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） A ,β= 91.594（5）°, V = 7143（3）A^3, Z = 2, F（000） = 4344, Dc = 2.070 g/cm^3,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-Mo8026]^4- and [β-Mo8026]^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.
