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大位阻烃基锡金属有机化合物的合成、结构和性质研究

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大位阻烃基锡金属有机化合物的合成、结构和性质研究

作者：蒋伍玖湘潭大学

学位级别：硕士

有机锡化合物具有优良的抗癌、杀菌、杀螨和催化性能,因而在工业、农业、医药上用途广泛,是极具研究价值的一类金属有机化合物。实验证明,有机锡化合物的性能与锡原子的配位形式有关,而中心锡原子的配位形式不仅与烃基的结构有关,还与... 详细信息

有机锡化合物具有优良的抗癌、杀菌、杀螨和催化性能,因而在工业、农业、医药上用途广泛,是极具研究价值的一类金属有机化合物。实验证明,有机锡化合物的性能与锡原子的配位形式有关,而中心锡原子的配位形式不仅与烃基的结构有关,还与配体的类型有关,尤其大位阻的烃基和复杂结构的配体与锡连接,能产生许多性质特殊、结构新奇的有机锡化合物。为了进一步探讨复杂配体与锡原子的配位方式以及大位阻烃基锡配合物的分子结构与性能的关系,本文设计并合成了三个系列31个大位阻烃基锡及其配合物,其中20个未见文献报道,并用元素分析、红外、核磁等对化合物进行了表征;研究了部分化合物的结构特征、量子化学和光谱性质。论文主要包括以下五部分工作: 一、合成了7个大位阻烃基锡原料及1个配体,测定了二对氰基苄基二氯化锡的晶体结构,分子之间通过氢键作用组装成三维超分子网络结构。二、以大位阻苯（苄）基锡为原料,与含N、S、O等杂原子的配体反应,合成了9个苯（苄）基锡配合物,测定了二苄基一氯化锡喹啉-2-甲酸酯的晶体结构,其中锡原子通过羧基的两个氧原子桥联成一维链状结构。三、以大位阻三环己基氢氧化锡为原料,与含N、S、O等杂原子的配体反应,合成了14个三环己基锡配合物,测定了其中11个化合物的晶体结构,结构数据可分成三大类:（Ⅰ）单体结构,（Ⅱ）一维链状结构,（Ⅲ）二维或三维超分子结构。四、采用B3LYP/LANL2DZ进行量化计算,探讨了四个化合物的稳定性、分子轨道能量、原子净电荷布居规律以及一些前沿分子轨道的组成特征。五、研究了部分化合物的紫外-可见光谱和荧光光谱,探讨了化合物的荧光发光机理。

关键词：大位阻有机锡合成晶体结构

四个基于间苯二(取代水杨醛酰腙)的有机锡配合物的溶剂热合成、结构和荧光性能

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无机化学学报 2022年第6期38卷 1171-1179页

作者：冯泳兰蒋伍玖张复兴邝代治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衡阳师范学院化学与材料科学学院衡阳421008

采用间苯二(取代水杨醛酰腙)(H_(4)L)与R^(2)_(3)SnOH溶剂热反应,或间苯二甲酰肼、3-叔丁基水杨醛和三环己基氢氧化锡一锅溶剂热法反应,合成了4个新的有机锡配合物(SnR_(2))_(2)L(1~4),其中,H_(4)L=m-Ph(CONH—N=CH(o-OH)PhR^(1))2;R^(1)=NEt_(2),R^(2)=Ph(1);R^(1)=3,5-di-tert-butyl=3,5-t-2Bu,R^(2)=Ph(2);R^(1)=3,5-t-2Bu,R^(2)=Cy(3);R^(1)=3-tert-butyl=3-t-Bu,R^(2)=Cy(4)。经元素分析、红外光谱和(^(1)H、^(13)C、^(119)Sn)核磁共振谱表征,并用X射线衍射方法确证配合物1~4的结构。配体H_(4)L的2个取代水杨醛酰腙链向内取向并与锡原子配位形成3个内向E型配合物1~3,取代水杨醛酰腙链向外取向并与锡原子配位形成外向E型配合物4。配合物1、2和4属于三斜晶系P1空间群,配合物3属于单斜晶系P21/c空间群。中心锡与配位原子构成畸形双角三锥构型。配体、配合物-三氯甲烷溶液的荧光性能表明,当具有弱荧光的配体m-Ph(CONH—N=CH(o-OH)PhNEt_(2))_(2)(H_(4)L^(1))和无荧光的配体m-Ph(CONH—N=CH(o-OH)Ph(3,5-t-2Bu))_(2)(H_(4)L^(2))分别与苯基锡、环己基锡配位后,配合物-三氯甲烷溶液发出强荧光。

