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作 者:冯泳兰 杨春林 Feng Yonglan;Yang Chunlin(Key Laboratory of Functional Metal-Organic Compounds of Hunan Province,Key Laboratory of Organometallic New Materials,College of Hunan Province,College of Chemistry and Material Science,Hengyang Normal University,Hengyang Hunan 421002,China)
机构地区:[1]衡阳师范学院化学与材料科学学院,功能金属有机化合物湖南省重点实验室,金属有机新材料湖南省高校重点实验室,湖南衡阳421002
出 处:《衡阳师范学院学报》2022年第6期47-52,共6页Journal of Hengyang Normal University
摘 要:3,5-二叔丁基水杨醛、硫代卡巴肼和二乙酸二丁基锡一锅法自组装反应,合成了一个基于双(3,5-二叔丁基水杨醛)缩偶氮二(硫代甲酰肼)和双(3,5-二叔丁基水杨醛)缩硫代卡巴肼混合配位的新型三核丁基锡配合物,经红外光谱、~1H和13C核磁共振谱表征,并用X-射线衍射方法确定了配合物的晶体分子结构。配合物C87H142N10O4S3Sn3,M=1844.35,单斜晶系,P21空间群,a=1.2357(4) nm,b=1.9121(6) nm,c=2.0355(7) nm,β=102.212(5)°,V=4.701(3) nm~3,Z=2,Dc=1.303 g/cm~3,最终R1=0.0607和wR2=0.14147。锡原子与配基原子形成六配位畸形八面体构型,由μ~2-S桥联2个二丁基锡形成“螺旋桨”状独立单元结构的配合物,通过分子间的氢键和σ-π作用,单元结构堆积形成一个三维超分子结构。A novel trinuclear butyltin complex based on the mixed-coordination of bis(3,5-di-tert-butylsalicylaldehyde) azodithiocarbazide and bis(3,5-di-tert-butylsalicylaldehyde) thiocarbazide was synthesized by one pot self-assembly reaction of 3,5-di-tert-butyl salicylaldehyde, thiocarbazide and dibutyltin diacetate. The crystal and molecular structure of the complex were characterized by IR,1H and13C-NMR and X-ray diffraction. Complex C87H142N10O4S3Sn3, M=1 844.35, monoclinic P21space group, a=1.235 7(4), b=1.912 1(6), c=2.035 5(7) nm,β=102.212(5)°, V= 4.701(3) nm3, Z=2, Dc=1.303 g/cm3, final R1=0.060 7 and w R2=0.141 47. Tin and ligand atoms form a six-coordination distorted octahedral configuration, which is composed of μ2-S bridges two dibutyltins to form a "propeller" like unit structure. And a three-dimensional supramolecular structure is formed by intermolecular hydrogen bonds and σ-π interaction.
关 键 词:三核混配丁基锡配合物 合成 晶体结构
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