Alibrahim Khuloud A, Al-Saif Foziah A, Alghamdi M T, El-Shahawi M S, Moustafa Y M, Refat Moamen S
College of Science, Princess Nourah bint Abdulrahman University, Department of Chemistry Kingdom of Saudi Arabia.
Department of Chemistry, Faculty of Science, King Abdulaziz University Jeddah P. O. Box 80203 Saudi Arabia.
RSC Adv. 2018 Jun 20;8(40):22515-22529. doi: 10.1039/c8ra03879a. eCollection 2018 Jun 19.
Three new solid complexes of pipemidic acid (Pip-H) with Ru, Pt and Ir were synthesized and characterized. Pipemidic acid acts as a uni-dentate chelator through the nitrogen atom of the -NH piperazyl ring. The spectroscopic data revealed that the general formulas of Pip-H complexes are [M(L) (Cl) ]·HO ((1) M = Ru, L: Pip-H, = 3, = 3, = 6; (2) M = Pt, L: Pip-NH, = 2, = 4, = 0 and (3) M = Ir, L: Pip-H, = 3, = 3, = 6). The number of water molecules with their locations inside or outside the coordination sphere were assigned thermal analyses (TG, DTG). The DTG curves refer to 2-3 thermal decomposition steps where the first decomposition step at a lower temperature corresponds to the loss of uncoordinated water molecules followed by the decomposition of Pip-H molecules at higher temperatures. Thermodynamic parameters (, Δ, Δ* and Δ*) were calculated from the TG curves using Coats-Redfern and Horowitz-Metzeger non-isothermal models. X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques were carefully used to assign properly the particle sizes of the prepared Pip-H complexes. The biological enhancement of Pip-H complexes rather than free chelate were assessed against four kinds of bacteria G(+) ( and ) and G(-) ( and ) as well as against the human breast cancer (MCF-7) tumor cell line.
合成并表征了三种新的哌酸(Pip-H)与钌、铂和铱的固体配合物。哌酸通过哌嗪基环的氮原子作为单齿螯合剂。光谱数据表明,Pip-H配合物的通式为[M(L)(Cl)]·H₂O((1) M = Ru,L: Pip-H,ν = 3,μ = 3,z = 6;(2) M = Pt,L: Pip-NH,ν = 2,μ = 4,z = 0;(3) M = Ir,L: Pip-H,ν = 3,μ = 3,z = 6)。通过热分析(TG、DTG)确定了配位球体内外水分子的数量及其位置。DTG曲线显示有2 - 3个热分解步骤,其中较低温度下的第一个分解步骤对应于未配位水分子的损失,随后在较高温度下是Pip-H分子的分解。使用Coats-Redfern和Horowitz-Metzeger非等温模型从TG曲线计算热力学参数(E*、ΔH*、ΔS和ΔG)。仔细使用X射线粉末衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)技术来正确确定所制备的Pip-H配合物的粒径。评估了Pip-H配合物而非游离螯合剂对四种细菌G(+)(金黄色葡萄球菌和枯草芽孢杆菌)和G(-)(大肠杆菌和铜绿假单胞菌)以及人乳腺癌(MCF-7)肿瘤细胞系的生物增强作用。