Hydrothermal synthesis and crystal structure of a novel compound: [Ni(phen)_3]_2[SiMo_10V_2~IVO_40(V~(IV)O)_2]·2H_2O

摘要

A novel compound [Ni(phen)_3]_2[SiMo_10V_2~IVO_40(V~(IV)O)_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, alpha = 105.9(2)°,gamma = 96.89(3)°, V = 2373.0(12) A~3 Z = 1, (lambdaMo_(Kalpha) = 0.71073A, Rl(wR2) = 0.0869(0.2174). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range of 1.51 < theta < 22.50°using the omega-scan technique. Empirical absorption correction (psi 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 crystallographicc study showed that the title compound contained a bi-capped alpha-Keggin-type [SiMo_10V_2~(iv)o_40(V_~(IV)O)_2]~(4-) polyoxoanion.