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Synthesis and crystal structure of [Nb2(S1.72Se2.28)(S2CNEt2)4]—A solid solution based on [Nb2(μ2, η2-X2)2(S2CNEt2)4], where X2=S2, SSe, and Se2. New model of structure refinement of [Nb2(S2)2(S2CNEt2)4], where X2=S2, SSe, and Se2. New model of structure refinement of [Nb2(S2)2(S2CNEt2)4]

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Abstract

The crystal structure of [Nb2(S1.72Se2.28)(S2CNEt2)4], which is a solid solution based on [Nb2(μ2, η2-X2)2(S2CNEt2)4], where X2=S2, SSe, and Se2, is determined. The compound was obtained by the reaction of NaS2CNEt2 in CH3CN with the product of the reaction of the NbSe2Cl2-KNCS fusion cake with an aqueous solution of Bu4NBr (yield 30%). The crystals are monoclinic, a=21.319(11), b=7.008(1), c=16.673(8) Å, β=133.99(2)°, Vcell=1792(1) Å3, space group C2/m, Z=2, dcalc=1.879 g/cm3 for C20H40N4Nb2S9.72Se2.28, Syntex P21, λCukα, Nmeas/corr=2423/1191, R(F)=0.0569 and wR(F2)=0.1282 for 889 Fhkl>4σ(F). The compound is isostructural to the thio analog Nb2S4(S2CNEt2)4 studied earlier; in both cases, the molecule is disordered in crystals over two positions. The composition was refined by diffraction data. The results are in good agreement with the Raman and FMB (fast molecule bombardment) mass spectrometry data. The structure of Nb2S4(S2CNEt2)4 was refined for the second time using a new model of disorder; as a result of the refinement, a normal value of S−S bond length in the S2 ligand [2.027(5) Å] was obtained.

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Authors
  1. A. V. Virovets
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  2. M. N. Sokolov
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  3. N. V. Podberezskaya
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  4. V. E. Fedorov
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Additional information

Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences. Translated formZhurnal Strukturnoi Khimii, Vol. 37, No. 3, pp. 528–533, May–June, 1996.

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Virovets, A.V., Sokolov, M.N., Podberezskaya, N.V. et al. Synthesis and crystal structure of [Nb2(S1.72Se2.28)(S2CNEt2)4]—A solid solution based on [Nb2(μ2, η2-X2)2(S2CNEt2)4], where X2=S2, SSe, and Se2. New model of structure refinement of [Nb2(S2)2(S2CNEt2)4], where X2=S2, SSe, and Se2. New model of structure refinement of [Nb2(S2)2(S2CNEt2)4]. J Struct Chem 37, 458–463 (1996). https://doi.org/10.1007/BF02578601

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  • DOI: https://doi.org/10.1007/BF02578601

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