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The tris(cyanoethyl)phosphine (tcep) complexes trans-[PtCl2(tcep)2], cis-[PtMe2(tcep)2], and trans-[PtMeCl(tcep)2] are prepared by treatment of the corresponding [PtXY(cod)] (cod = 1,5-cyclooctadiene) with tcep. Reduction of trans-[PtCl2(tcep)2] with NaBH4 gives trans-[PtHCl(tcep)2] which, in the presence of tcep and NEt3, gives the coordinatively unsaturated platinum(0) complex [Pt(tcep)3]. This coordinatively unsaturated species is also formed when [Pt(norbornene)3] reacts with tcep. [Pt(tcep)3] is very unreactive compared to its PEt3 analogue: it is air-stable and does not react with further tcep to form an 18-electron species. It is protonated by HBF4 · OEt2 to form [PtH(tcep)3]BF4. The complex trans-[PdCl2(tcep)2] is made from [PdCl2(NCPh)2] and tcep and the derivatives trans-[PdX2(tcep)2] (X = Br or I) are made by metathesis of the dichloro complex. Reduction of trans-[PdCl2(tcep)2] with LiOMe in the presence of tcep gave the palladium(0) complex [Pd(tcep)3] which, like its platinum(0) analogue, undergoes exchange with free tcep on the NMR timescale. The palladium complex reacts with dibenzylideneacetone (dba) to form [Pd(eta2-dba)(tcep)2]; the same product is formed in the reaction of [Pd(eta2-dba)2] and tcep. Reaction of [Pd2Cl2(eta3-C3H3) 2] and tcep gives [PdCl(tcep)(eta3-C3H3)] or [Pd(tcep)2(eta3-C3H3)]Cl depending on stoichiometry. The rhodium(I) and iridium(I) complexes trans-[MCl(CO)(tcep)2], [MCl(tcep)(cod)] and [MCl(tcep)3] are all readily made from tcep and an appropriate precursor. All new compounds have been fully characterised by a combination of elemental analysis, IR, 31P, 13C, 1H and 195Pt NMR spectroscopy. The crystal structure of [IrCl(tcep)3] as a MeCN solvate shows a distorted square planar coordination geometry (trans angles at Ir(I) ca. 164, cis P-Ir-P av. 96, cis P-Ir-Cl av. 85). Analysis of the conformations of tcep ligands in this and other published tcep complexes shows there is a preference for conformations in which aaa, aag or g+g- (a = anti, g = gauche) arrangements of the three M-P-C-C chains are avoided.
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Reference：
Synthesis and Crystal Structure of a Chiral C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis,
Chiral lanthanide(III) complexes of sulphur–nitrogen–oxygen ligand derived from aminothiourea and sodium D-camphor-β-sulfonate