Summary
The reactions of titanium(III) and (IV) chlorides with the crown thioether [9]aneS3 were investigated. [TiCl3- (MeCN)3] gives a purple 1:1 adduct with a proposed octahedral structure involving tridentate fac-attachment of the ligand. With [TiCl4(MeCN)2] the identity of the yellow 1∶1 adduct obtained is discussed in terms of a six-coordinate species with bidentate ligand chelation. The title compound was isolated from the reactions of [9]aneS3 with [TiCl3(MeCN)3] [SbCl6] (by accident) and iron filings/SbCl5 in MeCN solution and characterised crystallographically. The cation has two macrocyclic ligands coordinated facially to a six-coordinate Fe2+ ion; the anion comprises dimeric [(SbCl4)2] units linked together into a polymeric chain by weak halogen bridging.
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Willey, G.R., Palin, J., Lakin, M.T. et al. Reactions of 1,4,7-trithiacyclononane, [9]aneS3, with early transition metal halides: synthesis and X-ray structure of {Fe([9]aneS3)2}[Sb2Cl8]. Transition Met Chem 19, 187–190 (1994). https://doi.org/10.1007/BF00161886
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DOI: https://doi.org/10.1007/BF00161886