CAJ | 학술논문

本文研究了Ln2O3/Sb/Se/en溶剂热反应体系,合成了2个镧(Ⅲ)系锑硒化合物[Ln(en)4]SbSe4·0.5en[Ln=Dy (1),Ho (2)],用元素分析和红外光谱对化合物进行了表征,并用X-射线单晶衍射测定了化合物的单晶结构,两者都属于单斜晶系,P21/n空间群.结构对比研究发现,在en溶剂中,SbSe43-离子可以与半径较大的La3+和Nd3+离子配位,而不与半径较小的Dy3+和Ho3+离子配位,可见镧系收缩效应对SbSe43-离子与镧系金属离子Ln3+的配位有重要影响.
본문연구료Ln2O3/Sb/Se/en용제열반응체계,합성료2개란(Ⅲ)계제서화합물[Ln(en)4]SbSe4·0.5en[Ln=Dy (1),Ho (2)],용원소분석화홍외광보대화합물진행료표정,병용X-사선단정연사측정료화합물적단정결구,량자도속우단사정계,P21/n공간군.결구대비연구발현,재en용제중,SbSe43-리자가이여반경교대적La3+화Nd3+리자배위,이불여반경교소적Dy3+화Ho3+리자배위,가견란계수축효응대SbSe43-리자여란계금속리자Ln3+적배위유중요영향.
Organic hybrid lanthanide(Ⅲ) selenidoantimonates [Dy(en)4]SbSe4·0.5en (1) and [Ho(en)4]SbSe4·0.5en (2) (en=ethylenediamine) were synthesized under mild solvothermal conditions and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. 1 and 2 are isostructural-crystallizing in the monoclinic space group P21/n. Crystallographic data for 1: a=1.140 69(14) nm, b=1.314 19(16) nm, c=1.628 3(2) nm, β=92.324(3)°, V=2.439 0(5) nm3, Z=4, Mr=870.56, Dc=2.371 g·cm-3, F(000)=1 624, the final R=0.038 6 and wR=0.073 3 for observed reflections 3 874 with I>2σ(I). For 2: a=1.140 20(17) nm, b=1.314 70(18) nm, c=1.623 2(2) nm, β=92.358(4)°, V=2.431 1(6) nm3, Z=4, Mr=872.99, Dc=2.385 g·cm-3, F(000)=1 628, the final R=0.070 1 and wR=0.121 9 for observed reflections 3 471 with I>2σ(I). 1 and 2 consist of tetrahedral anion SbSe43-, lanthanide complex cation [Ln(en)4]3+ (Ln=Dy, Ho) and free en molecule. The lanthanide Ln3+ ion is in an eight coordinated environment involving in eight N atoms of four en ligands forming a bicapped trigonal prism. In the crystal structure of 1 and 2, extensive N-H…Se hydrogen bonding interactions lead to a 3-dimensional network structure of the cations and anions. CCDC: 777749, 1; 777750, 2.