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摘要
Complexes of three related 1-azapentadienyl ligands [N(SiMe(2)R(1))C(Bu(t))(CH)(3)SiMe(2)R](-), abbreviated as L (R = Bu(t), R(1) = Me), L' (R = Me = R(1)), and L '' (R = Bu(t) = R(1)), are described. The crystalline compounds Sn(L)(2) (1), Sn(L')(2) (2), [Sn(L')(mu-Cl)](2) (3) and [Sn(L '')(mu-Cl)](2) (4) were prepared from SnCl(2) and 2 K(L), 2 K(L'), K(L') and K(L ''), respectively, in thf. Treatment of the appropriate lithium 1-azapentadienyl with Si(Cl)Me(3) yielded the yellow crystalline Me(3)Si(L) (5) and the volatile liquid Me(3)Si(L') (6) and Me(3)Si(L '') (7), each being an N,N,C-trisilyldieneamine. The red, crystalline Fe(L)(2) (8) and Co(L')(2) (9) were obtained from thf solutions of FeCl(2) with 2 Li(L)(tmeda) and CoCl(2) with 2 K(L'), respectively. Each of 1-9 gave satisfactory C, H, N analyses; 6 and 7 (GC-MS) and 1, 2, 8 and 9 (MS) showed molecular cations and appropriate fragments (also 3 and 4). The (1)H, (13)C and (119)Sn NMR (1-4) and IR spectra support the assignment of 1-4 as containing Sn-N(SiMe(2)R(1))C( Bu(t))(CH)(3)SiMe(2)R moieties and 5-7 as N(SiMe(3))(SiMe(2)R(1))C(Bu(t))(CH)(3)SiMe(2)R molecules; for 1-4 this is confirmed by their X-ray structures. The magnetic moments for 8 (5.56 mu(B)) and 9 (2.75 mu(B)) are remarkably close to the appropriate Fe and Co complex [M{eta(3)-N(SiMe(3))C(Bu(t))C(H)SiMe(3)}(2)]; hence it is proposed that 8 and 9 have similar metal-centred, centrosymmetric, distorted octahedral structures.
- 出版日期2009-11-1
- 单位中国科学技术大学
