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Volumn 26, Issue 7, 2007, Pages 1560-1562

A novel dinuclear ruthenium(I)/ruthenium(III) half-sandwich complex containing two chelating 1,2-dicarba-closo-dodecaborane-1,2-dithiolate ligands and its reactivity with alkynes

(4) Wu, De Hong a Ji, Cheng a Li, Yi Zhi a Yan, Hong a

a NANJING UNIVERSITY (China)

Author keywords

[No Author keywords available]

Indexed keywords

ADDITION REACTIONS; COMPLEXATION; HYDROCARBONS; SULFUR;

ADDITION COMPLEXES; DINUCLEAR COMPLEX;

RUTHENIUM;

EID: 34047273636 PISSN: 02767333 EISSN: None Source Type: Journal
DOI: 10.1021/om070014e Document Type: Article

Times cited : (29)

References (18)

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2
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- (1999) J. Organomet. Chem , vol.587 , pp. 252
- Herberhold, M.¹ Jin, G.-X.² Yan, H.³ Milius, W.⁴ Wrackmeyer, B.⁵

3
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- (b) Eur. J. Inorg. Chem. 1999, 873.
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- Liu, S.; Wang, X.; Jin, G.-X. J. Organomet. Chem. 2006, 691, 261.
- (2006) J. Organomet. Chem , vol.691 , pp. 261
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5
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- Bae, J.-Y.; Lee, Y.-J.; Kim, S.-J.; Ko, J.; Cho, S.; Kang, S.-O. Organometallics 2000, 19, 1514.
- (2000) Organometallics , vol.19 , pp. 1514
- Bae, J.-Y.¹ Lee, Y.-J.² Kim, S.-J.³ Ko, J.⁴ Cho, S.⁵ Kang, S.-O.⁶

6
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- (a) Herberhold, M.; Yan, H.; Milius, W.; Wrackmeyer, B. Chem. Eur. J. 2002, 8, 388.
- (2002) Chem. Eur. J , vol.8 , pp. 388
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12
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- Jin, G.-X.; Wang, J.-Q.; Zhang, C.; Weng, L.-H.; Herberhold, M. Angew. Chem., Int. Ed. 2005, 44, 259.
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- Jin, G.-X.¹ Wang, J.-Q.² Zhang, C.³ Weng, L.-H.⁴ Herberhold, M.⁵

13
- 34047252114
- Synthesis of 1: o-carborane (58 mg, 0.4 mmol) was dissolved in diethyl ether (15 mL) and lithiated by the addition of a 2.0 M cyclohexane solution of n-butyllithium (0.6 mL, 1.2 mmol, The addition of sulfur (43 mg, 1.34 mmol) led to a slightly yellow suspension, and then a solution of, p-cymene)RuCl 2]2 (123 mg, 0.2 mmol) in THF (40 mL) was added at ambient temperature. The color of the resultant mixture gradually changed from orange to green. After 10 h the solvents were removed under reduced pressure and the residue was chromatographed on silica. Elution with petroleum ether/CH 2Cl2 (1:2) gave a green compound of 1. Suitable single crystals for X-ray analysis were obtained from petroleum ether/CH 2Cl2 in 2 weeks. 1: yield 105 mg (65, mp 205°C dec. Anal. Calcd for C14H34B20-Ru2S 6: C, 20.68; H, 4.21. Found: C, 20.80; H, 4.13. ESI-MS m/z, calcd for C14
- -1, 6513 reflections observed, 4778 independent reflections, R1(I > 2σ(I)) = 0.0477, wR2(I > 2σ(I)) = 0.0924, GOF = 1.042.

