我们感谢德意志研究联合会（DFG）的资金支持，我们感谢丹尼尔·沃纳博士有益的讨论。

注意！请咨询使用前的所有相关材料安全数据表（MSDS）。几个在这些合成中使用的化学品是剧毒，发火，和致癌性。相比，他们的大部分对手纳米材料可能有额外的危害。进行反应时，包括利用工程控制（通风柜和手套箱）和个人防护装备（护目镜，手套，实验室外套，全长裤，封闭趾鞋）的请使用所有适当的安全措施。下面的过程部分涉及标准无空气的Schlenk技术。施加的共缩合装置包含一个20千瓦的高频发生器。有心脏起搏器的人可以有严格的禁止入。 HCl气体是高度腐蚀性的。存放在通风良好的地方或在通风橱中。液氮和干冰是非常冷的物质;特殊手套必须用于防止冻伤。 1.前期工作<ol><li> 石墨反应堆的安装 <ol><li>取五反应室，一个终端环，其中一个空心石墨管淋上石英玻璃管和两个0.7毫米石墨棒。装满元素锡（件）全部五个反应室，在总共6克堆叠反应室在端子环，他们每个人的扭转30°，并修正与石墨棒的堆栈。确保杆并不比堆栈更长。 </li><li>插入堆栈到石墨管，使得终端环的孔配合在所述石墨管上的孔。固定有第二石墨棒的设置。确保杆并不比管的直径长。称重带刻度的整个安装并注意，以确定在反应过程中消耗的锡的量的值。 </li></ol></li><li> 制备溶剂混合物 注:甲苯必须超过钠/二苯甲酮预干燥和蒸馏。 TributylphosphinE必须是真空蒸馏后才能使用。 <ol><li>附加的200ml Schlenk管与玻璃活栓到实验室的Schlenk线。疏散和冲洗系统与惰性气体三次。圣火第一次疏散周期之后加热疏散Schlenk管。 注意:使用任一干燥氮气或干燥氩气作为惰性气体。 </li><li>用180毫升甲苯和20毫升三丁基膦填充。通过手动摇动瓶中混合溶剂。 注:三丁基用纸巾反应。不要擦拭三丁基滴纸。 </li><li>冷却用干冰的混合物至少20分钟，并通过轻微蒸发和摇动冷烧瓶脱气混合物。关闭阀在真空下，让混合物热至室温。 注:混合物可剧烈蒸发，这可以通过连续地摇动烧瓶来避免。 </li></ol></li></ol> 2.设置联合冷凝装置<ol><li> 反应 <ol><li>放置铜感应线圈内部的石墨反应器中并通过顶部铜板材的中心孔，设置在感应线圈上面通过石英管。固定在石英管的气体供给用垫圈和螺母。检查线圈内的反应器的位置。确保该反应器由5±0.5 mm的线圈突出。 注:铜感应线圈是共缩合装置的中心部分。线圈是用冷却水冲洗，并连接到一个高频发生器。因此，该石墨管将被感应加热。为了获得可重复的条件下，在线圈内部的石墨管的位置是至关重要的。它应位于线圈的腔的中心，以5±0.5毫米伸出的底部。 </li><li>冷却防护罩连接至与螺钉螺母连接器的水销。固定冷却防护罩在另一侧用螺钉。测试由运算冷却循环的水密性厄宁水龙头30秒。 注:由于内部的高电压，必须有没有直接的金属 - 金属接触，以防止旁路或电弧，特别是在顶部铜板材。如果有联系，更改与一个棒铜片的位置。如果这是不可能的，删除所有的部件和从2.1.1重启。 </li><li>修复高温计（温度控制）的光纤的支架在用螺丝的铜屏蔽。放的石英玻璃在保持器在光学用相同的SnCl化学品，以防止光学系统的污染。 </li><li>固定用螺丝螺母溶剂蒸气扩散器。确保扩散器的铜屏蔽的腔体中的中心。重新检查石墨反应器仍然在感应线圈的中心，而且是没有线圈的接触顶端铜片。 </li><li>装入Schlenk容器中，蒸发溶剂，在阀，其通过一个钢管连接到蒸气DIF定影器。在制备溶剂混合物的烧瓶安装到Schlenk容器中。半球形加热套加入蒸发Schlenk容器。 </li><li>长钢性插管连接到具有一个螺母的装置。用小圆底烧瓶关闭外尾。放置大不锈钢容器内的磁性搅拌棒（10厘米），将垫圈成平面凸缘的空腔，该容器连接到共缩合装置。 </li></ol></li><li> 供气 <ol><li>含盐酸的玻璃容器连接到一个小钢管，然后到一四点适配器。 注:在玻璃容器内的盐酸压力必须低于1个大气压，以使压差压力计可以工作。 </li><li>关闭四点适配器的后部出口用盲板法兰。差压压力表连接到前退出并成立了阀门顶部出口。连接细针阀到阀在四点adapte的顶部出口河然后，使用一个长的钢管到气体供给部的共缩合装置连接。 注:代替细针阀，可使用质量流量控制器。 </li></ol></li><li> 进一步的准备工作 <ol><li>的双壁钢杜瓦桶连接到真空泵和撤离双壁空间至少30分钟。 注意:此步骤也可在共缩合装置的反应部的设置过程中完成的。 </li><li> 2毫巴，这需要60分钟-用旋转叶片泵10的最终压力抽空整个共缩合装置。 </li><li>达到最终压力之后，预热油扩散泵。打开冷却水循环和疏散用加热期间旋转叶片泵的油扩散泵。 注意:在此期间，该装置的静态真空下保持，直到扩散泵进行加热。这至少需要45分钟。 </li><li>疏散APPAratus与预加热的扩散泵过夜以达到约8×10的最终压力- 6毫巴第二天早晨。 </li></ol></li></ol> 3.共缩合反应<ol><li> 设置在反应 <ol><li>填扩散泵的冷却阱用4L液氮。