Crystal structure of [SP-5-(R
 *,R
 *)]-(+/−)-chloro(1,1,4,7,10,10-hexaphenyl-1,4,7,10-tetraphosphadecane)nickel(II) hexafluorophosphate, C42H42ClF6NiP5

Airey, Anthea L.; Hockless, David C. R.; Swiegers, Gerhard F.; Wild, S. B.

doi:10.1524/zkri.1996.211.12.939

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“…X-ray crystal structure analyses identified the orange crystals as ( M Ni )-[Ni{( R , R )-tetraphos}]·0.5Et 2 O and the yellow crystals as ( M Ni , M Ni )-[Ni 2 {( R , R )-tetraphos}]·0.5Et 2 O. Crystallographic data and associated experimental details for the complexes are given in Table . The crystal structures of the racemates (±)-[NiCl{( R *, R *)-tetraphos}]PF 6 and (±)-[Ni{( R *, R *)-tetraphos}](ClO 4 ) 2 have been determined previously.…”

Section: Resultsmentioning

confidence: 99%

Synthesis, Structure, and Electrochemistry of Di- and Zerovalent Nickel, Palladium, and Platinum Monomers and Dimers Derived from an Enantiopure (S,S)-Tetra(tertiary Phosphine)

et al. 2007

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The ligand (S,S)-1,1,4,7,10,10-hexaphenyl-1,4,7,10-tetraphosphadecane, (S,S)-tetraphos, reacts with hexa(aqua)nickel(II) chloride in the presence of trimethylsilyl triflate (TMSOTf) in dichloromethane to give the yellow square-planar complex [Ni{(R,R)-tetraphos}](OTf)2, which has been crystallographically characterized as the square-pyramidal, acetonitrile adduct [Ni(NCMe){(R,R)-tetraphos}]OTf. Cyclic voltammograms of the nickel(II) complex in dichloromethane and acetonitrile at 20 degrees C showed two reduction processes at negative potentials with oxidative (E(p)(ox)) and reductive (E(p)(red)) peak separations similar to those observed for ferrocene/ferrocenium under identical conditions, suggesting two one-electron steps. The cyclic voltammetric data for the divalent nickel complex in acetonitrile at temperatures below -20 degrees C were interpreted according to reversible coordination of acetonitrile to the nickel(I) and nickel(0) complexes. The divalent palladium and platinum complexes [M{(R,R)-tetraphos}](PF6)2 and [M2{(R,R)-tetraphos}2](OTf)4 have been prepared. The reduction potentials for the complexes [M{(R,R)-tetraphos}](PF6)2 increase in the order nickel(II) < palladium(II) < platinum(II). The reaction of (S,S)-tetraphos with bis(cycloocta-1,5-diene)nickel(0) in benzene affords orange [Ni{(R,R)-tetraphos}], which slowly rearranges into the thermodynamically more stable, yellow, double-stranded helicate [Ni2{(R,R)-tetraphos}2]; the crystal structures of both complexes have been determined. The reactions of (S,S)-tetraphos with [M(PPh3)4] in toluene (M = Pd) or benzene (M = Pt) furnish the double-stranded helicates [M2{(R,R)-tetraphos}2]; the palladium complex crystallizes from hot benzene as the 2-benzene solvate and was structurally characterized by X-ray crystallography. In each of the three zerovalent complexes, the coordinated (R,R)-tetraphos stereospecifically generates tetrahedral M(PP)2 stereocenters of M configuration.

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Section: Resultsmentioning

confidence: 99%

Synthesis, Structure, and Electrochemistry of Di- and Zerovalent Nickel, Palladium, and Platinum Monomers and Dimers Derived from an Enantiopure (S,S)-Tetra(tertiary Phosphine)

et al. 2007

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Crystal structure of [SP-5-(R ^,R ^)]-(+/−)-chloro(1,1,4,7,10,10-hexaphenyl-1,4,7,10-tetraphosphadecane)nickel(II) hexafluorophosphate, C₄₂H₄₂ClF₆NiP₅

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Synthesis, Structure, and Electrochemistry of Di- and Zerovalent Nickel, Palladium, and Platinum Monomers and Dimers Derived from an Enantiopure (S,S)-Tetra(tertiary Phosphine)

Synthesis, Structure, and Electrochemistry of Di- and Zerovalent Nickel, Palladium, and Platinum Monomers and Dimers Derived from an Enantiopure (S,S)-Tetra(tertiary Phosphine)

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Crystal structure of [SP-5-(R *,R *)]-(+/−)-chloro(1,1,4,7,10,10-hexaphenyl-1,4,7,10-tetraphosphadecane)nickel(II) hexafluorophosphate, C42H42ClF6NiP5

Cited by 1 publication

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Synthesis, Structure, and Electrochemistry of Di- and Zerovalent Nickel, Palladium, and Platinum Monomers and Dimers Derived from an Enantiopure (S,S)-Tetra(tertiary Phosphine)

Synthesis, Structure, and Electrochemistry of Di- and Zerovalent Nickel, Palladium, and Platinum Monomers and Dimers Derived from an Enantiopure (S,S)-Tetra(tertiary Phosphine)

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Crystal structure of [SP-5-(R ^,R ^)]-(+/−)-chloro(1,1,4,7,10,10-hexaphenyl-1,4,7,10-tetraphosphadecane)nickel(II) hexafluorophosphate, C₄₂H₄₂ClF₆NiP₅