Department of Chemistry, Jadavpur University, Kolkata -700 032, India.
Department of Chemistry, Jadavpur University, Kolkata -700 032, India.
J Photochem Photobiol B. 2017 Aug;173:1-11. doi: 10.1016/j.jphotobiol.2017.05.025. Epub 2017 May 20.
An osazone based ligand, hexane-3,4-dione-bis(2'-phenylhydrazone) (LH), was synthesized by 1:2M Schiff base condensation of 3,4-hexanedione and phenylhydrazine in dehydrated methanol. Its palladium(II) complex (1) has also been synthesized. LH and 1 have thoroughly been characterized by several spectroscopic and analytical means. DFT optimized structure of 1 shows that it is a monomeric Pd(II) complex having 'NCl' coordination chromophore. Our BVS analysis also satisfactorily reproduces the oxidation number of the palladium center. 1 shows irreversible Pd(II)/Pd(I) reduction in its CV in methanol. 1 is three-fold more emissive than LH. This enhanced emission has also been supported by time correlated single photon counting (TCSPC) measurements at room temperature. Human serum albumin (HSA) binding aspects of both LH and 1 have been investigated through various biophysical techniques. The binding constants as determined from Benesi-Hilderbrand plot using the absorbance spectral analyses were found respectively to be 1.18×10 and 4.38×10M for LH and 1. The experimental findings confirm that both are good HSA binders. The thermodynamic parameters (∆G°, ∆H° and ∆S°) have also been evaluated by isothermal titration calorimetric (ITC) experiments. These parameters indicate that the binding processes are spontaneous both for LH and 1. Molecular docking analyses reveal that both LH and 1 reside in domain-I of HSA.
一种基于奥沙酮的配体，己烷-3,4-二酮-双（2'-苯腙）（LH），是通过 3,4-己二酮和苯肼在脱水甲醇中以 1:2M 的希夫碱缩合反应合成的。它的钯（II）配合物（1）也已被合成。LH 和 1 已经通过多种光谱和分析手段进行了彻底的表征。DFT 优化的 1 的结构表明，它是一种具有'NCl'配位发色团的单体钯（II）配合物。我们的 BVS 分析也令人满意地再现了钯中心的氧化数。1 在其在甲醇中的 CV 中表现出不可逆的 Pd(II)/Pd(I)还原。1 比 LH 三波长发光。这一增强的发射也得到了室温下时间相关单光子计数（TCSPC）测量的支持。通过各种生物物理技术研究了 LH 和 1 的人血清白蛋白（HSA）结合方面。通过吸收光谱分析用 Benesi-Hilderbrand 图确定的结合常数分别为 1.18×10 和 4.38×10M 用于 LH 和 1。实验结果证实，两者都是良好的 HSA 结合物。通过等温滴定量热（ITC）实验还评估了热力学参数（∆G°、∆H°和 ∆S°）。这些参数表明，结合过程对于 LH 和 1 都是自发的。分子对接分析表明，LH 和 1 都位于 HSA 的域-I 中。
