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85033160065
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note
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4·4HF (1): All operations were carried out under argon using standard Schlenk techniques. Solvents (dioxane, tetrahydrofuran, diethyl ether, toluene) were distilled under argon from sodium/benzophenone shortly prior to use. Mesityl bromide (5.5 g, 28 mmol) was added slowly to a slight excess of magnesium (0.70 g, 29 mmol) in 50 mL of THF. The solution was stirred for 12 h, whereafter it was centrifuged and the brownish supernatant was withdrawn and added to purified CuCl (3.0 g, 30 mmol) at -30 °C. The reaction solution was then slowly allowed to warm to ambient temperature, yielding a yellow solution and a white precipitate. Dioxane (20 mL) was added, stirring was continued for 2 h, and the solution was then centrifuged. The supernatant was evaporated to dryness under reduced pressure, dissolved in 50 mL of toluene, and centrifuged. The supernatant was evaporated to dryness under reduced pressure and crystals of 1 were grown from THF/diethyl ether (1:1 v:v) at -20 °C.
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85033167213
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3, respectively. The THF molecules exhibit some ring spinning causing the oxygen positions to be somewhat ambigous.
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18
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0000012966
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(h) Soloveichik, G. L.; Eisenstein, O.; Poulton, J. T.; Streib, W. E.; Huffmann, J. C.; Caulton, K. G. Inorg. Chem. 1992, 31, 3306.
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Caulton, K.G.6
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0001420306
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(i) Håkansson, M.; Örtendahl; M.; Jagner, S.; Sigalas, M. P.; Eisenstein, O. Inorg. Chem. 1993, 32, 2018.
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Håkansson, M.1
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Sigalas, M.P.4
Eisenstein, O.5
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0030593391
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(j) Belanzoni, P.; Rosi, M.; Sgamelotti, A.; Baerends, E. J.; Floriani, C. Chem. Phys. Lett. 1996, 257, 41.
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Belanzoni, P.1
Rosi, M.2
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Floriani, C.5
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85033173702
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note
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3, respectively.
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24
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85033189313
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note
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3, respectively.
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