Name: combining solid-state and solution-based techniques: synthesis and reactivity of chalcogenidoplumbates(ii or iv)
Uploaded: 2016-12-29T15:00:00.000+00:00
Duration: 10 min 42 s
Description: Watch this Scientific Journal Video about Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of ChalcogenidoplumbatesII or IV at JoVE.com

这项工作是由最高人民检察院1708 GT感谢的框架内利奥波尔迪纳国立Akademie的德学问的博士后奖学金内德意志研究联合会（DFG）的支持。

注意:化学品时，一定要小心谨慎。应用共同安全预防措施，包括手套，护目镜的适当利用，并且在任何时候都白大褂。特别是，要知道，含重元素，以及它们的元素来源的所有讨论的化合物，是高毒性的。 1,2-二氨基乙烷是一种腐蚀性液体。碱金属和三元的固态产品可能与空气和水分pyrophorically反应。 注意:所有的操作都采用在空气和外部湿气的严格排除标准Schlenk或手套箱技术在氩气氛中进行。含重元素金属化物种或前体的固体或溶液通过包裹用铝箔各自的容器用于抑制光诱导分解的存储的光的排斥下。 1，溶剂和溶液的制备<ol><li>加入1升新鲜购买1,2-diaminoethane至25g氢化钙2并搅拌过夜。回流（T B = 116℃），直到没有H 2的情况下（大约12小时）。 <ol><li>蒸馏在环境压力。 </li></ol></li><li> 1升氧杂环戊烷（THF）中添加至10克的NaK合金并搅拌过夜。返流（T B = 66°C）至少12小时。蒸馏在环境压力。 </li><li>加入150毫克的[Rh（PPH 3）3氯]的10毫升THF中作出的[Rh（PPH 3）3氯]的饱和溶液。在室温（RT）和滤液与低孔隙率的惰性气体过滤器的玻璃料搅拌过夜。 </li></ol> 2.高温固态反应<ol><li> 的PbSe合成2- <ol><li>将3.81克元素硒的硼硅酸盐安瓿并在上面添加元素铅5克。直到熔体的光学均匀性达到（约10分钟）用氧/甲烷燃烧器加热。用软木塞轻轻环敲安瓿整个合成分离从安瓿壁，然后将回落到反应混合物升华硒。 </li><li>允许安瓿冷却至室温。打破用杵安瓿在研钵和手动移除安瓿的所有剩余的碎片。杵粗硒化铅2淋漓尽致。 </li></ol></li><li> K 2的PbSe 2的合成 <ol><li>将0.95克元素钾和厚壁硼硅安瓿5克元素铅。慢慢地用氧/甲烷燃烧器增加热量，直到熔体的光学均匀性达到（约20分钟）。 </li><li>仔细1.9克元素硒粒料添加到熔融合金。一旦完全加入，提高温度，直至反应混合物发出明亮的黄色/白色辐射（约10分钟）并保持温度10分钟。降低反应温度，如果稍微辐射颜色将变为纯，亮白色（TE的温度接近安瓿的熔点）。 </li><li>使反应混合物冷却至室温。打破安瓿并手动删除安瓿的所有剩余的碎片和元素铅轩辕。杵粗K 2硒化铅2淋漓尽致。 </li></ol></li></ol> 3. 在原位还原<ol><li> 中的溶液的合成〔K（18-冠-6）] 2 [铅2硒3] <ol><li>放置2克的PbSe 2，3.1克18-冠-6，250毫升1,2-二氨基乙烷，并在一个圆底的 N 2 -flask上的搅拌盘的大型搅拌棒。