Coordination Chemistry Research Laboratory, Department of Chemistry, DDU Gorakhpur University, Gorakhpur 273 009, India.
Spectrochim Acta A Mol Biomol Spectrosc. 2012 Dec;98:302-6. doi: 10.1016/j.saa.2012.08.030. Epub 2012 Aug 21.
A convenient method has been explored to synthesize some nano-sized, mixed-ligand complexes of titanium(IV) with the general formula [Ti(acac)Cl(2-n)(L)(n)(OOCC(15)H(31))] (where Hacac=acetylacetone, HL=dibenzoylmethane or benzoylacetone and n=1 or 2). They have been synthesized by stepwise substitutions of chloride ions from titanium(IV) chloride with straight chain carboxylic acid and β-diketones. These were characterized by elemental analyses, molecular weight determinations, spectral (electronic, FTIR, (1)H NMR and powder XRD) and TEM studies. Conductance measurements indicated their non-conducting nature which may behave like insulators. Bidentate chelating nature of carboxylate and β-diketones anions in the complexes was established by their infrared spectra. LMCT bands were observed in the electronic spectra. Molecular weight determinations indicated mononuclear nature of the complexes. Powder XRD and transmission electron microscopy (TEM) studies indicated the particles of these were lying in the nano-size range. The complexes exhibited high resistance to hydrolysis. On the basis of these studies, coordination number 7 or 8 is assigned for titanium in the synthesized complexes.
一种方便的方法被探索出来，用于合成一些纳米级的、混合配体的钛(IV)配合物，其通式为[Ti(acac)Cl(2-n)(L)(n)(OOCC(15)H(31))]（其中 Hacac=乙酰丙酮，HL=二苯甲酰甲烷或苯乙酮，n=1 或 2）。它们是通过逐步取代钛(IV)氯化物中的氯离子与直链羧酸和β-二酮来合成的。这些配合物通过元素分析、分子量测定、光谱（电子、FTIR、(1)H NMR 和粉末 XRD）和 TEM 研究进行了表征。电导测量表明它们是非导体，可能表现为绝缘体。配合物中羧酸盐和β-二酮阴离子的双齿螯合性质通过它们的红外光谱得到证实。电子光谱中观察到 LMCT 带。分子量测定表明这些配合物具有单核性质。粉末 XRD 和透射电子显微镜（TEM）研究表明，这些颗粒处于纳米尺寸范围内。这些配合物表现出对水解的高抵抗力。基于这些研究，合成配合物中钛的配位数被指定为 7 或 8。
