经过三步反应合成了红色晶体,双六甲基二硅胺基二甲基硅基环戊二烯基稀土二价镱配合物[η5-C5H4SiMe3N(SiMe3)2]2Yb(Ⅱ)·2THF,X射线衍射结果表明,[η5-C5H4SiMe2N(SiMe3)2]2Yb(Ⅱ)·2THF属于单斜晶系,空间群为P21/c,α=1.646 87(12)nm,b=0.90770(6)nm,c=3.049 4(3)nm,β=93.642(4)°,V=4.549 3(6)nm3,Z=2,C34H72N2O2Si6Yb,Mr=1 905.41,Dc=1.288g/cm3,F(000)=1 840.00,μ(MoKα)=22.42cm-1(λ=0.071 070nm).收集独立衍射点7 814个,将其中J>3.00σ(1)的用于结构解析,用全矩阵最小二乘法校正,得最终偏离因子R=0.039,Rw=0.050.8配位的中心镱原子与2个四氢呋喃的氧及2个环戊二烯基配位形成扭曲的四面体结构.
参考文献
[1] | Evans W J,Engerer S C,Piliero P A, et al. J Chem Soc Chem Commun[J] ,1979:1 007 |
[2] | Andrews M P. Organometallics[J] ,1988,743:7 |
[3] | Slater J L,Devore T C,Calder V. Inorg Chem[J] ,1973,12:1 918 |
[4] | Wedler M,Recknagel A,Edelmann F T. J Organomet Chem[J] ,1990,395(2) :C26 |
[5] | Shen Q,Zheng D,Lin L, et al. J Organomet Chem[J] ,1990,391:307 |
[6] | Shen Q,Zheng D,Lin L, et al. J Organomet Chem[J] ,1990,391:321 |
[7] | Fisher E O,Fisher H. Angew Chem[J] ,1964,76:52 |
[8] | QIAN Chang-Tao(钱长涛) ,WANG Bing(王兵). Chemistry(化学通报) [J] ,1993,12:17 |
[9] | Suleimanor C E,Rybakoka L F,Forsyth C M, et al. J Organomet Chem[J] ,1982,235:C19 |
[10] | Deacon G B,Koplick A J. J Organomet Chem[J] ,1978,146:C4 |
[11] | Taylor M D,Cartar C P. J Inorg Nucl Chem[J] ,1962,24:387 |
[12] | Bradely D C,Ghotra J S,Hart F A, et al. J Chem Soc Dalton Trans[ J] ,1973:1 021 |
[13] | Gilman H,Fred W,Atwood A, et al. J Am Chem Soc[ J] ,1940,62:1843 |
[14] | Wilkinson G,Birmingham J M. JAm Chem Soc[J] ,1954,76:6 210 |
[15] | Tilley D T,Andersen R A,Spencer B, et al. Inorg Chem[J] ,1980,19:2 999 |
[16] | Evans W J. Polyhedron[J] ,1987,6:803 |
[17] | Swamy S J,Loebel J,Schumann H. J Organomet Chem[ J] ,1989,379:51 |
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