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Issue 21, 2004
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Purposeful construction versusself-assembly in approaches to single source precursors of spinel materials. Synthesis, structure and stability studies of MiiAl2(acac)3(OiPr)4(OAc), Mii = Mn, Co, Zn – a new class of heterometallic heteroleptic alkoxide complexes

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Abstract

The reaction of Mn(acac)3 with 3 eq. of Al(OiPr)3 in toluene at reflux provided with minor yield single crystals of MnAl2(acac)3(OiPr)4(OAc)(C7H8)0.5 (1), incorporating into the molecular structure the acetate ligand originating from oxidation of the OiPr-groups. 1 was obtained with high yield (76%) via the reaction of Mn(acac)3 with 2.2 eq. of Al(OiPr)3 with subsequent addition of 1 eq. of HOAc to the reaction mixture cooled to room temperature. The analogs of 1, CoAl2(acac)3(OiPr)4(OAc)(C7H8)0.5 (2), and ZnAl2(acac)3(OiPr)4(OAc)(C7H8)0.5 (3), were obtained with almost quantitative yields by reaction of the corresponding MII(acac)2 with 2 eq. of Al(OiPr)3 in toluene at reflux with subsequent addition of 1 eq. of Hacac and 1 eq. of HOAc after cooling the reaction mixture to the room temperature. In the molecules 1–3 the late transition metal atom is tetrahedrally coordinated (η2-acac plus 2 bonds to μ-OiPr-groups), and the Al atoms have a slightly distorted octahedral coordination (hexacoordinated) (η2-acac plus 3 bonds to μ-OiPr-groups plus one bond to μ-OAc-group). 1–3 are stable to solvolysis in toluene and are volatile under reduced pressure. Thermal decomposition of CoAl2(acac)3(OiPr)4(OAc)(C7H8)0.5 leads to nanoparticles of CoAl2O4, while homogeneous coatings of the spinel can be easily obtained using MOCVD.

Graphical abstract: Purposeful construction versus self-assembly in approaches to single source precursors of spinel materials. Synthesis, structure and stability studies of MiiAl2(acac)3(OiPr)4(OAc), Mii = Mn, Co, Zn – a new class of heterometallic heteroleptic alkoxide complexes

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Article information


Submitted
19 Apr 2004
Accepted
25 May 2004
First published
27 Sep 2004

J. Mater. Chem., 2004,14, 3150-3157
Article type
Paper

Purposeful construction versus self-assembly in approaches to single source precursors of spinel materials. Synthesis, structure and stability studies of MIIAl2(acac)3(OiPr)4(OAc), MII = Mn, Co, Zn – a new class of heterometallic heteroleptic alkoxide complexes

G. A. Seisenbaeva, E. V. Suslova, M. Kritikos, V. G. Kessler, L. Rapenne, M. Andrieux, F. Chassagneux and S. Parola, J. Mater. Chem., 2004, 14, 3150
DOI: 10.1039/B405771F

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