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Unusual selective reactivity of the rare-earth metal complexes bearing a ligand with multiple functionalities

Science China Chemistry 2023年第1期66卷 117-126页

作者： Dongjing Hong Thayalan Rajeshkumar Shan zhu Zeming Huang Shuangliu Zhou xiancui zhu Laurent Maron Shaowu Wang Key Laboratory of Functional Molecular Solids Ministry of EducationAnhui Laboratory of Molecule-Based MaterialsCollege of Chemistry and Materials ScienceAnhui Normal UniversityWuhu 241000China Anhui Laboratory of Clean Catalytic Engineering Anhui Laboratory of Functional Coordinated Complexes for Materials Chemistiry and ApplicationCollege of Chemical and Environmental EngineeringAnhui Polytechnic UniversityWuhu 241000China LPCNO CNRS&INSAUniversite Paul Sabatier 135 Avenue de Rangueil31077 ToulouseFrance

Ligands play a key role in controlling activity of organometallic complexes so that development of new ligands to overcome the challenge is the main topic of modern *** first example of 1,1-hydride migratory insertion and intramolecular redox reaction has been realized in this work by applying a new ligand in rare-earth metal *** novel rare-earth metal complexes L^(Mes)RECH2TMS(THF)(RE=Y(1a),Dy(1b),Er(1c),Yb(1d),L^(Mes)=1-(3-(2,6-iPr_(2)C_(6)H_(3)N=CH)C8H4N)-CH_(2)CH_(2)-3-(2-CH2–4,6-Me_(2)C_(6)H_(2))-(N(CH)_(2)NC),THF=tetrahydrofuran)bearing a ligand with imino,indolyl,NHC(N-heterocyclic carbene)multiple functionalities were synthesized and *** of complexes 1 with silanes(PhSiH3or PhSiH2Me or PhSiD3)selectively produced the unprecedented 1,1-hydride(or deuterated H)migratory insertion of the indolyl moiety of the novel unsymmetrical dinuclear rare-earth metal complexes *** complex 2a reacts with Ph_(2)C=O to give the selective C=O double bond insertion to the RE–Co-methylene-Mesbond product 3a which further reacts with another Ph_(2)C=O(or DMAP,4-N,N-dimethylaminopyridine)affording the novelμ-η^(2):η^(3)-dianionic 3-iminoindolyl dinuclear rare-earth metal complex *** latter is formed through an unusual intramolecular redox reaction(through electron migration from the 2-carbanion of the indolyl ring to the imino motif)resulting in the re-aromatization of the indolyl ring.

关键词： rare-earth metal complexes indole N-heterocyclic carbene Fischer-type carbene 1 1-migratory insertion dianionic 3-iminoindolyl

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Synthesis,Characterization of Rare-Earth Metal Chlorides Bearing Indolyl-Based NCN Pincer Ligand and Their Catalytic Activity toward 1,4-cis Polymerization of Isoprene

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Chinese Journal of Chemistry 2021年第12期39卷 3360-3368页

作者： Zeming Huang Shaowu Wang xiancui zhu Yun Wei Qingbing Yuan Shuangliu Zhou Xiaolong Mu Hua Wang Key Laboratory of Functional Molecular Solids Ministry of EducationAnhui Laboratory of Molecule-Based MaterialsCollege of Chemistry and Materials ScienceAnhui Normal UniversityWuhuAnhui 241000China Anhui Laboratory of Clean Catalytic Engineering Anhui Laboratory of Functional Coordinated Complexes for Materials Chemistry and ApplicationCollege of Chemical and Environmental EngineeringAnhui Polytechnic UniversityWuhuAnhui 241000China State Key Laboratory of Organometallic Chemistry Shanghai Institute of Organic ChemistryChinese Academy of SciencesShanghai 200032China

