Organometallic macrocycle chemistry. 5.¹ σ-vinyl and σ-aryl complexes of ruthenium(II) ligated by 1,4,7-trithiacyclononane: X-ray crystal structure of [Ru(CH=CH₂)(CO)(PPh₃)([9]aneS ₃)]PF6·2CH₂Cl₂

Abstract

The reaction of coordinatively unsaturated σ-vinyl complexes [Ru(CR=CHR′)Cl(CO)(PPh3)2] with 1,4,7-trithiacyclononane ([9]aneS3) provides chiral salts of the "half-sandwich" complexes [Ru(CR=CHR′)(CO)(PPh3)([9]aneS3)]+. The synthesis of the σ-aryl complex [Ru(C6H4Me-4)(CO)(PPh3)([9]aneS 3)]+ is also described. A representative NMR study of one example allowed the assignment of individual chemical shifts for the 12 diastereotopic proton environments of the macrocycle. The crystal structure of [Ru(CH=CH2)(CO)(PPh3)-([9]aneS3)]PF 6·2CH2Cl2 is also reported.