A new complex [Ni（en）3]4[HVⅣ12VⅤ6O42（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.
A new complex[Ni(en) 2V 6O 14] n was hydrothermally synthesized and characterized by 2-dimensional vanadium oxide framework pillared by Ni(en) 2 group. Single crystal X-ray analysis indicates that this compound crystallizes in monoclinic system, space group P2 1/c with a= 0.892 17(18) nm, b= 1.711 1(3) nm, c=0.662 73(13) nm, β=111.58(3)°, V=0.940 8(3) nm 3, Z=2, D c= 2.501 g/cm 3, R=0.042 3, wR=0.060 9, S=1.006.
The title compound[Co(2,2-bipy) 3] 4[Mo 10V 6O 40(PO 4)] 2·4H 2O was synthesized by hydrothermal method and its structure was determined with single crystal X-ray analysis. The cluster anion is double tetracapped Pseudo-Keggin cluster anions. The crystal is triclinic, space group P-1 with a=\{1\^316 5(3)\} nm, b=1\^438 2(3) nm, c=2\^764 4(6) nm, α=79\^51°, β=89\^95°, γ=68\^89°, V=\{4\^789 3(17)\} nm 3, Z=1, D c=2\^176 g/cm 3, R=0\^075 5, wR=0\^205 3, S=0\^995.
A novel two-dimensional compound [Ni0.5(H2O)1.5{Ni(en)2}3V18O42(Cl)]3.5H2O 1 has been hydrothermally synthesized and characterized by IR, elemental analysis, and single-crystal X-ray diffraction analysis. Crystal data for 1: monoclinic, space group C2/c with a = 12.824(3), b = 27.873(6), c = 21.092(4) , b = 92.93(3), V = 7529(3) 3, Z = 4, Dc = 2.012 g/cm3, Mr = 2280.56, F(000) = 4476 and m = 3.092 mm-1. The final R and wR are 0.0769 and 0.1783, respectively for 4203 observed reflections with I>2s(I). The structure consists of [V18O42(Cl)]7- clusters linked by trans- {Ni(en)2} groups into linear chains, while cis-{Ni(en)2} groups provide the cross-linking adjacent chains to form a two-dimensional structure.
A new open-framework zincophosphite, Zn2(HPO3)3H2DACH 1, was hydro- thermally synthesized in the presence of 1,2-diaminocyclohexane (DACH) as structure-directing agent. Its structure was determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, powder X-ray diffraction and thermogravimetric analysis. Crystal data for 1: Mr = 486.88, monoclinic, space group P21/c with a = 10.2287(11), b = 9.7624(11), c = 16.1686(18) , b = 92.573(2), V = 1612.9(3) 3, Z = 4, Dc = 2.005 g/cm3, F(000) = 984, = 3.314 mm-1 and S = 1.152. The final R = 0.0473 and wR = 0.1121 for 2456 observed reflections with I > 2s(I). The inorganic layer consisting of four- and eight-membered rings is constructed of alternating ZnO4 tetrahedra and HPO3 pseudo pyramids by sharing vertices. The organic template molecules reside in the interlayer region and interact with the inorganic network through H-bonds.
