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1,4,7-trithiacyclononane ([9]aneS3) and 2,5,8-trithia[9]orthocyclophane complexes of molybdenum(II) and tungsten(II): Crystal structures of [WI(CO)3([9]aneS3)][BPh4] and [WI2(CO)3(NCMe)(PPh3)]

DOI: 10.1039/dt9960004003

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 4003 - 4010 (1996)

Update date:2022-08-04

Topics:

Authors:

Baker, Paul K.Baker, Paul K.

Coles, Simon J.Coles, Simon J.

Durrant, Marcus C.Durrant, Marcus C.

Harris, Sharman D.Harris, Sharman D.

Hughes, David L.Hughes, David L.

Hursthouse, Michael B.Hursthouse, Michael B.

Richards, Raymond L.Richards, Raymond L.

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Article abstract of DOI:10.1039/dt9960004003

Reaction of [MI2(CO)3(NCMe)2] (M = Mo or W) with a slight excess of 1,4,7-trithiacyclononane ([9]aneS3) in CH2Cl2 at room temperature gave the cationic complexes [MI(CO)3([9]aneS3)]I 1 and 2 in high yield. Treatment of 1 and 2 with an excess of Na[BPh4] in methanol gave [MI(CO)3([9]aneS3)][BPh4] 3 and 4. The molecular structure of [WI(CO)3([9]aneS3)][BPh4] 4 has been determined by X-ray crystallography. It shows that the geometry around the tungsten centre is distorted capped octahedral with a capping carbonyl ligand. Room-temperature 13C NMR studies on complexes 1 and 2 indicate a unique CO ligand, demonstrating that their structures in solution are similar to that found for 4 in the solid state. Reaction of [MI2(CO)3(NCMe)L] [M = Mo or W, L = PPh3; M = W, L = P(OPh)3] with an equimolar quantity of [9]aneS3 gave the seven-co-ordinate cation/anion complexes [MI(CO)2L([9]aneS3)][MI3(CO)4] 5-7. Treatment of [MI2(CO)3(NCMe)2] with 1 equivalent of 2,5,8-trithia[9]orthocyclophane (ttoc) in CH2Cl2 at room temperature gave the dicarbonylmolybdenum complex [MoI2(CO)2(ttoc)] 8 or the seven-co-ordinate cation/anion tungsten complex [WI(CO)3(ttoc)][WI3(CO)4] 9. Reaction of [MI2(CO)3(NCMe)L] with an equimolar amount of ttoc gave [MI(CO)2L(ttoc)][MI3(CO)4] 10-12. The complex [WI2(CO)3(NCMe)(PPh3)] was also shown to have a distorted capped-octahedral geometry by X-ray crystallography.

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Product name:MoI(CO)2(P(C6H5)3)(C6H12S3)(1+)*MoI3(CO)4(1-) = [MoI(CO)2(P(C6H5)3)(C6H12S3)][MoI3(CO)4]

Cas No:184287-94-3

184287-94-3

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