JOHN N. LOW et al. 2037
References
Cobo, J. (1995). PhD thesis, University of Ja6n, Spain.
Enraf-Nonius (1992). CAD-4/PC Software. Version 1.1. Enraf-
Nonius, Delft, The Netherlands.
Gabe, E. J., Le Page, Y., Charland, J.-P., Lee, F. L. & White, P. S.
(1989). J. Appl. Cryst. 22, 384-387.
Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge
National Laboratory, Tennessee, USA.
Low, J. L., Ferguson, G., Godino, M. L., Cobo, J., Lopez, R.,
Melguizo, M., Nogueras, M. & Sanchez, A. (1996). Acta Cryst.
C52, 418-420.
Sheldrick, G. M. (1993). SHELXL93. Programfor the Refinement of
Crystal Structures. University of Grttingen, Germany.
Spek, A. L. (1995a). PLATON. Molecular Geometry Program. Version
of July 1995. University of Utrecht, The Netherlands.
Spek, A. L. (1995b). PLUTON. Molecular Graphics Program. Version
of July 1995. University of Utrecht, The Netherlands.
Comment
As a part of our study of the Beckmann fragmentation
reaction in a series of steroidal tertiary a-hydroxy-
imino alcohols, the synthesis of 17a-benzyl-17~-hydro-
xy - 16 - hydroxyimi no - 3 - methoxyestra- 1,3,5 (10) - triene,
(2), was performed (Miljkovir, Ga~i, Medir-Mijarevir,
Stankovi6 & Lazar, 1995). Regioselective addition of
benzyllithium to the 17-carbonyl group of 16-hydroxy-
imino-3-methoxyestra-1,3,5 (1)-triene- 17-one, (1), afforded
the title compound, (2). Its structure, deduced from
chemical spectroscopic evidence, was confirmed by X-
ray diffraction analysis.
/~o . , /OH
H H 3 C O - ' ~ OH
H3CO
(1) (2)
Acta Cryst. (1996). C52, 2037-2040
17c~-Benzyl-17/3-hydroxy-16-hydroxyimino-
3-methoxyestra-l,3,5(10)-triene
SLOBODANKA STANKOVIC, a DU~AN LAZAR, ~ DU~AN
MILJKOVI6, b LJUBICA MEDIC-MIJACEVI6,b KATARINA
GA~I, b RADMILA KOVA~VI6 c AND CHRIS]lANE
COURSEILLE d
alnstitute of Physics, Faculty of Sciences, University of Novi
Sad, Trg Dositeja Obradovida 4, 21000 Novi Sad, Serbia,
blnstitute of Chemistry, Faculty of Sciences, University of
Novi Sad, Novi Sad, Serbia, Clnstitute of Biology, Faculty
of Sciences, University of Novi Sad, Novi Sad, Serbia, and
dLaboratoire de Cristallographie et de Physique Cristalline,
Facultd des Sciences, Universitd de Bordeaux L Talance,
France
(Received I May 1995; accepted 28 November 1995)
Abstract
The asymmetric unit of the title compound, 17c~-benz-
yl- 16 - hydroxyimino - 3 - methoxyestra- 1,3,5( 10 ) - trien-
17/3-ol, C26H31NO3, contains two molecules which
differ in the orientations of the methoxy groups at
C(3). The 17-hydroxy and 16-hydroxyimino moieties
are involved in intramolecular N...O and intermolecular
N-..O and O...O hydrogen bonds. The hydrogen-bond
network accounts for the differences in bond and torsion
angles of the a-hydroxyimino moieties of the symmetry-
independent molecules. This has been confirmed by
molecular-mechanics calculations on the individual mol-
ecules which indicate that they have the same geometry
in their energy minimum states.
@ 1996 International Union of Crystallography
Printed in Great Britain - all rights reserved
Perspective views of the two symmetry-independent
molecules, (I) and (II), of compound (2) are shown in
Fig. 1. Selected geometric parameters are given in Ta-
ble 2, together with corresponding values (in square
brackets) obtained from molecular-mechanics calcula-
tions. The puckering (Cremer & Pople, 1975) and asym-
metry parameters (Duax, Weeks & Rohrer, 1976) listed
in Table 3 reveal usual ring conformations. Ring B
has a 7a,8~-half-chair conformation; the distances of
atoms C(7) and C(8) from the best plane of the remain-
ing four atoms are -0.369(7) and 0.413 (6),~,, respec-
tively, for molecule (I), and -0.319 (7) and 0.437 (6)A
for molecule (II). Ring C has a chair conformation,
while ring D exhibits a conformation between a 13~-
envelope [the distance of atom C(13) from the best
Molecule (I)
c%c,
Molecule ClI)
Fig. 1. A perspective view of the two symmetry-independent mol-
ecules, (I) and (II), of the title compound. Displacement ellipsoids
are plotted at the 40% probability level.
Acta C~.stallographica Section C
ISSN 0108-2701 © 1996