Hydrothermal synthesis,structural characterization of molybdophosphate and vanadium molybdophosphates polyoxometalates

The V 2O 5/Na 2MoO 4·2H 2O/HF/Ni(NO 3) 2·6H 2O/H 3PO 4/pyridine system was investigated using hydrothermal techniques.Three new phases, 3[PMo 12 O 40 ](1), 4[PVMo 11 O 40 ](2)and 4[HPV 2Mo 12 O 40 ](3)have been prepared and structurally characterized.Crystal data:compound (1),monoclinic, C/2c space group, a=2.186 7 (6)nm, b=1.397 8(4) nm, c =1.663 3(3)nm, β=105.73(10)°,V= 4.892 8 nm 3,R=0.060 4,Z=4; compound(2),monoclinic, C/2 cspace group, a=2.185 8(4) nm, b=1.397 1(3) nm, c=1.663 5(3) nm, β=105.83(3)°,V=4.887 3(17) nm 3, Z=4,R=0.046 3; compound(3),monoclinic, P2 1/n space group, a=1.112 2(2) nm, b= 1.941 2 (3) nm, c=1.248 4(3) nm, β=99.89(3)°,V=2.656 5(9) nm 3, Z=2,R=0.069?0.