Electrochemical Synthesis of [NEt4]2[enH]2[Ge2Se6] and [NEt4]4[Sn4Se10]

Chang Woo Park*, Michael A. Pell, James A Ibers

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

46 Scopus citations

Abstract

[NEt4][enH]2[Ge2Se6] and [NEt4]4[Sn4Se10] have been synthesized electrochemically by the reduction of metal chalcogen alloys in an electrolyte solution of NEt4Br in ethylenediamine. The structures of both compounds have been determined by single-crystal X-ray methods. [NEt4]2[Ge2Se6] crystallizes in the triclinic space group Ci1-P1̄ with one formula unit in a cell of dimensions a = 7.805(4) Å, b = 10.747(6) Å, c = 11.445(6) Å, α = 110.33(2)°, β = 97.19(3)°, γ = 92.62(2)°, and V = 889.0(8) Å3 (T = 115 K). Final agreement indices for [NEt4]2[enH]2[Ge2Se6] are 0.116 for RW(Fo2) for all the 2982 data and 0.055 for R1 for the 1958 reflections with Fo2 ≥ 2σ(Fo2) (158 variables). [NEt4]4[Sn4Se10] crystallizes in the cubic space group Td4-P4̄3n with eight formula units in a cell of dimensions a = 22.170(7) and V= 10897(6) Å33 (T= 115 K). Final agreement indices for [NEt4]4[Sn4Se10] are 0.123 for Rw(Fo2 for all the 1490 data and 0.057 for R1 for the 1138 data with Fo2 ≥ 2σ(Fo2) (90 variables). The [Ge2Se6]4- anion is composed of a pair of edge-sharing tetrahedra. Each of the two independent [Sn4Se10]4- anions has the adamantane-type structure consisting of four Sn tetrahedra, each of which shares three edges with three similar tetrahedra; the symmetry of one anion is 4̄ (S4) while that of the other is 23 (T). Although both the [Ge2Se6]4- and [Sn4Se10]4-]4' anions are new, each has group 14 structural analogues.

Original languageEnglish (US)
Pages (from-to)4555-4558
Number of pages4
JournalInorganic Chemistry
Volume35
Issue number16
StatePublished - Dec 1 1996

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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