在室温下搅拌严格，慢慢地加入0.45克元素的K. </li><li>在RT搅拌过夜，并筛选具有低孔隙率的惰性气体过滤玻璃料的溶液（孔径:D3，16-40微米或D 4，10-16微米）。 </li></ol></li></ol> 4.溶剂热反应<ol><li> K 4 [的PbSe 4]的合成＆＃183;恩·NH 3 <ol><li>放置0.5克K 2的PbSe 2和2mL 1,2-二氨基乙烷的在10毫升的小玻璃瓶中在标准的不锈钢高压釜15mL的聚四氟乙烯瓶中。紧紧关闭高压釜，并将其在烘箱中加热至150℃5天。 </li><li>关掉烤箱，并搁置1天慢慢冷却至室温。反应混合物转移到paratone石油和手动选择K 4 [硒化铅4]的晶体·恩·NH 3在15-40X倍的标准光学显微镜下。 </li></ol></li></ol> 5.无分层<ol><li> [（RhPPh 3）6（μ3 -Se）8]·0.5en的合成 <ol><li>放置10毫升的THF〔K（18-冠-6）] 2 [铅2硒3]在一个50毫升烧瓶中，添加饱和溶液的10毫升的[Rh（PPH 3）3氯]的溶液，并搅拌过夜。 </li><li>费尔之三与低孔隙率的惰性气体过滤玻璃料的反应溶液，并在24小时慢慢除去在动态真空下除去溶剂。粗反应产物转移到paratone油和15-40X倍率手动选择标准光学显微镜下[（RhPPh 3）6（μ3 -Se）8]·0.5en的晶体。 </li></ol></li><li> 合成{[K（18-冠-6）〕 - 〔K（烯）2] K的[Rh 3（CN）2（PPH 3）4（μ3 -Se）2（μ-的PbSe）]} 2· 1.3en <ol><li>放置10毫升的溶液〔K（18-冠-6）] 2 [铅2硒3]在Schlenk管和小心地用10毫升的饱和溶液的[Rh（PPH 3）3氯]在层它THF。完全覆盖Schlenk管中铝箔和离开它不受干扰4周。 </li><li>转移所产生的固体进入paratone油和李下快速选择单晶GHT显微镜。 </li></ol></li></ol> 6.解决方案和化合物的分析<ol><li>放置50毫克的"K 2的PbSe 2"上的丙烯酸类玻璃样品载体（化合物与元素硅反应），并用胶带覆盖。将其放置在环境条件下，在粉末X射线衍射装置（PXRD）和1小时23内记录的衍射数据。 </li><li>放置的溶液0.6毫升〔K（18-冠-6）] 2 [铅2硒3]核磁共振（NMR）管并彻底密封后者用保护胶带。迅速转移入核磁共振探测并记录77 Se和205铅NMR至少有2000和5000的脉冲，分别为25。 </li><li>在光学显微镜下选择单个晶体和它安装在衍射仪的测角头。具有高冗余测量它能够充分吸收校正23-33。 </li><li>执行simultaneo的电子和几何结构的我们优化的[Rh 3（CN）2（PPH 3）4（μ3硒）2（μPbSe）3 - 。与默认半径的增加了10％，占电荷补偿28施加导体状筛选模型（COSMO）。 <ol><li>计算振动频率，以保证精力充沛的最低28。 </li><li>执行马利肯和/或自然键轨道（NBO）基于密度泛函理论（DFT）波函数来获得原子电荷28分析。 </li><li>计算在轨道贡献的"松弛"和一个原结构）的完整的群集，b）该CO /自由的PbSe群集，和c）该CO /的PbSe配体，结果28进行比较。 </li></ol></li></ol>

