A new carboxylate-phosphonate, [Zn3（O3PCH（CH3）COO）2（H2O）] 1, has been successfully synthesized by hydrothermal technique and characterized by X-ray single-crystal structure analysis, elemental analysis and infrared spectroscopy. It crystallizes in monoclinic, space group P2 1/c with a = 4.9521（5）, b = 21.953（3）, c = 13.2266（18） A, β = 100.704（2）°, V= 1412.9（3） A3, Z= 4, Mr = 516.19, Dc= 2.427 g/cm^3, F（000） = 1016,μ（MoKα） = 5.332 mm^-1 and T= 293（2） K. The final R = 0.0605 and wR = 0.1354 for 2957 observed reflections with I 〉 2σ（I）. The thermogravimetric analysis （TGA） and fluorescent measurement have been done. The structure of compound 1 is a 3D open framework with 32-atom channels.
LAI Zhu-ZhiFU Rui-BiaoSHENG Tian-LuLI Ya-MinHUANG Xi-HeWU Xin-Tao
A 3-D coordination polymer [PbNH(CH2COO)2] 1 has been prepared under hydrothermal conditions and its crystal structure was studied by single-crystal X-ray diffraction. The compound belongs to orthorhombic system, space group Fdd2 with unit cell parameters: a = 13.6304(6), b = 36.295(1), c = 5.0821(2) ? V = 2514.19(17) 3, Z = 16, Mr = 338.28, Dc = 3.575 g/cm3, F(000) = 2400 and m(MoKa) = 2.679 cm-1. The final R and wR are 0.0290 and 0.0685, respectively, for 874 observed reflections with I > 2s(I). The lead has a distorted tetragonal pyramid environment with four oxygen donors in the basal plane and one nitrogen donor in the axial site. Micro-channels are observed in the neutral 3-D network of 1.
The hydrothermal reaction of 1,2-dicyanobenzene with NaN3 in the presence of CuC12, 2,2＇-bipyridine and H2O affords a novel dinuclear copper（Ⅱ）-ditetrazolate, [Cu（bpy）- （pdtz）]2 （Hpdtz = 5,5＂-1,2-phenylene-ditetrazole, bpy = 2,2＇-bipyridine）. The pdtz ligand is generated in situ through Sharpless 2＋3 cycloaddition reaction. Its crystal structure was determined by single-crystal X-ray diffraction method. The crystal crystallizes in the monoclinic system, space group P211n with a = 8.2096（16）, b = 18.580（4）, c = 11.838（2） A, β = 103.12（3）°, V = 1758.5（6） A^3, Z = 2, Mr = 863.83, Dc = 1.631 g/cm^3, F（000） = 876 and μ = 1.272 mm^-1. In this novel dinuclear structure, the pdtz ligand adopts a peculiar μ2-η1,η2 coordination mode.
HUANG Xi-He SHENG Tian-Lu XIANG Sheng-Chang FU Rui-Biao HU Sheng-Min LI Ya-Min WU Xin-Tao
