HYDRIDE ABSTRACTION FROM [PPN](2)[HSB(FE(CO)(4))(3)] BY ALKYL IODIDES- SYNTHESIS AND CHARACTERIZATION OF [PPN][SB(ME)I(FE(CO)(4))(2)]

[PPN](2)[HSb{Fe(CO}(4))(3)] ([PPN](2)[I]) was reacted with Mel and EtI . The reaction with Mel yielded [PPN][Sb(Me)I{Fe(CO)(4)}(2)] ([PPN][II ]) whereas the reaction with EtI yielded [PPN](2)[ISb(Fe(CO)(4)}(3)] ( [PPN](2)[III]) instead. The structure of [PPN](2)[II] was determined b y single crystal X-ray diffraction. [PPN][II] crystallizes in the mono clinic space group C2/c (# 15) with a = 14.115(3) Angstrom, b = 17.123 (3) Angstrom, c = 18.913(4) Angstrom, beta = 97.06(3), V= 4536.4(16) A ngstrom(3), Z = 4, R-1 (I > 2 sigma(I)) = 0.0691 and wR(2) = 0.1900. A nalysis of the off gases indicated the presence of methane for [PPN][I I] and ethane for [PPN](2)[III]. The possibility of the formation of [ PPN](2)[III] via a radical chain mechanism was excluded by performing the reaction at high dilution, in the dark and in the presence of BHT. (C) 1998 Elsevier Science S.A. All rights reserved.