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Attempted crystallizations are reported in ref. [9].
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61
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30444446275
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62
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30444436830
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The four independent C-Fe-C angles are 113.67(15), 109.24(9), 109.28(9), and 105.83(15)°.
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30444445061
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note
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The standard uncertainty of the average edge is within three times the average standard uncertainties of each individual edge.
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4 is 2.31(5) Å, the average C-Li distance in 1 is 2.25(6) Å.
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30444440830
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see Scheme 4
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Although GC shows seemingly clean conversions, the isolated yields of 5 remained disappointingly low using either defined 1 or the in situ system, see Scheme 4.
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81
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Complex 1, however, seems to be unable to transfer electrons to dialkyl ketones as evident from the clean addition to 4-tert-butylcyclohexanone. This result is again in excellent agreement with the report by Ashby et al. who showed that the iron content in the magnesium has no effect in Grignard additions to aliphatic carbonyl compounds. Moreover, they are in line with the finding that certain iron salts beneficially effect the stereoselective course of addition of cyclic ketones as reported by Reetz et al., see: M. T. Reetz, S. Stanchev, J. Chem. Soc. Chem. Commun. 1993, 328-330.
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30444433903
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3): δ = 200.5, 145.2, 142.0, 141.9, 135.2, 31.9, 29.7, 19.5, 19.4, 15.5 ppm.
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|