关键词：间苯二(取代水杨醛酰腙) 有机锡配合物溶剂热合成晶体结构荧光性质

Syntheses,Crystal Structures,Anticancer Activities and DNA-Binding Properties of the Dibutyltin Complexes Based on Benzoin Aroyl Hydrazone

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Chinese Journal of Structural Chemistry 2022年第2期41卷 105-113,I0010页

作者：蒋伍玖谭宇君满家泰谭宇星 Key Laboratory of Functional Metal-organic Compounds of Hunan Province Key Laboratory of Functional Organometallic MaterialsUniversity of Hunan ProvinceHunan Provincial Engineering Research Center for Monitoring and Treatment of Heavy Metals Pollution in the Upper Reaches of Xiang Jiang RiverCollege of Chemistry and Materials ScienceHengyang Normal UniversityHengyangHunan 421008China Emergency Department Xiangya HospitalCentral South UniversityChangsha 410008China

Dibutyltin benzoin benzoyl hydrazone complex Ⅰ[C_(6)H_(5)(O)C=N-N=C(Ph)CH(Ph)O]_(2)[(n-Bu)_(2)Sn]_(2)and dibutyltin benzoin salicyl hydrazone complex Ⅱ[2-(OH)-C_(6)H_(4)(O)C=N-N=C(Ph)CH(Ph)O]_(2)[(n-Bu)_(2)Sn]_(2)were synthesized and characterized by IR,^(1)H,^(13)C and^(119)Sn NMR spectra,HRMS,elemental analysis and thermal stability analysis,and the crystal structures were determined by X-ray diffraction.The crystal of complex I belongs to monoclinic system,space group P2_(1)/n with a=11.1942(8),b=10.4754(7),c=23.6700(17)?,?=101.529(2)?,Z=2,V=2719.6(3)?^(3),D_(c)=1.371 Mg·m^(–3),?(Mo Kα)=0.966 mm^(–1),F(000)=1152,R=0.0458and w R=0.1312.The crystal of complex II is of triclinic system,space group P1 with a=9.9960(4),b=11.2466(4),c=14.0509(5)?,α=69.4190(10)?,?=70.0600(10)?,γ=81.8090(10)?,Z=1,V=1389.69(9)?^(3),D_(c)=1.380 Mg·m^(–3),?(Mo Kα)=0.950 mm^(–1),F(000)=592,R=0.0284 and w R=0.0690.In vitro antitumor activities of both complexes were evaluated by CCK8 method against three human cancer cell lines(MCF7,NCI-H460 and Hep G2),and complex II exhibited better antitumor activity than I.The interaction between complexes and calf thymus DNA was studied by UV-vis,fluorescence spectroscopy and viscosity measurements.

关键词： dibutyltin complex synthesis crystal structure DNA

Syntheses,Crystal Structures and Property of Pyridine Zinc(Ⅱ)Complexes Based on Halogenated Salicylaldehyde Schiff Base

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Chinese Journal of Structural Chemistry 2022年第3期41卷 12-18,I0007页

作者：蒋伍玖倪鹏辉毛芳芳谭宇星 Key Laboratory of Functional Metal-organic Compounds of Hunan Province Key Laboratory of Organometallic New MaterialsCollege of Hunan ProvinceHunan Provincial Engineering Research Center for Monitoring and Treatment of Heavy Metals Pollution in the Upper Reaches of Xiangjiang RiverCollege of Chemistry and Materials ScienceHengyang Normal UniversityHengyangHunan 421008China

