Synthesis and characterisation of nitrile complexes of iron

Autor: Leslie D. Field, Graham R. Purches, Adrian V. George, David C. R. Hockless, Allan H. White, A. Ewan D. McQueen, Brian W. Skelton, Trevor W. Hambley, Elizabeth Y. Malouf, Irmi E. Buys, Stuart R. Pike
Rok vydání: 1997
Předmět:
Zdroj: Journal of Organometallic Chemistry. 538:101-110
ISSN: 0022-328X
DOI: 10.1016/s0022-328x(96)06912-4
Popis: The reaction of cis-[FeH2(DMPE)2] (DMPE = 1,2-bis(dimethylphosphino)ethane) (1a) and trans-[FeCl2(DMPE)2] (7a) with acetonitrile, 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][2PF6] (3a) are monoclinic, space group P2/c, with a = 8.697(3), b = 9.165(5), c = 20.026(5) A, β = 107.54(3)°, Z= 2 and R = 0.058 (2300 F values). Crystals of trans-[Fe(N≡CC3H5)2(DEPE)2][2BF4] (4b) are monoclinic, space group P21/n, with a = 11.146(1), b = 15.396(2), c = 11.810(2) A, β = 111.06(1)°, Z = 2 and R = 0.050 (3011 F values). Crystals of trans-[Fe(N≡CPh)2(DMPE)2][2PF6] (5a) are monoclinic, space group P21/n, with a = 11.006(2), b = 12.351(3), c = 13.650(4) A, β = 93.60(2)°, Z = 2 and R = 0.035 (2650 F values). Crystals of trans-[Fe(p-N≡CC6H4Br)2(DMPE)2][2PF6][0.5KPF6] (6a) are tetragonal, space group I4¯c2, with a = b = 20.015(6), c = 21.610(3) A, β = 90.00°, Z = 8 and R = 0.049 (2235 F values).
Databáze: OpenAIRE
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