摘要
Two manganese complexes, [Mn3(2-cba)6(phen)2] 1 (2-cba = 2-cyanobenzoic acid, phe11 = 1,10-phenanthroline) and [MnE(4-fbaO)E(phen)4](PF6)E.EHEO 2 (4-fbao = 4-formylbenzoic acid oxime), have been synthesized by the reaction of 2-formylbenzoic acid oxime (2-fbao, HELl) or 4-formylbenzoic acid oxime (4-fbao, HELE) with phen and manganese acetate in ethanol or methanol solution. A translation from the oximino (-CHN=OH) of HELl to cyano (-C-N) was found in the formation of complex 1 at room temperature. The complexes were structurally determined by single-crystal X-ray diffraction. The crystal of compound I belongs to monoclinic, space group C2/c, with a = 17.983(6), b = 23.364(7), c =14.589(5) A, β = 92.401(5)° V = 6124(3) A^3, Z = 4, C72H40Mn3N10O12, Mr= 1401.96, Dc = 1.521 g/cm^3, F(000) = 2852.0, Rint = 0.0372, T= 293(2) K,μ = 0.686 mm^-1, the final R = 0.0644 and wR = 0.1813 for 5803 observed reflections with I 〉 2δ(I). The crystal of compound 2 is of monoclinic system, space group P21/n, with a = 13.050(4), b = 20.577(5), c = 13.323(4)A,β = 113.578(3)°, V = 3227.2(14)A3, Z = 2, C64H48F12Mn2N10O8P2, Mr = 1484.94, Dc = 1.528 g/cm^3, F(000) = 1508.0, Rint= 0.0295, T= 293(2) K,μ = 0.539 mm^-1, the final R = 0.0629 and wR = 0.1789 for 5298 observed reflections with I 〉 2σ(I). Compounds 1 and 2 are linear trinuclear and dinuclear manganese complexes respectively, which are both bridged by carboxylate groups of the ligands.
Two manganese complexes, [Mn3(2-cba)6(phen)2] 1 (2-cba = 2-cyanobenzoic acid, phe11 = 1,10-phenanthroline) and [MnE(4-fbaO)E(phen)4](PF6)E.EHEO 2 (4-fbao = 4-formylbenzoic acid oxime), have been synthesized by the reaction of 2-formylbenzoic acid oxime (2-fbao, HELl) or 4-formylbenzoic acid oxime (4-fbao, HELE) with phen and manganese acetate in ethanol or methanol solution. A translation from the oximino (-CHN=OH) of HELl to cyano (-C-N) was found in the formation of complex 1 at room temperature. The complexes were structurally determined by single-crystal X-ray diffraction. The crystal of compound I belongs to monoclinic, space group C2/c, with a = 17.983(6), b = 23.364(7), c =14.589(5) A, β = 92.401(5)° V = 6124(3) A^3, Z = 4, C72H40Mn3N10O12, Mr= 1401.96, Dc = 1.521 g/cm^3, F(000) = 2852.0, Rint = 0.0372, T= 293(2) K,μ = 0.686 mm^-1, the final R = 0.0644 and wR = 0.1813 for 5803 observed reflections with I 〉 2δ(I). The crystal of compound 2 is of monoclinic system, space group P21/n, with a = 13.050(4), b = 20.577(5), c = 13.323(4)A,β = 113.578(3)°, V = 3227.2(14)A3, Z = 2, C64H48F12Mn2N10O8P2, Mr = 1484.94, Dc = 1.528 g/cm^3, F(000) = 1508.0, Rint= 0.0295, T= 293(2) K,μ = 0.539 mm^-1, the final R = 0.0629 and wR = 0.1789 for 5298 observed reflections with I 〉 2σ(I). Compounds 1 and 2 are linear trinuclear and dinuclear manganese complexes respectively, which are both bridged by carboxylate groups of the ligands.
基金
grants from the 973 Program (2007CB815301 and 2006CB932900)
the National Natural Science Foundation of China (20733003 and 20673118)
the Science Foundation of CAS (KJCX2-YW-M05)
Fujian Province (2006F3132 and 2005HZ01-1)