A novel indolyl-based NCN pincer ligand precursor HL(HL=(1-(2-(CH_(2))_(4)NCH_(2)CH_(2))-3-(2,6-ipr_(2)C_(6)H_(3)N=CH)C_(8)H_(5)N))was rationally and precisely designed,and successfully prepared in a high *** of HL with ^(n)BuLi in n-hexane,followed by treatment with RECl_(3) in THF led to the isolation of rare-earth metal chlorides in monomeric form(κ^(3)-L)RECI_(2)(THF)(RE=Sc(2),Yb(3)),and dimeric form[(κ^(3)-L)RECI(THF)(μ-Cl)]_(2)(RE=Er(4),Y(5))bearing the novel indolyl-based NCN pincer ligand in designed pincer ligation depending on different metal ionic radii;and the chloride bridged rare-earth metal and lithium mixed complexes in form(κ^(2)-L)_(2)RE(μ-Cl)_(2)Li(THF)_(2)(RE=Y(6),Dy(7)).All complexes were fully characterized and their structures were *** diamagnetic complexes 2,5 and 6 were furtherly characterized by the NMR spectroscopic *** catalytic activity studies revealed that the central metal ions,borates,aluminum alkyls,and ligation of the central metal ions have influences on catalytic activity,and regio-and stereoselectivity for the polymerization of *** cooperation of the cocatalysts,the pincer-type yttrium chloride 5 initiated the isoprene polymerization with a high activity producing polymers with high regio-and stereoselectivity(1,4-cis polymers up to 99.6%),and the Mn as high as 8.76×10^(5).

关键词： Rare earth Pincer-ligand Indolyl Polymerization Selectivity

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Rare-Earth Metal Alkyl Complexes with 3-Arylamido-Functionalized Indolyl Ligands:Synthesis,Characterization and Reactivity

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Chinese Journal of Chemistry 2020年第5期38卷 478-488页

作者： xiancui zhu Yuzhe Jiang Jun Chen Shaowu Wang Zeming Huang Shan zhu Xu Zhao Wenrun Yue Jun Zhang Weikang Wu Xiangyang Zhong Key Laboratory of Functional Molecular Solids Ministry of EducationAnhui Laboratory of Molecule-Based MaterialsCollege of Chemistry and Materials ScienceAnhui Normal UniversityWuhuAnhui 242000China Anhui Laboratory of Clean Catalytic Engineering Anhui Laboratory of Functional Coordinated Complexes for Materials Chemistry and ApplicationCollege of Biological and Chemical EngineeringAnhui Polytechnic UniversityWuhuAnhui 241000China State Key Laboratory of Organometallic Chemistry Shanghai Institute of Organic ChemistryChinese Academy of SciencesShanghai 200032China

A series of dinuclear rare-earth metal alkyl complexes{[μ-η^2:η^1:η^1-3-(LNCH)(CH2SiMe3)Ind]RE-(CH2SiMe3)(THF)}2(L^1=2-tBuC6H4,RE=Y,Gd,Dy,Er,Yb;L^2=2,4,6-Me3C6H2,RE=Dy,Er;Ind=indolyl)and{[μ-η^2:η^1:η^1-3-(LNCH2)Ind]RE(CH2SiMe3)(THF)}2(L^1,RE=Y,Dy,Er,Yb;L^2,RE=Er,Yb)bearing 3-arylamido functionalized indolyl ligands having diverse bonding modes with metal ions were synthesized either by the insertion reaction of the imino group to the RE-C bond or by the alkane elimination *** the preparation of above complexes,rare-earth metal alkyl complexes{[μ-η^5:η^1:η^1-3-(L^2 NCH)(CH2SiMe3)Ind]Gd(CH2SiMe3)(THF)}2 with aμ-η^5:η^1:η^1 coordination mode to the gadolinium ion and{[μ-η^3:η^1:η^1-3-(L^2NCH2)Ind]Dy(CH2SiMe3)(THF)}2 with aμ-η^3:η^1:η^1 coordination mode to the dysprosium ion were unexpectedly *** reactions of 3-(L^2N=CH)lnd with Er(CH2SiMe3)3(THF)2 at room temperature,generated a tetranuclear imino-indolyl erbium intermediate{[μ-η^1:η^1-3-(L^2N=CH)Ind]Er(CH2SiMe3)2(THF)}4,which can transform into the amido functionalized indolyl erbium complex in hot ***,the reactivities of the newly synthesized ytterbium complex with N-heterocyclic compounds were investigated,affording the corresponding products of the mixed pyridyl-indolyl,imidazolyl-indolyl,and ortho-metalated *** yttrium complexes showed a high regioselectivity and steroselectivity for the isoprene polymerization with 1,4-trans selectivity up to 91.7%and 1,4-cis selectivity up to 96.1%in the presence of cocatalysts,respectively.

