期刊文献+

Synthesis and Structures of New Cyclopalladated Ferrocenylimines

Synthesis and Structures of New Cyclopalladated Ferrocenylimines
下载PDF
导出
摘要 The new complexes, [PdCl{C5H4FeC5H4CHRN=CHC4H3O}(Ph3P)] (R= H, CH3) were synthesized via two novel Schiff bases (C5H5FeC5H4CHRN=CHC4H3O, R= H, CH3) with lithium tetrachloropalladate (Ⅱ), and characterized by IR, elemental analysis, ^1H NMR. Complex 5a was further determined by X-ray single crystal diffraction. We found that it contained an intramolecular N→Pd coordination in the compound 5a, and the palladium atom was bound to the unsubstituted Cp ring. The Pd-N, Pd-C (I) and Pd-O bond lengths were 2.121 (3), 2.008 (4) and 2.990 )A, respectively. The new complexes, [PdCl{C5H4FeC5H4CHRN=CHC4H3O}(Ph3P)] (R= H, CH3) were synthesized via two novel Schiff bases (C5H5FeC5H4CHRN=CHC4H3O, R= H, CH3) with lithium tetrachloropalladate (Ⅱ), and characterized by IR, elemental analysis, ^1H NMR. Complex 5a was further determined by X-ray single crystal diffraction. We found that it contained an intramolecular N→Pd coordination in the compound 5a, and the palladium atom was bound to the unsubstituted Cp ring. The Pd-N, Pd-C (I) and Pd-O bond lengths were 2.121 (3), 2.008 (4) and 2.990 )A, respectively.
出处 《Chinese Chemical Letters》 SCIE CAS CSCD 2006年第3期317-320,共4页 中国化学快报(英文版)
基金 the National Natural Science Foundation of China (No. 20472074) the Natural Science Foundation of Henan Province (411020200) for financial support of this work.
关键词 Heteroannular FERROCENYLIMINE cyclopalladated. Heteroannular, ferrocenylimine, cyclopalladated.
  • 相关文献

参考文献8

  • 1[1](a) B.M.Trost,D.V.Voranke,Chem.Rev.,1996,96,39.(b) X.L.Cui,Y.J.Wu,C.X.Du,et al.,Tetrahedron:Asymmetry,1999,10,1255.(c) A.D.Ryabov,Chem.Rev.,1990,90,403.(d) C.Navarro-Ranninger,J.López Solera,J.M.Pérez,et al.,Appl.Organomet.Chem.,1993,7,57.
  • 2[2](a) S.Q.Huo,Y.J.Wu,C.X.Du,et al.,J.Organomet.Chem.,1994,483,139.(b) Y.J.Wu,S.Q.Huo,Y.Zhu,J.Organomet.Chem.,1995,485,161.(c) Y.J.Wu,Y.H.Liu,X.L.Cui,Polyhedron,1996,15,3315.(d) Y.J.Wu,Y.H.Liu,Polyhedron,1997,16,335.(e) G.Zhao,Q.G.Wang,T.C.W.Mark,J.Organomet.Chem.,1999,574,311.(f) R.Bosque,C.López,J.Sales,J.Organomet.Chem.,1995,498,147.
  • 3[3]F.Ossola,P.Tomasin,F.Benetollo,et al.,Inorganica Chimica Acta.,2003,353,292.
  • 4[4](a) Selected analytical and spectral data:Compound 4a,Yellow crystals,yield:70%; m.p.85-87℃.Anal.Calcd.for C16H15FeNO:C,65.56,H,5.16,N,4.78.Found:C,65.60,H,5.06,N,4.80%.1H NMR:(400 MHz,CDCl3,δ ppm):4.54 (s,2H),4.21 (d,2H,J=1.6 Hz),7.50 (s,1H),4.15 (s,5H),6.74 (d,2H,J=3.6 Hz),4.14 (d,2H,J=1.2 Hz),6.46 (2d,1H,J=1.6Hz),8.04 (s,1H).IR (KBr):v 1642.99 (Vc=N),1000.69,1100 (unsubstituted cyclopentaldienylring) cm-1.(b) Selected analytical and spectral data:Compound 4b,Yellow crystals,yield:56%; m.p.91-94°; Anal.Calcd.For C17H17FeNO:C,66.47,H,5.58,N,4.56.Found:C,66.50,H,5.56,N,4.56%.1H NMR:(400 MHz,CDCl3,δ ppm):4.14-4.49 (m,4H,substituded Cp-ring H),4.14 (s,5H,unsubstituded H),1.59 (d,3H,J= 6.6),4.21 (m,1H),6.47,6.72,7.26 (m,3H),7.51 (s,1H).IR (KBr):v 1642.00 (vc=N),1000.59,1100 (unsubstituted cyclopentaldienyl ring)cm-1.
  • 5[5](a) Selected analytical and spectral data:Compound 5a,Yield:76%; m.p.176-179℃; Anal.Calcd.for C34H29ClFeNOPPd:C,58.65,H,4.20,N,2.01.Found:C,58.60,H,4.22,N,2.05%.1H NMR:(400 MHz,CDCl3,δ ppm):3.40-4.87 (m,10H),6.58-7.99 (m,18H),8.17 (s,1H);IR:(KBr):v 1637.69,1479.58,1436.38,1097.68,1027.25 cm-1.(b) Selected analytical and spectral data:Compound 5b,Yield:59%; m.p.205-207 ℃; Anal.Calcd.for C35H31ClFeNOPPd:C,59.02,H,4.34,N,1.88.Found:C,59.15,H,4.36,N,1.97%.1H NMR:(400 MHz,CDCl3,δ ppm):3.52-4.44 (m,8H),6.58-7.99 (m,18H),8.13 (s,1H),2.02(d,3H),1.54 (m,1H); IR:(KBr):v 3447,1712,1639,1479,1223,1096,1019,868,535,494 cm-1.
  • 6[6]G.M.Sheldrick SHELXL97 Program for Crystal Structure Refinement,University of Gottingen,Germany 1997.
  • 7[7](a) M.Rosenblum,R.B.Woodward,J.Am.Chem.Soc.,1958,80,5443.(b) K.L.Rinehart,Jr.K.L.Motz,S.Moon,J.Am.Chem.Soc.,1957,79,2749.(c) S.P.Moinarand,M.Orchin,J.Organomet.Chem.,1969,16,169.(d) M.Orchin,P.L.Schimdt,Coord.Chem.Rev.,1968,2,345.(e) M.Onoue,K.Minami,K.Nakagawa,Bull Chem.Soc.Jpn.,1970,43,3480
  • 8[8]Crystal structural determinations of 5a:Intensity data were collected at 291(2) K on a Rigaku RAXIS-Ⅳ diffractometer.The crystal data were as follows:5a,C34H29ClFeNOPPd,monoclinic,space group P2(1)/c,a = 9.673(19),b = 17.583(4),c = 17.351(4) A,β = 92.19(3)°,Z = 4,V = 2949.0(10)A3,R = 0.0351,wR = 0.0611.

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部