Name: combining solid-state and solution-based techniques: synthesis and reactivity of chalcogenidoplumbates(ii or iv)
Uploaded: 2016-12-29T15:00:00
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...

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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。

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	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:247px;">Ethan-1,2-diamine</td>
			<td style="width:81px;">Sigma-Aldrich</td>
			<td style="width:136px;">E26266-2.5L</td>
			<td style="width:191px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:247px;">Calcium hydride</td>
			<td style="width:81px;">Sigma-Aldrich</td>
			<td>213268-100G</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:247px;">Tetrahydrofuran</td>
			<td style="width:81px;">Sigma-Aldrich</td>
			<td>401757-1L</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:247px;">Sodium</td>
			<td style="width:81px;">Sigma-Aldrich</td>
			<td>71172-1KG</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:247px;">Potassium</td>
			<td style="width:81px;">Sigma-Aldrich</td>
			<td>244864-50G</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:247px;">Tris-triphenylphosphine rhodium chloride</td>
			<td style="width:81px;">Sigma-Aldrich</td>
			<td>199982-5G</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:247px;">Lead</td>
			<td style="width:81px;">Acros</td>
			<td align="right">222625000</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:247px;">Selenium</td>
			<td style="width:81px;">Sigma-Aldrich</td>
			<td>209643-50G</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:247px;">18-crown-6</td>
			<td style="width:81px;">Acros</td>
			<td align="right">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 ...

Research

JoVE Journal

Chemistry

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

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes

The Synthesis, Characterization and Reactivity of a Series of Ruthenium N-triphosPh Complexes

一系列钌的合成，表征和反应<em&gt;Ñ</em&gt; -triphos<sup&gt;博士</sup&gt;配合

Herein we report the synthesis of a tridentate phosphine ligand N(CH2PPh2)3 (N-triphosPh) (1) via a phosphorus based Mannich reaction of the ...

科研

化学

Synthesis and Characterization of Supramolecular Colloids

超分子胶体的合成与表征

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects

X射线粉末衍射在保护科学：迈向文物艺术品腐蚀产物的常规晶体结构测定

The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder ...

Synthesis of Plant Phenol-derived Polymeric Dyes for Direct or Mordant-based Hair Dyeing

对于直接或媒介为基础的头发染色厂苯酚衍生的高分子染料的合成

Effective hair dyeing through in situ incubation of keratin hair with the products of fungal laccase-catalyzed polymerization of plant phenols has been ...

Measurement of Particle Size Distribution in Turbid Solutions by Dynamic Light Scattering Microscopy

通过动态光散射显微镜混浊解决方案粒度分布的测定

A protocol for measuring polydispersity of concentrated polymer solutions using dynamic light scattering is described. Dynamic light scattering is a ...

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

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

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 ...

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

直接溶液还原法快速合成金、钯、铂气凝胶的研究

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

两栖金纳米粒子的合成与表征

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...

High-Contrast and Fast Photorheological Switching of a Twist-Bend Nematic Liquid Crystal

扭曲弯曲的液晶的高对比度和快速光圈开关

Smart viscoelastic materials that respond to specific stimuli are one of the most attractive classes of materials important to future technologies, such ...