| 苯甲酸与4-羟基-2，2′∶6′，2″-三联吡啶镧系配合物的合成、晶体结构、热分解机理及荧光性能 | |
| Synthesis, crystal structure, thermal decomposition mechanism, and fluorescence properties of benzoic acid and 4-hydroxy-2,2′:6′,2″-terpyridine lanthanide complexes | |
| 摘要: 用混合配体苯甲酸(HBA)和4-羟基-2，2'∶6'，2″-三联吡啶(4-OH-terpy)，与镧系硝酸盐通过超声溶解和常规溶液法成功合成了2种新型镧系元素配合物：[Sm2(BA)6(4-OH-terpy)2]·2H2O·2EtOH (1)和[Pr2(BA)6(4-OH-terpy)2(H2O)2]·HBA·H2O (2)。在合成过程中，4-羟基-2，2'∶6'，2″-三联吡啶作为中性配体参与反应，而苯甲酸则以去质子化形式(BA-)作为酸性配体与镧系离子配位。这2种配合物的晶体结构通过单晶X衍射得到了精确解析。同时还采用了元素分析、红外和拉曼光谱以及粉末X射线衍射技术来深入探究这2种配合物的物理化学性质。单晶X射线衍射数据显示，尽管2种配合物的结构存在差异，但它们均属于三斜晶系$P \overline{1}$空间群，且中心镧系元素离子具有相同的配位数，但配位环境却有所不同。为了全面评估这2种配合物的热稳定性，进一步实施了包括热重分析-微分热重分析-差示扫描量热法、傅里叶变换红外光谱分析以及质谱联用(TG-DTG-DSC/IR/MS)技术在内的综合测试。同时对配合物逸出气体的三维红外堆积图和质谱图进行了深入探究。此外，对配合物1的荧光特性研究表明，它能够展现出与Sm3+特征跃迁相匹配的荧光发射。 | |
| 关键词: 镧系配合物 晶体结构 热化学 荧光光谱 | |
| 基金项目: 国家自然科学基金(No.22273015)资助。 | |
| Abstract: Two novel lanthanide complexes, [Sm2(BA)6(4-OH-terpy)2]·2H2O·2EtOH (1) and [Pr2(BA)6(4-OH-terpy)2 (H2O)2]·HBA·H2O (2), where HBA=benzoic acid, 4-OH-terpy=4-hydroxy-2,2'∶6',2″-terpyridine, were successfully synthesized using ultrasonic dissolution and the conventional solution method with two mixed ligands HBA and 4OH-terpy. During the synthesis, 4-OH-terpy was involved in the reaction as a neutral ligand, while HBA, in its deprotonated form (BA-), coordinated with the lanthanide ions as an acidic ligand. The crystal structures of these two complexes were precisely determined by single crystal X ray diffraction. Elemental analysis, infrared and Raman spectroscopy, and powder X-ray diffraction techniques were also employed to further explore the physicochemical properties of the two complexes. The single-crystal X-ray diffraction data indicate that, despite their structural differences, both complexes belong to the triclinic crystal system $P \overline{1}$ space group. The central lanthanide ions have the same coordination number but exhibit different coordination environments. To comprehensively evaluate the thermal stability of these two complexes, comprehensive tests including thermogravimetric analysis, differential thermogravimetric analysis, differential scanning calorimetry, Fourier transform infrared spectroscopy, and mass spectrometry were conducted. Meanwhile, an in depth investigation was conducted into the 3D infrared stacked images and mass spectra of the gases emitted from the complexes. In addition, studies of the fluorescence properties of complex 1 showed that it exhibited fluorescence emission matching the Sm3+ characteristic transition. CCDC: 2394469, 1; 2394447, 2. | |
| Keywords: lanthanide complexes crystal structure thermochemistry fluorescence spectrum | |
| 投稿时间：2024-11-04 修订日期：2025-03-18 | |
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