Casas José S, Castellano Eduardo E, Couce María D, Ellena Javier, Sánchez Agustín, Sordo José, Taboada Carmen
Departamento de Química Inorgánica, Facultade de Farmacia, Universidade de Santiago de Compostela, 15782 Santiago de Compostela, Galicia, Spain.
J Inorg Biochem. 2006 Jan;100(1):124-32. doi: 10.1016/j.jinorgbio.2005.10.009. Epub 2005 Dec 7.
The reaction of oxythiamine chloride hydrochloride (HOxTCl x HCl) with ZnCl2, CdCl2 and HgCl2 in ethanol yielded the complexes [ZnCl3(HOxT)], [CdCl3(HOxT)] and [HgCl3(HOxT)]. In water, the reaction with CdCl2 afforded [CdCl2(OxT)], but reaction with ZnCl2 or HgCl2 yielded unidentified products. The four new complexes were characterized by mass spectrometry and IR spectroscopy in the solid state and by 1H, 13C and 15N nuclear magnetic resonance (NMR) spectroscopy in hexadeuterated dimethylsulfoxide (DMSO-d6), and three were also studied by X-ray diffractometry. In [ZnCl3(HOxT)] and [HgCl3(HOxT)] the oxythiamine ligand is bound to the metal via N(1') and adopts the V conformation exhibited by thiamine in biological contexts. The infrared (IR) spectrum of [CdCl3(HOxT)] suggests a similar coordination mode. In [CdCl2(OxT)] each OxT zwitterion coordinates to one Cd(II) ion via its N(1') atom and to another via its N(3') and O atoms, giving rise to a polymeric chain along the x-axis. The coordination number of the metal is made up to six by Cdc...Cl interactions, two of which link the polymeric chains in pairs. This seems to be the first metal complex containing the oxythiamine ligand as a zwitterion, with the N(3')-H/O(4'alpha)-H group deprotonated. Neither HOxTCl nor its zinc(II) complex showed any significant activity in vitro against HeLa cells.
盐酸氧硫胺(HOxTCl·HCl)与氯化锌、氯化镉和氯化汞在乙醇中反应生成配合物[ZnCl3(HOxT)]、[CdCl3(HOxT)]和[HgCl3(HOxT)]。在水中,与氯化镉反应生成[CdCl2(OxT)],但与氯化锌或氯化汞反应生成不明产物。通过质谱和固态红外光谱以及在十六氘代二甲亚砜(DMSO-d6)中的1H、13C和15N核磁共振(NMR)光谱对这四种新配合物进行了表征,其中三种还通过X射线衍射法进行了研究。在[ZnCl3(HOxT)]和[HgCl3(HOxT)]中,氧硫胺配体通过N(1')与金属结合,并采用硫胺在生物环境中呈现的V构象。[CdCl3(HOxT)]的红外(IR)光谱表明其配位模式相似。在[CdCl2(OxT)]中,每个OxT两性离子通过其N(1')原子与一个Cd(II)离子配位,并通过其N(3')和O原子与另一个Cd(II)离子配位,从而沿x轴形成聚合物链。金属的配位数通过Cdc...Cl相互作用达到六个,其中两个相互作用将聚合物链成对连接。这似乎是第一个以两性离子形式包含氧硫胺配体且N(3')-H/O(4'α)-H基团去质子化的金属配合物。盐酸氧硫胺及其锌(II)配合物在体外对HeLa细胞均未显示出任何显著活性。