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 MP 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 AlP 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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