Department of Chemistry, College of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou, 510640, China.
Dalton Trans. 2010 Mar 14;39(10):2497-503. doi: 10.1039/b920987e. Epub 2010 Jan 19.
Three isostructural heterobimetallic nitrilotriacetatoperoxotitanate complexes of general formula M(H(2)O)(5)[Ti(2)(O(2))(2)O(nta)(2)].7H(2)O [M = Co (1), Ni (2) and Zn (3)] have been isolated in pure crystals directly from the quaternary system of M(2+)-Ti(OC(4)H(9))(4)-H(2)O(2)-H(3)nta (H(3)nta = nitrilotriacetic acid) at pH = 4.0 and have been characterized by elemental analyses, IR, thermal analysis (TGA), and single-crystal X-ray diffraction. Single crystal X-ray analysis reveals that the titanium atom in these complexes features seven-fold-coordination, each surrounded by six oxygen atoms and one nitrogen atom. The divalent transition metal ions in these compounds are hexa coordinated, surrounded by five water molecules and one bridged carboxylato oxygen atom. The TGA and XRD results prove that complexes 1-3 undergo facile thermal decomposition to form pure CoTiO(3), NiTiO(3) and ZnTiO(3) at 700 degrees C respectively. The morphologies, microstructures, and crystallinity of the residues obtained after pyrolysis were characterized by transmission electron microscopy and powder X-ray diffraction.
已从 pH = 4.0 的 M(2+)-Ti(OC(4)H(9))(4)-H(2)O(2)-H(3)nta (H(3)nta = 氮基三乙酸)四元体系中直接以纯晶体形式分离出通式为M(H(2)O)(5)[Ti(2)(O(2))(2)O(nta)(2)].7H(2)O 的三种同结构的异双核硝氮三乙酸过氧钛酸盐配合物[M = Co(1)、Ni(2)和 Zn(3)]，并用元素分析、IR、热分析（TGA）和单晶 X 射线衍射对其进行了表征。单晶 X 射线分析表明，这些配合物中的钛原子具有七配位，每个钛原子被六个氧原子和一个氮原子包围。这些化合物中的二价过渡金属离子均为六配位，由五个水分子和一个桥接的羧基氧原子包围。TGA 和 XRD 结果证明配合物 1-3 可在 700°C 下容易地热分解，分别形成纯 CoTiO(3)、NiTiO(3)和 ZnTiO(3)。通过透射电子显微镜和粉末 X 射线衍射对热解后得到的残留物的形貌、微观结构和结晶度进行了表征。
