Direct observation of reversible C(sp3)-H bond activation. Characterization of the structures of both Ir complexes before and after C-H bond activation by using a flexible P-N heterochelate hybrid ligand

Organometallics

Volumn 18, Issue 18, 1999, Pages 3563-3565

  Kataoka, Yasutaka ^a   Imanishi, Masahiro ^a   Yamagata, Tsuneaki ^a   Tani, Kazuhide ^a  

^a OSAKA UNIVERSITY   (Japan)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0000954546     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om990443f     Document Type: Article

References (41)

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27. 6 in dichloromethane were foiled because the reaction gave only complex mixtures.
28. 5OH: C, 48.05; H, 4.61; N, 1.60.
29. int = 0.0205, R1(all) = 0.0387, R1(obsd) = 0.0292 (>2.0σ(I)), wR2(all) = 0.0345, wR2-(obsd) = 0.0707 (>2.0σ(I)).
30. Selected bond lengths, bond angles, and crystal and data collection parameters are given in the Supporting Information.
31. Huheey, J. E. Inorganic Chemistry, 3rd ed.; Harper & Row: New York, 1983; pp 258-259.
32. n=1 ligand was also coordinated as a P-O-N tridentate ligand. The rhodium complex, however, did not show any indication of similar C-H bond activation at ambient temperature. Preparation and properties of the rhodium complex will be reported separately.
33. 2: C, 47.82; H, 4.13; N, 1.69.
34. int = 0.0205, R1(all) = 0.0548, R1(obsd) = 0.0335 (>2.0σ(I)), wR2(all) = 0.0956, wR2(obsd) = 0.0807 (>2.0σ(I)).
35. 3; however, the effect of the decomposition was negligible for the estimation of the kinetic parameters.
36. Schunn, R. A. In Transition Metal Hydrides; Muetterties, E. L., Ed.; Marcel Dekker: New York, 1971; pp 244-246.
37. 17 the reverse process from the Ir(III) complex to the Ir(I) complex is not clear.
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39. The observed kinetic isotope effect of 2.8 (50 °C) in the oxidative addition indicates that an alkane complex is not a key intermediate in this reversible C-H bond activation.
40. An ORTEP drawing and crystal data for 2b are provided in the Supporting Information.
41. 3 at 30 °C for 7 days, a small amount of hydride species (<5%) was observed, but it could not be characterized.