新的四帽Keggin结构的金属-氧簇合物[NiMo12O40H10{Ni(H2O)3}4]的水热合成与结构表征

多金属氧酸盐 (也称金属 -氧簇 )由于在催化、材料及医药等领域的应用日益广泛而备受关注 .近年来 ,一些新颖的非经典结构的化合物不断被合成出来 .如带二帽的 Keggin结构化合物 V15O4 2 ]9- 1] ,PV14 O4 2 ]9- 2 ] ,As V14 O4 2 ]9- 3 ] ,{ Mo8V7O4 2 } 2 ]14 - 4 ] ,

Hydrothermal Synthesis and Structure Characterization of a New Four-capped Metal-oxygen Cluster [NiMo12O40H10{Ni(H2O)3}4]

A Hydrothermal reaction of MoO₃, NiCl₂·6H₂O, WO₃ and H₂O with a molar ratio of 1:0.6:1:83.3 gives a rhombic-shaped black crystal NiMo₁₂O₄0H₁₀{Ni(H₂O)₃}₄]. It crystallizes in a tetragonal system with space group I4₁/amd and unit cell parameters a=b=1.518 4(2) nm, c=3.082 9(6) nm, Z=4, V=7.108(2) nm³, R=0.067 1, _wR=0.217 8. The compound possesses a four-capped Keggin structure. The structure of the Keggin-NiMo₁₂O₄0H₁₀]^8- consists of twelve MoO₆ octahedrons and a NiO₄ tetrahedron on the center. Four Ni(H₂O)₃]²⁺ at the cap positions are linked to Keggin-structure by three μ 3-O, respectively. The calculation of bond valence shows that the oxidation state of Mo in the compound is +5.