A novel inorganic-organic hybrid compound [Cu(dpq)2]4[As8V14O42(H2O)]·2H2O(dpq=dipyrido[3,2-d:2’,3’-f]quinoxaline) was synthesized under the hydrothermal condition and its structure was characterized via single-crystal X-ray diffraction,elemental analysis,IR and XPS spectra.The title compound crystallizes in a monoclinic crystal system,space group P21/c with crystal parameters a=1.8973(3) nm,b=2.5816(2) nm,c=2.8941(2) nm,β=106.61(2)°,V=13.5846(12) nm3,Z=4,R1=0.0674,wR2=0.1750.It possesses a spherical [As8V14O42(H2O)]4-cluster anion,four [CuI(dpq)2]+ counter cations and two lattice water molecules.The cationic complexes form ca.0.8 nm×0.8 nm stellate channels along the c axis through strong π…π stacking interactions due to the multiple aryls in the dpq ligands.The polyoxoanions are embedded in the channels through extensive C—H…O short contact interactions.
The title compound,[Ni(C8N3H7)3]4[Mo8O26]2·6H2O 1,has been synthesized from the reaction of 2-(1H-pyrazol-3-yl)-pyridine (L) with (NH4)2MoO4·2H2O and NiCl2·6H2O. Elemental analysis,IR,UV spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure of the compound. Crystal data:C96H96Mo16N36Ni4O58,Mr = 4451.97,monoclinic system,space group P21/n,a = 20.846(5),b = 14.825(5),c = 23.122(5),β = 91.594(5)°,V = 7143(3) 3,Z = 2,F(000) = 4344,Dc = 2.070 g/cm3,μ = 1.968 mm-1,R = 0.0452 and wR = 0.1056 for 17102 independent reflections (Rint = 0.0442) and 11074 observed reflections (Ⅰ > 2σ(Ⅰ)). Structural analysis indicates that two kinds of octamolybdates ([α-Mo8O26]4-and [β-Mo8O26]4-) co-exist in the compound. This is the first example of a supramolecular structure containing L complex as well as both α-and β-octamolybdate clusters.