通过打开水龙头开关在高频发生器的冷却水的循环。然后，接通高频发生器。 </li><li>通过手动增加高频发生器的输出功率，在0.1至0.5千瓦的增量步慢慢预加热石墨反应器中，直至反应温度为大约1,300℃。 注:温度与光学高温计监测，并应不高于1300℃。在正常情况下，该过程需要约30分钟，最终温度是在3.5千伏实现。在此过程中，在不锈钢容器中也变热。 </l我&gt; <li>发电机的值调整为1.0千伏至冷却反应器。填充钢杜瓦约30升液氮。解除与升降平台杜瓦使得反应容器放置在杜瓦瓶内。添加更多的液态氮对钢杜瓦达到液氮的最终水平。 注意:在以下步骤中，液态氮的水平应该总是在不锈钢容器的上部三分之一。 </li></ol></li><li> 进行反应 <ol><li>蒸发溶剂溶液。固定下降率，使得反应（4小时）期间使用的所有溶剂。切换的半球形加热套对的最低水平，以保持蒸发。 </li><li>关闭细针和燃气阀。打开容器盐酸。确保在差压压力表显示的电压高于1600毫伏。如果不是这种情况下，通过连接的EVAC施加低压的压力计的第二连接uated容器的压力计的外部连接。记下显示的初始值。 </li><li>由发电机的值调整为3.5千伏加热石墨反应器中以1300℃的最终温度。打开燃气阀。慢慢打开细针阀将反应气体（HCl）的中让与的8毫伏/分钟的恒定速率。检查率至少每10分钟，并记下的测量值。 注:以恒定气体流量的控制为可再现的反应绝对必要的。如果使用质量流量控制器，所述流量可以通过计算机程序来控制。否则，该控制可以通过气体入口中指出的压差压力计的下降值来实现。率应为7-8毫伏/ min内，并当显示的值是通过1600毫伏，它等于40毫摩尔的HCl消耗降低的反应就完成了。 注意:当反应运行时，产生氢气，它可以监测由该装置内的压力增加，从约8×10 -至约4×10 6毫巴- 5毫巴。 </li><li>把2升液态氮在杜瓦大约每10分钟，使液氮的电平总是在不锈钢容器的上部三分之一。这个过程需要4小时。 </li><li>差动压力计的值由1600毫伏下降后，关闭气体阀。然后，引入是气体供给部内慢慢打开细针阀剩余HCl气体。等到在该装置中的压力变得比4×10低级- 5毫巴和然后关闭高频发生器和如果需要的话让剩余的溶剂混合物中。 </li><li>充满液体的氮钢杜瓦改为置于磁力搅拌器的绝缘桶。通过关闭主阀断开油扩散泵和用干燥氮气（5.0）的装置周围刷新到的压力1个大气压（粗糙的晴雨表）。添加〜5公斤细粉状干冰的到水桶，使得不锈钢容器中会从外面和开关上的磁力搅拌器进行冷却。 </li><li>等到磁力搅拌器旋转自如。这表明，在反应混合物为熔融态。让溶液搅拌至少45分钟。 注:在加热过程中，压力增大和可能获得高于1.2个大气压，这可以在粗晴雨表看到。过压可通过阀的圆底烧瓶中，在长按插管被释放。 </li><li>关闭搅拌器。在压套管的圆底烧瓶改变到双阀Schlenk管，同时仍然用在氮气流量恒定干冰冷却。固定压套管的高度，以便它接触的不锈钢容器的底部。 </li><li>通过在双阀Schlenk管打开阀压出的Sn（I）的氯与轻微过压溶液。 注意:搜索解决方案n应是深红色，深褐色至黑色，浓的时候。 </li></ol></li><li> 确定溶液的质量 <ol><li>卤化物滴定 取2毫升溶液和在20毫升的稀硝酸溶解。加入1ml 30％的H 2 O 2并搅拌10分钟。执行硝酸银的电位滴定法对甘汞电极。 注:卤化物的浓度应为〜0.2 M. </li><li>取石墨管并称重，以确定所消耗的锡的量，应4克和4.8克之间是英寸 注意:在正常的情况下，反应的锡的量小于溶液内的卤化物的量降低，由于副反应: SN + 2盐酸→2氯化亚锡 注:此反应在少量，但它不会降低溶液的质量和歧化反应，以形成锡簇物种的能力。阿锡:1 C比:1.2在正常范围内。 </li></ol></li></ol> 4.锡10脯氨酸（Hyp）4 2的合成- <ol><li> 前期工作 <ol><li>放置LiHyp•3的THF 2克（4.4毫摩尔），按文献24和小磁性搅拌棒放入一个Schlenk管中手套箱制备。 </li><li>在-78℃制备2-丙醇/干冰冷却浴。不要使用低温恒温器。 </li><li>放置Schlenk容器冷却浴内，并放置两个在磁力搅拌器上。 </li></ol></li><li> 反应 <ol><li>加入20毫升的0.2M的SnCl溶液含有通过钢或特氟隆套管•3的THF LiHyp 2克（4.4毫摩尔）的冷却Schlenk容器的。开启磁力搅拌器。让反应跑3小时内慢慢地暖机至室温。观察反应液变化到深褐色的颜色。 注意:如果该溶液的浓度没有的0.2M，调节添加量，使得4毫摩尔卤化物的应用（ 例如加入 40ml的0.1M溶液）。 </li></ol></li><li> 的处理过程 <ol><li>停止搅拌器并允许Schlenk管内的所有不溶性沉淀物沉降。倒出黑色溶液到另一个Schlenk容器。 注:在大多数情况下，在倾析过程中，它是有用的有灯检查沉淀物，以确保将上清液完全转化。非溶性的沉淀氯化锂可以被标识为在底部的灰色固体。 </li><li>增加±毫升TMEDA（TMEDA = N，N，N&#39;，N&#39;四甲基乙二胺）该混合物中，并允许它放置过夜。黑，四面体晶体生长在该溶液中。一旦隔离，通过质子核磁共振李2（TMEDA）4锡10羟脯氨酸4 月23日确定的结晶。 注:随着时间的推移，该母液生产的产品的更多的晶体。因此，存储所述拉莫特为至少一个月ř酒建议以增加产量。母液的浓度也可能是有益的以引发进一步结晶。 </li><li>以获得用于X射线晶体结构分析的晶体，再结晶以下列方式集群:将150毫克的 Li 2（TMEDA）4的Sn 10脯氨酸4在-40℃的在15毫升绝对THF中。加在1ml 12-冠-4（5克在25毫升甲苯），将混合物的。溶液应深绿色和必须储存在-30℃，作为集群并不稳定在THF中于室温。 </li><li>一天后，得到的 Li 2（12冠4）4锡10羟脯氨酸4（140毫克）的大块。使用单晶利用X射线晶体23的结构分析（ 图9）中的一个。 </li></ol></li></ol>

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Ed. 41, 3532-3554 (2002).</li><li>Ecker, A., Weckert, E., Schn&#246;ckel, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+structural+characterization+of+an+Al77+cluster.">Synthesis and structural characterization of an Al77 cluster.</a> Nature. 387, 379-381 (1997).</li><li>Schnepf, A., Schn&#246;ckel, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+structure+of+a+Ga84R204-+cluster-a+link+between+metalloid+clusters+and+fullerenes?.">Synthesis and structure of a Ga84R204- cluster-a link between metalloid clusters and fullerenes?.</a> Angew. Chem. Int. Ed. 40, 712-715 (2001).</li><li>Schrenk, C., K&#246;ppe, R., Schellenberg, I., P&#246;ttgen, R., Schnepf, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+tin(I)bromide.+A+novel+binary+halide+for+synthetic+chemistry.">Synthesis of tin(I)bromide. A novel binary halide for synthetic chemistry.</a> Z. Anorg. Allg. Chem. 635, 1541-1548 (2009).</li><li>Schnepf, A., K&#246;ppe, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthese+von+Germanium(I)bromid.+Ein+erster+Schritt+zu+neuen+Clusterverbindungen+des+Germaniums?.">Synthese von Germanium(I)bromid. Ein erster Schritt zu neuen Clusterverbindungen des Germaniums?.</a> Z. Anorg. Allg. Chem. 628, 2914-2918 (2002).</li><li>Uhlemann, F., K&#246;ppe, R., Schnepf, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+metastable+Si(II)X2solutions+(X+=+F,+Cl).+A+Novel+Binary+Halide+for+Synthesis.">Synthesis of metastable Si(II)X2solutions (X = F, Cl). A Novel Binary Halide for Synthesis.</a> Z. Anorg. Allg. Chem. 640, 1658-1664 (2014).