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首页> 外文期刊>Crystal growth & design >From zero-to three-dimensional thioantimonates: [Ni(aepa)_2] _3Sb_6S_(12) (aepa = C_5H _(15)N_3 = N -(aminoethyl)-1,3-propandiamine), containing the unique [Sb_6S_(12)]~(6-) cyclic anion, [Ni(aepa) _2]_6(Sb_3S_6)_2(SO _4)
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From zero-to three-dimensional thioantimonates: [Ni(aepa)_2] _3Sb_6S_(12) (aepa = C_5H _(15)N_3 = N -(aminoethyl)-1,3-propandiamine), containing the unique [Sb_6S_(12)]~(6-) cyclic anion, [Ni(aepa) _2]_6(Sb_3S_6)_2(SO _4)

机译:从零到三维硫代锑酸盐:[Ni(aepa)_2] _3Sb_6S_(12)(aepa = C_5H _(15)N_3 = N-(氨基乙基)-1,3-丙二胺),其中包含独特的[Sb_6S_(12) )]〜(6-)环状阴离子,[Ni(aepa)_2] _6(Sb_3S_6)_2(SO _4)

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摘要

The new thioantimonates [Ni(aepa)_2]_3Sb _6S_(12) (1), [Ni(aepa)_2]_6(Sb _3S_6)_2(SO_4)_3?2H _2O (2), and [Ni(aepa)_2]Sb_4S_7 (3) (aepa = C_5H_(15)N_3 = N-(aminoethyl)-1,3- propandiamine) were obtained under solvothermal conditions by slightly varying the reaction conditions. In all compounds the [Ni(aepa)_2] ~(2+) complexes were formed in situ during the chemical reactions. Compound 1 features the new unique [Sb_6S_(12)]~(6-) cyclic anion composed by vertex-linked SbS3 trigonal pyramids. This [Sb_6S_(12)]~(6-) cyclic anion represents the largest isolated thioantimonate(III) anion. In the structure of [Ni(aepa) _2]_6(Sb_3S_6)_2(SO _4)_3?2H_2O, three SbS_3 units are corner-linked to form a Sb_3S_3 hetero ring adopting a twist conformation. Additionally, the new nickel complex [Ni(aepa)_2] _2Cl_2 was isolated from the same reaction slurry and was structurally characterized. Compound 3 represents a rare example of a three-dimensional thioantimonate(III) network. The [Sb_4S _7]~(2-) anion contains large Sb_(14)S_(14) rings with dimension of 6.1 × 16.1 ?~2. The structure directing effect of the in situ formed cations is obvious because [Ni(aepa) _2]~(2+) molecules are located in pairs above and below the large rings. The first photocatalytic hydrogen evolution tests exhibit promising results for compound 3.
机译:新的硫代锑酸盐[Ni(aepa)_2] _3Sb _6S_(12)(1),[Ni(aepa)_2] _6(Sb _3S_6)_2(SO_4)_3?2H _2O(2)和[Ni(aepa)_2通过稍微改变反应条件,在溶剂热条件下获得] Sb_4S_7(3)(aepa = C_5H_(15)N_3 = N-(氨基乙基)-1,3-丙二胺)。在所有化合物中,[Ni(aepa)_2]〜(2+)络合物都是在化学反应中原位形成的。化合物1具有新的独特的[Sb_6S_(12)]〜(6-)环状阴离子,该阴离子由顶点连接的SbS3三角金字塔组成。该[Sb_6S_(12)]〜(6-)环状阴离子代表最大的分离硫代锑酸根(III)阴离子。在[Ni(aepa)_2] _6(Sb_3S_6)_2(SO_4)_3→2H_2O的结构中,三个SbS_3单元被角连接以形成采用扭曲构象的Sb_3S_3杂环。另外,从相同的反应浆料中分离出新的镍络合物[Ni(aepa)_2] _2Cl_2,并对其结构进行了表征。化合物3代表三维硫代锑酸盐(III)网络的罕见实例。 [Sb_4S _7]〜(2-)阴离子包含尺寸为6.1×16.1?〜2的大Sb_(14)S_(14)环。由于[Ni(aepa)_2]〜(2+)分子成对地位于大环的上方和下方,因此原位形成的阳离子具有明显的结构导向作用。首次光催化氢析出试验显示了化合物3的有希望的结果。

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