Synthesis and characterisation of nitrile complexes of iron

A.V. George, L.D. Field, E.Y. Malouf, A.E.D. Mcqueen, S.R. Pike, G.R. Purches, T.W. Hambley, I.E. Buys, Allan White, D.C.R. Hockless, Brian Skelton

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Abstract

The reaction of cis-[FeH2(DMPE)(2)] (DMPE = 1,2-bis(dimethylphosphino)ethane) (la) and trans-[FeCl2(DMPE)(2)] (7a) with acetornitrile, cyanocyclopropane. benzonitrile p-bromobenzonitrile and terephthalonitrile and reaction of trans-[FeCl2(DEPE)(2)] (DEPE = 1,2-bis(diethylphosphino)ethane) (7b) with acetonitrile, cyanocyclopropane and benzonitrile in methanol solution resulted in a series of nitrile chloride complexes trans-[FeCl(N=C-R)(PP)(2)](+) and bis-nitrile complexes trans-[Fe(N=C-R)(2)(PP)(2)](2+) of iron. All of the complexes have been characterised spectroscopically and four bis-nitrile complexes have been characterised crystallographically. Crystals of trans-[Fe(N=CCH3)(2)(DMPE)(2)][2PF(6)] (3a) are monoclinic, space group P 2/c, with a = 8.697(3), b = 9.165(5), c = 20.026(5) Angstrom, beta = 107.54(3)degrees, Z = 2 and R = 0.058 (2300 F values).Crystals of trans-[Fe(N=CC3H5)(2)(DEPE)(2)][2BF(4)] (4b) are monoclinic, space group P2(1)/n, with a = 11.146(1), b = 15.396(2), c = 11.810(2) Angstrom, beta = 111.06(1)degrees, Z = 2 and R = 0.050 (3011 F values). Crystals of trans-[Fe(N=CPh)(2)(DMPE)(2)][2PF(6)] (5a) are monoclinic, space group P2(1)/n, with a = 11.006(2), b = 12.351(3), c = 13.650(4) Angstrom, beta = 93.60(2)degrees, Z = 2 and R = 0.035 (2650 F values). Crystals of trans-[Fe(p-N=CC6H4Br)(2)(DMPE)(2)][2PF(6)][0.5KPF(6)] (6a) are tetragonal, space group , with a = b = 20.015(6), c = 21.610(3)Angstrom, beta = 90.00 degrees, Z = 8 and R = 0.049 (2235 F values).
Original languageEnglish
Pages (from-to)101-110
JournalJournal of Organometallic Chemistry
Volume538
DOIs
Publication statusPublished - 1997

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