</li><li>Schenk, C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Formal+Combination+of+Three+Singlet+Biradicaloid+Entities+to+a+Singlet+Hexaradicaloid+Metalloid+Ge14[Si(SiMe3)3]5Li3(THF)6Cluster.">The Formal Combination of Three Singlet Biradicaloid Entities to a Singlet Hexaradicaloid Metalloid Ge14[Si(SiMe3)3]5Li3(THF)6Cluster.</a> J. Am. Chem. Soc. 133, 2518-2524 (2011).</li><li>Schrenk, C., Schellenberg, I., P&#246;ttgen, R., Schnepf, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+formation+of+a+metalloid+Sn10[Si(SiMe3)3]6cluster+compound+and+its+relation+to+the+&#945;&#8596;&#946;+tin+phase+transition.">The formation of a metalloid Sn10[Si(SiMe3)3]6cluster compound and its relation to the &#945;&#8596;&#946; tin phase transition.</a> Dalton Trans. 39, 1872-1876 (2010).</li><li>Schrenk, C., Winter, F., P&#246;ttgen, R., Schnepf, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term={Sn10[Si(SiMe3)3]4}2-+:+A+high+reactive+metalloid+tin+cluster+with+an+open+ligand+shell+for+further+applications.">{Sn10[Si(SiMe3)3]4}2- : A high reactive metalloid tin cluster with an open ligand shell for further applications.</a> Chem. Eur. J. 21, 2992-2997 (2015).</li><li>Gutekunst, G., Brook, A. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tris(trimethylsilyl)silyllithium.3+THF:+a+stable+crystalline+silyllithium+reagent.">Tris(trimethylsilyl)silyllithium.3 THF: a stable crystalline silyllithium reagent.</a> J. Organomet. Chem. 225, 1-3 (1982).</li><li>Timms, P. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Techniques+of+Preparative+Cryochemistry.">Techniques of Preparative Cryochemistry.</a> Cryochemistry. , 61-136 (1976).</li><li>Schrenk, C., Gerke, B., P&#246;ttgen, R., Clayborne, A., Schnepf, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reactions+with+a+Metalloid+Tin+Cluster+{Sn10[Si(SiMe3)3]4}2-:+Ligand+Elimination+versus+Coordination+Chemistry.">Reactions with a Metalloid Tin Cluster {Sn10[Si(SiMe3)3]4}2-: Ligand Elimination versus Coordination Chemistry.</a> Chemistry. 21, 8222-8228 (2015).</li><li>Schnepf, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chemistry+Applying+Metalloid+Tin+Clusters.">Chemistry Applying Metalloid Tin Clusters.</a> Phosphorus, Sulfur and Silicon and the Related Elements. 191, 662-664 (2016).</li></ol>

The authors do not declare any conflicts of interest.

