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The selective Gaussian-shaped pulse was applied at the central methine proton: T. Fäcke, S. Berger, J. Magn. Reson. A 1995, 113, 257-259. A 1D TOCSY experiment was employed in order to identify the H proton whose signal overlaps with that of the Cp groups.
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Fäcke, T.1
Berger, S.J.2
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16
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85163241051
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note
-
Note that the NH proton resonance occurred at a considerably higher field than in previously reported β-enaminoimine systems,[3,6] possibly due to the presence of the zirconated metal fragment bonded to the nitrogen atoms.[7]
-
-
-
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17
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0034049651
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See this work and: P. H. M. Budzelaar, N. N. P. Moonen, R. de Gelder, J. M. M. Smits, A. W. Gal, Eur. J. Inorg. Chem. 2000, 753-769.
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Moonen, N.N.P.2
De Gelder, R.3
Smits, J.M.M.4
Gal, A.W.5
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18
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[7a] P. J. Walsh, A. M. Baranger, R. G. Bergman, J. Am. Chem. Soc. 1992, 114, 1708-1719.
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19
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[7b] P. J. Walsh, J. Hollander, R. G. Bergman, J. Am. Chem. Soc 1988, 110, 8729-8731.
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20
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0000445956
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The 1D GROESY experiment is a combination of the DPFGSE sequence; see: [8a] K. Stott, J. Stonehouse, J. Keeler, T-L. Hwang, A.-J. Shaka, J. Am. Chem. Soc. 1995, 117, 4199-4200 and the TROESY spin-lock, see:
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24
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[9c] K. Feldmann, E. Daltrozzo, G. Scheibe, Z. Naturforsch., Teil B 1967, 22, 722-731.
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25
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0012508955
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H(2)-H(1) > 10Hz; see: [10a] C. Jutz, A. F. Kirschner, R.-M. Wagner, Chem. Ber. 1977, 110, 1259.
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28
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-
85163237939
-
-
note
-
13C NMR [CH(1)]: For the cis-cis configuration, 130 ppm < δ < 150 ppm. For the trans-trans configuration 90 ppm < δ < 110 ppm; see ref.[11]
-
-
-
-
29
-
-
33748855338
-
-
2ClZr metal moieties are not observed for a C-N-Zr angle lower than 130° in the amido and ketimide subunits. For a good discussion of orbital constraints and symmetry requirements of the bent metallocene derivatives, see: J. W. Lauher, R. Hoffmann, J Am. Chem. Soc. 1976, 98, 1729.
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See for example: G. L. Hillhouse, A. R. Bulls, B. D. Santarsiero, J. E. Bercaw, Organometallics 1988, 7, 1309-1312.
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Hillhouse, G.L.1
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31
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0002232923
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[14a] G. Erker, W. Frömberg, J. L. Atwood, W. E. Hunter, Angew. Chem. 1984, 96, 72-73; Angew. Chem. Int. Ed Engl. 1984, 23, 68-69. [14b] W. Frömberg, G. Erker, J. Organomet. Chem. 1985, 280, 343-354. [14c] G. Erker, W. Frömberg, C. Krüger, E. Raabe, J. Am. Chem. Soc. 1988, 110, 2400-2405.See also for the X-ray structures of (alkylideneamido)zirconocene complexes: [14d] D. R. Armstrong, K. W. Henderson, I. Little, C. Jenny, A. R. Kennedy, A. E. McKeown, R. E. Mulvey, Organometallics 2000, 19, 4369-4375. [14e] U. Segerer, S. Blaurock, J. Sieler, E. Hey-Hawkins, Organometallics 1999, 18, 2838-2842.
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33845278063
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[14a] G. Erker, W. Frömberg, J. L. Atwood, W. E. Hunter, Angew. Chem. 1984, 96, 72-73; Angew. Chem. Int. Ed Engl. 1984, 23, 68-69. [14b] W. Frömberg, G. Erker, J. Organomet. Chem. 1985, 280, 343-354. [14c] G. Erker, W. Frömberg, C. Krüger, E. Raabe, J. Am. Chem. Soc. 1988, 110, 2400-2405.See also for the X-ray structures of (alkylideneamido)zirconocene complexes: [14d] D. R. Armstrong, K. W. Henderson, I. Little, C. Jenny, A. R. Kennedy, A. E. McKeown, R. E. Mulvey, Organometallics 2000, 19, 4369-4375. [14e] U. Segerer, S. Blaurock, J. Sieler, E. Hey-Hawkins, Organometallics 1999, 18, 2838-2842.
