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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Synthesis and crystal structure of Ca(en) _4Ca(en) _3[Sn _2Se _6] and Ca(en) _4Se _4 in superheated and supercritical ethylenediamine
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Synthesis and crystal structure of Ca(en) _4Ca(en) _3[Sn _2Se _6] and Ca(en) _4Se _4 in superheated and supercritical ethylenediamine

机译:Ca(en)_4Ca(en)_3 [Sn _2Se _6]和Ca(en)_4Se _4在过热和超临界乙二胺中的合成和晶体结构

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摘要

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$ar{1}$ (No. 2) with a = 10.2708(4) ?, b = 12.2739(5) ?, c = 16.3103(6) ?, α = 93.576(3)°, β = 90.609(3)°, = 109.269(4)°, Z = 1 and V = 1936.09(13) ? ~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) ?, b= 9.2738(6) ?, c = 16.9880(6) ?, Z = 8 and V = 4333.0(4) ? ~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.
机译:在乙二胺中在过热和超临界溶剂热条件下合成了两个新化合物Ca(en)_4Ca(en)_3 [Sn _2Se _6](1)和Ca(en)_4Se _4(2)。化合物1在三斜晶空间群P $ bar {1} $(第2号)中结晶,a = 10.2708(4)α,b = 12.2739(5)α,c = 16.3103(6)α,α= 93.576(3 )°,β= 90.609(3)°,= 109.269(4)°,Z = 1且V = 1936.09(13)? 〜3。 1的晶体结构由孤立的[Sn _2Se _6]〜(4-)阴离子以及Ca(en)_4〜(2+)和Ca(en)_3〜(2+)阳离子组成。化合物2在正交晶体空间群Fdd2(43号)中结晶,其a = 27.5034(10)δ,b = 9.2738(6)δ,c = 16.9880(6)δ,Z = 8,V = 4333.0(4)δ。 〜3。 2的晶体结构由Se _4〜(2-)阴离子和Ca(en)_4〜(2+)阳离子组成。在1和2中,硒酸锡酸盐[Sn _2Se _6]〜(4-)和四硒化物Se_4〜(2-)阴离子互连到Ca(en)_4〜(2+)的胺基上和/或Ca(en)_3〜(2+)通过氢桥形成三维网络。而在1 CaO中作为Ca〜(2+)的来源,使用Zintl相CaSi _2和硒粉合成了2 CaO。

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