关键词： reaction. complexes selectivity

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The Application of Solid Waste in Thermal Insulation Materials: A Review

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Journal of Renewable Materials 2024年第2期12卷 329-347页

作者： Ming Liu Pinghua zhu xiancui Yan Haichao Li Xintong Chen School of Environmental Science and Engineering Changzhou UniversityChangzhou213164China School of Urban Construction Changzhou UniversityChangzhou213164China

As socioeconomic development continues,the issue of building energy consumption has attracted significant attention,and improving the thermal insulation performance of buildings has become a crucial strategic ***,the application of solid waste in insulation materials has also become a hot *** paper reviews the sources and classifications of solid waste,focusing on research progress in its application as insulation materials in the domains of daily life,agriculture,and *** research shows that incorporating household solid waste materials,such as waste glass,paper,and clothing scraps into cementitious thermal insulation can significantly reduce the thermal conductivity of the materials,leading to excellent thermal insulation *** materials prepared from agricultural solid waste,such as barley straw,corn stalk,chicken feather,and date palm fibers,possess characteristics of lightweight and strong thermal *** solid waste,including waste tires,iron tailings,and coal bottom ash,can also be utilized in the preparation of insulation *** innovative applications not only have positive environmental significance by reducing waste emissions and resource consumption,but also provide efficient and sustainable insulation solutions for the construction ***,to further optimize the mix design and enhance the durability of insulation materials,continuous research is required to investigate the mechanisms through which solid waste impacts the performance of insulation materials.

关键词： Solid waste building energy consumption insulation material sustainability

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Synthesis, structure, and catalytic activity of rare-earth metal amides with a neutral pyrrolyl-functionalized indolyl ligand

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Science China Chemistry 2014年第8期57卷 1090-1097页

作者： YANG Song zhu xiancui ZHOU ShuangLiu WANG ShaoWu FENG ZhiJun WEI Yun MIAO Hui GUO LiPing WANG FenHua ZHANG GuangChao GU XiaoXia MU XiaoLong Key Laboratory of Functional Molecular Solids Ministry of Education Anhui Laboratory of Molecule-Based Materials School of Chemistry and Materials Science Anhui Normal University State Key Laboratory of Organometallic Chemistry Shanghai Institute of Organic Chemistry Chinese Academy of Sciences

The reactions of neutral pyrrolyl-functionalized indole with rare-earth metal amides [(Me3Si)2N]3RE(μ-Cl)Li(THF)3 produced the rare-earth metal complexes [(Me3Si)2N]2RE([η1:μ-η2-3-(2-(N–CH3)C4H3NCH=N–CH2CH2)C8H5N])(μ-Cl)Li(THF)(RE = Er, Y) having indolyl ligand η1 bonded to rare-earth metal ion and η2 bonded to lithium ion. The catalytic activities of these lanthanide amido complexes for addition of terminal alkynes to aromatic nitriles were explored. Results reveal that these complexes displayed a good catalytic activity for the addition reaction under mild conditions.

