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Volumn 37, Issue 9, 2008, Pages 966-967

Heptanuclear nickel(II) wheel with eight redox active ferrocenyl groups

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EID: 53649097697 PISSN: 03667022 EISSN: 13480715 Source Type: Journal
DOI: 10.1246/cl.2008.966 Document Type: Article

Times cited : (8)

References (17)

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14
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- Hfcpp was prepared by slight modification of reported procedure (W. R. Thiel, T. Priermeier, D. A. Fiedler, A. M. Bond, M. R. Mattner, J. Organomet. Chem. 1996, 514, 137, Synthesis of 1-ferrocenyl-3-(2- pyridyl)-1,3-propanedione: A solution of sodium ethoxide (1.09 g, 15.9 mmol, acetylferrocene (2.00g, 8.77 mmol) and picolinic acid ethyl ester (2.89 g, 19.1 mmol) in 30 mL of toluene was refluxed for 2 h under nitrogen atmosphere. The solvent was removed under reduced pressure, and aqueous acetic acid was added to the residue. The resulting aqueous solution was extracted with diethyl ether and dried with sodium sulfate. The solvent was evaporated, and the recrystallization of crude products from methanol yielded a purple crystalline solid of 1-ferrocenyl-3-(2-pyridyl)-1,3-propanedione (Yield 2.35 g, 81, Anal. Calcd (Found) for C18H15NO2Fe· 0.1H 2O: C, 64.54 (64.51, H 4.53 (4.63, N, 4.18 4.16, 1HN
- 4), 6.81 (s, IH), 7.22 (m, 1H), 7.76 (m, 2H), 8.62 (d, 1H).

15
- 53649104165
- Synthesis of 1: An acetonitrile solution (30 mL) of Ni(ClO 4)2·6H2O (55 mg, 0.15 mmol) was added to a mixture of Hfcpp (50 mg, 0.15 mmol) and Et3N (15 mg, 0.15 mmol, The resulting red solution was allowed to stand for a week at room temperature to give red plate crystals of 1 (Yield 6.9mg, 13, ESIMS observed m/z 1551.7, M, 2ClO4]2, Anal. Calcd (Found) for Q 44H116N24-Cl2Fe8Ni 7O12·2CH3CN·5H2O: C, 51.15 (50.98, H, 3.82 (3.62, N, 10.48 10.55
- 3CN·5H2O: C, 51.15 (50.98); H, 3.82 (3.62); N, 10.48 (10.55)%.

16
- 53649107316
- Crystallographic data for 1: red plates (0.4 × 0.3 × 0.2 mm3) C156H134N30Cl 2Fe8Ni7Oi2, Mr, 3549.60, Monoclinic, space group P21/n, a, 16.287(3, b, 26.451(5, c, 17.158(3)Å, β=108.135(4)°, V, 7025(2)Å3, Z, 2, T, 200K. A total of 31424 were collected (3° < θ < 46°) of which 10102 unique reflections (Rint, 0.0717) were measured. R1, 0.0607, wR2, 0.1266 (I > 2σI
- 2 = 0.1266 (I > 2σ(I)).

17
- 20344404752
- K. Matsufuji, H. Shiraishi, Y. Miyasato, T. Shiga, M. Ohba, T. Yokoyama, H. Ōkawa, Bull. Chem. Soc. Jpn. 2005, 78, 851.
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- Matsufuji, K.¹ Shiraishi, H.² Miyasato, Y.³ Shiga, T.⁴ Ohba, M.⁵ Yokoyama, T.⁶ Ōkawa, H.⁷

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