MJ Atherton
Pentafluorophenylphosphine complexes of Rhodium(I): Extended x-rayabsorption fine structure studies of[{Rh[PPh(x)(C6F5)(3-x)](2)(mu-Cl)}(n)] (x=0-2) and[{Rh[(C6F5)(2)PCH2CH2P(C6F5)(2)](mu-Cl)}(2)]. Crystal structures of[RhCl(PPh(3)){(C6F5)(2)PCH2CH2P(C6F5
Atherton, MJ; Coleman, KS; Fawcett, J; Holloway, JH; Hope, EG; Karacar, A; Peck, LA; Saunders, GC
Authors
Professor Karl Coleman k.s.coleman@durham.ac.uk
Academic Visitor
J Fawcett
JH Holloway
EG Hope
A Karacar
LA Peck
GC Saunders
Abstract
The NMR spectroscopic properties of the rhodium pentafluorophenylphosphine complexes [{Rh[PPh(x)(C6F5)(3-x)](2)(mu-Cl)}(n)] (x = 0 1, 1 2 or 2 3) and trans-[Rh{PPh(x)(C6F5)(3-x)}Cl-2(CO)] (x = 0 5, 1 6 or 2 7) have been investigated. The new complexes [{Rh[(C6F5)(2)PCH2CH2P(C6F5)(2)] (mu-Cl)}(2)] 4 and cis-[Rh{(C6F5)(2)PCH2CH2P(C6F5)(2)}Cl(CO)] 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 [d(Rh-P) 2.16-2.21, d(Rh-CI) 2.38-2.39, d(Rh ... Rh') 3.50-3.58 Angstrom], whereas complex 1 is a polymer with each Rh ... Rh' distance bridged by one chloride [d(Rh-P) 2.18, d(Rh-CI) 2.36, d(Rh ... Rh') 4.30 Angstrom]. The reaction between [{Rh[(C6F5)(2)PCH2CH2P(C6F5)(2)](mu-Cl)}(2)] and PPh(3) yields the four-coordinate mononuclear rhodium(I) complex [RhCl(PPh(3)){(C6F5)(2)PCH2CH2P(C6F5)(2)}] 9. The crystal structures of 9 and of (C6F5)(2)PCH2CH2P(C6F5)(2) have been determined by X-ray crystallography. Complex 9 crystallizes in the monoclinic space group P2(1)/c with a = 12.707(2), b = 17.066(2), c = 22.003(3) Angstrom, beta = 101.41(1)degrees, Z = 4. Refinement gave final R(1) and wR(2) 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 Angstrom) indicative of an agostic interaction. The phosphine (C6F5)(2)PCH2CH2P(C6F5)(2) crystallizes in the triclinic space group P (1) over bar with a = 5.833(1). b = 10.011(2), c = 11.514(4) Angstrom, alpha = 75.25(2), beta = 88.69(2), gamma = 84.28(2)degrees, Z = 1. Refinement gave final R(1) and wR(2) values of 0.0482 and 0.0987 respectively for 1339 observed reflections.
Citation
Atherton, M., Coleman, K., Fawcett, J., Holloway, J., Hope, E., Karacar, A., …Saunders, G. (1995). Pentafluorophenylphosphine complexes of Rhodium(I): Extended x-rayabsorption fine structure studies of[{Rh[PPh(x)(C6F5)(3-x)](2)(mu-Cl)}(n)] (x=0-2) and[{Rh[(C6F5)(2)PCH2CH2P(C6F5)(2)](mu-Cl)}(2)]. Crystal structures of[RhCl(PPh(3)){(C6F5)(2)PCH2CH2P(C6F5. Journal of the Chemical Society. Dalton transactions, 4029-4037
Journal Article Type | Article |
---|---|
Publication Date | 1995-12 |
Journal | Dalton transactions. |
Print ISSN | 0300-9246 |
Publisher | Royal Society of Chemistry |
Peer Reviewed | Peer Reviewed |
Issue | 24 |
Pages | 4029-4037 |
Keywords | CURVED-WAVE THEORY; EXAFS CALCULATIONS |
Public URL | https://durham-repository.worktribe.com/output/1576290 |
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