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. 2021 Aug 9;60(33):17866-17870.
doi: 10.1002/anie.202107587. Epub 2021 Jul 9.

A Versatile Silver(I) Pentafluorooxosulfate Reagent for the Synthesis of OSF5 Compounds

Axel Haupt  1 , Daniel Duvinage  2 , Enno Lork  2 , Maksym Ponomarenko  1 , Gerd-Volker Röschenthaler  1
Affiliations

A Versatile Silver(I) Pentafluorooxosulfate Reagent for the Synthesis of OSF5 Compounds

Axel Haupt et al. Angew Chem Int Ed Engl. .

Abstract

Herein, we report the preparation of silver(I) pentafluorooxosulfate from commercially available AgF and OSF4 . The compound is surprisingly stable in a MeCN solution. Apart from that, AgOSF5 has been stabilised by the addition of 2,2'-bipyridine ligands. Starting from solutions of the unstabilised silver(I) salt, OSF5 complexes with NiII , CuI , and CuII -centres have been obtained. In addition, AgOSF5 has proven to be generally capable of mediating the transfer of OSF5 groups to aryne moieties, thus furnishing a new and safe method for the preparation of OSF5 -substituted arenes. X-ray crystal structure analysis of selected transition-metal OSF5 compounds have revealed distorted octahedral [OSF5 ]- anions which are extensively stabilised by hydrogen bonding.

Keywords: arynes; chalcogens; fluorine; silver; synthetic methods.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Scheme 1
Scheme 1
Preparation of silver(I) pentafluorooxosulfate 3.
Scheme 2
Scheme 2
Stabilisation of AgOSF5 by 2,2′‐bipyridine ligands.
Scheme 3
Scheme 3
Salt metathesis of transition‐metal halides using AgOSF5 3 and direct synthesis of nickel(II) complex 9.
Figure 1
Figure 1
Left: extract of the solid‐state packing of [Cu(MeCN)4][OSF5]⋅⋅⋅MeCN 6, revealing layers of [OSF5]− anions, which are stabilised by numerous H−F and H−O contacts. For clarification, cations and free MeCN ligands with short contacts to the anions are shown exclusively using the stick model. Right: distorted octahedral [OSF5]− anion with selected bond lengths (in Å) and bonding angles. Ellipsoids are at a probability level of 50 %.
Figure 2
Figure 2
Top: extract of the solid‐state packing of [Cu(bpy)2(OSF5)][OSF5]⋅⋅⋅0.5 MeCN 8, revealing the two different types of [OSF5]− anions. Bottom: distorted trigonal bipyramidal [Cu(bpy)2(OSF5)]+ cation with selected bond lengths (in Å) and bonding angles. Hydrogen atoms are omitted for clarity; ellipsoids are at a probability level of 50 %.
Scheme 4
Scheme 4
Synthesis of the stable OSF5 − salt 11 and preparation of OSF5‐substituted dimethylbenzene 13.
See this image and copyright information in PMC

References

    1. For a review on OEF5 compounds, see: Seppelt K., Angew. Chem. Int. Ed. Engl. 1982, 21, 877–888;
    2. Angew. Chem. 1982, 94, 890–901.
    1. None
    1. Seppelt K., Nothe D., Inorg. Chem. 1973, 12, 2727–2730;
    1. Engelbrecht A., Sladky F., Inorg. Nucl. Chem. Lett. 1965, 1, 15;
    1. Mayer E., Sladky F., Inorg. Chem. 1975, 14, 589–592.

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