The reaction of a new salicylideneaniline ligand, （Z）-4-（2-hydroxybenzylideneamino）-2-hydroxybenzoic acid （HL） with COCl2-6H2O yields one Co（Ⅱ） complex, [CoL2（CH3OH）2 （H2O）2]. This complex crystallizes in monoclinic P21/n space group, with a = 5.4992（5）, b = 18.2200（15）, c = 14.8678（14） ,A, β= 98.64（1）°, V = 1472.8（2）A3, C30H32CoN2O12, Mr = 671.51, Z = 2, Dc = 1.51416 g/cm^3, F（000） = 698, μ = 0.652 mm^-1, T = 298（2） K, R = 0.0514 and wR = 0.1735 for all 2675 observed reflections （I 〉 2σ（I））. In this complex, the imine N does not link to Co（H） and a remarkable torsion around C=N bond is observed. Through hydrogen bonds, the monomers aggregate into an interesting ＂Z-shape＂ framework.
A new manganese compound [Mn8（tmp）2（Htmp）4（（CH3）3CCO2）4（py）2Cl2]·2py （1·2py, H3tmp = 1,1,1-tri（hydroxymethyl）propane, py = pyramid） has been synthesized and its structure was characterized by IR, elemental analysis and X-ray diffraction. Compound 1 belongs to the triclinic system, space group P1 with a = 13.378（5）, b = 14.334（5）, c = 15.012（6） , α = 107.637（5）, β = 95.635（3）, γ = 92.825（4）°, V = 2720.7（17） 3, Z = 1, C76H124N4O26Cl2Mn8, Mr = 2022.23, Dc = 1.234 Mg/m3, μ = 1.007 mm-1, F（000） = 1052, T = 293（2） K, the final R = 0.0755 and wR = 0.2163 for all 6463 observed reflections （I 〉 2σ（I））. X-ray analysis shows that the core of 1 contains a [Mn8] mixed-valence rod-like unit consisting of six edge-sharing triangles （Mn3）, each of which is bridged by a μ3-oxygen atom.
Two mononuclear Mn compounds of Mn III （salen）（L 1） and Mn III （salen）（L 2） （H 2 salen=N,N-ethylenebis-（salicylideneaminato）,L 1=4-（2-hydroxybenzylideneamino）benzoic acid and L 2=4-（2-hydroxybenzylideneamino）-2-hydroxybenzoic acid） have been prepared and characterized by X-ray crystallography.Both compounds crystallize in the monoclinic system,space group P2 1 /c with a=14.351（4）,b=14.955（3）,c=11.869（3） and β=91.529（3）° for 1;and those for 2：a=14.439（9）,b=15.217（9）,c=11.660（7） and β=91.648（1）°.The compounds have similar structures,in which the Mn III center adopts a distorted square-pyramidal geometry with the basal plane constructed by two N and two O atoms from the salen ligand and the apical position occupied by the carboxylate O atom from L 1 or L 2 ligand.The voltammetric behavior of the compounds is examined,which shows quasi-reversible one-electron reduction of Mn（Ⅲ） to Mn（Ⅱ）.The reduction potentials of both compounds fall between-0.33 V [E 0 （O 2 /O 2 ·）] and 0.65 V [E 0 （1 O 2 /O 2 ·）],which suggest that 1 and 2 could be potential mimics of Mn-SOD.
