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note
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3. Cell dimensions and intensities were measured at 200 K on a diffractometer with graphite-monochromated Mo Ka radiation (λ = 0.71073 Å). Of 49644 measured reflections, 24214 were unique and 9272 were observed (|Fo| > 4σ (Fo)). Data were corrected for Lorentz and polarization effects and for absorption: R = 0.044, ωR = 0.042, S = 1.28(2), Flack parameter x = 0.06(10). Both ion pairs of the asymmetric unit are similar. CCDC-297893 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/conts/retrieving.html (or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, U.K. Fax: (+ 44) 1223-336-033 or deposit@ccdc.cam.ac.uk).
-
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63
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note
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No evidence has so far been found to demonstrate the predominance of this relative configuration in solution. Configuration assignment of 1 by circular dichroism analysis of salts [1][Δ-2] and [1][Δ-3] could not be readily achieved because of the presence of the CD-active anions and of the aromatic solvent.
-
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64
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33748989292
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note
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-]), this being possibly the result of charge-assisted C-H⋯O interactions. On the contrary, a high field shift is observed for the minor diastereomer.
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-
91
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33749033385
-
-
note
-
exchange.
-
-
-
-
92
-
-
33748997974
-
-
note
-
exchange is thus undefined.
-
-
-
-
93
-
-
33749035317
-
-
note
-
enantio.
-
-
-
-
94
-
-
33748997697
-
-
note
-
TRISPHAT 2 is the better NMR chiral solvating agent and, at the same time, the less effective asymmetry-inducing moiety. As such, it is more effective for the kinetic mechanistic analysis.
-
-
-
-
95
-
-
33749021391
-
-
note
-
exchange on the very same proton spectra as to minimize the temperature error which would have been, otherwise, not negligible.
-
-
-
-
96
-
-
33749005692
-
-
note
-
exchange value is in perfect agreement with previous experiments (see ref 7).
-
-
-
-
97
-
-
33749026115
-
-
note
-
Unlike in the organometallic phosphane chemistry, an eventual dissociation-association enantiomerization pathway can essentially be ruled out.
-
-
-
-
98
-
-
33748994850
-
-
work in progress
-
Lepetit, C.; Laleu, B.; Bernardinelli, G.; Lacour, J.; Chauvin, R., work in progress.
-
-
-
Lepetit, C.1
Laleu, B.2
Bernardinelli, G.3
Lacour, J.4
Chauvin, R.5
-
99
-
-
33749024769
-
-
note
-
maj and min identify signals from the major and minor conformers, respectively.
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-
-
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