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Chem. 640 (14), 2684-2700 (2014).</li><li>Thiele, G., Lichtenberger, N., Tonner, R., Dehnen, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Syntheses,+Structures+and+Electronic+Properties+of+a+New+Series+of+Tellurides+of+the+Type+[Sequestrated+Cation]2[Tex]+(x+=+1-4).">Syntheses, Structures and Electronic Properties of a New Series of Tellurides of the Type [Sequestrated Cation]2[Tex] (x = 1-4).</a> Z. Anorg. Allg. Chem. 639 (15), 2809-2815 (2013).</li></ol>

The authors have nothing to disclose.

经典的高温的结合，以基于溶液的方法的固态反应允许用于不能仅通过这些途径中的一个来合成的新化合物的产生和分离。尽管在大多数情况下，该中间物质的清晰识别和充分表征是难以或基本上不可能的，一般的想法是直截了当的并且可以应用于各种元素的组合。此外，对于一个具体的化合物的生成的实际的合成条件是相当灵活，并且进一步离子物质和/或不同的所涉及的元件的相对比例的存在...

金属硫属化物，如SNSE或的CuInSe，是具有广泛的应用，例如通用的材料，如半导体，热电，或非线性光学材料1-6。类似的元素的组合物硫属化合物中发现的，其中所述金属处于正式正氧化态和由负（聚）硫属化物配体配位，以产生一个总的阴离子物质。不同于上述材料，例如金属化物附加地包括反离子，其是公由阴离子子隔开。典型的阳离子是（溶剂化）碱金属或碱土金属，铵或鏻离子。大多数情况下，与chalcogenidometalate阴离子例如盐具有的物理性质是类似于亲本的二元或三元化合物，如类似的带隙或光和半导电性能。然而，由于各元素内c的广泛范围的可能的阴离子结构ombination，从通过股线和互联的阴离子为扩展三维框架片分离的分子种类，各种性质的一个更精细的调谐，可以实现最终瞄准具有所需性质的化合物的设计合成。内降维的概念，它已经表明，每式单元，伴随经由二维和一维从3D还原以0D阴离子结构（0D表示分子物质）的反离子的相对增加，降低所观察到的带隙7。此外，通过不同的（或混合物）硫属化物的配位体的使用，它甚至有可能达到的带隙8,9-超细调整。 除了这些实际应用的有远见relevancies，硫属化合物仍在研究对基本理解，诸如用于新颖的阴离子结构类型的产生或发现和INTE一个不寻常的粘接rpretation，以及它们的前所未有的属性。而较轻的同源物（ 即，oxidometalates，通常被称为oxometalates）已被广泛研究，尤其是用于潜在催化应用，较重的硫属化合物是少得多的探讨。 我们自己的兴趣一直集中在合成，属性和chalcogenidotetrelates进一步反应（即硅酸盐较重的同源物）10,11。有各种各样这样的化合物，从水稳定且可溶的二元阴离子，如[SNTE 4] 4-阴离子12;有机的，官能化和multinary簇化合物，如{[铱3（鳕鱼）3（μ3 -S）2]（μ3 -S）的SnCl} 2（COD =环辛-1,5-二烯）13。我们最近的研究处理chalcogenidoplumbates，用铅作为中心金属在OM（S）。在与重原子的惰性，对理念，解决6S轨道的稳定，由于相对论效应，率先在正规+ II氧化态所观察的通常。像的PbO 2的例外是强氧化剂，和较重的铅（IV）的硫属化物，"PBCH 2，"没有被发现的日期14。这同样适用于所述chalcogenidoplumbate（Ⅳ）的阴离子，其中只有[的PbO 4] 4 -已经报道15直到最近（见下文）。 除了一个不同的小组结构调查oxidoplumbates（Ⅱ，Ⅳ），已经出现了chalcogenidoplumbates（Ⅱ），即只有几个例子[的PbTe 3] 4 - ，具有三角锥型阴离子16;和[铅2 CH 3] 2 - ，其中CH = Se或Te，具有三角双锥阴离子17。这些是由也被应用的路线合成为Zintl的产生离子18。经在高温下的元素融合制备multinary金属间相，随后在螯合剂的存在下提取由溶剂，得到在（单）晶体形式的所需产物。在的情况下，[铅2 CH 3] 2 -的阴离子，例如，标称成分的相位"KPbCh"已经在4,7,13,16存在下1,2-二氨基乙烷（烯）萃取，21,24六氧-1,10-二氮杂双环[8.8.8]二十六烷（双环[2.2.2]隐窝）。的穴状配体是必要既用于在在[KP [2.2.2]隐窝}有效阳离子半径+络合物抗衡离子的增加结晶，以更好地匹配阴离子大小，而对于正电荷的屏蔽，抑制电子回-donation从在溶液中的阴离子。相比于当封装的阳离子这样的盐通常揭示结晶高的倾向，因此，相当不错的收益相应的盐，而不封存剂。然而，相当麻烦的合成或穴状的高房价阻止这种方法的过度扩展。 与此相反，K 4 [的PbTe 3]·2en经由在溶液原位还原合成，如已经早在1891年用于著名铅9 4的产生-阴离子19,20。对于后者，元素碱金属加入到铅悬浮在液态氨在低温下，而对于telluridoplumbate，标称组合物"的PbTe 2"的合金，在室温下通过加入元素的钾降低，一次。 我们对这种金属化物种第一种方法将本文中所呈现的这两个途径的组合。这里，固态合成之后是在溶液中廉价螯合剂阿格纳的存在或减少TS，如1,4,7,10,13,16- hexaoxacyclooctadecane（18-冠-6），或通过减少与由溶剂本身螯合碱金属，而不需要额外的多价螯合剂，类似合成的[娜4（EN）7] [9锡] 21。我们的第二种方法也开始与高温合成，但它接着将得到的相的溶剂热提取（ 即，提取在升高的温度和压力下）22。在下文中，我们将提出两个合成方法和一些我们最近在这些反应途径的应用的结果。

