Abstract
S−F‐bond activation of sulfur tetrafluoride at [Rh(Cl)( tBuxanPOP)] (1; tBuxanPOP=9,9‐dimethyl‐4,5‐bis‐(di‐tert‐butylphosphino)‐xanthene) led to the formation of the cationic complex [Rh(F)(Cl)(SF2)( tBuxanPOP)][SF5] (2 a) together with trans‐[Rh(Cl)(F)2( tBuxanPOP)] (3) and cis‐[Rh(Cl)2(F)( tBuxanPOP)] (4) which both could also be obtained by the reaction of SF5Cl with 1. In contrast to that, the conversion of SF4 at the methyl complex [Rh(Me)( tBuxanPOP)] (5) gave the isolable and room‐temperature stable cationic λ4‐trifluorosulfanyl complex [Rh(Me)(SF3)( tBuxanPOP)][SF5] (6). Treatment of 6 with the Lewis acids BF3 or AsF5 produced the dicationic difluorosulfanyl complex [Rh(Me)(SF2)( tBuxanPOP)][BF4]2 (8 a) or [Rh(Me)(SF2)( tBuxanPOP)][AsF6]2 (8 b), respectively. Refluorination of 8 a was possible with the use of dimethylamine giving [Rh(Me)(SF3)( tBuxanPOP)][BF4] (9). A reaction of 6 with trichloroisocyanuric acid (TClCA) gave the fluorido complex [Rh(F)(Cl)(SF2)( tBuxanPOP)][Cl] (2 b) together with chloromethane and SF5Cl.
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