

A tridentate dibasic Schiff base ligand with an ONO donor set reacts with in ethanol to form a monomeric five-coordinated oxovanadium (Ⅴ) complex of the type .The title complex VOcrystallizes in the triclinic system,space group Pī with a=0.894 11(5)nm,b=1.006 3(2)nm,c=1.039 2(2)nm,α=110.171(7)°,β=95.219(3)°,γ=93.822(2)°;V=0.869 2(2)nm3,Z=2,The crystal structure was determined by direct methods and refined to R1=0.051 3,wR=0.153 2 on the basis of 3 717 independent reflections.X-ray structure analysis reveals that the VⅤ ion is in a distorted square pyramidal enviroment with the oxo ligand occupying the apical position and the three donor atoms of the tridentate ligand occupying three of the positions in the basal plane,the fourth position of the plane is defined by solvent molecule.The cyclic voltammetry measurements shows that the title complex appears quasi-reversible redox behavior of a one-electron transformation.