【Abstract】 A new complex [Ni（en）₃]₄[HV^Ⅳ₁₂V^Ⅴ₆O₄₂（PO₄）] has been hydrothermally synthesize d and characterized by X-Ray diffraction,IR and Elemental analysis.Single crystal X-ray analysis indicates that this compoud cry stallizes in cubic system,space group Im3m with a=17.4081（2）*!,V=5275.38（10）*! 3 ,R=0.0420,w R=0.1055,Z =2,D c =1.663g·cm -3 ,μ=2.297mm -1 ,F（000）=2636.The crystal structure consis ts of[Ni （en） 3 ] 2+ cations and{HV 18 O 42 （PO 4 ）} 8- cluster anion which construct from 18{VO 5 }.square pyramids.The VO 5 pyramids joined each other to form a {V 18 O 42 }cage hosting a tetrahedral{PO 4 } 3- moiety with disordered oxygen atoms .CCDC:185574.更多还原