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Journal article

Base-Free and Bisphosphine Ligand Dialkylmanganese(II) Complexes as Precursors for Manganese Metal Deposition

Abstract

The solid-state structures and the physical, solution magnetic, solid-state magnetic, and spectroscopic (NMR and UV/vis) properties of a range of oxygen- and nitrogen-free dialkylmanganese­(II) complexes are reported, and the solution reactivity of these complexes toward H2 and ZnEt2 is described. The compounds investigated are [{Mn­(μ-CH2SiMe3)2}∞] (1), [{Mn­(CH2CMe3)­(μ-CH2CMe3)2}2{Mn­(μ-CH2CMe3)2Mn}] (2), [Mn­(CH2SiMe3)2(dmpe)] (3; dmpe = 1,2-bis­(dimethylphosphino)­ethane), [{Mn­(CH2CMe3)2(μ-dmpe)}2] (4), [{Mn­(CH2SiMe3)­(μ-CH2SiMe3)}2(μ-dmpe)] (5), [{Mn­(CH2CMe3)­(μ-CH2CMe3)}2(μ-dmpe)] (6), [{Mn­(CH2SiMe3)­(μ-CH2SiMe3)}2(μ-dmpm)] (7; dmpm = bis­(dimethylphosphino)­methane), and [{Mn­(CH2CMe3)­(μ-CH2CMe3)}2(μ-dmpm)] (8). Syntheses for 1–4 have previously been reported, but the solid-state structures and most properties of 2–4 had not been described. Compounds 5 and 6, with a 1:2 dmpe/Mn ratio, were prepared by reaction of 3 and 4 with base-free 1 and 2, respectively. Compounds 7 and 8 were accessed by reaction of 1 and 2 with 0.5 equiv or more of dmpm per manganese atom. An X-ray structure of 2 revealed a tetrametallic structure with two terminal and six bridging alkyl groups. In the solid state, bisphosphine-coordinated 3–8 adopted three distinct structural types: (a) monometallic [LMnR2], (b) dimetallic [R2Mn­(μ-L)2MnR2], and (c) dimetallic [{RMn­(μ-R)}2(μ-L)] (L = dmpe, dmpm). Compound 3 exhibited particularly desirable properties for an ALD or CVD precursor, melting at 62–63 °C, subliming at 60 °C (5 mTorr), and showing negligible decomposition after 24 h at 120 °C. Comparison of variable-temperature solution and solid-state magnetic data provided insight into the solution structures of 2–8. Solution reactions of 1-8 with H2 yielded manganese metal, demonstrating the thermodynamic feasibility of the key reaction steps required for manganese­(II) dialkyl complexes to serve, in combination with H2, as precursors for metal ALD or pulsed CVD. In contrast, the solution reactions of 1–8 with ZnEt2 yielded a zinc–manganese alloy with an approximate 1:1 Zn/Mn ratio.

Authors

Price JS; Chadha P; Emslie DJH

Journal

Organometallics, Vol. 35, No. 2, pp. 168–180

Publisher

American Chemical Society (ACS)

Publication Date

January 25, 2016

DOI

10.1021/acs.organomet.5b00907

ISSN

0276-7333

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