A new carboxylate-phosphonate, [Zn3(O3PCH(CH3)COO)2(H2O)] 1, has been success- fully synthesized by hydrothermal technique and characterized by X-ray single-crystal structure analysis, elemental analysis and infrared spectroscopy. It crystallizes in monoclinic, space group P21/c with a = 4.9521(5), b = 21.953(3), c = 13.2266(18) ’, β = 100.704(2)o, V = 1412.9(3) ’3, Z = 4, Mr = 516.19, Dc = 2.427 g/cm3, 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 CuCl2, 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 deter- mined by single-crystal X-ray diffraction method. The crystal crystallizes in the monoclinic system, space group P21/n with a = 8.2096(16), b = 18.580(4), c = 11.838(2) , β = 103.12(3)o, V = 1758.5(6) 3, Z = 2, Mr = 863.83, Dc = 1.631 g/cm3, 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
