Abstract: 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. |
王 娇,潘迎利,陈江芳,张 勇,顾建胜,贾定先.镧(Ⅲ)系锑硒化合物[Ln(en)4]SbSe4·0.5en(Ln=Dy,Ho)的溶剂热合成与晶体结构(英文)[J].无机化学学报,2010,26(8):1339-1344. |