[V^(Ⅳ)O{salen(3-OMe)}_2(CH_3OH)]·H_2O的合成与晶体结构

Synthesis and Structural Characterization of [V^(Ⅳ)O{salen(3-OMe)}_2(CH_3OH)]·H_2O

1,3-二氨基硫脲双缩邻香草醛,偏钒酸铵,乙二胺,加入吡啶,甲醇和水的混合溶剂合成一种新的[V(Ⅳ)O{salen(3-OMe)}2(CH3OH)].H2O配合物,并进行了红外和晶体结构表征.该晶体属于三斜晶系,P1群.晶胞参数为:a=0.671 50(14)nm,b=0.965 20(19)nm,c=1.600 7(3)nm,α=100.715(3)°,β=101.587(3)°,γ=94.787(3)°,V=0.990 7(3)nm3,Z=2,Dc=1.486 g.cm-3,μ=0.545 mm-1,F(000)=462,R1=0.034 8,ωR2=0.066 6,配合物中钒中心为六配位的扭曲八面体构型.

A new complex [V^（Ⅳ））O{salen（3-OMe）}2（CH_3OH）]·H2O was synthesized by the reaction of 1,5-bis（3-methoxyl-salicylaldehyde）-dithiocarbohydrazone,ammonium metavanadate,ethylenediamine,in a mixed solvent of methanol,water and pyridine.The vanadium complex was characterized by IR and X-ray diffraction.The title complex belongs to triclinic,space group P1 with unit cell parameters a=（6.715 0）（14） nm,b=9.652 0（19） nm,c=16.007（3） nm,α=100.715（3）°,β=101.587（3）°,γ=94.787（3）°,V=990.7（3） nm^3,Z=2,Dc=1.486 kg·m^-3, μ= 0.545^ -1 mm , F（000） =462, R1 =0.034 8, ωR2 =0.066 6.