Isolation of β-Ag3AsSe3, (Me3NH)[Ag3As2Se5], K5Ag2As3Se9, and KAg3As2S5: Novel solid state silver thio- and selenoarsenates from solvento-thermal synthesis

Mercouri G. Kanatzidis, Jun Hong Chou

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Abstract

Three new solid state silver selenoarsenates and one thioarsenate prepared from hydro- and methanothermal synthesis are described. β-Ag3AsSe3 (I) and (Me3NH)[Ag3As2Se5] (II) were synthesized hydrothermally at 110°C from a mixture of AgBF4/3K3AsSe3 and AgBF4/3K3AsSe3/6Me3NHCl, while K5[Ag2As3Se9] (III) and K[Ag3As2S5] (IV) were synthesized methanothermally at 110°C from a mixture of AgBF4/3K3AsS3 and AgBF4/3K3AsSe3, respectively. β-Ag3AsSe3(I) crystallizes in the orthorhombic space group Pnma (No. 62) with a = 8.111(1) Å, b = 11.344(2) Å, c = 20.728(3) Å, Z = 8, V = 1907(1) Å3. This compound is a new allotrope of α-Ag3AsSe3 and has a complex three-dimensional structure composed of distorted trigonal planar and tetrahedral Ag+ ions and [AsSe3]3- units. (Me3NH)[Ag3As2Se5] (II) crystallizes in the triclinic space group P - 1 (No. 2) with a = 10.119(2) Å, b = 18.010(4) Å, c = 14.932(3) Å, α = 110.20 (1)°, β = 103.98(2)°, γ = 99 99(1)°, Z = 2, V = 729.3(8) Å3. The [Ag3As2Se5]n-n anion in (II) has a complex two-dimensional layered structure with tetrahedral Ag+ ions and [As2Se5]4- units. K5[Ag2As3Se9] (III) crystallizes in the orthorhombic space group Pnma (No. 62) with a = 12.599(2) Å, b = 12.607(4) Å, c = 14.067(3) Å, Z = 8, V = 2234(1) Å3. The [Ag2As3Se9]5n-n anion in (III) has a two-dimensional layered structure with tetrahedral Ag+ ions and two different kinds of selenoarsenate units, [AsSe4]3- and [As2Se5]4-. K[Ag3As2S5] (IV) also crystallizes in the orthorhombic space group Pnma (No. 62) with a = 19.210(2) Å, b = 16.867(2) Å, c = 6.3491(7) Å, Z = 8, V = 2057.2(7) Å3. The [Ag3As2S5]n-n anion in (IV) possesses a complicated two-dimensional structure with tetrahedral Ag+ ions and two kinds of thioarsenate ligands, [AsS3]3- and [As3S7]5-. The thermal stability and optical absorption properties of these compounds are reported.

Original languageEnglish
Pages (from-to)186-201
Number of pages16
JournalJournal of Solid State Chemistry
Volume127
Issue number2
DOIs
Publication statusPublished - Dec 1996

ASJC Scopus subject areas

  • Electronic, Optical and Magnetic Materials
  • Ceramics and Composites
  • Condensed Matter Physics
  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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