Synthesis and oxidation of dirhenium C4, C6, and C8 complexes of the formula (η5-C5 Me5)Re(NO)(PR3)(C≡C)n(R3P) (ON)Re(η5-C5Me5)

Organometallics

Volumn 20, Issue 6, 2001, Pages 1115-1127

  Meyer, Wayne E ^a   Amoroso, Angelo J ^a   Horn, Clemens R ^b   Jaeger, Monika ^a   Gladysz, J A ^a,b  

^a UNIVERSITY OF UTAH   (United States)

^b UNIVERSITY OF ERLANGEN NUREMBERG   (Germany)

Author keywords

[No Author keywords available]

Indexed keywords

ALKYNYL COMPLEXES; BUTADIYNYL COMPLEXES; CHLOROBENZENE; CYCLIC VOLTAMMOGRAM; DELOCALIZED MIXED-VALENCE; PHOSPINE;

CHLORINE COMPOUNDS; COMPLEXATION; CYCLIC VOLTAMMETRY; GROUND STATE; MOLECULAR STRUCTURE; OXIDATION; POSITIVE IONS; SPECTROSCOPIC ANALYSIS; SYNTHESIS (CHEMICAL);

RHENIUM COMPOUNDS;

EID: 0035912017     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om000961m     Document Type: Article

References (54)

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14. 4Re complexes isolable in multiple oxidation states: Brady, M.; Weng, W.; Zhou, Y.; Seyler, J. W.; Amoroso, A. J.; Arif, A. M.; Böhme, M.; Frenking, G.; Gladysz, J. A. J. Am. Chem. Soc. 1997, 119, 775.
15. 4Re complexes isolable in multiple oxidation states: Paul, F.; Meyer, W. E.; Toupet, L.; Jiao, H.; Gladysz, J. A.; Lapinte, C. J. Am. Chem. Soc. 2000, 122, 9405.
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20. 6 polyynediyl complexes not included in the preceding references: (a) Bruce, M. I.; Hall, B. C.; Kelly, B. D.; Low, P. J.; Skelton, B. W.; White, A. H. J. Chem. Soc., Dalton Trans. 1999, 3719.
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22. Meyer, W. E.; Amoroso, A. J.; Jaeger, M.; Le Bras, J.; Wong, W.-T.; Gladysz, J. A. J. Organomet. Chem. 2000, 616, 44.
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24. Much of this work is taken from: Meyer, W. E. Ph.D. Thesis, University of Utah, 1999.
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33. Complexes 8b-d are moderately stable toward silica and, if necessary, could be purified by a quick filtration using THF/hexane (1:1).
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40. For some class III mixed-valence diiron complexes that give several near-IR bands, see: Le Stang, S.; Paul, F.; Lapinte, C. Organometallics 2000, 19, 1035 (spin-orbit coupling is much weaker for first-row transition metals).
41. Le Bras, J.; Meyer, W. E.; Gladysz, J. A. Unpublished results.
42. 5. Pyridine was distilled from KOH or NaOH.
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44. 2.
45. 2 or benzene unless noted (8c,d, 2-nitrophenyloctyl ether/benzene).
46. 31P NMR spectra were recorded at 300, 75.5, and 121 MHz, respectively. Chemical shifts and J values are given in δ and Hz, respectively. In disubstituted aryl rings, the designations ipso/ortho/meta/para are with respect to the phosphorus substituent.
47. These assignments follow from coupling constant and chemical shift patterns rigorously established earlier. For the syn/anti sense, see II in Chart 1.
48. 2/hexane solution was kept at -20 °C for 14 h. Orange needles of 3b were obtained (ca. 90%).
49. 2.
50. These assignments follow from coupling constant and chemical shift patterns rigorously established earlier.
51. 1H} 18.6 (s).
52. 2: C, 55,20; H, 6.34. Cl, 3.43. Found: C, 55.25; H, 6.40. Cl, 2.19.
53. 2. Anal. Calcd: C, 59.46; H, 4.92, Cl, 1.97. Found: C, 59.03; H, 4.89, Cl, 1.92.
54. The sample for microanalysis was filtered through Alox (neutral; Fluka) in place of Celite.