Schiff base pyridine zinc(II)complexes 1~4 were synthesized by the reaction of the 2-((2-hydroxybenzylidene)amino)phenol Schiff base with appended donor functionality,zinc acetate,and pyridine.The results of the structural characterization of the complex show that they have the same coordination mode and similar steric structure.Complexes 1 and 3 form a one-dimensional chain structure and two-dimensional grid struc-ture by lots of hydrogen bonds,respectively.Thermogravimetric analysis shows complexes 1~4 can exist stably be-low 150℃.The results of the fluorescence quenching experiments between the complexes and DNA-EB show that the interaction between them is intercalation,and the effect of complex 1 is the most obvious.It is speculated that the steric hindrance of complex 1 is relatively small,and the aromatic ring on the ligand is more likely to inserted into the base pair of DNA.

关键词： zinc complex Schiff base synthesis crystal structure property

双(3⁃乙氧基水杨醛)缩间苯二甲酰腙四丁(苯)基二锡的合成、结构和荧光性质

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无机化学学报 2022年第1期38卷 103-110页

作者：冯泳兰王莹蒋伍玖庾江喜张复兴邝代治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功能金属有机材料湖南省普通高等学校重点实验室衡阳421008

在乙醇溶液中以3⁃乙氧基水杨醛和间苯二甲酰肼反应,制备双(3⁃乙氧基水杨醛)缩间苯二甲酰腙(H_(4)L)配体。用H_(4)L分别与二丁基氧化锡和三苯基氢氧化锡甲醇溶剂热反应,合成了双(3⁃乙氧基水杨醛)缩间苯二甲酰腙四丁(苯)基二锡配合物:Bu_(... 详细信息

在乙醇溶液中以3⁃乙氧基水杨醛和间苯二甲酰肼反应,制备双(3⁃乙氧基水杨醛)缩间苯二甲酰腙(H_(4)L)配体。用H_(4)L分别与二丁基氧化锡和三苯基氢氧化锡甲醇溶剂热反应,合成了双(3⁃乙氧基水杨醛)缩间苯二甲酰腙四丁(苯)基二锡配合物:Bu_(4)Sn_(2)L(T1)和Ph_(4)Sn_(2)L(T2)。用元素分析、红外光谱、紫外可见光谱、核磁共振谱以及单晶X射线衍射表征了H_(4)L和配合物的结构。H_(4)L的分子式为C_(26)H_(26)N_(4)O_(6),晶体属单斜晶系C2/c空间群,2个甲酰肼缩(3⁃乙氧基)水杨醛呈顺式对称构型。T1的分子式为C_(42)H_(58)N_(4)O_(6)Sn_(2),晶体属正交晶系Pbcn空间群,H_(4)L的2个甲酰肼缩(3⁃乙氧基)水杨醛链向内翻转180°,配位原子与锡配位构成畸形三角双锥构型,分子结构关于C2…C4轴对称。T2的分子式为C_(50)H_(42)N_(4)O_(6)Sn_(2),晶体属三斜晶系P1空间群,配体的一个甲酰肼缩(3⁃乙氧基)水杨醛保持原构型,另一个甲酰肼缩(3⁃乙氧基)水杨醛向内翻转180°,形成2个不同构型取向的配位链,分别与二苯基锡配位形成反式双核不对称畸形三角双锥构型的配合物。H_(4)L、T1、T2的氯仿溶液(50μmol·L^(-1))的荧光光谱表明:H_(4)L在520 nm有弱荧光,T1和T2在518 nm具有比配体强14~15倍的荧光发射峰。

关键词：双(3⁃乙氧基水杨醛)缩间苯二甲酰腙有机锡配合物溶剂热合成晶体结构荧光性质

两个具有Sn4O8簇结构的二丁基锡芳氧乙酸酯配合物的合成、晶体结构及除草活性

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无机化学学报 2023年第4期39卷 649-658页

作者：谭宇星冯泳兰张复兴庾江喜蒋伍玖邝代治衡阳师范学院化学与材料科学学院金属有机新材料湖南省普通高等学校重点实验室功能金属有机化合物湖南省重点实验室湘江上游重金属污染监测与治理湖南省工程研究中心衡阳421008

