Synthesis and reactivity of fluoro complexes: Part 2. Rhodium(I) fluoro complexes with alkene and phosphine ligands. Synthesis of the first isolated rhodium(I) bifluoride complexes. Structure of [Rh3(mu3-OH)2(COD)(3)](HF2) by X-ray powder diffraction

Inorganic Chemistry
José VicenteNorberto Masciocchi

Abstract

The reaction between [Rh(mu-OH)(COD)](2) (COD = 1,5-cyclooctadiene) and 73% HF in THF gives [Rh(3)(mu(3)-OH)(2)(COD)(3)](HF(2)) (1). Its crystal structure, determined by ab initio X-ray powder diffraction methods (from conventional laboratory data), contains complex trimetallic cations linked together in 1D chains by a mu(3)-OH...F-H-F...HO-mu(3) sequence of strong hydrogen bonds. The complex [Rh(mu-F)(COE)(2)](2) (COE = cyclooctene; 2), prepared by reacting [Rh(mu-OH)(COE)(2)](2) with NEt(3).3HF (3:2), has been characterized. Complex 1 reacts with PR(3) (1:3) to give [RhF(COD)(PR(3))] [R = Ph (3), C(6)H(4)OMe-4 (4), (i)Pr (5), Cy (6)] that can be prepared directly by reacting [Rh(mu-OH)(COD)](2) with 73% HF and PR(3) (1:2:2). The reactions of 1 with PPh(3) or Et(3)P have been studied by NMR spectroscopy at different molar ratios. Complexes [RhF(PEt(3))(3)] (7), [RhF(COD)(PEt(3))] (8), and [RhF(PPh(3))(3)] (9) have been detected. The complex [Rh(F)(NBD)(iPr(3)P)] (NBD = norbornadiene; 10) was prepared by the sequential treatment of [Rh(mu-OMe)(NBD)](2) with 1 equiv of NEt(3).3HF and (i)Pr(3)P. The first isolated bifluoride rhodium(I) complexes [Rh(FHF)(COD)(PR(3))] [R = Ph (11), (i)Pr (12), Cy (13)], obtained by reacting fluoro...Continue Reading

References

Mar 12, 2004·Journal of the American Chemical Society·Vladimir V Grushin, William J Marshall

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Citations

Jul 18, 2015·Dalton Transactions : an International Journal of Inorganic Chemistry·Mateusz K CybulskiMichael K Whittlesey
Nov 2, 2014·Chemical Communications : Chem Comm·Byron J TruscottSteven P Nolan
Dec 16, 2011·Chemistry : a European Journal·Thomas VergoteTom Leyssens
Aug 4, 2015·ChemCatChem·Fady NahraSteven P Nolan
Sep 14, 2018·Dalton Transactions : an International Journal of Inorganic Chemistry·Kai YueFeng-Bo Xu
Sep 30, 2005·Dalton Transactions : an International Journal of Inorganic Chemistry·Thomas BraunHans-Georg Stammler
Nov 2, 2006·Dalton Transactions : an International Journal of Inorganic Chemistry·Thomas BraunHans-Georg Stammler
Jun 11, 2015·Chemistry : a European Journal·Brandon K TateJoseph P Sadighi
Jan 24, 2014·Angewandte Chemie·Lada ZámostnáBeatrice Braun
Jul 9, 2011·Dalton Transactions : an International Journal of Inorganic Chemistry·Richard C BauerJarl Ivar van der Vlugt
Aug 26, 2010·Inorganic Chemistry·Sung Ok KangKristin Bowman-James
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Oct 27, 2005·Journal of the American Chemical Society·Stuart A MacgregorVladimir V Grushin

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