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For the synthesis of 5: To a stirred n-hexane solution (60 mL) of freshly sublimed Cb*CoCp (1.00 g; 4.31 mmol) was added freshly distilled PMDETA (2.70 mL; 13 mmol; 3 equiv) and BuLi (1.6 M in n-hexane; 8.0 mL; 13 mmol) at RT. The reaction mixture was stirred at RT for 1620 h, after which the precipitate was allowed to settle. The supernatant solution was removed, and the precipitate was washed with n-hexanes (2 × 20 mL) followed by n-pentane (5 × 15 mL) until no visible color was extracted into the n-pentane layer. The light brown solid was dried for 18 h in vacuo to give (Co(η4-Me 3C4CH2Li)(η5-C5H 4Li)]·PMDETA (5, yield 1.19 g, 66, Anal. Caled for C22H38N3Co1Li2 (found, C 63.32 (63.20, H 9.18 (8.78, N 10.07 9.41, For the synthesis of 6a/b: To an n
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1H NMR spectra are available in the Supporting Information as an indication of the level of purity obtained.
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