A novel layered compound, [Ni(C 10 H 8N 2) 2V 3O 8 5 ], was hydrothermally synthesized and structurally characterized by single crystal X ray diffraction. The compound crystallizes in monoclinic system, space group P2 1/c with a =1 551 8(3) nm, b =1 476 1(3) nm, c =1 048 3(2) nm, β=92 02(3)°, V = 2 399 8 (8) nm 3, Z=4, R=0 046 7, wR 2= 0 085 9.
A new compound, \[Ni(en)\-3\]\-2\[Ni(en)\-2(H\-2O)\-2\]\[As\-6V\-\{15\}O\-\{42\}\]·4H\-2O, was first prepared by hydrothermal synthesis and characterized by elemental analysis, IR, TGA\|DSC, ESR and single crystal X\|ray diffraction. Crystal data: monoclinic, space group \%C\-c, a\%=1\^523 6(3) nm, \%b\%=2\^051 8(4) nm, \%c\%=2\^395 9(5) nm, \%β=97\^41(3)°, V\%=7\^427(3) nm\+3, \%Z=4, R=0\^057 0, wR\-2=0\^135 7\%. The polyanion consists of six AsO\-3 pyramids and fifteen VO\-5 pyramids. Counterions are complex ions with octahedral structure, which consist of NH\-2CH\-2CH\-2NH\-2 and Ni\+\{2+\}.
A new isopolyoxovanadate [Ni(1,10′-phen) 3] 2 [V Ⅳ 2V Ⅴ 8O 26] was hydrothermally synthesized and structurally characterized by the single crystal X-ray diffraction. The compound crystallizes in orthorhombic system, space group Pbcn with a=1.362 9(3) nm, b=2.215 6(4) nm, c= 2.571 2(4) nm, V=7.764(2) nm 3, Z=4, R=0.040 3, wR 2=0.044 6. The compound exhibits an unusual empty ellipsoidal cage, which is constructed by eight {V ⅤO 4} tetrahedra and two {V ⅣO 5} square pyramids via corner-sharing modes. The chiral [Ni(1,10′-phen) 3] 2+ complexes act as the counter cations.
