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• W2065325553 abstract "Abstract The complex Os3(CO)12 (1) is alkylated with organolithium reagents to give [Li][Os3{η1-C(O)R}(CO)11−] ([Li][2]). Attempts at electrophilic alkylation of such salts has been unsuccessful. Acidification of a tetrahydrofuran (THF) solution of [Li][2] leads to Os3(CO)11(THF) (3). Metathesis of [Li][2] with [PPN]Cl ([PPN]+ = (Ph3P)2N]+) accompanied by exchange of THF by CHCl3, leads to a solution of [PPN][Os3{1,2-μ-OC(Me)}(CO)10] ([PPN][4]). Acidification of the latter gives Os3{1,2-μ-H; 1,2-μ-OC(Me)}(CO)10 (5). Alkylation of [PPN][4] with ROSO2CF3 gives the bis-acyl derivative Os3{ηx-C(O)R}{μ-OC(Me)}(CO)9 (6). This reacts with water to give a small amount of Os3{1,2-μ-X; 1,2-μ-OC(Me)}(CO)10 (7, X = Cl, or I) along with the two principal products, the Fischer carbene complex Os3{1,2-μ-H; 1,2-μ-OC(Me)}{1-C(OR)Me}(CO)9 (8, R = CH3, CD3, C6H5), and Os3{1,2-μ-(OH); 1,2-μ-OC(Me)}(CO)10 (9). Complex 5 is deprotonated by alkyl lithium reagents at 25°C; at −30°C, however, it is alkylated to give [Li][Os3{C(O)R}{μ-H,μ-OC(Me)}(CO)9] ([Li](10)). Electrophilic alkylation of this salt with R′OSO2CF3 at 25°C leads to cluster complexes containing a Fischer carbene group, Os3{1-η1-C(OR′)R}{1,2-μ-H; 1,2-μ-OC(Me)}(CO)9 (8, R = R′= Me; R = Me, R′ = Et; R = Ph, R′ = Et) in high yield. Treatment of Ru3{1,2-μ-H; 1,2-μ-OC(Me)}(CO)10 (11) with LiR at −30°C leads to [Li][Ru3{C(O)R}{μ-H,μ-OC(Me)}(CO)9] ([Li][12]). Electrophilic alkylation of these salts, however, leads to the elimination of acetaldehyde along with the formation of double CH oxidative addition products, Ru3{μ-H}2 {η2,μ3-C(OEt)C(H)}(CO)9 (13). Starting with Me2NH instead of alkyllithium in this sequence gives Ru3{μ-H}2{η2,μ3-C(OEt)N(Me)C(H)}(CO)9 (14)." @default.
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• W2065325553 date "1988-01-01" @default.
• W2065325553 modified "2023-10-18" @default.
• W2065325553 title "Contrasts in the chemistry of trinuclear cluster complexes of osmium and ruthenium. Formation of a fischer carbene or a functionalized μ3,η2-vinylidene group" @default.
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• W2065325553 doi "https://doi.org/10.1016/s0277-5387(00)86323-8" @default.
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