Synthesis and characterisation of tungsten and rhenium aluminopolyhydrides: X-ray crystal structures of (Me3P)3H3W(µ-H)2Al(H)(µ-OBun)2Al(H)(µ-H)2WH3(PMe3)3and (Me3P)3H3W(µ-H)2Al(H)(µ-H)2WH3(PMe3)3
Andrew R. BarronD. LyonsGeoffrey WilkinsonMajid MotevalliAndrew HowesMichael B. Hursthouse
Abstract
The reaction of WCl4(PMe3)3 with LiAlH4 in refluxing tetrahydrofuran leads to the aluminopolyhydride, (Me3P)3H3W(µ-H)2Al(H)(µ-OBun)2Al(H)(µ-H)2WH3(PMe3)3(1), whereas in diethyl ether the product is (Me3P)3H3W(µ-H)2Al(H)(µ-H)2Al(H)(µ-H)2WH3(PMe3)3(2). Addition of NNN′N′-tetramethylethylenediamine to a toluene solution of (2) results in the formation of (Me3P)3H3W(µ-H)2Al(H)(µ-H)2WH3(PMe3)3(3). The rhenium analogues of (1) and (2), namely compounds (Me2PhP)3H2Re(µ-H)2Al(H)(µ-OBun)2Al(H)(µ-H)2ReH2(PMe2Ph)3(4) and (Me2PhP)3H2Re(µ-H)2Al(H)(µ-H)2Al(H)(µ-H)2ReH2(PMe2Ph)3(5) have been obtained from ReCl3(PMe2Ph)3. The heavy-atom structures of (1) and (3) have been confirmed by X-ray crystallography. Hydrogen-1, 31P, and 27Al n.m.r. spectra are reported and the fluxional behaviour of the compounds discussed.
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