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Protonation of triosmium clusters Os3(CO)9(μ−CO)(μ3−2σ,η2−HCCR) and Os3(μ−H)(CO)9(μ3−σ,2η2−CCR) (R = CH2OH, CMe2OH, C(Me) = CH2

Authors
Journal
Journal of Organometallic Chemistry
0022-328X
Publisher
Elsevier
Publication Date
Volume
508
Identifiers
DOI: 10.1016/0022-328x(95)05871-l
Keywords
  • Triosmium Clusters
  • Protonation
  • Six-Electronic Propargyl Ligand
  • Phosphonium Complexes
  • Phosphoniun Allenyl Ligand
  • Crystal Structure

Abstract

Abstract Protonation of Os 3(CO)( μ−CO( μ 3−2 σ, η 2−HCCR) (R = CH 2OH ( 1) R = CMe 2OH ( 2) and Os 3( μ−H)(CO) 9( μ 3− σ,2 η 2−CCR) (R = CH 2OH ( 3), R = CMe 2OH ( 4), R = C(Me) = CH 2 ( 5)) affords cationic complexes with the 5e-and 6e-propargyl ligands [Os 3(CO) 9( μ−CO)( μ 3−3 σ, η 2−HCCCR′ 2)] + (R′ = H ( 6), R′ = Me ( 7) and [Os 3( μ−H)(CO) 9( μ 3−2 σ,2 η 2−CCR′ 2) + ( R′ = H ( 8) , R′ = Me ( 9) respectively. Reactrions of the cationic complexes with PPh 3 were studied. The treatment of solutions of complexes 6–9 with triphenylphosphine leads to the phosphonium derivatives of the Os 3 clusters Os 3( CO) 9(μ 2−2σ,η 2- HC CCR′ 2 P + Ph 3) ( R′ = H, (10); R′ = Me, ( 11)) as well as complexes Os 3(μ- H(CO) 9(μ 3−σ,2η 2− P + Ph in3 CCCR′ 2) ( R = H ( 12, R′ = Me ( 13)) with the novel phosphonium allenyl ligand. The cluster Os 3(CO) 8( μ−CO){HC 2[C(Me)CH 2]COC[C(Me)CH 2]CH} ( 4) synthesized and its X-ray study was carried out ( R = 0.0504 for 5510 observed reflections). Crystals of 14 are triclinic, at 20°C: a = 8.591(2), b = 11.437(2), c = 12.642(3) A ̊ , α = 93.17(2), β = 104.67(2), γ = 101.83(2)°, V = 1168.6(4) A ̊ , d calc = 2.793 g cm −3, Z = 2 , space group P 1 .

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