101011-69-2Relevant articles and documents
Organometallic chemistry of fluorocarbon acids. Synthesis, structure, and solvolysis of a sulfinate-bridged diruthenium dihydride cluster, [(Ph3P)4Ru2(μ-H)2(μ-CF 3SO2)(CO)2]HC(SO2CF 3)2
Siedle,Newmark,Pignolet
, p. 1345 - 1351 (2008/10/08)
Reaction of (Ph3P)3RuH2(CO) with 2 equiv of the fluorocarbon acids H2C(SO2CF3)2 or PhCH(SO2CF3)2 in toluene at >80°C produces the HC(SO2CF3)2- or PhC(SO2CF3)2- salts of (Ph3P)4Ru2(μ-H)2(μ-CF 3SO2)(CO)2+, in which the bridging hydrides were located by very high field 1H NMR. The bridging bidentate CF3SO2 group in [(Ph3P)4Ru2(μ-H)(μ-CF3SO 2)(CO)2]HC-(SO2CF3) 2·CH2Cl2 was established by single-crystal X-ray diffraction [P1 (triclinic), a = 16.300 (3) A?, b = 17.783 (4) A?, c = 14.496 (2) A?, α = 92.74 (1)°, β = 90.84 (1)°, γ = 111.82 (1)°, Z = 2]. This compound reacts with acetonitrile to form salts of (Ph3P)2RuH(CO)(CH3CN)2+. In the HC(SO2CF3)2- derivative [P21/n (monoclinic), a = 14.561 (3) A?, b = 16.858 (3) A?, c = 19.122 (4) A?, β = 93.55 (2)°, Z = 4], d(Ru-N, trans to CO) is 2.108 (5) A? while d(Ru-N, trans to H) is 2.163 (5) A? and one of the acetonitrile ligands rapidly exchanges with CD3CN.