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Issue 15, 2012
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Opening the paddlewheel: unusual coordination of [Mo2] dumbbells in the chain structures of A[Mo2(CF3SO3)5]·2CF3SO3H (A = Na, Rb, Cs)

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Abstract

The reaction of Mo(II)acetate, concentrated triflic acid and the alkaline metal triflates A(CF3SO3) (A = Na, Rb, Cs) in sealed glass ampoules at 110 °C yielded red single crystals of A[Mo2(CF3SO3)5]·2CF3SO3H (A = Na: triclinic, P-1, Z = 4, a = 13.714(1) Å, b = 14.339(1) Å, c = 21.340(2) Å, α = 81.78(1)°, β = 75.21(1)°, γ = 62.65(1)°; A = Rb/Cs: monoclinic, P21/m, Z = 2, a = 11.561(1)/11.584(1) Å, b = 14.817(1)/14.9472(8) Å, c = 11.6208(1)/11.744(1) Å, β = 112.38(1)/113.48(1)°). The crystal structures contain dumbbell shaped [Mo2] moieties surrounded by three chelating and four monodentate triflate anions leading to an opening of the typical paddlewheel fragment at one of its edges. The monodentate triflate anions are connected to further [Mo2] dumbbells leading to infinite anionic chains according to 1[Mo2(CF3SO3)3/1(CF3SO3)4/2]. The charge balance is achieved by the alkaline metal ions that are additionally coordinated by triflic acid molecules. Theoretical investigations were preformed on the open paddlewheel fragment and are in good agreement with the experimental findings. According to DTA/TG measurements and the XRD investigations the decomposition of the compounds occurs in multiple steps and leads to MoO2 and A2MoO4.

Graphical abstract: Opening the paddlewheel: unusual coordination of [Mo2] dumbbells in the chain structures of A[Mo2(CF3SO3)5]·2CF3SO3H (A = Na, Rb, Cs)

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Supplementary files

Article information


Submitted
16 Nov 2011
Accepted
27 Jan 2012
First published
01 Mar 2012

Dalton Trans., 2012,41, 4685-4691
Article type
Paper

Opening the paddlewheel: unusual coordination of [Mo2] dumbbells in the chain structures of A[Mo2(CF3SO3)5]·2CF3SO3H (A = Na, Rb, Cs)

K. Neuschulz, M. Penning, L. Groß, T. Klüner and M. S. Wickleder, Dalton Trans., 2012, 41, 4685
DOI: 10.1039/C2DT12196D

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