Pentafluorophenylphosphine Complexes of Rhodium(I): Extended X-Ray Absorption Fine Structure Studies of x(C6F5)3-x>2(μ-Cl))n> (x = 0-2) and (μ-Cl))2>. Crystal Structures of *C4H8O and (C6F5)2PCH2CH2P(C6F5)2

DOI: 10.1039/DT9950004029

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 4029 - 4038 (1995)

Update date:2022-07-30

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Authors:

Atherton, Malcolm J.

Coleman, Karl S.

Fawcett, John

Holloway, John H.

Hope, Eric G.

et al. et al.

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Article abstract of DOI:10.1039/DT9950004029

The NMR spectroscopic properties of the rhodium pentafluorophenylphosphine complexes <(Rhx(C6F5)_3-x>2(μ-Cl))_n> (x = 0 1, 1 2 or 2 3) and trans-x(C6F5)_3-x)2Cl(CO)> (x = 0 5, 1 6 or 2 7) have been investigated.The new complexes <(Rh<(C6F5)2PCH2CH2P(C6F5)2>(μ-Cl))2> 4 and cis- 8 have been prepared.A rhodium K-edge extended X-ray absorption fine structure (EXAFS) study of complexes 1-4 has been performed, and confirms that complexes 2, 3 and 4 are dimers with each Rh...Rh' distance bridged by two chlorides , whereas complex 1 is a polymer with each Rh...Rh' distance bridged by one chloride .The reaction between <(Rh<(C6F5)2PCH2CH2P(C6F5)2>(μ-Cl))2> and PPh3 yields the four-co-ordinate mononuclear rhodium(I) complex 9.The crystal structures of 9 and of (C6F5)2PCH2CH2P(C6F5)2 have been determined by X-ray crystallography.Complex 9 crystallizes in the monoclinic space group P2₁/c with a = 12.707(2), b = 17.066(2), c = 22.003(3) Angstroem, β = 101.41(1) deg, Z = 4.Refinement gave final R₁ and wR₂ values of 0.0429 and 0.0715 for 5193 observed reflections.The geometry about the rhodium atom is distorted-square planar and there is a short distance between an ortho-hydrogen atom of the triphenylphosphine ligand and the rhodium atom (2.699 Angstroem) indicative of an agostic interaction.The phosphine (C6F5)2PCH2CH2P(C6F5)2 crystallizes in the triclinic space group P1<*> with a = 5.833(1), b = 10.011(2), c = 11.514(4) Angstroem, α = 75.25(2), β = 88.69(2), γ = 84.28(2) deg, Z = 1.Refinement gave final R₁ and wR₂ values of 0.0482 and 0.0987 respectively for 1339 observed reflections.

Full text of DOI:10.1039/DT9950004029

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