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合成了 {[( n-Bu) 2 Sn( 4-Fc-C6 H4COO) ]2 O}2 ( 1 )和 {[( n-Oct) 2 Sn( 4-Fc-C6 H4COO) ]2 O}2 ( 2 ) ( Fc=ferrocenyl)两种新的配合物 ,对其进行了元素分析 ,并用 IR,NMR( 1 H ,1 3C,1 1 9Sn)进行了谱学表征 .单晶 X射线衍射法测定表明 ,配合物 1的晶体属单斜晶系 ,P2 1 / c空间群 ,晶胞参数 a=1 .2 988( 1 ) nm,b=2 .4 655( 1 ) nm,c=3 .4 50 6( 1 ) nm,β=91 .556( 2 )°,V=1 1 .0 4 54( 1 ) nm3,Z=4 ,最终可靠因子 Rf=0 .0 71 ,Rw=0 .0 70 .分子 1为具有一个 Sn2 O2 四元中心内环的二聚结构 ,桥氧原子又各连接一个外环 Sn原子 ,呈三配位 .内环锡和外环锡采用略有不同的加帽三角双锥配位几何 . 4个羧酸酯基具有两种不同的配位方式 ,其中两个羧酸酯基通过其两个氧原子以桥式双齿分别跨接于一个内环锡和一个外环锡 ,而另外两个羧酸酯基则以单齿配位方式各与一个外环锡相连接 . Sn2 O2 中心内环与苯甲酸酯基、茂环等共轭体系之间相互未能共平面 .整个分子结构中无对称中心
Synthesis of {[(n-Bu) 2 Sn (4-Fc-C6 H4COO)] 2 O} 2 (1) and {[(n-Oct) 2 Sn (4-Fc-C6 H4COO)] 2 O} 2 (2) (Fc = ferrocenyl) were synthesized and characterized by elemental analysis and spectroscopic characterization by IR, NMR (1 H, 1 3C, 1 1 9Sn). Single crystal X-ray diffraction The results show that the crystal of complex 1 belongs to the monoclinic system, the P2 1 / c space group has a unit cell parameter of a = 1.988 (1) nm, b = 2.655 (1) nm and c = 3.4 50 6 (1) nm, β = 91 .556 (2) °, V = 1 1 .0 4 54 (1) nm3, Z = 4 and final reliability factors Rf = 0.71 and Rw = 0.70 . Molecular 1 is a dimeric structure with a Sn2 O 2 quaternary central inner ring, and the oxygen atoms of the bridges are each connected to an outer ring Sn atom in the form of a three coordinate system. The inner ring tin and the outer ring tin adopt a slightly different capping triangle Biconical coordination geometry. Four carboxylic acid ester groups have two different coordination modes in which two carboxylic acid ester groups bridge one end ring tin and one outer end by bridging bidentate through two oxygen atoms Ring tin, and the other two carboxylate ester groups are monodentate coordination with an outer ring tin connection Sn2 O2 center and the benzoic acid ester group, the ring between the conjugated ring system It failed coplanar whole molecular structure without a center of symmetry