Abstract
The reactions of ditungsten hexa- t-butoxide, W 2(OCMe 3) 6, with dicyclohexylcarbodiimide, C 6H 11NCNC 6H 11, and diisopropylcarbodiimide, Me 2CHNCNCHMe 2, afford the 1:1 adducts, [W(OCMe 3) 3] 2(μ-C 6H 11NCNC 6H 11), 1, and [W(OCMe 3) 3] 2(μ-C 3H 7NCNC 3H 7), 2, respectively. These products were each shown by X-ray crystallography to be structurally homologous to the previously reported [W(OCMe 3) 3] 2(μ-CH 3C 6H 4NCNC 6H 4CH 3) and similar to [W(OCMe 3) 3(μ-C 6H 5NCO). It has been shown that the [W(OCMe 3) 3] 2(μ-RNCNR) compounds fail to react with further RNCNR, with PhNCO, PMe 3, LiOCMe 3 or LiOCHMe 2, CO or CO 2, and also that [W(OCMe 3) 3] 2(μ-PhNCO) does not afford any defined product when treated with C 6H 11NCNC 6H 11. Compounds 1 and 2 were fully characterized by IR and NMR spectroscopy and by X-ray crystallography. Compound 1 crystallizes in space group C2/ c with unit cell dimensions a = 13.481(3) Å, b = 18.129(4) Å, c = 18.244(2) Å, β = 97.54(1)°, V = 4420(2) Å 3, Z = 4. It was refined to R = 0.0375, R w = 0.0475. Compound 2 crystallizes in space group P2 1/ c with unit cell dimensions a = 14.752(2) Å, b = 12.157(3) Å, c = 22.189(3) Å, β = 97.03(2)°, V = 3949(2) Å 3, Z = 4. The structure was refined to R = 0.053, R w = 0.059. Each molecule has C 2-symmetry, with two W(OCMe 3) units united by RNCNR bridges across WW distances of 2.490(1) and 2.485(1) Å for 1 and 2, respectively.
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