M. Kowalewski, B. Krumm, P. Mayer, A. Schulz, A. Villinger
SHORT COMMUNICATION
[6] See the Supporting Information: a) chemical shifts (31P{1H},
31P MAS) and assignment was carried out on the basis of the
excellent agreement between theoretically (utilizing the two
structures obtained from X-ray elucidation) and experimentally
obtained shifts (δ[31P]); b) crystal data; c) full description of
the experimental data, technique and details; d) computational
details [B3LYP/6-31G(d,p)]; e) summary of the NBO analysis
for 3: (i) partial charges, (ii) hybridization effects, and (iii) po-
larization.
1401 (8), 1363 (7), 1309 (2), 1309 (2), 1288 (2), 1141 (2), 1118 (3),
1094 (2), 1021 (2), 982 (1), 848 (2), 819 (2), 785 (2), 771 (2), 658
(2), 621 (2), 596 (6), 527 (8), 501 (7), 446 (8), 397 (8), 363 (4) cm–1.
31P{1H} NMR (121.5 MHz, CD2Cl2, 25 °C): δ = 253 (br.) ppm.
31P MAS NMR (25 °C, ωrot = 20 kHz): δ = 240.7 (s), 264.0 (s)
ppm. MS (EI, 70 eV, Ͼ5%): m/z (%) = 168 (26.2) [C6F5], 277 (26.8),
345 (19.5) [B(C6F5)2], 365 (28.0), 629 (58.4) [½ 3Me], 644 (100) [½
3], 1288 (30.6) [3]. C42H18N4B2F30P2Si2 (1288.3): calcd. C 39.16, H
1.41, N 4.35; found C 40.62, H 1.00, N 4.22.
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Crystals suitable for single-crystal X-ray studies were obtained by
cooling the reaction solution slowly to 5 °C. An X-ray quality crys-
tal of 3 was selected in silicon oil at ambient temperature and was
cooled to 200(2) K during measurement. The data for compound
3 was collected with a Nonius Kappa CCD diffractometer by using
graphite-monochromated Mo-Kα radiation (λ = 0.71073). The
structure was solved by direct methods and refined by full-matrix
least-squares procedures (SHELXL-97).[16] All non-hydrogen
atoms were refined anisotropically; hydrogen atoms were included
in the refinement at calculated positions by using a riding model.
The P(C6F5) unit was split over two positions and the occupancy
of each part (A and B) refined. For the carbon atoms of the split
C6F5 rings, rigid group refinement was performed. A second X-
ray study from a different experiment gave the same result (see
Supporting Information). CCDC-653980 contains the supplemen-
tary crystallographic data for this paper. These data can be ob-
tained free of charge from the Cambridge Crystallographic Data
Centre via www.ccdc.cam.ac.uk/data_request/cif.
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[14] Single-point calculations were computed with a tight conver-
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computational details see the Supporting Information. M. J.
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Supporting Information (see footnote on the first page of this arti-
cle): Full experimental details and characterization data, X-ray
crystallographic refinement data, selected bond lengths and angles,
and computational details of 3.
Acknowledgments
Financial support by the Deutsche Forschungsgemeinschaft
(SCHU 1170/4-1) is gratefully acknowledged. We thank Dr. Jörn
Schmedt auf der Günne for recording the MAS NMR spectra.
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Received: August 7, 2007
Published Online: October 25, 2007
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Eur. J. Inorg. Chem. 2007, 5319–5322