Hydrothermal synthesis and crystal structure of a novel compound: [Ni(phen) 3] 2[SiMo 10V IV2O 40(V IVO) 2]·2H 2O

Abstract

A novel compound [Ni(phen) 3] 2[SiMo 10V IV 2O 40(V IVO) 2]·2H 2O has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the triclinic system, space group P-1, a=12.378(4) A ̊ , b=14.148(5) A ̊ , c=14.316(2) A ̊ , α=105.91(2)°, β=95.31(2)°, γ=96.89(3)°, V=2373.0(12) A ̊ 3 , Z=1, (λ Mo Kα )=0.71073 A ̊ , R1( wR2)=0.0869(0.2174). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range of 1.51< θ<22.50° using the ω-scan technique. Empirical absorption correction (ψ scan) was applied. The structure was solved by the direct method and refined by the Full-matrix least-squares on F 2 using the SHELXL-97 software. X-ray crystallographic study showed that the title compound contained a bi-capped α-Keggin-type [SiMo 10V IV 2O 40(V IVO) 2] 4− polyoxoanion.