Organometallics
Article
(
(
(
125 MHz, toluene-d , 25 °C): δ = 8.84 (BeC (CH ) I), 110.13
Chemistry; Cundan, T. R., Ed.; Marcel Dekker: New York, 2001; p
397.
8
5
3 5
1
BeC (CH ) I) ppm. H NMR (300 MHz, THF-d , 25 °C): δ = 1.97
5
3
5
8
9
s, 15H, BeC (CH ) I) ppm. Be (42.2 MHz, THF-d ): δ = −16.00 (s,
(3) Fernan
3206.
́
dez, R.; Carmona, E. Eur. J. Inorg. Chem. 2005, 3197−
5
3
5
8
1
3
BeC (CH ) I) ppm. C NMR (125 MHz, THF-d , 25 °C): δ = 9.29
(
5
3
5
8
BeC (CH ) I), 111.00 (BeC (CH ) I) ppm.
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5
3 5
Single-Crystal X-ray Analyses. Crystallographic data for 1−3,
which were collected on a Bruker AXS APEX 2 diffractometer (Mo Kα
radiation, λ = 0.71073 Å), are summarized in Table S1 in the
Supporting Information. Figures 1−3 show diagrams of the solid-state
structures of 1−3. Data were collected at 121(1) K (1), 100(1) K (2),
and 150(1) K (3). The structures were solved by direct methods
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SHELXS-97) and refined anisotropically by full-matrix least-squares
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2
38
on F (SHELXL-97/SHELXL2013). Absorption corrections were
performed semiempirically from equivalent reflections on the basis of
multiscans (Bruker AXS APEX2). 1 was a nonmerohedral twin of two
components of approximately equal size and refined against HKL5
data. Absorption correction was performed with TWINABS.
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Monge, A.; Carmona, E. Angew. Chem. 2000, 112, 2025−2027; Angew.
Chem., Int. Ed. 2000, 39, 1949−1951. (b) del Mar Conejo, M.;
The crystallographic data for 1−3 (excluding structure factors) have
́
́
Fernandez, R.; del Río, D.; Carmona, E.; Monge, A.; Ruiz, C. Chem.
been deposited with the Cambridge Crystallographic Data Centre
Commun. 2002, 2916−2917. (c) del Mar Conejo, M.; Fernan
́
dez, R.;
quez, A. M.; Sanz, J.
(
1
CCDC) as supplementary publications CCDC-1051315 (1), CCDC-
051317 (2), and CCDC-1051316 (3). Copies of the data can be
́
del Río, D.; Carmona, E.; Monge, A.; Ruiz, C.; Mar
́
F. Chem.Eur. J. 2003, 9, 4452−4461. (d) Hung, I.; Macdonald, C. L.
obtained free of charge upon application to the CCDC, 12 Union
B.; Schurko, R. W. Chem.Eur. J. 2004, 10, 5923−5935.
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(
ASSOCIATED CONTENT
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*
S
Supporting Information
(c) Jemmis, E. D.; Alexandratos, S.; Schleyer, P. v. R.; Streitwieser, A.,
A CIF file giving X-ray crystallographic data for 1−3;
Jr.; Schaefer, H. F., III. J. Am. Chem. Soc. 1978, 100, 5695−5700.
1
9
13
(
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d) Gleiter, R.; Bohm, M.; Haaland, A.; Johansen, R.; Lusztyk, J. J.
crystallographic details for 1−3 and 5; H, Be, and
C
Organomet. Chem. 1979, 170, 285−292.
NMR data for 1−3; and computational details (gas-phase
structures, NBO analyses, and ELF and LOL plots) for 1−3.
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03, 683−690. (b) McKee, M. L. Wiley Interdiscip. Rev.: Comput. Mol.
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(11) del Mar Conejo, M.; Fernan
A.; Gutierrez-Puebla, E.; Monge, M. A. Chem.Eur. J. 2003, 9, 4462−
4471.
AUTHOR INFORMATION
Corresponding Author
■
́
dez, R.; Carmona, E.; Andersen, R.
́
(12) (a) Goddard, R.; Akhtar, J.; Starowieyski, K. B. J. Organomet.
Chem. 1985, 282, 149−154. (b) Saulys, D. A.; Powell, D. R.
Organometallics 2003, 22, 407−413.
Author Contributions
The manuscript was written through contributions of all
authors. All authors have given approval to the final version of
the manuscript.
(
13) Himmel, D.; Scheer, H.; Kratzert, D.; Krossing, I. Z. Anorg. Allg.
Chem. 2015, 641, 655−659.
14) (a) Naglav, D.; Blaser, D.; Wo
2014, 53, 1241−1249. (b) Naglav, D.; Neumann, A.; Blas
Wolper, C.; Haack, R.; Jansen, G.; Schulz, S. Chem. Commun. 2015, 51,
889−3891.
15) Burns, C. J.; Andersen, R. A. J. Organomet. Chem. 1987, 325,
1−37.
16) Pratten, S. J.; Cooper, M. K.; Aroney, M. J. J. Organomet. Chem.
990, 381, 147−153.
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18) del Mar Conejo, M.; Fernan
(
̈
̈
lper, C.; Schulz, S. Inorg. Chem.
er, D.;
Notes
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The authors declare no competing financial interest.
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ACKNOWLEDGMENTS
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S.S. thanks the University of Duisburg-Essen for financial
support. We thank Materion Company for the donation of
beryllium metal.
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