以二丁基氧化锡分别与苯氧乙酸(L1)、邻氯苯氧乙酸(L2)反应,合成了2个四核二丁基锡芳氧乙酸酯配合物[(o-R—C6H4—OCH_(2)COOSn(n-Bu)_(2))_(2)O]_(2)(R=H (C1)、Cl (C2))。经元素分析、IR、^(1)H和^(13)C NMR以及X射线单晶衍射表征其... 详细信息

以二丁基氧化锡分别与苯氧乙酸(L1)、邻氯苯氧乙酸(L2)反应,合成了2个四核二丁基锡芳氧乙酸酯配合物[(o-R—C6H4—OCH_(2)COOSn(n-Bu)_(2))_(2)O]_(2)(R=H (C1)、Cl (C2))。经元素分析、IR、^(1)H和^(13)C NMR以及X射线单晶衍射表征其结构。在配合物C1、C2的独立分子中,分别存在1个以Sn2O_(2)平面四元环为中心的Sn4O_(4)梯形结构,梯的两侧分别由羧基的2个O原子与梯边的Sn—O—Sn链桥联成六元环,形成一个含Sn4O8的锡氧簇结构。配合物在220℃(C1)、250℃(C2)的空气气氛下具有较好的热稳定性。除草活性结果表明,配合物C1对决明具有较好的生长调节作用,配合物C2在50 mg·L^(-1)浓度下可高效、选择性地抑制刺苋的茎和根的生长。

关键词：二丁基锡芳氧乙酸酯合成晶体结构热稳定性除草活性

Synthesis,Structural Characterization,Fluorescence Properties and Herbicidal Activity of Bis(substituted salicylaldehyde)Carbohydrazide Dibutyltin Complexes

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Chinese Journal of Structural Chemistry 2021年第12期40卷 1639-1646,1553页

作者：冯泳兰蒋伍玖张复兴邝代治 Key Laboratory of Functional Metal-organic Compounds of Hunan Province Key Laboratory of Functional Organometallic Materials of College of Hunan ProvinceDepartment of Chemistry and Material ScienceHengyang Normal UniversityHengyangHunan 421008China

A series of dibutyltin complexes,(Bu_(2)Sn)_(2)L,[(Bu_(2)Sn)_(2)L]3 and H_(2)LSnBu_(2),were synthesized by microwave-assisted methanolic solvothermal method,where H4L is[_(2)-(OH)-R-ArCH=NNH]_(2)CX,and X=O,R=4-NEt_(2)(Tl),5-Br(T_(2));X=S,R=H(T3);R=5-Br(T4).Their structures were characterized by elemental analysis,IR and(^(1)H,^(13)C)-NMR spectra.The molecular structure of T_(2) was confirmed by X-ray diffraction.The crystal of T_(2) belongs to monoclinic system,space group la.Five-coordinated distorted triangular bipyramids and six-coordinated distorted octahedral configurations were formed by the coordination of oxygen and nitrogen atoms of ligand with two dibutyltins,thus forming a trimeric hexanuclear butyltin complex by the cross coordination of three units(Bu_(2)Sn)_(2)L with enol imines.The T_(2) and T4 exhibit fluorescence emission in DMF solvents and DMF-water mixture.The fluorescence intensity of T_(2)-DMF-H_(2)0 system decreases almost linearly with the increase of water volume fraction(WVF).The aggregation fluorescence enhancement effect of T4-DMF-H_(2)0 solution system increases with the increase of WVF at the range of 0-_(2)0%WVF.When WVF is more than _(2)0%,the fluorescence intensity decreases with the increase of WVF.In addition,T1〜T4 have broad growth activities on target plants,such as Portulaca oleracea L.,Amaranthus spinosus L.,Cassia tora L.,Brassica campestris L.ssp.chinensis var.utilis Tsen et Lee,and Amaranthus tricolor L.,and can be used as a candidate herbicide for further research.

