Two thioamide pro-ligands, R¹N(H)C(═S)R² (R¹ = t-Bu, R² = i-Pr and R¹ = i-Pr, R² = i-Pr), were synthesized by treatment of the corresponding amides with Lawesson’s reagent. Reactions of [Sn{N(SiMe₃)₂}₂] with two molar equivalents of each thioamide pro-ligand yielded the tin(II) thioamidate species, bis(2-methyl-N-(1-methylethyl)-propanethioamide)tin(II) and Bis[N-(1,1-dimethylethyl)-2-methylpropanethioamide]tin(II). Both of the new tin compounds have been characterized by ¹H, ¹³C{¹H}, and ¹¹⁹Sn NMR spectroscopy and elemental analysis. In addition, the solid-state structure of bis(2-methyl-N-(1-methylethyl)-propanethioamide)tin(II) has been determined through a single crystal X-ray diffraction analysis and shown to display a monomeric constitution in which the tin(II) center occupies a distorted pseudo square pyramidal geometry defined by the N₂S₂ donors and the stereochemically active lone pair. Both tin(II) derivatives have been assessed for their potential as single source precursors to SnS by TGA and by NMR spectroscopic analysis of the volatile organic products produced during their thermolysis. Both compounds have been utilized in the growth of thin films by aerosol-assisted chemical vapor deposition (AACVD). These latter studies provided film growth at temperatures as low as 200 °C. The films have been analyzed by PXRD, Raman spectroscopy, XPS, AFM, and SEM and are shown to comprise primarily the orthorhombic (Herzenbergite) phase of SnS, which is contaminated by only low levels of residual carbon (<5 at %). Although further films deposited onto Mo-coated substrates produced only limited photocurrents when illuminated, these results demonstrate the potential of such simple thioamidate derivatives to act as single source precursors to useful metal sulfide thin film materials.

中文翻译：

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硫胺酸锡（II）前驱体沉积SnS薄膜

有两个硫酰胺原配体R ¹ N（H）C（= S）R ²（R ¹ = t -Bu，R ² = i-Pr和R ¹ = i-Pr，R ² = i-Pr）通过用Lawesson试剂处理相应的酰胺合成。[Sn {N（SiMe ₃）₂ } ₂ ]与两个摩尔当量的每种硫代酰胺原配体的反应产生了氨基锡锡（II）物种双（2-甲基-N-（1-甲基乙基）-丙烷硫代酰胺）锡（II）和双[ N-（1,1-二甲基乙基）-2-甲基丙硫酰胺]锡（II）。两种新的锡化合物的特征均是¹ H，¹³C { ¹ H}和¹¹⁹ Sn NMR光谱及元素分析。此外，双（2-甲基-N-（1-甲基乙基）-丙硫酰胺）锡（II）的固态结构已通过单晶X射线衍射分析确定，并显示出单体结构，其中锡（II）中心占据由N ₂ S ₂定义的扭曲的伪正方形金字塔形几何形状供体和具有立体化学活性的孤对。两种锡（II）衍生物均已通过TGA和热裂解过程中产生的挥发性有机产物的NMR光谱分析评估了它们作为SnS单一来源的前体的潜力。两种化合物都已通过气溶胶辅助化学气相沉积（AACVD）用于薄膜的生长。后面的这些研究提供了在低至200°C的温度下薄膜的生长。薄膜已通过PXRD，拉曼光谱，XPS，AFM和SEM进行了分析，显示主要包含SnS的斜方晶（Herzenbergite）相，该相仅被少量的残留碳（<5 at％）污染。尽管沉积在涂有Mo的基材上的其他薄膜在照射时仅产生有限的光电流，