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Synthesis of analogous complexes with perfluoroglutaric acid or succinic acid yielded intractable solids, which were not further investigated. A complex analogous to 2 with two 2,2-difluorosuccinic acid ligands was successfully synthesized, but catalytic performance was inferior to that of the perfluorosuccinic acid complex.
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33644519848
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1H NMR and elemental analysis.
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33644529932
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1H NMR and elemental analysis.
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33644512651
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The difference between both C-O bond lengths is 0.00 ± 0.02 and 0.009 ± 0.011 Å for both complexes in the unit cell of (rac)-4d and 0.12(4) Å for (R,S)-4d.
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33644506360
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note
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The batch of catalyst 3d that was used for dehydrogenation was synthesized using conventional heating, and this resulted in an approximately 1:1 ratio of (rac)-3d vs (R,S)-3d.
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26
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33644535715
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note
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Complex 3d was screened as well. Despite the presence of ∼80% of the racemic isomer, its low solubility - in contrast to that of optically pure 3e - prevented efficient dehydrogenation.
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27
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33644543659
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3 could be observed for the bridging hydride ligands.
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