Abstract

The following adducts of Group III trialkyls with phosphines have been prepared, either by direct reaction in hydrocarbon solution or by displacement of ether from the metal trialkyl etherate: Me 3M·PPh 3 (M = Ga, In); Me 3In·P(2-MeC 6H 4) 3; (R 3M) 2·(Ph 2PCH 2) 2 (R = Me, M = Al, Ga, In; R = Et, M = Ga, In; R = Bu i, M = Al); (Me 3M) 3·(Ph 2PCH 2CH 2) 2PPh (M = Al, Ga, In) and (Me 3M) 4·(Ph 2PCH 2CH 2PPhCH 2) 2 (M = Al, Ga, In). The compounds were analysed by 1H and 31P NMR spectra of (Me 3M) 2·(Ph 2PCH 2) 2 (M = Ga, In) showed little change between 193 K and room temperature. Thermal dissociation of the adducts in vacuo gave the free metal trialkyl with no detectable contamination by the respective phosphine. Crystals of (Me 3M) 2·(Ph 2PCH 2) 2 (M = Al, Ga, In) are iso-structural and the molecules contain two distorted tetrahedral metals bridged by the (Ph 2PCH 2) 2; the MP distances are 2.544(4), 2.546(4) and 2.755(4) Å, respectively. The X-ray crystal structure of (Me 3Al) 3·(Ph 2PCH 2CH 2) 2PPh shows the molecule to contain distorted tetrahedral aluminium atoms bonded to each of the three phosphorus atoms, with AlP distances of 2.536(9) and 2.510(9) Å for the terminal and central moieties, respectively; the unit cell contains two such molecules plus one benzene molecule (the crystallizing solvent).

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