Sivakumar T, Ok Kang Min, Halasyamani P Shiv
Department of Chemistry and Center for Materials Chemistry, University of Houston, 136 Fleming Building, Houston, Texas 77204-5003, USA.
Inorg Chem. 2006 May 1;45(9):3602-5. doi: 10.1021/ic052103u.
Two new vanadates, Ba(2.5)(VO2)3(SeO3)4.H2O and La(VO2)3(TeO6).3H2O, have been synthesized by hydrothermal methods using BaCO3, Ba(OH)2.H2O, La(NO3)3.6H2O, V2O5, TeO2, and H2SeO3 as reagents. The structures were determined by single-crystal X-ray diffraction. Ba(2.5)(VO2)3(SeO3)4.H2O exhibits a two-dimensional layered structure consisting of VO(5) square pyramids and SeO3 polyhedra, whereas La(VO2)3(TeO6).3H2O has a three-dimensional framework structure composed of VO(4) tetrahedra and TeO6 octahedra. Infrared and Raman spectroscopy, UV-vis diffuse reflectance spectroscopy, and thermogravimetric analysis are also presented. Crystal data: Ba(2.5)(VO2)3(SeO3)4.H2O, trigonal, space group P (No. 147) with a = b = 12.8279(15) A, c = 7.2631(9) A, V = 1035.1(2) A(3), and Z = 2; La(VO2)3(TeO6).3H2O, trigonal, space group R3c (No. 161) with a = b = 9.4577(16) A, c = 23.455(7) A, V = 1816.9(7) A3, and Z = 6.
采用水热法,以碳酸钡、氢氧化钡·水、硝酸镧·六水合物、五氧化二钒、二氧化碲和亚硒酸为试剂,合成了两种新的钒酸盐,即Ba(2.5)(VO2)3(SeO3)4·H2O和La(VO2)3(TeO6)·3H2O。通过单晶X射线衍射确定了其结构。Ba(2.5)(VO2)3(SeO3)4·H2O呈现出由VO(5)四方锥和SeO3多面体组成的二维层状结构,而La(VO2)3(TeO6)·3H2O具有由VO(4)四面体和TeO6八面体构成的三维骨架结构。还给出了红外光谱、拉曼光谱、紫外可见漫反射光谱和热重分析。晶体数据:Ba(2.5)(VO2)3(SeO3)4·H2O,三方晶系,空间群P(编号147),a = b = 12.8279(15) Å,c = 7.2631(9) Å,V = 1035.1(2) ų,Z = 2;La(VO2)3(TeO6)·3H2O,三方晶系,空间群R3c(编号161),a = b = 9.4577(16) Å,c = 23.455(7) Å,V = 1816.9(7) ų,Z = 6。