<table><tbody><tr><td>Ethan-1,2-diamine</td><td>Sigma-Aldrich</td><td>E26266-2.5L</td><td></td></tr><tr><td>Calcium hydride</td><td>Sigma-Aldrich</td><td>213268-100G</td><td></td></tr><tr><td>Tetrahydrofuran</td><td>Sigma-Aldrich</td><td>401757-1L</td><td></td></tr><tr><td>Sodium</td><td>Sigma-Aldrich</td><td>71172-1KG</td><td></td></tr><tr><td>Potassium</td><td>Sigma-Aldrich</td><td>244864-50G</td><td></td></tr><tr><td>Tris-triphenylphosphine rhodium chloride</td><td>Sigma-Aldrich</td><td>199982-5G</td><td></td></tr><tr><td>Lead</td><td>Acros</td><td>222625000</td><td></td></tr><tr><td>Selenium</td><td>Sigma-Aldrich</td><td>209643-50G</td><td></td></tr><tr><td>18-crown-6</td><td>Acros</td><td>181561000</td><td></td></tr></tbody></table>

combining solid-state and solution-based techniques: synthesis and reactivity of chalcogenidoplumbates(ii or iv)

"PBCH 2"（CH =硒，碲）的相位从固态合成得到的（ 即 ，通过在石英玻璃安瓿在惰性条件下的元件的融合）。通过在胺元素碱金属如相减，得到结晶chalcogenidoplumbate（Ⅱ）由[的PbTe 3] 2的盐-或[铅2 CH 3] 2 -阴离子，这取决于其中螯合剂为阳离子存在:冠醚，像18-冠-6，或穴状配体，如[2.2.2]隐窝。与过渡金属化合物产量（聚）硫系阴离子或过渡金属簇硫族化合物，其中包括一个具有μ-硒化铅配体（ 即 ，最重的知名CO同源物）这样的阴离子溶液的反应。 与此相反，标称组成的一相的固态合成的"K 2的PbSe 2"的元素的连续反应S和由在胺随后溶剂热处理产生第一非氧化物/卤化物无机铅（IV）的化合物: 邻 -selenidoplumbate（IV）的阴离子的盐[的PbSe 4] 4 - 。这是出乎意料的，由于铅（IV）和硒（-II）的氧化还原电位。这样的方法可以进一步应用于其它元素的组合，导致二进制[HGTE 2] 2溶液形成-或[BISE 3] 3 -的阴离子，或至K 2汞柱2硒3或K 3的大规模合成碧色3通过固态路线。 所有化合物的特征在于由单晶X射线衍射和元素分析;铅酸盐溶液可通过205 Pb和77或硒碲127核磁共振技术来研究。采用密度泛函理论方法量子化学计算使能量比较。他们还允许为分析上市的电子组态，从而，接合情况。含铑分子被发现谢夫尔型化合物显示出离域混合价，而类似telluridopalladate阴离子电子精确;与μ-硒化铅配体集群正在大力赞成对一个假设的CO模拟，符合其合成失败的尝试。正式铅（IV）中的[的PbSe 4] 4内的稳定性-阴离子主要是由于晶格内的适当稳定化。

邻 -selenidoplumbate阴离子的存在[的PbSe 4] 4 - 23（参见图1，右上）已经由单晶衍射实验，元素分析，和量子化学计算证实。晶体结构细化证实了几乎完美的四面体配位几何形状，如所预期的铅（Ⅳ）离子，而DFT计算合理化大力稳定一个 1表示，这有助于阴离子的整体稳定性（参见图1，右下角）。...

