Cobalt(II) Complexes of Homoscorpionate, Heteroscorpionates and Chiral Tris(pyrazolyl)borates
FULL PAPER
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J. Juang, L. Lee, B. S. Haggerty, A. L. Rheingold, M. A.
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[6]
9
: C30
H
34BCoN
7
S (594.44): calcd. C 60.61, H 5.76, N 16.49; found
1
C 60.63, H 5.80, N 16.59. H NMR (CD
3
OD, 298 K): δ ϭ Ϫ78.2
2 H, o-H(3-Ph)], Ϫ70.2 [1 H, CH(3-iPr)], Ϫ57.2 (1 H, 3-CH ),
(3-iPr)], Ϫ4.2 [2 H, m-H(3-Ph)], 0.8
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[
3
[
[
7]
8]
Ϫ30.1, Ϫ28.1 [3 H, 3 H, CH
3
[1 H, p-H(3-Ph)], 14.4 [1 H, p-H(5-Ph)], 17.4, [2 H, m-H(3-Ph)],
21.5, 22.8 [3 H, 3 H, CH
3
(5-iPr)], 24.3 [2 H, o-H(3-Ph)], 33.1 (3 H,
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-CH ), 50.0, 51.9, 52.9 [1 H, 1 H, 1 H, 4-H(pz)], 64.7 [1 H, CH(5-
3
2
682Ϫ2684.
iPr)], 85.0 (1 H, BH) ppm. IR (KBr): ν˜ ϭ 2557 (νBH), 2121, 2058
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Ϫ1
S. Trofimenko, A. L. Rheingold, L. M. Liable-Sands, Inorg.
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(νNCS) cm
.
1
[10]
Methods: H NMR spectra were obtained with a Bruker AMX300
spectrometer operating in the quadrature mode at 300 MHz. The
residual peaks of deuterated solvents were used as internal stand-
ards. IR spectra were recorded with a PerkinϪElmer 1725X spec-
trophotometer. Elemental analyses were performed with an EA
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Mass spectra were obtained using a Finnigan MAT TSQ 700 spec-
trometer by the ESI method from chloroform with a 4.5-kV ioniz-
ation potential and a capillary temperature of 250 °C. Crystal data
are given in Table 1 together with refinement details. Measurements
were performed at 293 K for 1-THF and at 100 K for 3-THF, 4 and
19, 2119Ϫ2125.
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2
using an Oxford Cryosystem device with a Kuma KM4CCD κ-
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α
8
9Ϫ93.
ation. The crystals were positioned at 65 mm from the CCD cam-
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time of 10Ϫ15 s. Accurate cell parameters were determined and
refined by least-squares fit of 2500Ϫ3800 of the strongest reflec-
tions. The data were corrected for Lorentz and polarization effects.
No absorption correction was applied for 1-THF, 3-THF and 3,
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. Data re-
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34]
SHELXS-97)
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(1-THF), -200533 (3-THF), -200534 (4) and -189010 (9 ) contain
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Acknowledgments
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We thank KBN (Poland) for a Grant (no. 3 T09A 05219).
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1
Received January 13, 2003
Eur. J. Inorg. Chem. 2003, 2475Ϫ2485
www.eurjic.org
2003 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
2485