programme XABS2.49 The H atoms on the NH2ϩ moieties and
the water molecule were located in the difference map and
refined without geometric constraints. All other H atoms were
refined in their calculated geometric positions and refined using
an atom riding model. Anisotropic thermal parameters were
refined for all non-hydrogen atoms.
7 T. H. Bennur, S. Sabne, S. S. Deshpande, D. Srinivas and
S. Sivasanker, J. Mol. Cat. A: Chem., 2002, 185, 71.
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11 B. R. Bodsgard and J. N. Burstyn, Chem. Commun., 2001, 647.
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19 See for example: (a) E. N. Jacobsen, Comprehensive Asymmetric
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The programs ORTEP-3,50 and PLATON51 were used for
graphical representations and WINGX52 was used to prepare
material for publication for all structures.
Crystal data for 15. C18H27N3O3S, M = 365.49, tetragonal,
a = 11.164(2), b = 11.164(2), c = 14.910(3) Å, U = 1858.3(6) Å3,
T = 180(2) K, space group P41, Z = 4, µ(Mo-Kα) = 0.196 mmϪ1
,
1553 reflections measured, 1351 unique (Rint = 0.0364) which
were used in all calculations. The final wR [I>2σ(I )] was 0.1382.
Crystal data for 17bؒ2HClؒH2O. C10H24Cl2N2O2, M = 275.21,
orthorhombic, a = 7.9736(4), b = 12.2913(6), c = 14.1517(9) Å,
U = 1386.95(13) Å3, T = 120(2) K, space group P212121, Z = 4,
µ(Mo-Kα) = 0.459 mmϪ1, 3042 reflections measured, 1778
unique (Rint = 0.0877) which were used in all calculations. The
final wR [I>2σ(I )] was 0.0830.
Crystal data for [Cu(17b)Cl2]. C10H18Cl2CuN2O, M = 316.70,
tetragonal, a = 26.629(4), b = 26.629(4), c = 7.506(2) Å, U =
5322.5(18) Å3, T = 293(2) K, space group I41,§ Z = 16, µ(Mo-Kα)
= 2.024 mmϪ1, 2688 reflections measured, 2521 unique (Rint
=
0.0197) which were used in all calculations. The final wR
[I>2σ(I )] was 0.1524 (all data).
CCDC reference numbers 188705, 195733 and 195734.
lographic data in CIF or other electronic format.
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Acknowledgements
We are grateful to Queen Mary, University of London for a
studentship (S. P.) and also to the EPSRC for a studentship
(K. F. S., GR/R19182/01), EPSRC and Warwick International
Limited for a CASE award for New Academics (K. S.) (Award
No. 00800316) and GlaxoSmithKline for an Industrial CASE
studentship (H. W.) (Ref. No. 9931546X). We are indebted to
The University of London Research Instruments Service
(ULRIS) for mass spectra (London School of Pharmacy) and
for NMR spectra at 400 MHz (Queen Mary). We also thank the
EPSRC National X-ray service (University of Southampton)
for the collection of data for 17bؒ2HClؒH2O. In addition we
thank The University of London Central Research Fund,
The Nuffield Foundation and The Royal Society for financial
support and Dr I. Abrahams for final refinements of two of the
X-ray structures.
32 (a) S. Bromidge, P. Wilson and A. Whiting, Tetrahedron Lett., 1998,
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33 S. Danishefsky and T. Kitahara, J. Am. Chem. Soc., 1974, 96, 7807.
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37 D. H. Busch, D. J. Olszanski, J. C. Stevens, W. P. Schammel,
M. Kojima, N. Herron, L. L. Zimmer, K. A. Holter and J. Mocak,
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§ The Patterson map could not be refined using the I41a space group.
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D a l t o n T r a n s . , 2 0 0 3 , 2 0 4 3 – 2 0 5 2
2051