Synthesis of CsCuS6 and Cs6Cu2(TeS3)2(S6)2 in Molten Cs2SxTey Salts. Novel Compounds Containing Polychalcogenide Ligands

Timothy J. McCarthy, Xiang Zhang, Mercouri G. Kanatzidis

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Abstract

The reaction of Cu with excess Cs2Sx and Cs2SxTey produced two new copper/polychalcogenides CsCuS6 (1) and Cs6Cu2(S6)2(TeS3)2 (2). Orange-red 1 was synthesized by the reaction of copper powder with CS2S11 in the 1.25:1 molar ratio at 270 °C for 4 days. Red 2 was synthesized by the reaction of copper powder with Cs2S6Te0.7 in the 2:3 molar ratio at 230 °C for 96 h or by the reaction of CuTe with Cs2S6 in a 2:3 molar ratio at 250 °C for 96 h. Crystal data for 1: triclinic P1̄, Z = 2, a = 10.664(2) Å, b = 11.223(1) Å, c = 7.1599(8) Å, α = 94.64(1)°, β = 101.32(1)°, γ = 74.04(1)°, V= 807.5(4) Å3, 2θmax = 60°. Number of data measured: 4709. Number of data having Fo2 > 3σ(Fo2): 2800. Final R/Rw = 0.036/0.044. Crystal data for 2: a = 21.072(4) Å, b= 13.173(3) Å, c = 11.948(2) Å,V= 3317(1) Å3 at 20 °C, 2θmax = 55°, space group Cmca, Mo Kα radiation. Number of data having Fo2> 3 θ-(Fo2): 1437. Final R/Rw = 0.031/0.026. The structure of CsCuS6 is assembled from one-dimensional [Cu(S6)]nn− centrosymmetric chains (running parallel to the crystallographic [011] direction) separated by Cs+ atoms. Cs6Cu2(S6)2(TeS3)2 contains a dimeric anion assembled from two tetrahedral Cu+ atoms joined by two trigonal pyramidal TeS32− ligands and two chelating S62− ligands. The infrared and UV/vis/near-IR spectra of these compounds are reported.

Original languageEnglish
Pages (from-to)2944-2948
Number of pages5
JournalInorganic Chemistry
Volume32
Issue number13
DOIs
Publication statusPublished - Jan 1 1993

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ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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