Preparation of a N-ferrocenyl-amidinate complex was achieved by employing (TMEDA)Li[(CpFeC5H4)NC(Ph)NSiMe3] (1) to prepare Cp*Zr[(CpFeC5H4)NC(Ph)NSiMe3]Cl2(2). Complex 2exhibited poor polymerization activity and thus a series of C-ferrocenyl bis(amidinate) complexes of the type M(L)2Cl2(M = Zr, 4; M = Ti, 5; L = (CyNC(CpFeC5H4)NCy) were synthesized viareaction of ferrocenyl-amidine, H(L) and M(NMe2)2Cl2(M = Ti, Zr·2THF). Half sandwich mono(amidinate) complexes, Cp′ZrLCl2(Cp′ = Cp, 7; Cp′ = Cp*, 8), were prepared by the reaction of Cp′ZrCl3with Li(L) and subsequently alkylated to give M(L)2Me2(M = Zr, 9; M = Ti, 11), CpZr(L)(CH2Ph)2(12) and Cp*Zr(L)Me2(10) with the appropriate alkylating agent. Abstraction of a methyl group from 7with B(C6F5)3and [Ph3C][B(C6F5)4] proceeded cleanly to give [{CyNC(CpFeC5H4)NCy}2ZrMe][MeB(C6F5)3] 13and [{CyNC(CpFeC5H4)NCy}2ZrMe][B(C6F5)4] 14, respectively. Similarly, the analogous CpZr and Cp*Zr derivatives LZr{CyNC(CpFeC5H4)NCy}CH2Ph] [PhCH2B(C6F5)3] L = Cp 15, Cp* 17and [LZr{CyNC(CpFeC5H4)NCy}CH2Ph][B(C6F5)4] L = Cp 16, Cp* 18were prepared. Cyclic voltammetry studies on the metal complexes containing ferrocenyl-amidinates reveal quasi reversible oxidation and reduction waves for the ferrocene/ferrocenium couple. The dichloride complexes (4–8) activated with MAO and dialkyl complexes (9,10) activated with B(C6F5)3and [Ph3C][B(C6F5)4] showed low ethylene polymerization activities. [ABSTRACT FROM AUTHOR]