Watch this Scientific Journal Video about Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of ChalcogenidoplumbatesII or IV at JoVE.com

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of ChalcogenidoplumbatesII or IV

The synthesis of chalcogenidoplumbates(II,IV) via the in situ reduction of nominal "PbCh2" (Ch = Chalcogen) and via a solid-state reaction and subsequent solvothermal reactions is presented. Additionally, reactivities of plumbate(II) solutions are portrayed, which yield the heaviest-known CO homolog known to date: the &#181;-PbSe ligand.

结合固态和基于解决方案的技术合成及Chalcogenidoplumbates的反应（II或IV）

The phases of &#34;PbCh2&#34; (Ch = Se, Te) are obtained from solid-state syntheses (i.e., by the fusion of the elements under inert conditions in silica ...

combining-solid-state-solution-based-techniques-synthesis-reactivity

Research

JoVE Journal

Chemistry

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of Chalcogenidoplumbates(II or IV)

10.6K 次观看.  University of California, Berkeley. The synthesis of chalcogenidoplumbates(II,IV) via the in situ reduction of nominal "PbCh2" (Ch = Chalcogen) and via a solid-state reaction and subsequent solvothermal reactions is presented. Additionally, reactivities of plumbate(II) solutions are portrayed, which yield the heaviest-known CO homolog known to date: the µ-PbSe ligand. 

视频: Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of ChalcogenidoplumbatesII or IV

Activating Molecules, Ions, and Solid Particles with Acoustic Cavitation

The chemical and physical effects of ultrasound arise not from a direct interaction of molecules with sound waves, but rather from the acoustic cavitation: the nucleation, growth, and implosive collapse of microbubbles in liquids submitted to power ultrasound. The violent implosion of bubbles leads to the formation of chemically reactive species and to the emission of light, named sonoluminescence. In this manuscript, we describe the techniques allowing study of extreme intrabubble conditions and chemical reactivity of acoustic cavitation in solutions. The analysis of sonoluminescence spectra of water sparged with noble gases provides evidence for nonequilibrium plasma formation. The photons and the "hot" particles generated by cavitation bubbles enable to excite the non-volatile species in solutions increasing their chemical reactivity. For example the mechanism of ultrabright sonoluminescence of uranyl ions in acidic solutions varies with uranium concentration: sonophotoluminescence dominates in diluted solutions, and collisional excitation contributes at higher uranium concentration. Secondary sonochemical products may arise from chemically active species that are formed inside the bubble, but then diffuse into the liquid phase and react with solution precursors to form a variety of products. For instance, the sonochemical reduction of Pt(IV) in pure water provides an innovative synthetic route for monodispersed nanoparticles of metallic platinum without any templates or capping agents. Many studies reveal the advantages of ultrasound to activate the divided solids. In general, the mechanical effects of ultrasound strongly contribute in heterogeneous systems in addition to chemical effects. In particular, the sonolysis of PuO2 powder in pure water yields stable colloids of plutonium due to both effects.

Acoustic cavitation in liquids submitted to power ultrasound creates transient extreme conditions inside the collapsing bubbles, which are the origin of unusual chemical reactivity and light emission, known as sonoluminescence. In the presence of noble gases, nonequilibrium plasma is formed. The "hot" particles and the photons generated by collapsing bubbles are able to excite species in solution.

活化分子，离子和固体颗粒与声空化

The chemical and physical effects of ultrasound arise not from a direct interaction of molecules with sound waves, but rather from the acoustic ...

