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  

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

作　　者：罗兰[1] 魏明礼[1] 阎世平[1] 王耕霖[1] 王宏根[1] 姚心侃[1] 

机构地区：[1]南开大学化学系分析测试中心,天津300071

出　　处：《高等学校化学学报》1992年第10期1201-1204,共4页Chemical Journal of Chinese Universities

基　　金：国家自然科学基金

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.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,UV spectra,IR spectra and TG-DAT analyses.The crystal and molecular structures of C19H21N4O4S3ClSm 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.

关 键 词：冠醚 晶体结构 稀土金属 络合物 

分 类 号：O614.33[理学—无机化学]