Abstract
tris(4-N,N-Dimethylaminophenyl)antimony dichloride (I) was prepared by the reaction of tris(4-N,N-dimethylaminophenyl)antimony with copper dichloride. tris(4-N,N-Dimethylaminophenyl)antimony difluoride benzene disolvate II was synthesized from dichloride I and sodium fluoride in aqueous acetone with the subsequent crystallization from benzene. tris(4-N,N-Dimethylaminophenyl)antimony dibenzoate III was obtained from tris(4-N,N-dimethylaminophenyl)antimony and benzoic acid in the presence of hydrogen peroxide in ether or from silver benzoate and the corresponding dichloride in acetone. According to X-ray studies Sb atoms in two crystallographically independent molecules of dichloride, difluoride benzene solvate, and dibenzoate have the distorted trigonal bipyramide coordination [ClSbCl, FSbF, and OSbO trans angles are 178.12(2)°, 178.57(3)°, 177.30°, and 176.49° respectively). Sb-Cl, Sb-F, and Sb-O interatomic distances are 2.4719(7)-2.505(7); 2.106(4); 2.438(2); 2.1212(13) Å respectively. The oxygen atoms of carbonyl groups of the molecule III (C 2v molecular symmetry) are coordinated to the central atom [Sb-O distance 2.987(1) Å].
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Original Russian Text © V.V. Sharutin, V.S. Senchurin, O.K. Sharutina, E.V. Akulova, 2008, published in Zhurnal Obshchei Khimii, 2008, Vol. 78, No. 12, pp. 1999–2006.
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Sharutin, V.V., Senchurin, V.S., Sharutina, O.K. et al. Synthesis and structure of tris(4-N,N-dimethylaminophenyl)antimony(V) difluoride, dichloride, and dibenzoate. Russ J Gen Chem 78, 2344–2352 (2008). https://doi.org/10.1134/S1070363208120098
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DOI: https://doi.org/10.1134/S1070363208120098