科研

化学

The Synthesis of [Sn10(Si(SiMe3)3)4]2- Using a Metastable Sn(I) Halide Solution Synthesized via a Co-condensation Technique

The number of well-characterized metalloid tin clusters, synthesized by applying the disproportionation of a metastable Sn(I) halide in the presence of a sterically demanding ligand, has increased in recent years. The metastable Sn(I) halide is synthesized at&#160;&#34;outer space conditions&#34; via the preparative co-condensation technique. Thereby, the subhalide is synthesized in an oven at high temperatures, around 1,300 &#176;C, and at reduced pressure by the reaction of elemental tin with hydrogen halide gas (e.g., HCl). The subhalide (e.g., SnCl) is trapped within a matrix of an inert solvent, like toluene at -196 &#176;C. Heating the solid matrix to -78 &#176;C gives a metastable solution of the subhalide. The metastable subhalide solution is highly reactive but can be stored at -78 &#176;C for several weeks. On heating the solution to room temperature, a disproportionation reaction occurs, leading to elemental tin and the corresponding dihalide. By applying bulky ligands like Si(SiMe3)3, the intermediate metalloid cluster compounds can be trapped before complete disproportionation to elemental tin. Hence, the reaction of a metastable Sn(I)Cl solution with Li-Si(SiMe3)3 gives [Sn10(Si(SiMe3)3)4]2- 1 as black crystals in high yield. 1 is formed via a complex reaction sequence including salt metathesis, disproportionation, and degradation of larger clusters. Further, 1 can be analyzed by various methods like NMR or single crystal X-ray structure analysis.

The Synthesis of [Sn10SiSiMe334]2- Using a Metastable SnI Halide Solution Synthesized via a Co-condensation Technique

The disproportionation reaction of a metastable Sn(I) chloride solution, obtained via the preparative co-condensation technique, is used for the synthesis of a metalloid tin cluster compound.

的合成[锡<sub&gt; 10</sub&gt;（SI（SIME<sub&gt; 3</sub&gt;）<sub&gt; 3</sub&gt;）<sub&gt; 4</sub&gt;]<sup&gt; 2</sup<sup&gt; -</sup&gt;使用亚稳锡（I）卤溶液通过共缩聚合成技术

The number of well-characterized metalloid tin clusters, synthesized by applying the disproportionation of a metastable Sn(I) halide in the presence of a ...

A Protocol for Safe Lithiation Reactions Using Organolithium Reagents

Organolithium reagents are powerful tools in the synthetic chemist&#39;s toolbox. However, the extreme pyrophoric nature of the most reactive reagents warrants proper technique, thorough training, and proper personal protective equipment. To aid in the training of researchers using organolithium reagents, a thorough, step-by-step protocol for the safe and effective use of tert-butyllithium on an inert gas line or within a glovebox is described. As a model reaction, preparation of lithium tert-butyl amide by the reaction of tert-butyl amine with one equivalent of tert-butyl lithium is presented.

The safe and proper use of organolithium reagents is described.

使用有机锂试剂的一个协议安全的锂化反应

Organolithium reagents are powerful tools in the synthetic chemist&#39;s toolbox. However, the extreme pyrophoric nature of the most reactive reagents ...

Preparation and Reactivity of a Triphosphenium Bromide Salt: A Convenient and Stable Source of Phosphorus(I)

We present herein the optimized synthesis of a triphosphenium bromide salt. Apart from being a versatile metathesis reagent, this unusually stable low-valent-phosphorus-containing compound acts as a useful P+ transfer agent. Unlike traditional methods employed to access low-coordinate phosphorus species which usually require pyrophoric phosphorus-containing precursors (white phosphorus, Tris(trimethylsilyl)phosphine, etc.), or harsh reducing agents (alkali metals, potassium graphite, etc.), the current approach does not involve pyrophoric or explosive reagents and can be done on large scales (&#62;20 g) in excellent yields by undergraduates with basic air-free synthetic training. The bromide counter ion is readily exchanged with other anions such as tetraphenyl borate (described herein) using typical salt metathesis reagents to obtain materials with desired properties and reactivities. The versatility of this P+ transfer approach is exemplified by the reactions of these triphosphenium precursors with an N-heterocyclic carbene and an anionic bisphosphine, each of which readily displace the neutral bisphosphine to give an NHC-stabilized phosphorus(I) cation and a phosphorus(I) containing zwitterion, respectively.