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35
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0034299952
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[14a] G. Erker, W. Frömberg, J. L. Atwood, W. E. Hunter, Angew. Chem. 1984, 96, 72-73; Angew. Chem. Int. Ed Engl. 1984, 23, 68-69. [14b] W. Frömberg, G. Erker, J. Organomet. Chem. 1985, 280, 343-354. [14c] G. Erker, W. Frömberg, C. Krüger, E. Raabe, J. Am. Chem. Soc. 1988, 110, 2400-2405.See also for the X-ray structures of (alkylideneamido)zirconocene complexes: [14d] D. R. Armstrong, K. W. Henderson, I. Little, C. Jenny, A. R. Kennedy, A. E. McKeown, R. E. Mulvey, Organometallics 2000, 19, 4369-4375. [14e] U. Segerer, S. Blaurock, J. Sieler, E. Hey-Hawkins, Organometallics 1999, 18, 2838-2842.
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Organometallics
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Armstrong, D.R.1
Henderson, K.W.2
Little, I.3
Jenny, C.4
Kennedy, A.R.5
McKeown, A.E.6
Mulvey, R.E.7
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36
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0001764296
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[14a] G. Erker, W. Frömberg, J. L. Atwood, W. E. Hunter, Angew. Chem. 1984, 96, 72-73; Angew. Chem. Int. Ed Engl. 1984, 23, 68-69. [14b] W. Frömberg, G. Erker, J. Organomet. Chem. 1985, 280, 343-354. [14c] G. Erker, W. Frömberg, C. Krüger, E. Raabe, J. Am. Chem. Soc. 1988, 110, 2400-2405.See also for the X-ray structures of (alkylideneamido)zirconocene complexes: [14d] D. R. Armstrong, K. W. Henderson, I. Little, C. Jenny, A. R. Kennedy, A. E. McKeown, R. E. Mulvey, Organometallics 2000, 19, 4369-4375. [14e] U. Segerer, S. Blaurock, J. Sieler, E. Hey-Hawkins, Organometallics 1999, 18, 2838-2842.
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Segerer, U.1
Blaurock, S.2
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Hey-Hawkins, E.4
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[15a] G. Erker, W. Frömberg, R. Benn, R. Mynott, K. Angermund, C. Krüger, Organometallics 1989, 8, 911-920.
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[15b] G. Erker, Angew. Chem. 1989, 101, 411-417; Angew. Chem. Int. Ed. Engl. 1989, 28, 397-412.
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[15b] G. Erker, Angew. Chem. 1989, 101, 411-417; Angew. Chem. Int. Ed. Engl. 1989, 28, 397-412.
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-
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40
-
-
85163236359
-
-
note
-
Alternative structures for 2 which involve the formation of dimers, trimers, or oligomers with the zirconated metal fragment cannot be totally ruled out, but it is highly unlikely as it will prevent any fluxional process within the alkylideneamido subunit.
-
-
-
-
41
-
-
85163238782
-
-
note
-
Rate constants were derived from band-shape analysis using the software MEXICO (available from A. D. Bain, Department of Chemistry, McMaster University, Hamilton, Ontario, Canada). NMR parameters were optimized to match the simulated and the experimental data. Activation parameters were determined by a standard Eyring analysis.
-
-
-
-
42
-
-
85163237276
-
-
note
-
2] at 293 K revealed two "half-hydrogen" atoms in the N⋯N region of the molecule, similar to what might be obtained by the superposition of one half molecule of A′ on one half molecule of A″.
-
-
-
-
43
-
-
20544433165
-
-
The observed nitrogen-nitrogen separation [N1-N2 = 2.657(6) Å] is smaller than the sum of the nitrogen van der Waals radii (3.10 Å); see: A. Bondi, J. Chem. Phys. 1964, 68, 441. R. C. Weast, Handbook of Chemistry and Physics, CRC, Boca Raton, FL, 1974.
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Bondi, A.1
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0003998388
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CRC, Boca Raton, FL
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The observed nitrogen-nitrogen separation [N1-N2 = 2.657(6) Å] is smaller than the sum of the nitrogen van der Waals radii (3.10 Å); see: A. Bondi, J. Chem. Phys. 1964, 68, 441. R. C. Weast, Handbook of Chemistry and Physics, CRC, Boca Raton, FL, 1974.
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(1974)
Handbook of Chemistry and Physics
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