A binuclear complex [Cu2(phen)2(ip)(Hip)2]·4H2O has been synthesized by the reaction of Cu(CH3COO)2·H2O, phen(1,10-phenanthroline) and isophthalic acid (H2ip) under hydrothermal condition. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex: mono- clinic, space group C2/c, a = 19.214(3), b = 10.6973(14), c = 22.567(3) , β = 105.081(2)°, C24H19N2O8Cu, Mr = 526.95, Z = 8, F(000) = 2160, V = 4478.6(10) 3, Dc = 1.563 g/cm3, μ = 1.030 mm-1, –24≤h≤16, –13≤k≤13, –28≤l≤28, R = 0.0369 and wR = 0.0819 for 4615 (Rint = 1.0357) independent reflections and 3290 observed ones (I > 2σ(I)). Structural analysis shows that coordination geometry of Cu(Ⅱ) is a planar square, and the title complex exhibits a 2-D framework supramolecular structure by hydrogen bonds and π-π stacking interactions.
SUN Ya-Guang GU Xiao-Fu GAO En-Jun REN Ling ZHANG Dong-Sheng XU Jie
A new complex [Ni(phen)(mal)(H2O)2]·3H2O (phen = 1,10-phenanthroline, mal2-= malonic acid) has been synthesized by the reaction of nickel nitrate, phen and malonic acid. EA, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure of the title complex. Crystal data: monoclinic system, space group P2/c, a = 8.937(3), b = 12.163(5), c = 9.725(3) , β = 119.36°, C15H19N2O9Ni, Mr = 430.03, Z = 2, F(000) = 446, V = 921.3 3, Dc = 1.550 g/cm3, μ = 1.104 mm-1, –10≤h≤10, –12≤k≤14, –11≤l≤7, R = 0.0261 and wR = 0.0609 for 4376 (Rint = 0.0203) independent reflections and 1631 observed ones (I > 2σ(I)). Ni(Ⅱ) exhibits an octahedral coordination geometry, with hydrogen bonds and π-π interactions stabilizing the whole structure. UV spectrum of the complex interacting with protamine DNA indicates that the title compound interacts with DNA via insertion mode with bonding constant Kb of 1.11×104.
A novel coordination polymer [Nd2(PDB)2(CH3COO)2(H2O)3] (H2PDB = pyridine- 3,4-dicarboxylic acid) has been synthesized by the reaction of Nd(CH3COO)3 with pyridine- 3,4-dicarboxylic acid under hydrothermal conditions. Elemental analysis, IR spectra and X-ray crystal structure analysis were carried out to determine the composition and crystal structure of the title complex which belongs to the triclinic system, space group P1 with a = 6.9409(14), b = 7.5497(15), c = 22.530(5) , α = 84.79(3), β = 88.15(3), γ = 75.55(3)°, C18H18N2O15Nd2, Mr = 790.82, Z = 2, V = 1138.5(4) 3, Dc = 2.307 g/cm3, μ = 4.593 mm-1, –6≤h≤8, –5≤k≤8, –26≤l≤ 26, F(000) = 760, Rint = 0.0298, R = 0.0314 and wR = 0.0695 (I > 2σ(I)). Nd(1) and Nd(2) are linked into zigzag chains by carboxylate groups of acetate with interesting μ3-η2:η2 fashion. The zigzag chains are bridged by PDB to form a 2D framework, and a 3D supramolecular network is further constructed via π-π stacking.
The 1-D chain coordination complex of {[Mn2(HCAM)3(H2bipy)]·5H2O}n(H3CAM=4-hydroxypyridine-2,6-dicarboxylic acid,bipy=4,4′-bipyridine) has been synthesized by the reaction of 4-hydroxypyridine-2,6-dicarboxylic acid,4,4′-bipyridine and manganese carbonate under hydrothermal conditions,and its crystal structure was determined by X-ray diffraction method.The crystal belongs to the monoclinic system,space group P21/n with a=10.110(2),b=20.159(4),c=17.861(4) ,β=99.67(3)°,V=3.5884(12) nm3,Mr=901.47,Z=4,Dc=1.669 g·cm-3,μ=0.798 mm-1,F(000)=1840,the final R=0.0713 and wR=0.1853.The complex forms a 1-D chain bridged by HCAM,protonated 4,4-bipyridines link the 1-D chains to construct 2-D networks via N-H…O hydrogen bonds,and networks are further extended via π-π stacking and hydrogen bonds into 3-D supramolecular framework.
Reaction of 8-hydroxyquinoline (HQ) with Pb(NO3)2 in water resulted in the formation of a tetranuclear complex [Pb4(HQ)6(NO3)2]1. It has been characterized by IR, elemental analyses and X-ray diffraction. Crystal data for this complex: triclinic system, space group P1, a=9.7399(6), b=11.6535(8), c=12.6806(8), α=62.8050(10), β=78.4910(10), γ=80.5490(10)°, C54H36N8O12Pb4, Mr=1817.67, Z=1, V=1250.04(14)3, Dc=2.415 g/cm3, μ=13.503 mm-1, -12≤h≤8, -14≤k≤13, -15≤l≤15, F(000)=840, Rint=0.0217, R=0.0348 and wR=0.0927. X-ray crystal structure analysis revealed that in 1 each Pb(Ⅱ ) contains a stereo-chemically active lone pair of electrons. The Pb…C interaction, C-H…O weak interaction and π···π stacking interactions are observed in the complex. In the solid state, the complex possesses strong photoluminescent emission at 485 and 528 nm.