Preparation and Reactivity of a Triphosphenium Bromide Salt: A Convenient and Stable Source of PhosphorusI

The synthesis of a triphosphenium bromide salt is described and its use as a P+ transfer agent is outlined by reactions with an N-heterocyclic carbene and an anionic bisphosphine, yielding an NHC-stabilized P(I) cation and a P(I) containing zwitterion, respectively.

制备及反应性的Triphosphenium溴化物盐:磷方便稳定来源（I）

We present herein the optimized synthesis of a triphosphenium bromide salt. Apart from being a versatile metathesis reagent, this unusually stable ...

Synthesis of a Thiol Building Block for the Crystallization of a Semiconducting Gyroidal Metal-sulfur Framework

We present a method for preparing thioester molecules as the masked form of the thiol linkers and their utilization for accessing a semiconducting and porous metal-dithiolene network in the highly ordered single crystalline state. Unlike the highly reactive free-standing thiols, which tend to decompose and complicate the crystallization of metal-thiolate open frameworks, the thioester reacts in situ to provide the thiol species, serving to mitigate the reaction between the mercaptan units and the metal centers, and to improve crystallization consequently. Specifically, the thioester was synthesized in a one-pot procedure: an aromatic bromide (hexabromotriphenylene) reacted with excess sodium thiomethoxide under vigorous conditions to first form the thioether intermediate product. The thioether was then demethylated by the excess thiomethoxide to provide the thiolate anion that was acylated to form the thioester product. The thioester was conveniently purified by standard column chromatography, and then used directly in the framework synthesis, wherein NaOH and ethylenediamine serve to revert in situ the thioester to the thiol linker for assembling the single-crystalline Pb(II)-dithiolene network. Compared with other methods for thiol synthesis (e.g., by cleaving alkyl thioether using sodium metal and liquid ammonia), the thioester synthesis here uses simple conditions and economical reagents. Moreover, the thioester product is stable and can be conveniently handled and stored. More importantly, in contrast to the generic difficulty in accessing crystalline metal-thiolate open frameworks, we demonstrate that using the thioester for in situ formation of the thiol linker greatly improves the crystallinity of the solid-state product. We intend to encourage broader research efforts on the technologically important metal-sulfur frameworks by disclosing the synthetic protocol for the thioester as well as the crystalline framework solid.

Here, we present a one-pot, transition-metal-free synthesis of thiols and thioesters from aromatic halides and sodium thiomethoxide, followed by the preparation of single crystals of a metal-dithiolene network using thiol species generated in situ from the more stable and tractable thioester.

半导体回转金属硫框架结晶的硫醇构建块的合成

We present a method for preparing thioester molecules as the masked form of the thiol linkers and their utilization for accessing a semiconducting and ...

Synthesis of In37P20(O2CR)51 Clusters and Their Conversion to InP Quantum Dots

This text presents a method for the synthesis of In37P20(O2C14H27)51 clusters and their conversion to indium phosphide quantum dots. The In37P20(O2CR)51 clusters have been observed as intermediates in the synthesis of InP quantum dots from molecular precursors (In(O2CR)3, HO2CR, and P(SiMe3)3) and may be isolated as a pure reagent for subsequent study and use as a single-source precursor. These clusters readily convert to crystalline and relatively monodisperse samples of quasi-spherical InP quantum dots when subjected to thermolysis conditions in the absence of additional precursors above 200 &#176;C. The optical properties, morphology, and structure of both the clusters and quantum dots are confirmed using UV-Vis spectroscopy, photoluminescence spectroscopy, transmission electron microscopy, and powder X-ray diffraction. The molecular symmetry of the clusters is additionally confirmed by solution-phase 31P NMR spectroscopy. This protocol demonstrates the preparation and isolation of atomically-precise InP clusters, and their reliable and scalable conversion to InP QDs.

