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首页> 外文期刊>Journal of chemical crystallography >The crystal structure of {[Pt(9S3)Cl2]2[Pt(9S3) 2]}Cl2?4H2O: An improved synthesis of [Pt(9S3)Cl2]
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The crystal structure of {[Pt(9S3)Cl2]2[Pt(9S3) 2]}Cl2?4H2O: An improved synthesis of [Pt(9S3)Cl2]

机译：{[Pt（9S3）Cl2] 2 [Pt（9S3）2]} Cl2？4H2O的晶体结构：[Pt（9S3）Cl2]的改进合成

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We wish to report the crystal structure for a solid-state solution, {[Pt(9S3)Cl2]2[Pt(9S3)2]}Cl2? 4H2O (1), which contains two different complexes of Pt(II) with the trithiacrown 9S3 (1,4,7-trithiacyclononane). One complex [Pt(9S3)Cl2] is neutral and contains a Pt(II) center with a single 9S3 ligand and two coordinated chloro ligands. The second Pt(II) complex is a dication and contains two coordinated 9S3 ligands and two non-coordinating chloride anions. There are two crystallographically equivalent [Pt(9S3)Cl2] complexes present for every single [Pt(9S3)2]2+ cation. Four water solvent molecules are also present. In the neutral complex ([Pt(9S3)Cl2], the Pt(II) center is surrounded by a cis-[S2Cl2 + S 1] ligand environment formed by the two chloro ligands and two of the three sulfur atoms from the 9S3 ligand. These two sulfurs are positioned 2.225(2) and 2.242(2) ? from the Pt(II), but the third sulfur shows a long distance interaction at 3.311(2) ? to form an elongated square pyramidal structure. This axial Pt-S distance is the longest observed in 57 crystal structures of Pt(II) 9S3 complexes. The cation [Pt(9S3)2] 2+ displays two centrosymmetrically coordinated 9S3 ligands forming a [S4 + S2] environment with an elongated octahedral shape. In the dication, the two equatorial Pt-S distances are 2.297(2) and 2.306(2) ? with the axial sulfur at 3.065(2) ?. The most interesting intermolecular aspects of the structure are hydrogen bonding interactions between two of the water molecules and two chloride counter-ions, resulting in a nearly square O2Cl2 ring. This ring shares an edge with a six-membered ring formed by four waters and two chlorides which are hydrogen bonded. The hydrogen bonding interactions, which result from the presence of water in the crystal, appear to be an important component in stabilizing the lattice for the unusual solid-state solution structure. Crystal Data for (1): P2 1 , a = 7.8327(10) ?, b = 25.152(4) ?, c = 12.382(2) ?, V = 2314.3(6) ?3, Z = 2. We also report an improved synthetic procedure for the preparation of two thiacrown complexes [Pt(9S3)Cl2] and [Pt(10S3)Cl2], which are commonly used as precursors for other heteroleptic thioether complexes. The new syntheses proceed at room temperature without the need for long reflux times and produce large crystals which are easily isolable without filtration. The simplicity of these new preparations results in improved yields over previously employed methods.
机译：我们希望报告{{Pt（9S3）Cl2] 2 [Pt（9S3）2]} Cl2固态溶液的晶体结构。 4H2O（1），其中包含Pt（II）与Trithiacrown 9S3（1,4,7-trithiacyclononane）的两种不同络合物。一种络合物[Pt（9S3）Cl2]是中性的，包含一个带有单个9S3配体和两个配位氯配体的Pt（II）中心。第二种Pt（II）配合物是双阳离子，包含两个配位的9S3配体和两个非配位的氯阴离子。对于每个[Pt（9S3）2] 2+阳离子，存在两种晶体学上等效的[Pt（9S3）Cl2]络合物。还存在四个水溶剂分子。在中性络合物（[Pt（9S3）Cl2]中，Pt（II）中心被由两个氯配体和9S3配体中的三个硫原子中的两个形成的顺式[S2Cl2 + S 1]配体环境包围。这两个硫原子位于距Pt（II）2.225（2）和2.242（2）？处，但是第三个硫在3.311（2）？处显示出长距离相互作用，从而形成细长的方形金字塔结构。 S距离是在Pt（II）9S3配合物的57个晶体结构中观察到的最长的距离，阳离子[Pt（9S3）2] 2+显示两个中心对称配位的9S3配体，形成具有细长八面体形状的[S4 + S2]环境。根据指示，两个赤道的Pt-S距离分别为2.297（2）和2.306（2）？，轴向硫为3.065（2）？。结构中最有趣的分子间方面是两个水分子之间的氢键相互作用和两个氯化物抗衡离子，形成一个接近正方形的O2Cl2环，该环与6个膜共享一个边由四个与氢键合的水和两个氯化物形成的红环。由晶体中水的存在引起的氢键相互作用似乎是稳定不寻常固态溶液结构晶格的重要组成部分。 （1）的晶体数据：P2 1 / n，a = 7.8327（10）？，b = 25.152（4）？，c = 12.382（2）？，V = 2314.3（6）？3，Z = 2还报道了一种改进的合成方法，用于制备两种噻唑酮配合物[Pt（9S3）Cl2]和[Pt（10S3）Cl2]，它们通常用作其他杂配硫醚配合物的前体。新的合成过程在室温下进行，不需要很长的回流时间，并且可以生成大晶体，无需过滤即可轻松分离。这些新制剂的简单性导致了比以前采用的方法更高的产率。

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