Ok Kang Min, Halasyamani P Shiv
Department of Chemistry and Center for Materials Chemistry, 136 Fleming Building, University of Houston, Houston, Texas 77204-5003, USA.
Inorg Chem. 2005 Apr 4;44(7):2263-71. doi: 10.1021/ic048428c.
Five new d0 transition metal iodates, BaTi(IO3)6, LaTiO(IO3)5, Ba2VO2(IO3)4.(IO3), K2MoO2(IO3)4, and BaMoO2(IO3)4.H2O, have been synthesized by hydrothermal methods using Ba(OH)2.8H2O, La2O3, K2CO3, TiO2, V2O5, MoO3, and HIO3 as reagents. The structures of these compounds were determined by single-crystal X-ray diffraction. All of the reported materials have zero-dimensional or pseudo-one-dimensional crystal structures composed of MO6 (M = Ti4+, V5+, or Mo6+) octahedra connected to IO3 polyhedra. Infrared and Raman spectroscopy, thermogravimetric analysis, and UV-vis diffuse reflectance spectroscopy are also presented. Crystal data: BaTi(IO3)6, trigonal, space group R-3 (No. 148), with a = b = 11.4711(10) A, c = 11.1465(17) A, V = 1270.2(2) A3, and Z = 3; LaTiO(IO3)5, monoclinic, space group P2(1)/n (No. 14), with a = 7.4798(10) A, b = 18.065(2) A, c = 10.4843(14) A, beta = 91.742(2) degrees , V = 1416.0(3) A3, and Z = 4; Ba2VO2(IO3)4.(IO3), monoclinic, space group P2(1)/c (No. 14), with a = 7.5012(9) A, b = 33.032(4) A, c = 7.2150(9) A, beta = 116.612(2) degrees , V = 1598.3(3) A3, and Z = 4; K2MoO2(IO3)4, monoclinic, space group C2/c (No. 15), with a = 12.959(2) A, b = 6.0793(9) A, c = 17.748(3) A, beta = 102.410(4) degrees , V = 1365.5(4) A3, and Z = 4; BaMoO2(IO3)4.H(2)O, monoclinic, space group P2(1)/n (No. 14), with a = 13.3368(17) A, b = 5.6846(7) A, c = 18.405(2) A, beta = 103.636(2) degrees , V = 1356.0(3) A3, and Z = 4.
采用水热法,以Ba(OH)₂·8H₂O、La₂O₃、K₂CO₃、TiO₂、V₂O₅、MoO₃和HIO₃为试剂,合成了五种新型d⁰过渡金属碘酸盐,即BaTi(IO₃)₆、LaTiO(IO₃)₅、Ba₂VO₂(IO₃)₄·(IO₃)、K₂MoO₂(IO₃)₄和BaMoO₂(IO₃)₄·H₂O。通过单晶X射线衍射测定了这些化合物的结构。所有报道的材料都具有由MO₆(M = Ti⁴⁺、V⁵⁺或Mo⁶⁺)八面体与IO₃多面体相连组成的零维或准一维晶体结构。还介绍了红外光谱、拉曼光谱、热重分析和紫外可见漫反射光谱。晶体数据:BaTi(IO₃)₆,三方晶系,空间群R-3(编号148),a = b = 11.4711(10) Å,c = 11.1465(17) Å,V = 1270.2(2) ų,Z = 3;LaTiO(IO₃)₅,单斜晶系,空间群P2(1)/n(编号14),a = 7.4798(10) Å,b = 18.065(2) Å,c = 10.4843(14) Å,β = 91.742(2)°,V = 1416.0(3) ų,Z = 4;Ba₂VO₂(IO₃)₄·(IO₃),单斜晶系,空间群P2(1)/c(编号14),a = 7.5012(9) Å,b = 33.032(4) Å,c = 7.2150(9) Å,β = 116.612(2)°,V = 1598.3(3) ų,Z = 4;K₂MoO₂(IO₃)₄,单斜晶系,空间群C2/c(编号15),a = 12.959(2) Å,b = 6.0793(9) Å,c = 17.748(3) Å,β = 102.410(4)°,V = 1365.5(4) ų,Z = 4;BaMoO₂(IO₃)₄·H₂O,单斜晶系,空间群P2(1)/n(编号14),a = 13.3368(17) Å,b = 5.6846(7) Å,c = 18.405(2) Å,β = 103.636(2)°,V = 1356.0(3) ų,Z = 4。