Synthesis and crystal structure of Ca(en) 4Ca(en) 3[Sn 2Se 6] and Ca(en) 4Se 4 in superheated and supercritical ethylenediamine

Prashanth W. Menezes, Thomas F. Fässler

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Abstract

Two new compounds Ca(en) 4Ca(en) 3[Sn 2Se 6] (1) and Ca(en) 4Se 4 (2) were synthesized under superheated and supercritical solvothermal conditions in ethylenediamine. Compound 1 crystallizes in triclinic space group P$\bar{1}$ (No. 2) with a = 10.2708(4) Å, b = 12.2739(5) Å, c = 16.3103(6) Å, α = 93.576(3)°, β = 90.609(3)°, = 109.269(4)°, Z = 1 and V = 1936.09(13) Å 3. The crystal structure of 1 comprises of isolated [Sn 2Se 6] 4- anion as well as Ca(en) 4 2+ and Ca(en) 3 2+ cations. Compound 2 crystallizes in the orthorhombic space group Fdd2 (No. 43) with a = 27.5034(10) Å, b= 9.2738(6) Å, c = 16.9880(6) Å, Z = 8 and V = 4333.0(4) Å 3. The crystal structure of 2 consists of Se 4 2- anion and Ca(en) 4 2+ cations. In both 1 and 2 the selenostannate, [Sn 2Se 6] 4- and the tetraselenide, Se 4 2- anions are interconnected to the amine group of Ca(en) 4 2+ and/or Ca(en) 3 2+ via hydrogen bridges forming a three-dimensional network. Whereas in 1 CaO serves as source for Ca 2+, was 2 synthesized using the Zintl phase CaSi 2 and selenium powder.

Original languageEnglish
Pages (from-to)1109-1113
Number of pages5
JournalZeitschrift fur Anorganische und Allgemeine Chemie
Volume638
Issue number7-8
DOIs
StatePublished - Jun 2012

Keywords

  • Selenides
  • Selenostannates
  • Supercritical
  • Superheated
  • Zintl phases

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