J. Beckmann, E. Fleige, N. Schnurbusch
dissolved in CHCl3 (20 mL) and cooled to 0 °C. Under vigorous
stirring, a slight excess of SO2Cl2 (776 mg, 5.75 mmol) was slowly
added via a syringe. After 15 min, the mixture was allowed to warm
to room temperature and stirring was continued for 60 min. The
colourless precipitate was collected and dissolved in CH2Cl2
(20 mL). A very small amount of insoluble material was filtered
off. Hexane was added (30 mL) and the solvent was slowly evapora-
ted to yield 2 as colourless crystals (0.54 g, 63 %, mp. 119 °C).
Anal. Calcd. for C10H28B2N2Cl4Te (467.41): C, 25.70; H, 6.04; N,
5.99; Found: C, 25.65; H, 5.77; N, 5.75 %.
refinements on F2, using all data, were carried out with anisotropic
displacement parameters applied to all non-hydrogen atoms. The
co-crystallized toluene molecule of 1·0.5 toluene was disordered
over two positions. H atoms attached to C atoms were included in
geometrically calculated positions for all structures using a riding
model and were refined isotropically. H atoms attached to B atoms
were located in the last refinement cycle and refined isotropically.
Figures were created with DIAMOND [11]. Crystallographic data
(excluding structure factors) for the structural analyses have been
deposited with the Cambridge Crystallographic Data Centre,
CCDC nos. 641951Ϫ641953(1Ϫ3). Copies of this information may
be obtained free of charge from The Director, CCDC, 12 Union
Road, Cambridge CB2 1EZ, UK (Fax: ϩ44-1223-336033; e-mail:
1H-NMR (acetone-d6) δ ϭ 3.9 (4H, t; NCH2), 3.6 (4H, t; TeCH2), 3.2 (12H, s;
N(CH3)2), 3.1 (4H, m; CH2CH2CH2). 13C-NMR (CD2Cl2) δ ϭ 60.0 (NCH2),
48.0 (N(CH3)2), 42.5 (TeCH2), 19.6 (CH2CH2CH2). 11B-NMR (CD2Cl2) δ ϭ
Ϫ3.5 (very broad). 125Te-NMR (CD2Cl2) δ ϭ 862.9. IR: ν˜(B-H) ϭ 2471
(shoulder), 2453 s, 2386 m cmϪ1
.
Acknowledgement. Mrs. Irene Brüdgam (Freie Universität Berlin) is
thanked for the X-ray data collection. The Deutsche Forschungsge-
meinschaft (DFG) is gratefully acknowledged for financial support.
Synthesis of [Cl3BNMe2(CH2)3]2TeCl2 (3). A Schlenk flask connec-
ted with a gas outlet was charged with 1 (500 mg, 1.53 mmol), dis-
solved in CH2Cl2 (15 mL) and cooled to 0 °C. Under vigorous stir-
ring, a slight excess of SO2Cl2 (1.65 g, 12.2 mmol) was slowly added
via a syringe. After 15 min, the mixture was allowed to warm to
room temperature and stirring was continued for 60 min. The co-
lourless precipitate was collected and dissolved in acetone (20 mL).
A very small amount of insoluble material was filtered off. Ethanol
was added (30 mL) and the solvent was slowly evaporated to yield
3 as colourless crystals (0.82 g, 88 %, mp. 140 °C (dec.)). Anal.
Calcd. for C10H24B2N2Cl8Te (605.19): C, 19.85; H, 4.00; N, 4.63;
Found: C, 19.98; H, 3.92; N, 4.58 %.
References
[1] K. Jurkschat, N. Pieper, S. Seemeyer, M. Schürmann, M.
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1H-NMR (acetone-d6) δ ϭ 4.9 (4H, t; NCH2), 4.6 (4H, t; TeCH2), 4.2 (12H, s;
N(CH3)2), 4.1 (4H, q; CH2CH2CH2). 13C-NMR (acetone-d6) δ ϭ 59.5
(NCH2), 45.6 (N(CH3)2), 40.6 (TeCH2), 19.6 (CH2CH2CH2). 11B-NMR
(acetone-d6) δ ϭ 11.0. 125Te-NMR (acetone-d6) δ ϭ 910.3.
[4] D. Dakternieks, G. Dyson, K. Jurkschat, R. Tozer, E. R. T.
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X-ray crystallography
Intensity data were collected on Bruker SMART 1000 CCD area
[8] J. N. G. Faulks, N. N. Greenwood, J. H. Morris, J. Inorg. Nucl.
Chem. 1967, 29, 329.
detector (1) and a STOE IPDS 2T area detector (2, 3), equipped
˚
with graphite-monochromated Mo-Kα (0.7107 A) radiation. Data
[9] SMART, SAINT and SADABS, Siemens Analytical X-ray
Instruments Inc., Madison, Wisconsin USA, 1999.
[10] L. J. Farrugia, J. Appl. Cryst. 1999, 32, 837.
[11] DIAMOND V2.1d, Crystal Impact, K. Brandenburg & M.
Berndt GbR, 2002.
were reduced and corrected for absorption using the programs
SAINT and SADABS [9]. The structures were solved by direct me-
thods and difference Fourier synthesis using SHELXS-97 imple-
mented in the program WinGX 2002 [10]. Full-matrix least-squares
1264
2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Z. Anorg. Allg. Chem. 2007, 1261Ϫ1264