关键词： bis(substituted salicylaldehyde)carbohydrazide dibutyltin fluorescence properties herbicidal activity

Syntheses, Crystal Structures and in vitro Anticancer Activities of Dibenzyltin Compounds Based on the N-(2-Phenylacetic acid)-aroyl Hydrazone

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Chinese Journal of Structural Chemistry 2020年第4期39卷 673-681页

作者：蒋伍玖莫天姿张复兴邝代治谭宇星 Key Laboratory of Functional Metal-organic Compounds of Hunan Province Key Laboratory of Functional Organometallic MaterialsUniversity of Hunan ProvinceCollege of Chemistry and Materials ScienceHengyang Normal UniversityHengyangHunan 421008China

Two dibenzyltin compounds,{[C6H5O(O)C=N-N=C(Ph)COO](m-Cl-C6H4CH2)2-Sn(CH3OH)}2(1)and{[p-Me-C6H4O(O)C=N-N=C(Ph)COO](m-Cl-C6H4CH2)2Sn(CH3OH)}2(2),have been synthesized by microwave“one pot”reaction with benzoylhydrazine(or p-methyl benzhydrazine),phenylglyoxylic acid and di-m-chlorobenzyltin dichloride.Compound 2 contains two crystals 2a and 2b.The compounds have been characterized with IR,elemental analysis,1H,13C and 119Sn NMR spectra,H RMS.Three crystals are all binuclear molecules with a Sn2O2 four-membered ring plane,and each Sn atom center is seven-coordinated with[SnO4C2N]to form a distorted pentagonal bipyramidal configuration.In vitro antitumor activities of all compounds and carboplatin were evaluated by MTT against three human cancer cells such as NCI-H460(lung cancer cells),HepG2(liver cancer cells)and MCF7(breast cancer cells),and compound 2 exhibited better antitumor activity.

关键词： organotin complex hydrazine synthesis crystal structure biological activity

Microwave Solvothermal Synthesis, Crystal Structures and in Vitro Antitumor Activities of Di-n-butyltin Piperonylate with a Sn4O4 Ladder Framework

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Chinese Journal of Structural Chemistry 2018年第8期37卷 1265-1271页

作者：邝代治冯泳兰蒋伍玖朱小明庾江喜张复兴 Key Laboratory of Functional Metal-organic Compounds of Hunan Province Key Laboratory of Functional Organometallic Materials of Hengyang Normal UniversityCollege of Hunan ProvinceCollege of Chemistry and Material ScienceHengyang Normal University

A two-dimensional supramolecular compound di-n-butyltin piperonylate, {（μ3-O）（μ2-OMe）（n-Bu2Sn）2[O2CAr（C2H4O）]}2 constructed by hydrogen bonds with a Sn4O4 ladder-like framework, was obtained by the microwave-assisted solvothermal reaction of di-n-butyltin oxide precursor with the piperonylic acid in methanol environments. The composite was characterized by elemental analysis and IR（~1H, ^（13）C and ^（119）Sn） NMR spectra. The compound crystallizes in monoclinic system, space group P21/n with a = 13.3690（12）, b = 14.1442（14）, c = 16.4022（16） A, β = 107.191（6）°, V = 2963.0（5） A^3, Z = 2, Dc = 1.520 g/cm^3, F（000） = 1368, μ = 1.719 mm^（-1）, Mo Kα radiation（λ = 0.71073 A）, the final R = 0.0495 and w R = 0.1260 for 6780 observed reflections with I 〉 2σ（I）. Its X-ray crystallography diffraction analyses show a Sn4O4 ladder-like skeleton, in which two endocyclic tin and one exo tin atoms are bonded to the μ3-O atom. In addition, one endocyclic tin and one exo tin atoms are respectively bonded to the μ2-O atom from methanol. The ladder-like molecule has a three-ring fused skeleton, which is almost coplanar. The endocyclic and exocyclic tin atoms were all five-coordinated with distorted trigonal bipyramidal geometry. The antitumor activity showed that the compound had higher activities than cisplatin in HT-29, HepG2, MCF-7, KB and A549 cell line in vitro.

关键词： di-n-butyltin piperonylate microwave solvothermal synthesis ladder-likeframework in vitro antitumor activity