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The effect of temperature onto the crystal structure of thioantimonates: solvothermal syntheses and crystal structures of [Co(dien)2][Co(tren)SbS4]20.5 H2O and {[Co(tren)]2[CoSb2S6]}H2O

Abstract : The two new compounds [Co(dien)2][Co(tren)SbS4]20.5 H2O (1) and {[Co(tren)]2[CoSb2S6]}H2O (2) were synthesized applying mixtures of amines as structure directing molecules (dien = diethylenediamine; tren = tren = tris(2-aminoethyl)amine). Compound 1 crystallizes in the monoclinic space group C2/c with a = 29.378(3), b = 7.6643(4), c = 22.507(2) Å,  = 115.39(1)° and represents a pseudo-polymorph to the compound [Co(dien)2][Co(tren)SbS4]24H2O. The structure consists of the two complexes [Co(2)(dien)2]2+ and [Co(1)(tren)SbS4]- with the latter containing a [Sb(V)S4]3- anion bonded to the Co2+ cation. Compound 2 crystallizes in space group P21/c, a = 13.870(2), b = 14.708(1), c = 14.700(2) Å,  = 94.62(2)°. The central and new feature of the structure is a heterometallic [CoSb2S6] core composed of two [Sb(III)S3] pyramids and a [CoS4] tetrahedron. The [CoS4] tetrahedron shares two edges with two [Sb(III)S3] units. The remaining S atom of the [Sb(III)S3] groups are bonded to two independent [Co(tren)] complexes.
Keywords : Physical Sciences
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Wolfgang Bensch, Jessica Lichte, Henning Lühmann, Christian Näther. The effect of temperature onto the crystal structure of thioantimonates: solvothermal syntheses and crystal structures of [Co(dien)2][Co(tren)SbS4]20.5 H2O and {[Co(tren)]2[CoSb2S6]}H2O. Journal of Inorganic and General Chemistry / Zeitschrift für anorganische und allgemeine Chemie, Wiley-VCH Verlag, 2009, 635 (12), pp.2021. ⟨10.1002/zaac.200900177⟩. ⟨hal-00504927⟩

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