Hydrothermal Synthesis and Characterization of a Novel Two-dimensional Framework Materials Constructed from Polyoxometalate and Coordination Groups: [H_2Mo_(5.5)V_(10.5)O_(40)(PO_4)][Cu(en)_2]_4·7H_2O
Cui Xiao-bing
Abstract
Cui Xiao-bing
Abstract
A novel compound [H_2Mo_ 5.5V_ 10.5O_ 40(PO_4)][Cu(en)_2]_4·7H_2O(1) was synthesized from V_2O_5, MoO_3, CuCl_2·2H_2O, en, H_3PO4 and H_2O in an aqueous solution via the hydrothermal method and characterized by means of single-crystal X-ray diffraction, elemental analyses, IR, EPR spectra and thermal analyses. C_ 16H_ 80Cu_4Mo_ 5.5N_ 16O_ 51PV_ 10.5 crystallized in a triclinic system, the space group is P1 with M=2660.63, a= 1.283590(10) nm, b=1.289910(10) nm, c=1.387870(10) nm, V=1.80942(2) nm 3, Z=2, D_x=4.883 g/cm 3, F(000)=2599, μ=6.956 mm -1, (Δ/σ)=0.000, S=1.089. The crystal structure was solved by the direct methods with the final R=0.0752 and wR=0.1988 for 6311 observed reflections with I≥2σ(I). The X-ray crystallography reveals that compound 1 is a novel two-dimensional framework material constructed from the mixed Mo/V polyoxometalate and coordination groups.
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A novel compound [H_2Mo_ 5.5V_ 10.5O_ 40(PO_4)][Cu(en)_2]_4·7H_2O(1) was synthesized from V_2O_5, MoO_3, CuCl_2·2H_2O, en, H_3PO4 and H_2O in an aqueous solution via the hydrothermal method and characterized by means of single-crystal X-ray diffraction, elemental analyses, IR, EPR spectra and thermal analyses. C_ 16H_ 80Cu_4Mo_ 5.5N_ 16O_ 51PV_ 10.5 crystallized in a triclinic system, the space group is P1 with M=2660.63, a= 1.283590(10) nm, b=1.289910(10) nm, c=1.387870(10) nm, V=1.80942(2) nm 3, Z=2, D_x=4.883 g/cm 3, F(000)=2599, μ=6.956 mm -1, (Δ/σ)=0.000, S=1.089. The crystal structure was solved by the direct methods with the final R=0.0752 and wR=0.1988 for 6311 observed reflections with I≥2σ(I). The X-ray crystallography reveals that compound 1 is a novel two-dimensional framework material constructed from the mixed Mo/V polyoxometalate and coordination groups.
Key concepts: Polyoxometalate, Triclinic crystal system, Crystallography, Electron paramagnetic resonance, Hydrothermal synthesis, Hydrothermal circulation, Crystal structure, Aqueous solution