Journal of the Chemical Society, Dalton Transactions p. 4003 - 4010 (1996)
Update date:2022-08-04
Topics:
Baker, Paul K.
Coles, Simon J.
Durrant, Marcus C.
Harris, Sharman D.
Hughes, David L.
Hursthouse, Michael B.
Richards, Raymond L.
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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