Comprehensive Organometallic Chemistry 3ed Vol 06 Grp 8 by D M P Mingos; Robert H Crabtree

By D M P Mingos; Robert H Crabtree

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The 2JPP values of the 31P{1H} NMR spectra exhibited a strong negative correlation with the sum of the phosphine pKa values. This allows for the prediction of 2JPP values for transFe(CO)3L2 complexes. 156 While the all-Ph derivative did not give a spectrum, the methoxy derivatives did produce [M þ H]þ ions, presumably because of the presence of the basic OMe functions. When Fe(III), dppm, and LiAlH4 were reacted in the presence of CO, various iron carbonyl–halide complexes were formed. 158 FeCl2 .

Additional iron carbonyl fragments that are present can also add to the compound to produce dinuclear complex 35. 121 Based upon their infrared spectra, the complexes were proposed to have cis-carbonyl ligands, with the two iodide ligands trans to each other. Other related benzimidazolyl ligands led to complete CO loss and formation of FeI2(L) with no observed carbonyl-containing intermediates. 122 The product is diamagnetic. 123 The carbonyl ligand could be displaced by isocyanides. Similarly, synthesis and characterization of new monocarbonyl iron(II) complexes with macrocylic borylated bis(dimethylglyoximato) ligands has been reported (Scheme 34).

For 1,2-dibromoethane, a halogenated antimony complex was observed. With Cl(CH2)3Br, a monoalkylation product as observed for the R–I reactions was obtained along with a dialkylation product in which both the antimony and the iron were bonded to carbon (SbFeC3 ring). In contrast, with Br(CH2)4Br, a monoalkylation product as well as one in which the antimony was dialkylated were observed. When the starting compound was the antimony hydride [PPN]2[HSb{Fe(CO)4}3], however, a different reaction with alkyl iodides was observed (Scheme 68).

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