14
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- (a) Matsuura, N.; Kamiyama, A. I.; Kawamoto, T.; Konno, T. Inorg. Chem. 2006, 45, 401.
- (2006) Inorg. Chem , vol.45 , pp. 401
- Matsuura, N.¹ Kamiyama, A.I.² Kawamoto, T.³ Konno, T.⁴

15
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- (b) Maiti, R.; Shang, M.; Lappin, G. Dalton Trans. 2002, 244.
- (2002) Dalton Trans , pp. 244
- Maiti, R.¹ Shang, M.² Lappin, G.³

16
- 34047265940
- Synthesis of 2a and 2b: methyl propiolate (0.08 mL, 1 mmol) was added to 1 (81 mg, 0.1 mmol) in CH2Cl2 (15 mL, The mixture was stirred for 16 h at ambient temperature. After removal of the solvent the residue was chromatographed to give 2a (petroleum ether/CH2Cl2 (1:2, and 2b (petroleum ether/CH 2Cl2 (1:5, 2a: yield 36 mg (40, mp 230°C dec. Anal. Calcd for C18H38B20O 2Ru2S6: C, 24.09; H, 4.27. Found: C, 24.28; H, 4.35. MALDI-TOF MS (m/z, calcd for C18H38B 20O2Ru2S6, 897.130; found, 898.224, M, H, 75, 1H NMR (CDCl3, δ 1.21 (d, J, 7.0 Hz, 3H, CH(CH3)2, 1.35 (d, J, 7.0 Hz, 3H, CH(CH3)2, 2.19 (s, 3H, CH3, 2.68 (sept. J, 7.0 Hz, 1H, CHCH3
- -1): ν 2579 (νB-H).

17
- 34047260198
- Synthesis of 3b: phenylacetylene (0.1 mL, 1 mmol) was added to 1 (81 mg, 0.1 mmol) in CH2Cl2 (15 mL, The mixture was stirred for 18 h at ambient temperature. After removal of the solvent the residue was chromatographed to give 3b (petroleum ether/CH 2Cl2 (1:4, 3b: yield 73 mg (80, mp 238°C dec. Anal. Calcd for C22H40B20Ru 2S6: C, 28.87; H, 4.40. Found: C, 28.69; H, 4.29. MALDI-TOF MS (mlz, calcd for C22H40B20Ru 2S6, 915.156; found, 916.218, M, H, 85, 1H NMR (CDCl3, δ 1.24 (d, J, 7.0 Hz, 3H, CH(CH3)2, 1.37 (d, J, 7.0 Hz, 3H, CH(CH 3)2, 2.23 (s, 3H, CH3, 2.71 (sept, J, 7.0 Hz, 1H, CH(CH3)2, 5.05 (d, J, 6.0 Hz, 1H, C 6H4, 5.12 d, J, 6.0 Hz, 1H, C6H4, 6
- -1, 7557 reflections observed, 5000 independent reflections, R1(I > 2σ(I)) = 0.0639, wR2(I > 2σ(I)) = 0.1366, GOF = 1.000.

18
- 34047261548
- Synthesis of 4: dimethyl acetylenedicarboxylate (0.1 mL, 1 mmol) was added to 1 (81 mg, 0.1 mmol) in CH2Cl2 (15 mL, The mixture was stirred for 18 h at ambient temperature. After removal of the solvent the residue was chromatographed to give 4 (petroleum ether/CH2Cl2 (1:2, 4: yield 74 mg (78, mp 236°C dec. Anal. Calcd for C20H40B20Ru 2S6: C, 25.14; H, 4.22. Found: C, 24.91; H, 4.34. MALDI-TOF MS (m/z, calcd for C20H40B20O 4Ru2S6, 955.136; found, 956.478, M, H, 45, 1H NMR (CDCl3, δ 1.23 (d, J, 7.0 Hz, 3H, CH(CH3)2, 1.36 (d, J, 7.0 Hz, 3H, CH(CH 3)2, 2.22 (s, 3H, CH3, 2.70 (sept, J, 7.0 Hz, 1H, CH(CH3)2, 3.92 (s, 3H, OCH3, 3.94 (s, 3H, OCH3, 5.06 d, J
- B-H).

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