关键词： terminal alkyne aromatic nitrile ynone rare-earth metal

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紫外、红外、核磁共振和质谱在醛亚胺合成中的应用

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安庆师范大学学报（自然科学版） 2022年第1期28卷 116-120页

作者：朱先翠冯天懿安徽师范大学化学与材料科学学院安徽芜湖241000

测定有机分子结构最常用的方法有紫外光谱、红外光谱、核磁共振和质谱等。在多数高校的综合化学实验课程设置中,很少有关于亚胺类物质的合成和结构表征实验。基于此,设计了2-吡咯甲醛与2,6-二异丙基苯胺在酸催化下通过加成消除反应合成... 详细信息

测定有机分子结构最常用的方法有紫外光谱、红外光谱、核磁共振和质谱等。在多数高校的综合化学实验课程设置中,很少有关于亚胺类物质的合成和结构表征实验。基于此,设计了2-吡咯甲醛与2,6-二异丙基苯胺在酸催化下通过加成消除反应合成醛亚胺的实验。利用紫外分析仪-薄层层析跟踪反应进程,用红外光谱、核磁共振和质谱表征目标化合物结构、分析产品纯度。在培养学生基本实验技能的同时,亦提升他们综合运用光谱知识分析问题、解决问题的能力。

关键词：综合化学实验醛亚胺表征合成

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钙溶蚀对混凝土抗氯离子侵蚀性能的影响

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材料导报 2024年第16期38卷 126-132页

作者：王少伟肖焰钰朱平华严先萃夏群常州大学城市建设学院江苏常州213164

面板堆石坝和水下隧道等构筑物因渗漏水而容易遭受钙溶蚀病害,在复杂水环境下将面临钙溶蚀和氯离子侵蚀耦合作用下的混凝土耐久性问题。采用化学溶液浸泡法,对不同水灰比混凝土开展了耦合加速腐蚀试验,研究了钙溶蚀和氯离子侵蚀评价指... 详细信息

面板堆石坝和水下隧道等构筑物因渗漏水而容易遭受钙溶蚀病害,在复杂水环境下将面临钙溶蚀和氯离子侵蚀耦合作用下的混凝土耐久性问题。采用化学溶液浸泡法,对不同水灰比混凝土开展了耦合加速腐蚀试验,研究了钙溶蚀和氯离子侵蚀评价指标的时空演变规律,量化了钙溶蚀对混凝土抗氯离子侵蚀性能的影响,并对其微观机理进行了解释。结果表明:混凝土完全溶蚀后的氯离子扩散系数和氯离子含量分别是未溶蚀状态下的3.5倍左右和1.3~2.0倍;扩散系数在溶蚀区由表及里呈线性衰减趋势,但在深度越大处,氯离子含量的增大倍率也越大;溶蚀混凝土的氯离子吸附能力呈明显增强的趋势,且仍遵循线性吸附模型;混凝土水灰比越大,其抗溶蚀和抗氯离子侵蚀性能越差。

关键词：混凝土钙溶蚀氯离子侵蚀加速效应

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含吡啶基β-烯酮亚胺NNO型钇双胺基配合物的合成及其催化异戊二烯聚合研究

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杭州师范大学学报（自然科学版） 2017年第4期16卷 398-403页

作者：谷晓霞朱先翠韦芸周双六吴运军王少印皖南医学院医用基础化学教研室安徽芜湖241002 安徽师范大学化学与材料科学学院分子材料实验室功能分子固体教育部重点实验室安徽芜湖241000

通过4-[(2-吡啶基)乙亚胺基]-2-戊烯-2-醇(1)与[(Me3Si)2N]3Y(μ-Cl)Li(THF)3的反应,制备含吡啶基β-烯酮亚胺NNO型钇双胺基配合物(2),采用1 H NMR,13 C NMR,元素分析,X-ray和IR等对该配合物进行了表征,并探索了其在催化异戊二烯聚合中... 详细信息

通过4-[(2-吡啶基)乙亚胺基]-2-戊烯-2-醇(1)与[(Me3Si)2N]3Y(μ-Cl)Li(THF)3的反应,制备含吡啶基β-烯酮亚胺NNO型钇双胺基配合物(2),采用1 H NMR,13 C NMR,元素分析,X-ray和IR等对该配合物进行了表征,并探索了其在催化异戊二烯聚合中的应用.结果表明,配合物2在催化异戊二烯聚合方面有较好的催化活性和立体选择性.

