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33645492399
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note
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3, Z = 6: R1 = 0.070; wR2 = 0.124. Further details are given in the Supporting Information.
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14
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0000421806
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25
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33645493240
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note
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1.7 equiv of t-BuLi was used to generate 2 for the consumption with the residual water.
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26
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33645475099
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note
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The calculated chemical shifts (G1AO/6-31G**) of 1 were in agreement with the experimental data: See Supporting Information.
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27
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33645487554
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note
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13C NMR of 2 and 3 were confirmed by 1D NOE, HMQC, and HMBC experiments; see Supporting Information.
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28
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33645491091
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note
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The benzylic protons of 5 were assigned to endo-protons, judging from ring current effect and comparison with those of 9-TMSfluorene and fluorene (see Supporting Information). It is consistent with the assignment of benzylic protons of 1, in which endo-protons at ca. 3.4 ppm are more than 1 ppm as high as exo-protons due to ring current effect. The calculation results given in ref 16 also supported the assignment of 5.
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29
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0001815647
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The exo-selective deuterogenation of the curved system was reported. See: Sygula, A.; Abdourazak, A. H.; Rabideau, P. W. J. Am. Chem. Soc. 1996, 118, 339-343.
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Sygula, A.1
Abdourazak, A.H.2
Rabideau, P.W.3
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