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• W2049439497 abstract "Cp*Os(CO)2H is protonated by triflic acid (HOTf) in CD2Cl2 solution to give an equilibrium mixture (87:13) of the dihydride [Cp*Os(CO)2(H)2]+OTf− and the dihydrogen complex [Cp*Os(CO)2(η2-H2)]+OTf−. The acidity of these protonated species is roughly comparable to HOTf, since only partial protonation was observed, e.g., 36% protonation with 1.2 equiv of HOTf. In the absence of acid, the T1 of the hydride ligand of Cp*Os(CO)2H is 5.9 s at −80 °C. When all of the Cp*Os(CO)2H is protonated by excess HOTf, the T1 (−80 °C) of the terminal hydride ligands of [Cp*Os(CO)2(H)2]+OTf− is 2.8 s, while the T1 of the dihydrogen ligand of [Cp*Os(CO)2(η2-H2)]+OTf− is 19 ms (−80 °C). The observed T1 values of the Os−H resonance of Cp*Os(CO)2H decreased significantly under conditions of partial protonation, indicating intermolecular proton transfer among [Cp*Os(CO)2(η2-H2)]+OTf−, [Cp*Os(CO)2(H)2]+OTf−, Cp*Os(CO)2H, and HOTf. IR spectra indicate that the two CO ligands of [Cp*Os(CO)2(H)2]+ (and hence the hydrides as well) are trans to each other in the four-legged piano stool geometry. Two resonances for HOTf are observed in the NMR spectra and are assigned as [HOTf]n (hydrogen bonded to itself) and TfOH···OTf− in which HOTf is hydrogen bonded to an OTf− counterion. [CpW(CO)3(H)2]+OTf− and [Cp*W(CO)3(H)2]+OTf− were formed by protonation of CpW(CO)3H and Cp*W(CO)3H. Protonation of the phosphine-substituted tungsten hydrides CpW(CO)2(PR3)H (R = Me, Cy, Ph) by HOTf or [H(Et2O)2]+ BAr‘4− (Ar‘ = 3,5-bis(trifluoromethyl)phenyl) gives dihydrides [CpW(CO)2(PR3)(H)2]+ which were isolated and fully characterized. The structure of [CpW(CO)2(PMe3)(H)2]+OTf− was determined by single-crystal X-ray diffraction and reveals weak hydrogen bonds between one hydride on W and two of the fluorines on the triflate anion." @default.
• W2049439497 created "2016-06-24" @default.
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• W2049439497 date "1996-05-14" @default.
• W2049439497 modified "2023-09-27" @default.
• W2049439497 title "Protonation of Metal Hydrides by Strong Acids. Formation of an Equilibrium Mixture of Dihydride and Dihydrogen Complexes from Protonation of Cp*Os(CO)₂H. Structural Characterization of [CpW(CO)₂(PMe₃)(H)₂]⁺OTf⁻" @default.
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• W2049439497 doi "https://doi.org/10.1021/om950976y" @default.
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