高等学校化学学报 ›› 1992, Vol. 13 ›› Issue (10): 1201.

• 论文 • 上一篇    下一篇

稀土硫氰酸盐与N-对氯苯基氮杂15-冠-5配合物的合成及晶体结构

罗兰, 魏明礼, 阎世平, 王耕霖, 王宏根, 姚心侃   

  1. 南开大学化学系, 分析测试中心, 天津, 300071
  • 收稿日期:1991-12-04 修回日期:1992-04-13 出版日期:1992-10-24 发布日期:1992-10-24
  • 通讯作者: 王耕霖
  • 基金资助:

    国家自然科学基金

Synthesis and Crystal Structure of Complexes of Rare Earth(Ⅲ) Isothiocyanate with N-(p-chlorophenyl)aza-15-Crown-5

LUO Lan, WEI Ming-Li, YAN Shi-Ping, WANG Geng-Lin, WANG Hong-Gen, YAO Xin-Kan   

  1. Department of Chemistry, Central Laboratory, Nankai University, Tianjin, 300071
  • Received:1991-12-04 Revised:1992-04-13 Online:1992-10-24 Published:1992-10-24

摘要: 合成了12种稀土金属硫氰酸盐与N-对氯苯基氮杂15-冠-5的固体配合物,进行了元素分析和电导、红外光谱、电子光谱测定及热重-差热分析,并对Sm(SCN)3·L作了X射线单晶结构分析,结果表明:Sm(Ⅲ)离子与冠醚上的5个杂原子及3个硫氰酸根上的氮原子配位,配位数为8.

关键词: 稀土配合物, 冠醚, 晶体结构

Abstract: Twelve 1:1 complexes of rare earth(Ⅲ) isothiocyanate with N-(p-chlorophenyl)aza 15-crown-5 were synthesized and characterized by elementary analyses,conductivity measurements,UVspectra,IRspectra and TG-DATanalyses.The crystal and molecular structures of C19H24N4O4S3ClSm were determined by single-crystal X-ray diffraction.The unit-cell is triclinic,space group P1 with a=0.8422(3) nm,b=0.9056(1) nm,c=1.7041(6) nm,α=93.88(1)°β=102.25(3)°,γ=98.85(2)°,V=1.2482 nm3,M=654.34,Z=2,Dx=1.74 g/cm3,R=0.045,Rw=0.056.The Sm3+ deviates from the plane of the four ether oxygens by 0.1482 (±0.006) nm and is coordinated to every hetero-atom in the polyether ring,and is also coordination to the nitrogen atoms of three isothiocyanates,and the average bond distance is as follows:Sm-O(ether)0.2500 nm,Sm-N(SCN)0.2390 nm,Sm-N 0.2712(5) nm.The coordination number of Sm3+ ion is eight.

Key words: Complexes of rare earth elements, Crown-ether, Crystal structure

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