Heterometallic 3d–4f Complex with Unusual [MnIV
Nd O ] Core Topology
4 4 4
unprecedented [MnIV Nd O ] core. Systematic problems with Supporting Information (see footnote on the first page of this article):
4
4 4
Details of X-ray data collection and structure refinement, as well as
EDX measurement.
the collection of suitable yields of a pure sample of this poten-
tial SMM have so far hampered the determination of magnetic
properties. However, according multiple reproduction experi-
ments are currently underway. The investigated system seems
to be promising for yielding further interesting compounds in
the future.
Acknowledgement
This work was supported by the Alexander von Humboldt Foundation.
Help of M. Hellwig (EDX) and R. Riedel (X-ray data collection) is
gratefully acknowledged.
Experimental Section
General: 2Ј-hydroxyacetophenoxime was synthesized from 2Ј-hy-
[
5]
droxysalicylaldoxime and hydroxylamine hydrochloride. All other References
chemicals and solvents were used as received and no inert gas tech-
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Synthesis and Characterization of 1
MnCl
2
1
2
·4H
mmol, 2 equiv.), 2Ј-hydroxyacetophenoxime (151 mg, 1 mmol,
equiv.) and NEt OH (25% in methanol; 2 mL, 3 mmol, 3 equiv.)
2 3 3 2
O (189 mg, 1 mmol, 1 equiv.), Nd(NO ) ·6H O (878 mg,
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4
were combined in methanol (60 mL). After stirring for 12 h, the solu-
tion was concentrated to a volume of ca. 45 mL, filtered, concentrated
again to ca. 20 mL and finally layered with diethyl ether (20 mL). A
few black crystals formed within about one month and were found
suitable for X-ray diffraction analysis. X-ray spectral analysis (Cam-
Scan 4DV + EDX Noran Instruments Voyager 4.0 with Pioneer Detec-
tor with ultrathin window) was used to confirm the elemental composi-
tion of a carbon-coated sample: Mn 55.43%, Nd 44.57% (Mn/Nd ratio
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1.2; see Suporting Information).
[
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α
with graphite-monochromated Mo-K radiation (λ = 0.71073 Å) at 100
K.[ The structure was solved by direct methods and refined on F by
6]
2
[
[
full-matrix least-squares methods using the SHELXTL program pack-
age.[ Details on structure refinement are available in ESI. The supple-
mentary crystallographic data CCDC-831615 (1) can be obtained free
of charge from The Cambridge Crystallographic Data Center via
www.ccdc.cam.ac.uk.data_request.cif. For further details and further
characterization see the Supporting Information.
7]
Received: July 1, 2011
Published Online: September 26, 2011
Z. Anorg. Allg. Chem. 2011, 2093–2095
© 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
www.zaac.wiley-vch.de
2095