Synthesis of In37P20O2CR51 Clusters and Their Conversion to InP Quantum Dots

A protocol for the synthesis of In37P20(O2C14H27)51 clusters and their conversion to indium phosphide quantum dots is presented.

37p20 (o2cr)51聚类中的合成及其转化为 inp 量子点

This text presents a method for the synthesis of In37P20(O2C14H27)51 clusters and their conversion to indium phosphide quantum dots. The In37P20(O2CR)51 ...

Metal Oxide Heterojunction for Photocatalytic Activities

There is a significant global demand for improvements in synthesis techniques and their optimal characteristics, especially for industrial-scale applications. Sol-gel-based solution combustion synthesis (SG-SCS) is a simple method to produce ordered porous materials. In this regard, Pearson&#39;s hard and soft acids and bases theory assists in selecting host-dopant reactivity to form a proper heterojunction.
The formation of a heterojunction also changes the essential properties of the materials, improving photocatalysis via charge transfer or synergistic activities. A calcination temperature of 500 &#176;C is ideal for this process based on the results of the stability assessment via a differential thermogravimetry ratio analysis (DTG).
The nanoscale dimensions of the nanoparticles (NPs) and nanocomposites (NCs) generated were validated using X-ray diffraction and high-resolution transmission electron microscopy (HRTEM). Furthermore, the scanning electron microscopy micrographs and BET analyses confirmed the porosity nature of the materials. HRTEM, X-ray photoelectron spectroscopy, and energy-dispersive X-ray investigations established the materials composition. The study found that NCs degraded the acid orange 8 (AO8) color more efficiently than bare ZnO.

<meta charset="utf8"></head><body>用于光催化活性的金属氧化物异质结

The development of a heterojunction boosts the photocatalytic activities of solution combustion synthesis, which is a time-/energy-efficient process. Advanced analytical characterization techniques were used in this protocol to evaluate the materials&#39; characteristics, and nanocomposites demonstrated improved acid orange-8 dye degradation.

用于光催化活性的金属氧化物异质结

There is a significant global demand for improvements in synthesis techniques and their optimal characteristics, especially for industrial-scale ...

从多主题膦接头合成低价 MOF

Experimental Approaches for the Synthesis of Low-Valent Metal-Organic Frameworks from Multitopic Phosphine Linkers

Metal-organic frameworks (MOFs) are the subject of intense research focus due to their potential applications in gas storage and separation, biomedicine, energy, and catalysis. Recently, low-valent MOFs (LVMOFs) have been explored for their potential use as heterogeneous catalysts, and multitopic phosphine linkers have been shown to be a useful building block for the formation of LVMOFs. However, the synthesis of LVMOFs using phosphine linkers requires conditions that are distinct from those in the majority of the MOF synthetic literature, including the exclusion of air and water and the use of unconventional modulators and solvents, making it somewhat more challenging to access these materials. This work serves as a general tutorial for the synthesis of LVMOFs with phosphine linkers, including information on the following: 1) the judicious choice of the metal precursor, modulator, and solvent; 2) the experimental procedures, air-free techniques, and required equipment; 3) the proper storage and handling of the resultant LVMOFs; and 4) useful characterization methods for these materials. The intention of this report is to lower the barrier to this new subfield of MOF research and facilitate advancements toward novel catalytic materials.

作者聚焦:从多主题膦接头合成低价金属有机框架的实验方法  

Here, we describe a protocol for the synthesis of low-valent metal-organic frameworks (LVMOFs) from low-valent metals and multitopic phosphine linkers under air-free conditions. The resulting materials have potential applications as heterogeneous catalyst mimics of low-valent metal-based homogeneous catalysts.

多位膦接头合成低价金属有机骨架的实验方法

Metal-organic frameworks (MOFs) are the subject of intense research focus due to their potential applications in gas storage and separation, biomedicine, ...

结合固态和基于解决方案的技术合成及Chalcogenidoplumbates的反应（II或IV）

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多位膦接头合成低价金属有机骨架的实验方法

多位膦接头合成低价金属有机骨架的实验方法