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报道了一个新型一维的多核锰的配合物 {[Mn( μ- maleate) ( phen) ( H2 O) 2 ]· 2 H2 O}n( I)( phen为邻菲罗啉 ,μ- maleate为马来酸根桥 )的合成、元素分析、晶体结构、红外光谱和热重分析 .( I)是通过马来酸锰与邻菲罗啉在乙醇的水溶液中制得的 .其晶体属于三斜晶系 ,空间群为 P- 1 ,a=0 .81 1 9( 1 )、b=0 .81 57( 1 )、c=1 .3632 ( 1 ) nm、α=99.0 8( 1 )、β=87.1 1 ( 1 )、γ=1 0 1 .94°、V=0 .872 1 ( 3) nm3 、Z=2、Dc=1 .60 4 g/cm3 、μ=7.73cm-1、F( 0 0 0 ) =434.结构解析采用直接法 ,R和 Rw 分别收敛到 0 .0 37和 0 .0 50 .单晶结构分析表明 ,( I)中 Mn原子是六配位的 ,配位原子分别为邻菲罗啉的两个 N原子、两个 H2 O中的 O原子和两个马来酸根的 O原子 .马来酸根配体通过两端的羧基氧与 Mn原子桥联进而形成一条无穷链 .配合物分子中存在两种氢键 :即一个未配位的羧酸氧原子与一个已配位的 H2 O分子间形成的分子内氢键 ;结晶水分子与配合物链上的 O原子及配位水分子间的分子间氢键 .红外光谱对羧基在 1 42 5、1 540 cm-1处的对称和不对称伸缩振动以及配位水分子和晶格水分子在 350 0～ 31 0 0 cm-1处的振动吸收进行了归属 .热重分析表明 ,晶体约在 60°C开始失去结晶水 ,紧接着开始失
A new one-dimensional multi-nuclear manganese complex {[Mn (μ-maleate) (phen) (H 2 O) 2] · 2 H 2 O} n (I) is reported. Phen is phenanthroline and μ-maleate is Maleate bridge), elemental analysis, crystal structure, infrared spectroscopy and thermogravimetric analysis. (I) is prepared by the reaction of manganese maleate and o-phenanthroline in ethanol aqueous solution. The crystals belong to triclinic The space group is P-1, a = 0.81 1 9 (1), b = 0 .81 57 (1), c = 1.3632 1 nm, α = 99.0 8, 87.1 1 (1), γ = 1 0 1 .94 °, V = 0 .872 1 (3) nm3, Z = 2, Dc = 1.60 4 g / cm 3, μ = 7.73 cm -1, F 0 0) = 434. The structure was analyzed using the direct method, and R and Rw converged to 0 .0 37 and 0 .050, respectively. The single crystal structure analysis showed that Mn atom in (I) was hexacoordinated, Two adjacent N-phenanthroline atoms, two O atoms in H 2 O, and two O atoms in the maleate group.The maleate ligand forms an infinite chain by bridging the carboxyl oxygen at both ends with the Mn atom. There are two kinds of hydrogen bonds in the complex molecule: the molecule formed between one uncoordinated carboxylic acid oxygen atom and one coordinated H2O molecule Hydrogen bond, the intermolecular hydrogen bond between crystal water molecules and O atoms and coordination water molecules in the complex chain, the symmetric and asymmetric stretching vibration of carboxyl groups at 1 42 5,1 540 cm -1 The vibrational absorptions of water molecules and lattice water molecules at 350 0 ~ 31 0 0 cm-1 were assigned .Thermal gravimetric analysis showed that the crystal began to lose its crystal water at about 60 ° C, and then began to lose