𝔖 Bobbio Scriptorium
✦   LIBER   ✦

Hydrocarbon Oxidation by β-Halogenated Dioxoruthenium(VI) Porphyrin Complexes: Effect of Reduction Potential (RuVI/V) and CH Bond-Dissociation Energy on Rate Constants

✍ Scribed by Chi-Ming Che; Jun-Long Zhang; Rui Zhang; Jie-Sheng Huang; Tat-Shing Lai; Wai-Man Tsui; Xiang-Ge Zhou; Zhong-Yuan Zhou; Nianyong Zhu; Chi Kwong Chang


Publisher
John Wiley and Sons
Year
2005
Tongue
English
Weight
383 KB
Volume
11
Category
Article
ISSN
0947-6539

No coin nor oath required. For personal study only.

✦ Synopsis


Abstract

β‐Halogenated dioxoruthenium(VI) porphyrin complexes [Ru^VI^(F~28~‐tpp)O~2~] [F~28~‐tpp=2,3,7,8,12,13, 17,18‐octafluoro‐5,10,15,20‐tetrakis(pentafluorophenyl)porphyrinato(2−)] and [Ru^VI^(β‐Br~8~‐tmp)O~2~] [β‐Br~8~‐tmp=2,3,7,8,12,13,17,18‐octabromo‐5,10,15,20‐ tetrakis(2,4,6‐trimethylphenyl)porphyrinato(2−)] were prepared from reactions of [Ru^II^(por)(CO)] [por=porphyrinato(2−)] with m‐chloroperoxybenzoic acid in CH~2~Cl~2~. Reactions of [Ru^VI^(por)O~2~] with excess PPh~3~ in CH~2~Cl~2~ gave [Ru^II^(F~20~‐tpp)(PPh~3~)~2~] [F~20~‐tpp=5,10,15,20‐tetrakis(pentafluorophenyl)porphyrinato(2−)] and [Ru^II^(F~28~‐tpp)(PPh~3~)~2~]. The structures of [Ru^II^(por)(CO)(H~2~O)] and [Ru^II^(por)(PPh~3~)~2~] (por=F~20~‐tpp, F~28~‐tpp) were determined by X‐ray crystallography, revealing the effect of β‐fluorination of the porphyrin ligand on the coordination of axial ligands to ruthenium atom. The X‐ray crystal structure of [Ru^VI^(F~20~‐tpp)O~2~] shows a RuO bond length of 1.718(3) Å. Electrochemical reduction of [Ru^VI^(por)O~2~] (Ru^VI^ to Ru^V^) is irreversible or quasi‐reversible, with the E~p,c~(Ru^VI/V^) spanning −0.31 to −1.15 V versus Cp~2~Fe^+/0^. Kinetic studies were performed for the reactions of various [Ru^VI^(por)O~2~], including [Ru^VI^(F~28~‐tpp)O~2~] and [Ru^VI^(β‐Br~8~‐tmp)O~2~], with para‐substituted styrenes p‐XC~6~H~4~CHCH~2~ (X=H, F, Cl, Me, MeO), cis‐ and trans‐β‐methylstyrene, cyclohexene, norbornene, ethylbenzene, cumene, 9,10‐dihydroanthracene, xanthene, and fluorene. The second‐order rate constants (k~2~) obtained for the hydrocarbon oxidations by [Ru^VI^(F~28~‐tpp)O~2~] are up to 28‐fold larger than by [Ru^VI^(F~20~‐tpp)O~2~]. Dual‐parameter Hammett correlation implies that the styrene oxidation by [Ru^VI^(F~28~‐tpp)O~2~] should involve rate‐limiting generation of a benzylic radical intermediate, and the spin delocalization effect is more important than the polar effect. The k~2~ values for the oxidation of styrene and ethylbenzene by [Ru^VI^(por)O~2~] increase with E~p,c~(Ru^VI/V^), and there is a linear correlation between log k~2~ and E~p,c~(Ru^VI/V^). The small slope (≈2 V^−1^) of the log k~2~ versus E~p,c~(Ru^VI/V^) plot suggests that the extent of charge transfer is small in the rate‐determining step of the hydrocarbon oxidations. The rate constants correlate well with the CH bond dissociation energies, in favor of a hydrogen‐atom abstraction mechanism.