摘要
以2-羰基丙酸水杨酰腙作为配体与二正丁基氧化锡(Ⅳ)在苯/乙醇混合溶剂中反应, 合成了新型配合物(n-Bu)2Sn(C10H8N2O4)(C2H5OH)(C10H8N2O42为2-羰基丙酸水杨酰腙负二价离子)。用单晶X-射线衍射分析法测定了该配合物的晶体结构。晶体属四方晶系, I41/a空间群, 晶胞参数a = 2.5113(7), b = 2.5113(7), c = 1.5062(6) nm, V = 9.499(5) nm3, Z = 16, Dc = 1.396 g/cm3, m(MoKa) = 1.105 mm1, F (000) = 4096。对于2499 (I >2s(I))个可观测点, 最终可靠因子R = 0.0349, wR = 0.0793。在该配合物的分子结构中, 中心锡原子与3个O原子、1个N原子和2个C原子形成扭曲的八面体几何构型, 其中3个O原子和1个N原子为赤道配位原子, 而CSnC为配合物的轴。相邻配合物分子间因Sn…O的弱相互作用和分子间氢键的作用而以二聚体的结构形式存在。
A novel six-coordinate complex (n-Bu)2Sn(C10H8N2O4)(C2H5OH) (C10H8N2O42 is the negative ion of 2- oxo-propionic acid salicyloyl hydrazone) has been synthesized by the reaction of (n-Bu)2SnO with 2-oxo- propionic acid salicyloyl hydrazone (molar ratio 1:1, metal:ligand) in benzene-ethanol (V/V, 3/1), and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to a tetragonal system with space group I41/a, a = 2.5113(7), b = 2.5113(7), c = 1.5062(6) nm, V = 9.499(5) nm3, Z = 16, Dc = 1.396 g/cm3, m(MoKa) = 1.105 mm-1, F(000) = 4096, R = 0.0349 and wR = 0.0793 for 2499 observed reflections (I > 2(I)) out of 4039 unique ones. In the crystal structure, the tin atoms are rendered in a distorted six-coordinate octahedral geometry, with one nitrogen N(1) and three oxygen atoms (O(1), O(3) and O(5)) forming the equatorial plane and C(11)Sn(1)C(15) being the axis. The structure of the title complex can also be described as a dimer mode through intermolecular SnLO and weak hydrogen-bonding interactions.
