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A novel inorganic-organic hybrid compound,{[Co(dien)]4[(PO4)MoV8(WVI0.56MoVI0.44)4-O33(OH)3]}·nH2O(1,n≈1,dien=diethylenetriamine),has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction.Compound 1 crystallizes in the triclinic system with a=11.927(2),b=13.328(3),c=19.306(4),α=93.76(3),β=94.14(3),γ=109.99(3)o,V=2863.2(12)3,space group P1 and Z=2 at 173 K.The final full-matrix least-squares refinement converged to R=0.049 for 9621 observed reflections with I>2σ(I)and wR=0.139 for all data(9871)and S=1.073.Crystal structure analysis shows that 1 contains a kind of the first reported mixed-valence and molybdenum-tungsten mixed-distributedε-Keggin structural polyanion capped by four Co(dien)fragments with the main group element P occupying the center site.These results were further confirmed by energy-dispersive X-ray spectroscopy(EDS),X-ray powder diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),Raman spectroscopy,Thermogravimetry(TG)and X-ray photoelectron spectroscopy(XPS)analyses.
A novel inorganic-organic hybrid compound, {[Co (dien)] 4 [(PO4) MoV8 (WVI0.56MoVI0.44) 4-033 (OH) 3]} nH2O (1, n≈1, dien = diethylenetriamine) , has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the triclinic system with a = 11.927 (2), b = 13.328 (3), c = space group P1 and Z = 2 at 173 K. The final full-matrix least-squares refinement converged to R = 0.049 (3), γ = 109.99 (3) o, V = 2863.2 for 9621 observed reflections with I> 2σ (I) and wR = 0.139 for all data (9871) and S = 1.073. Crystal structure analysis shows that 1 contains a kind of the first reported mixed-valence and molybdenum-tungsten mixed-distributed ε- Keggin structural polyanion capped by four Co (dien) fragments with the main group element P occupying the center site. These results were further confirmed by energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction infrared spectroscopy (FTIR), Raman spectroscopy, Thermogravimetry (TG) and X-ray photoelectron spectroscopy (XPS) analyzes.