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Reaction of a solution of [LaL3(Ph3PO)][L = N(SiMe3)2] with Ph2PH followed by Ph3PO yields [LaL2(PPh2)(Ph3PO)2], which has been isolated as highly air-sensitive orange crystals and characterised by solution NMR spectroscopy (31P and 1H) and X-ray crystallography. The structure was refined to a final R value of 0.056 and shows the complex to have a terminal PPh2– ligand with planar co-ordination at P. Variable-temperature 31P NMR spectroscopy indicates rapid exchange between free and co-ordinated Ph3PO at room temperature but at 193 K is consistent with the solid-state structure with two Ph3PO ligands.
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Aspinall et al. (1992) studied this question.
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