Synthesis and Spectroscopic Properties of the 'Mixed' Seven-co-ordinate Complexes and Rearrangement of Selected to . X-Ray Crystal Structure of <WI3(CO)3(S...

DOI: 10.1039/DT9880002729

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 2729 - 2734 (1988)

Update date:2022-08-04

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Authors:

Baker, Paul K.

Fraser, Stuart G.

Drew, Michael G. B.

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Article abstract of DOI:10.1039/DT9880002729

Reaction of the complexes (M=Mo or W) with 1 equivalent of L (L=PPh3, AsPh3, or SbPh3) in CH2Cl2 at room temperature followed by 1 equivalent of L' in situ affords the 'mixed' seven-co-ordinate compounds .Low-temperature (-70 deg C, CD2Cl2) (13)C n.m.r. spectra of the triphenylantimony complexes showed two carbonyl resonances.This indicated capped octahedral geometry with a carbonyl ligand in the unique capping position.Some of the neutral seven-co-ordinate complexes containing phosphines disproportionated in CH2Cl2 to give the salts . (31)P N.m.r. spectroscopy and negative ion mass spectrometry confirmed that the more electron-rich phosphine is protonated in .The structure of the complex *Et2O was determined by X-ray analysis.The co-ordination geometry about the tungsten is capped octahedral with a carbonyl ligand in the unique capping position.The capped face contains two carbonyl groups and the triphenylantimony ligand, with the three iodide ligands occupying the uncapping face.The low-temperature (-70 deg C, CD2Cl2) spectrum of the related complex n4> prepared by treating in situ with 1 equivalent of n4>I in CH2Cl2 showed two carbonyl resonances at δ=209.68 and 235.50 p.p.m. with an intensity ratio of 2:1.The lower-field resonance can be ascribed to the unique capping carbonyl ligand and the higher-field resonance to the two equivalent carbonyl ligands on the octahedron.The low-temperature (13)C n.m.r. spectrum of n4> shows a single resonance at δ=222.20 p.p.m. which suggests a different capped octahedral structure with the triphenyphosphine ligand capping the three carbonyl ligands.

Full text of DOI:10.1039/DT9880002729

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