Synthesis, characterization, structural elucidation and biological screening of some <i>bis</i>(diisobutyldithiophosphato)antimony(III) complexes

Seven complexes of type [(C₄H₉<i>ⁱ</i>-O)₂PS₂]₂SbR have been synthesized by the reaction of chloro<i>bis</i>(diisobutyldithiophosphato)antimony(III) with mixed thio and/or oxo donor ligands in 1:1 M stoichiometry, where R = SC₆H₅, OOCC₆H₅, SCH₂COOH, SOCCH₃, OOCCH₃, SC₆H₄COOH and OOC(OH)C₆H₄. These newly synthesized derivatives have been characterized by different physicochemical (elemental analysis (C, H, S, Sb), melting point, molecular weight determination), spectral (UV, IR, NMR (¹H, ¹³C and ³¹P)) studies, as well as ESI mass, thermal, powder XRD and biological studies. In the final step of weight loss in thermogravimetric analysis, occurring in the range of 245–505 °C, the degradation of the C₆H₃CO moieties takes place and antimony sulfide (1/2 Sb₂S₃) is obtained as remaining material, which is useful in various aspects. Bonded to antimony the diisobutyldithiophosphato substituent behaves as an anisobidentate ligand, which is confirmed through spectral analysis. Powder XRD studies indicate that these compounds crystallize in a monoclinic crystal system with an unit cell volume of ∼7074–7162 ų forming nano ranged (9.69–15.69 nm) crystallites. From the antimicrobial screening tests, <i>bis</i>(diisobutyldithiophosphato)antimony(III) thioglycolate (compound <b>3</b>) has shown a maximum zone of inhibition (19 mm) against <i>E. coli</i> at 200 μg mL⁻¹ concentration.

本研究通过氯代二(二异丁基二硫代磷酸根)合锑(III)与1:1摩尔比的混合硫供体和/或氧供体配体反应，合成了7种通式为[(C₄H₉ⁱ-O)₂PS₂]₂SbR的配合物，其中R分别为苯硫基(SC₆H₅)、苯甲酰氧基(OOCC₆H₅)、巯基乙酸基(SCH₂COOH)、硫代乙酰氧基(SOCCH₃)、乙酸根(OOCCH₃)、对羧基苯硫基(SC₆H₄COOH)以及对羟基苯甲酰氧基(OOC(OH)C₆H₄)。这些新合成的衍生物通过多类物理化学表征（包括C、H、S、Sb元素分析、熔点测定、分子量测定）、光谱学表征（紫外光谱、红外光谱、核磁共振氢谱(¹H NMR)、碳谱(¹³C NMR)与磷谱(³¹P NMR)），以及电喷雾电离质谱(ESI mass)、热分析、粉末X射线衍射(PXRD)与生物学实验完成了结构与性能表征。在热重分析的最终失重阶段，温度区间为245~505 ℃，该阶段中苯甲酰基(C₆H₃CO)片段发生降解，最终残留产物为三硫化二锑(1/2 Sb₂S₃)，该产物具备多方面应用价值。与锑原子配位的二异丁基二硫代磷酸根取代基呈现出不对称双齿配位模式，这一结论通过光谱学分析得到验证。粉末X射线衍射表征结果显示，此类化合物均结晶于单斜晶系，晶胞体积约为7074~7162 ų，所形成的微晶粒径处于纳米尺度（9.69~15.69 nm）。抗菌活性筛选实验表明，二(二异丁基二硫代磷酸根)合锑(III)巯基乙酸酯（化合物3）在浓度为200 μg·mL⁻¹时，对大肠杆菌(E. coli)的抑菌圈直径最大，可达19 mm。

搜集汇总

背景与挑战

背景概述

该数据集聚焦于七种双(二异丁基二硫代磷酸)锑(III)配合物的合成与综合表征研究。通过元素分析、光谱技术、热重分析和粉末XRD等手段，揭示了配合物的化学结构和晶体特性（单斜晶系，纳米级晶体尺寸）。生物筛选结果显示，其中一种硫基乙酸酯配合物对大肠杆菌表现出显著的抗菌活性（抑制区达19毫米），体现了其在生物医学应用中的潜在价值。