胺基桥联双芳氧基稀土金属氯化物的合成和表征(英文)

Synthesis and Characterization of Amine Bis(phenolate) Lanthanide Chlorides

无水三氯化稀土LnCl_3与1倍量的胺基桥联双芳氧基钠LNa_2[L=Me_2NCH_2CH_2N{CH_2-(2-O-C_6H_2- Bu^t-3-Me-5)}_2]在四氢呋喃中室温下反应生成胺基桥联双芳氧基稀土金属氯化物LLnCl(THF)(Ln=Yb(1),Ln=Er(2)).这些配合物都经过了元素分析和红外光谱表征,并测定了配合物1的晶体结构.配合物1·C_7H_8 (C_(39)H_(58)ClN_2O_3Yb,Mr=811.36)属于单斜晶系,P2_1/c空间群,a=9.361 5(8),b=14.287(1),c=29.493(3)(?),β=98.516(2)°,V=3901.1(6)(?)~3,Z=4,Dc=1.381g·cm^(-3),λ(Mo Kα)=0710 70(?),μ=2.502 mm^(-1),F(000)= 1668,R=0.026 7,wR=0.0616.中心金属与来自胺基桥联双芳氧基配体上的2个氧原子和2个氮原子以及1个氯原子和1个来自四氢呋喃的氧原子配位,形成1个六配位的扭曲的八面体几何构型.

Abstract： Reaction of anhydrous lanthanide trichlorides with 1 equiv of sodium amine bis（phenolate）LNa2[L=Me2NCH2CH2N{CH2-（2-O-C6H2-Bu^t-3-（Me.5）}2] in THF at room temperature gave the amine bis（phenolate） lanthanide chlorides LLnCl（THF） （Ln = Yb （1）, Ln = Er （2））. These complexes were well characterized by elemental analyses, IR spectra and, in the case of complex 1, single crystal X-ray diffraction study. Complex 1·C7H8（C39H58ClN2O3Yb,Mr=811.36） belongs to monoclinic, space group P21/c with a=9.3615（8）,b=14.287（1）,c=29.493（3）A,β=98.516（2）°,V=3901.1（6）A^3,Z=4,Dc=1.381g·cm^-3,λ（MoKα）=071070A,μ=2.502mm^-1,F（000）=1668,R=0.0267,wR=0.0616 for 6 723 observed reflections with I 〉 2σ（I）. The central metal atom is coordinated six fold by two oxygen atoms and two nitrogen atoms from the amine bis（phenolate） ligand, one THF molecule and one chlorine atom in a distorted octahedron.