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A new bisupporting metal-oxygen cluster with bicapped pseudo-Keggin compound [CuII{Cl0.5Cl(phen)}]2 {[PMoV 6MoVI 6O40(VIVO)2][CuII(phen)2]2}·2H2O (phen = 1,10-phenathroline) has been synthesized by hydrothermal method and characterized by elemental analysis, IR spectroscopy, TGA, XRPD, and single-crystal X-ray diffraction. The polyoxoanion consists of a bicapped vanadium Keggin polyoxoanion and two {[Cu(phen)]2}2+ subunits producing bisupporting bicapped Keggin-polyoxometalate structure. The isolated dinuclear unit [CuII{Cl0.5Cl(phen)}2]+ acts as the countercation in title compound. In the crystal structure π − π stacking interactions, multiform C‒H···O and O‒H···O hydrogen bonds lead to a three-dimensional network.

A polyoxometalate-based complex [Cu I (phen)2]4[HPW11.5 VI Cu0.5 II O40] (1) (phen = 1,10-phenathroline) has been synthesized by hydrothermal method and characterized by IR, elemental analysis, TG technique and X-ray crystallography. [Cu I (phen)2]+ ion balances the charge on the α-Keggin [HPW11.5 VI Cu0.5 II O40]4 − anion. The cooperativity of intermolecular π −π stacking, C─H… π interactions and C─H… O hydrogen bonds link the ions together to form a three-dimensional chiral structure. The luminescent properties of the title complex in the solid state were investigated.