The title complex was synthesized by reaction of taurine salicylic schiff base(TSSB), O-phenanthroline(phen) and cupric acetate in water-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 498.00. The crystal structure of the title complex belongs to orthorhombic system with space group Pbcn and cell parameters: a=3.107 2(4) nm, b=1.289 09(18) nm, c= 1.034 78(14) nm; and V=4.144 7(10) nm3, Z=8, Dc=1.596 g·cm-3, μ=1.197 mm-1, F(000)=2 048. The compound is an one-dimensional chain complex of infinite length which are connected with hydrogen bonds. The Cu(Ⅱ) was coordinated by two oxygen atoms and three nitrogen while the o atoms of Ac- groups did not participate in the coordination. The Cu(Ⅱ) formed a distorted tetragonal pyramid and the capacities of coordination to Cu(Ⅱ) of atoms was discussed. Besides, the TG-IR of the complex was analyzed. The kinetics of the thermal decomposition reaction of the complex was studied under a non isothermal condition by TG-IR. TG and DTG curves indicate that the complex decomposed in three stages: [Cu(TSSB)(Phen)]·1.5H2O Cu(TSSB)(Phen) Cu(TSSB) CuO The kinetic parameters were obtained from the analysis of TG,DTG cures by OZAWA-Flynn-Wall method, and the activation energy and the value of A of the three stages are 74.98 kJ·mol-1, 286.65 kJ·mol-1, 87.55 kJ·mol-1; 9.66×108 s-1,1.82×1028 s-1, 3.09×103 s-1, respectively.
Reactions of bitter salt with taurine-3,5-dibromo-salicylaldehyde schiff base gave one new Complex [Mg(Br2TSSB)(Phen)(H2O)]·H2O (Br2TSSB=Taurine 3,5-dibromo-Salicylaldehyde Schiff Base, phen=o-phenanthro- line), which was characterized by elemental analysis, IR and X-ray diffraction. The chemical formula weight of the complex is 625.58. It′s crystal belongs to monoclinic system with space group P21/c. The cell parameters are: a=1.8142(3) nm, b=0.81475(14) nm, c=1.641 7(3) nm, β=90.571(4)°, and Z=4, V=2.426 4(7) nm3, Dc=1.712 g· cm-3, F(000)=1248, μ=3.496 mm-1. The complexes form a 3D net structure in which they are connected with hy- drogen bonds and #-# stacking. The Mg! formed a distorted coordination tetragonal pyramid. CCDC: 286194.
The new compound, Ni(TSSB)(Phen)(H2O)·4H2O (TSSB=Taurine Salicylic Schiff Base, phen=O- Phenanthroline) has been synthesized and characterized by IR, elemental analysis and X-ray diffraction. The compound crystal data: triclinic, space group P1, a=1.0497(2), b=1.1225(2), c=2.3843(4) nm, α=87.676(3)°, β= 82.957(3)°, γ=62.924(3)°; V=2.482 3(7) nm3, Z=4; Dc=1.488 g·cm-3, μ=0.920 mm-1, F(000)=1 160, Goof=1.032, (Δρ)max=899 e·nm-3, (Δρ)min=- 624 e·nm-3. The compound is a dimmer. In the complex, two Ni! were coordinated by three oxygen atoms and three nitrogen atoms while the O atoms of Ac- groups did not coordinate. The Ni! formed a distorted octahedron geometry. The compound is an three dimensional net connecting with hydrogen bonding. CCDC: 275474. The TG-IR of the complex was analyzed. The kinetics of the thermal decomposition reaction of the complex was studied under a non isothermal condition by TG-IR. TG and DTG curves indicate that the complex decom- posed in four stages: Ni(TSSB)(phen)H2O·4H2O Ni(TSSB)(phen)H2O Ni(TSSB)(phen) Ni(TSSB)
A novel coordination polymer [Mg(L)(H2O)2]·H2O] (LH2 = L-cysteic acid) has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal crystallizes in orthorhombic system, space group P212121, with a = 5.962(3), b = 11.224(6), c = 13.664(7) , V = 914.3(8) 3, Z = 4, Mr = 245.50, Dc = 1.783 g/cm3, μ = 0.445 mm–1, flack parameter = 0.32(16), F(000) = 512, the final R = 0.0458 and wR = 0.1172 for 1578 observed reflections with I > 2σ(I). The Mg(II) atom shows an octahedral geometry defined by two carboxyl O atoms from two different L-cysteic acid ligands, one carboxyl O atom and one amino N atom from the adjacent ligand, and two aqua ligands. The Mg(II) atoms are bridged by L-cysteic acid ligands, leading to a 1D infinite zigzag chain. In the structure there are extensive hydrogen bonds, through which the complex completes its 3D framework structure.
LI Hai-Ye LIAO Bei-Ling JIANG Yi-Min ZHANG Shu-Hua LI Jun-Xia