关键词： β-烯酮亚胺钇合成聚合

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Effect of CO_(2) Curing on the Physical Properties of Recycled Coarse Aggregate with Different Attached Mortar Contents

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Journal of Wuhan University of Technology(Materials Science) 2022年第5期37卷 905-911页

作者： zhu Pinghua LI Haichao LIU Hui YAN xiancui WANG Xinjie CHEN Chunhong Department of Civil Engineering Changzhou UniversityChangzhou213164China

The effects of carbon dioxide (CO_(2)) curing conditions (temperature,relative humidity and CO_(2) curing time) on the physical properties of recycled coarse aggregate (RCA) with varying attached mortar (AM) contents were *** and after CO_(2) curing,the physical properties in terms of the apparent density,water absorption and crushing value of RCA were tested and the quality of RCA was ***,scanning electron microscope was used to observe the microstructure of *** show that the physical properties variation of RCA with higher AM content are more significant,and the quality of RCA with lower AM content is easier to be upgraded during CO_(2) *** physical properties of RCA with 40.8% AM content are earlier stable than that with no less than 44.5% AM content during CO_(2) *** optimal temperature and relative humidity are 50 ℃ and 55% for CO_(2) curing,***_(2) curing is incapable of upgrading the quality of RCA with AM no less than 50.6%.The quality of RCA with 44.5% AM content can be upgraded only under the optimum CO_(2) curing *** relative humidity higher than 40% and the CO_(2) curing time more than 12 h,CO_(2) curing upgrades the quality of RCA with 40.8% AM content.

关键词： recycled coarse aggregate attached mortar content carbon dioxide curing curing time relative humidity temperature

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Effect of High Temperature Curing on the Frost Resistance of Recycled Aggregate Concrete and the Physical Properties of Second-Generation Recycled Coarse Aggregate under Freeze-Thaw Cycles

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Journal of Renewable Materials 2023年第6期11卷 2953-2967页

作者： Xintong Chen Pinghua zhu xiancui Yan Lei Yang Huayu Wang Changzhou City Key Laboratory of Building Energy-Saving Technology Department of Civil EngineeringChangzhou UniversityChangzhou213164China

With the emphasis on environmental issues,the recycling of waste concrete,even recycled concrete,has become a hot spot in the field of *** the repeated recycling of waste concrete used in harsh environments is still a complex *** paper discusses the durability and recyclability of recycled aggregate concrete(RAC)as a prefabricated material in the harsh environment,the effect of high-temperature curing(60℃,80℃,and 100℃)on the frost resistance of RAC and physical properties of the second generation recycled coarse aggregate(RCA_(2))of RAC after 300 freeze-thaw cycles were *** frost resistance of RAC was characterized by compressive strength,relative dynamic elastic modulus,and mass *** the physical properties of RCA_(2),the apparent density,water absorption,and crushing value were *** the SEM images of RAC after 300 freeze-thaw cycles were *** results indicated that the frost resistance of RAC cured at 80℃ for 7 days was comparable to that cured in the standard condition(cured for 28 days at 20℃±2℃ and 95%humidity),and the RAC cured at 100℃ was slightly ***,the frost resistance of RAC cured at 60℃ deteriorated *** RAC cured at 80℃ for 7 days is the *** after the freeze-thaw cycle or not,the RCA that curd at 60℃,80℃,and 100℃ for 7 days can also meet the requirements of Grade III RCA and be used as the aggregate of non-bearing part of prefabricated concrete ***_(2) which is cured at 80℃ for 7 days had the best physical properties.

关键词： Freeze-thaw cycles curing condition recycled aggregate concrete second-generation recycled coarse aggregate

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