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Volumn 36, Issue 9, 2007, Pages 1154-1155

Alkoxo-bridged cobalt(II) cube and its radical adduct

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EID: 34948875180 PISSN: 03667022 EISSN: None Source Type: Journal
DOI: 10.1246/cl.2007.1154 Document Type: Article

Times cited : (5)

References (20)

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15
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- Synthesis of 1: To a stirred solution of NaH (53.8 mg, 2.2 mmol) in THF (20mL) at 0°C was added a THF (20mL) solution of H2heip (501 mg, 2.0 mmol) slowly, turning the solution from white to yellow. After stirring for 10 min at 0°C and further stirring at room temperature for 30 min, the solution was added to a THF (20mL) solution of CoCl2 (130mg, 1.0 mmol, and the resulting red solution was stirred at room temperature for 4h. After the solvent was evaporated, the residue was extracted into diethyl ether, which was washed with distilled water and dried (MgSO4, The red solution was concentrated to 10 mL, slow evaporation under dry nitrogen atmosphere gave red crystal of 1, 119 mg) in 35% yield. Anal. Caled (Found) for 1 (C32H36N4Co4F24O 12, C, 28.25 (28.26, H, 2.67 (2.64, N, 4.12 4.07, Synthesis of 2·4CH3CN-2CH3OH: To solution of 1
- 16): C, 42.08 (42.04); H, 3.90 (3.97); N, 10.33(10.16).

16
- 34948894234
- Crystallographic data for 1: red blocks (0.3 × 0.3 × 0.3 mm3) C32H36N4Co 4F24O12, Mt, 1360.352, tetragonal, space group P421C, a =14.197(3, c, 12.052(3)Å, V, 2429.2(9)Å3, Z, 2, T, 200K. A total of 11464 were collected (6° < 2θ < 46°) of which 1745 unique reflections (Rint, 0.0191) were measured. R1= 0.0189, wR2, 0.0518 (I > 2σ(I, 2·4CH3CN· CH3OH: dark bule plate (0.4 × 0.3 × 0.2 mm3) C88H84N2OCo4F24O 18, Mr, 2401.47, tetragonal, space group 14 1/a, a =18.723(2, c, 30.706(5) Å, V, 10764(2) Å3, Z, 4, T
- 2 = 0.1361 (I > 2σ(I)).

17
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- Supporting Information is available electronically on the CSJ-Journal Web site, http://www.csj.jp/journals/chem-lett/.
- Supporting Information is available electronically on the CSJ-Journal Web site, http://www.csj.jp/journals/chem-lett/.

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