Rhenium(V) Tris(pyrazolyl)borate Thiolate Complex with the Disulfide Bridging Ligand: Synthesis and Structure

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Resumo

The reaction of TpReOCl(StBu) (Tp = tris(pyrazolyl)borate anion) with sodium disulfide in dimethoxyethane affords the new binuclear rhenium complex [TpReO(μ-StBu)]2(μ-S2) (I). Complex I can also be synthesized by the reaction of TpReO(StBu)2 with a suspension of manganese(II) bromide in toluene accompanied by the dealkylation of one of the ligands to form one more new complex [TpReO]2(μ-S2)(μ-S) (II) containing the bridging sulfide and disulfide ligands. The structures of two crystalline solvates of complex I with dichloromethane containing the molecules with different conformations of the Re2S2 fragment (Ia and Ib) and complex II are studied by X-ray diffraction (XRD) (CIF files ССDC nos. 2262677, 2262678, and 2267423 for Ia, Ib, and II, respectively).

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Sobre autores

I. Skabitskii

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Autor responsável pela correspondência
Email: skabitskiy@gmail.com
Rússia, Moscow

S. Shapovalov

Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences

Email: skabitskiy@gmail.com
Rússia, Moscow

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2. Fig. 1. Molecular structure of Ia (a), Ib molecule 1 (b) and Ib molecule 2 (c) (independent molecules for Ib are shown in separate projections).

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3. Fig. 2. Molecular structure II (the solvate molecule of methylene chloride is not shown). Selected bond lengths: Re(1)—O(1) 1.702(4), Re(2)—O(2) 1.687(4), Re(1)—S(1) 2.320(1), Re(2)—S(1) 2.335(1), Re(1)—S(2) 2.237(2), Re(2)—S(3) 2.251(2), Re(1)—N(1) 2.251(5), Re(1)—N(3) 2.138(5), Re(1)—N(5) 2.165(5), Re(2)—N(7) 2.270(5), Re(2)—N(9) 2.106(5), Re(2)—N(11) 2.176(5), S(2)—S(3) 2.122(2) Å and valence angles: Re(1) S(1) Re(2) 119.84(6)oh, S(3) S(2) Re(1) 113.75(7)oh, S(2) S(3) Re(2) 113.74(8) fr.

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4. Scheme 1.

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5. Scheme 2.

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