Abstract Two novel compounds: polynuclear catena-poly[bis(μ3-O,O′-di-cyclo-hexyldithiophosphato-S,S,S′)digold(I)] (Au Au) (1) and crystalline bis(O,O′-di-cyclo-hexylthiophosphoryl)disulphide, (cyclo-C6H11O)2P(S)S S(S)P(O-cyclo-C6H11)2 (2) were prepared using heterogeneous reaction between freshly precipitated binuclear cadmium(II) dithiophosphate (Dtph), [Cd2{S2P(O-cyclo-C6H11}4] and H[AuCl4] in 2 M hydrochloric acid. The isolated compounds 1 and 2 (the fixation mode of gold from the solution and the oxidised form of Dtph groups, respectively) have been studied by means of single-crystal X-ray diffraction, 13C and 31P cross-polarisation/magic-angle-spinning (CP/MAS) NMR spectroscopy and simultaneous thermal analysis (STA). Centrosymmetric binuclear molecule of 1, [Au2{S2P(O-cyclo-C6H11)2}2] comprises a pair of μ-bridging di-cyclo-hexyl Dtph ligands, linking two neighbouring gold atoms, and displays additional intramolecular aurophilic bond Au⋯Au. At the supramolecular level of structural self-organisation of complex 1, infinite polymeric zigzag chains arise due to pairs of the secondary bonds Au···S between neighbouring binuclear molecules. Centrosymmetric molecule of 2 displays two O,O′-di-cyclo-hexythiophosphoryl fragments, which are connected by the chemical bond S(1) S(1)a, and a planar zigzag array [S P S S P S] passing through the central part of the molecule. To characterise additionally the Dtph groups in both compounds 1 and 2, chemical shift anisotropy (CSA) parameters (δaniso and η) were calculated from spinning sideband manifolds in experimental 31P MAS NMR spectra. The thermal behaviour of complex 1 was studied using simultaneous thermal analysis (a combination of TG and DSC) under an argon atmosphere. The thermal behaviour displays stepwise mass loss, comprising thermal decompositions of the organic and inorganic parts of 1 with gold(I) dithio-meta-phosphate and reduced metallic gold as the intermediate and the final products, respectively.

中文翻译：

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使用二环己基二硫代磷酸镉与 H[AuCl4] 的非均相反应从溶液中固定金的模式。结晶聚合金 (I) 二环己基二硫代磷酸和双 (二环己基硫代磷酰) 二硫化物的结构和 (13C, 31P) CP/MAS NMR 研究和热行为

[Au2{S2P(O-cyclo-C6H11)2}2] 包含一对 μ-桥连二环己基 Dtph 配体，连接两个相邻的金原子，并显示出额外的分子内亲金键 Au⋯Au。在复合物 1 的结构自组织的超分子水平上，由于相邻双核分子之间的次级键 Au...S 对，产生了无限的聚合锯齿形链。2 的中心对称分子显示两个 O,O'-二环己硫代磷酰基片段，它们通过化学键 S(1) S(1)a 和穿过中心部分的平面锯齿形阵列 [SPSSPS] 连接分子。为了另外表征化合物 1 和 2 中的 Dtph 基团，化学位移各向异性 (CSA) 参数（δaniso 和 η）从实验 31P MAS NMR 光谱中的旋转边带流形计算。在氩气气氛下使用同步热分析（TG 和 DSC 的组合）研究配合物 1 的热行为。热行为显示出逐步的质量损失，包括 1 的有机和无机部分的热分解，其中二硫代偏磷酸盐金 (I) 和还原的金属金分别作为中间产物和最终产物。