摘要
A Schiff base ligand（H2CSF,C13H11NO4,1） derived from 3-carboxylsalicylaldehyde and furfurylamine,and its trinuclear complex [Ni3（CSF）2（CH3COO）2（DMF）2（H2O）2]（2） were synthesized.Compound 1 was characterized by elemental analysis,1H NMR,IR,MS and X-ray diffraction analysis.The crystal of 1 belongs to the monoclinic system,space group P21/c with a = 8.472（2）,b = 19.743（5）,c = 7.2300（18） ,β = 110.278（4）°,V = 1134.4（5） 3,Z = 4,Mr = 245.23,Dc = 1.436 g·cm-3,μ = 0.108 mm-1,F（000） = 512,λ = 0.71073 ,the final R = 0.0440 and wR = 0.1199 for 1426 observed reflections（I 2σ（I））.In the crystal of 1,there exist intramolecular hydrogen bonds and weak intermolecular C-H···O hydrogen bonds.Compound 2 was characterized by elemental analysis,IR,TG and X-ray diffraction analysis.The crystal of 2 is of triclinic system,space group P1 with a = 10.1237（17）,b = 10.4086（18）,c = 10.4884（18） ,α = 82.528（2）,β = 67.339（2）,γ = 83.010（2）°,V = 1008.1（3） 3,Z = 1,Mr = 962.87,Dc = 1.586 g·cm-3,μ = 1.463 mm-1,F（000） = 498,λ = 0.71073 ,the final R = 0.0517 and wR = 0.0805 for 2065 observed reflections（I 2σ（I））.The geometry of the trinuclear molecule is centrosymmetric,in which every Ni（Ⅱ） ion is coordinated in a slightly distorted octahedron.The three Ni（Ⅱ） ions are arranged in a straight line.The two CSF2-ions act as NOO tridentate ligands with the phenolate and carboxylate oxygen as bridging atoms.The coordination atoms of CSF2-anions and water molecules are coordinated on the equatorial plane,while the two bridging acetate ions and two DMF are trans-coordinated on the apical sites.
A Schiff base ligand（H2CSF,C13H11NO4,1） derived from 3-carboxylsalicylaldehyde and furfurylamine,and its trinuclear complex [Ni3（CSF）2（CH3COO）2（DMF）2（H2O）2]（2） were synthesized.Compound 1 was characterized by elemental analysis,1H NMR,IR,MS and X-ray diffraction analysis.The crystal of 1 belongs to the monoclinic system,space group P21/c with a = 8.472（2）,b = 19.743（5）,c = 7.2300（18） ,β = 110.278（4）°,V = 1134.4（5） 3,Z = 4,Mr = 245.23,Dc = 1.436 g·cm-3,μ = 0.108 mm-1,F（000） = 512,λ = 0.71073 ,the final R = 0.0440 and wR = 0.1199 for 1426 observed reflections（I 2σ（I））.In the crystal of 1,there exist intramolecular hydrogen bonds and weak intermolecular C-H···O hydrogen bonds.Compound 2 was characterized by elemental analysis,IR,TG and X-ray diffraction analysis.The crystal of 2 is of triclinic system,space group P1 with a = 10.1237（17）,b = 10.4086（18）,c = 10.4884（18） ,α = 82.528（2）,β = 67.339（2）,γ = 83.010（2）°,V = 1008.1（3） 3,Z = 1,Mr = 962.87,Dc = 1.586 g·cm-3,μ = 1.463 mm-1,F（000） = 498,λ = 0.71073 ,the final R = 0.0517 and wR = 0.0805 for 2065 observed reflections（I 2σ（I））.The geometry of the trinuclear molecule is centrosymmetric,in which every Ni（Ⅱ） ion is coordinated in a slightly distorted octahedron.The three Ni（Ⅱ） ions are arranged in a straight line.The two CSF2-ions act as NOO tridentate ligands with the phenolate and carboxylate oxygen as bridging atoms.The coordination atoms of CSF2-anions and water molecules are coordinated on the equatorial plane,while the two bridging acetate ions and two DMF are trans-coordinated on the apical sites.
