Bis-indenyl molybdenum(IV) halide complexes: synthesis and X-ray studies


A stepwise route to bis-indenyl halide derivatives of molybdenum is reported. Treatment of [Ind(2)Mo(CO)(2)][BF4](2) with one equivalent of Bu4NBr in CH2Cl2 yielded [Ind(2)Mo(CO)Br][BF4] (1). When 1 was refluxed in NCMe and irradiated with a 60 W tungsten bulb [Ind(2)Mo(NCMe)Br][BF4] (2) was isolated. The reaction of [Ind(2)Mo(CO)Br][BF4] with LiBr afforded Ind(2)MoBr(2) (3). The Ind(2)MoCl(2) (4) analogue has been prepared directly by reaction of [Ind(2)Mo(CO)(2)][BF4](2) with LiCl. The reaction of Ind(2)MoBr(2) with AlMe3 in toluene produces the bromo-methyl species Ind(2)MoBrMe (5). Treatment of Ind(2)MoBr(2) with TlPF6 in the presence of P(OMe)(3) afforded [Ind(2)Mo{P(OMe)(3)}(2)][PF6](2) (6) which was readily reduced by two equivalents of cobaltocene to yield the neutral species Ind(2)Mo{P(OMe)(3)}(2) (7). Reaction of [Ind(2)Mo( CO)(2)][BF4](2) with P(OMe)(3) in dichloromethane yielded [Ind(2)Mo(CO)Cl][BF4] (8). The molecular structures of [Ind(2)Mo(CO)X][BF4] [X = Cl (8) or Br (1)], Ind(2)MoBr(2) (3) and [Ind(2)Mo{P(OMe)(3)}(2)][PF6](2) (6) have been determined by single crystal X-ray diffraction. The synthesis and characterisation of [(eta(3)-Ind)Mo(CO)(2)](2)[mu-eta(5)-eta(5)-(C5H4)(2)SiMe2] (9) is also reported.



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Drew, MGB; Felix, V; Romao, CC; Royo, B

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