通过将制备共缩合技术（ 图1）25的基础上，分子新型材料，如得到SnBr。由于在温度，压力，金属，和反应性气体的高弹性，大量的各种高反应性物质的亚稳态溶液可以合成。例如，以这种方式已经获得的硅和锗的subhalides。然而，寻找合适的条件以获得用于进一步合成亚稳溶液是不平凡的，并且溶液通常必须在非常低的温度进行处理（ 例如，-78℃）。此外，该合成需?...

由于在纳米技术领域的最新进展，分子和固态之间的纳米级尺寸范围内变得越来越重要，并且各种研究工作1的焦点。研究与纳米级化合物是特别适用于金属或半金属的兴趣，如剧变小分子物质的转化过程中发生（ 例如，氧化物，卤化物:非导通; 例如， 三氯化铝，AUCL 3，GeO 2的等 ）到的通式Mn为R M金属簇2（N&gt; M; M =金属，如铝，金，锡等 ; R =配位体如SC 6 H 4 -COOH，-N（SIME 3）2， 等 ），到最终散装元素相（金属:导电;半金属:半导体; 例如，元素的Al，Au或Ge）的3。 一个明确的分子纳米级compou的合成第二是具有挑战性的，由于其性质稳。许多合成方法得到具有一定粒径分布4的金属纳米颗粒，这意味着不同大小的金属原子簇化合物的混合物。因此，要建立一个基础，纳米级材料的结构与性能的关系，合成方法必须制定明确的访问分子纳米级化合物。这些明确的分子化合物（在金属5，6，7的情况下金属簇，8）将在复杂性和看似简单的化学的基本原则，如溶解和金属9的形成线索。 访问各种金属的金属簇一种合成路线，从稳定前体的还原被还原形成金属簇，主要是在低产量（ 例如，准金属基14簇像锡15开始</suB&gt;（DippNSiMe 3）6（迪普= 2,6-的iPr 2 -C 6 H 3）10，铅10脯氨酸（Hyp）6脯氨酸（Hyp =硅（森3）3）11，或Ge 5（CH（SIME 3 2）2）4 12）。 此外，越来越多的硬币金属的金属团簇通过前体的一个俘获配体的存在，如减少合成 将[Ag 44（对MBA）30] 4 - （对- MBA =对-巯基苯甲酸）13和Au 102（对MBA）44 14。旁施加还原脱卤，Schnöckel 等的合成路线。通过将相应的元素的高反应性的亚稳单卤化物的歧化反应引入到金属基13簇的合成路线（ 例如，3AlCl→2AL + 三氯化铝）。 的合成所需的单卤化物经由制备型共缩合技术，其中在高温下，ALX和GAX的气相分子（X =氯，溴，I）的合成和随后捕获在冷冻溶剂的矩阵（ 图1由此进行）15。因此，该技术可以访问新试剂，开辟了道路化学新颖区域（ 例如，从亚稳态单卤化物开始，直径在纳米范围内像金属团簇[铝77（N（森3）2）20] 2 -或[镓84（N（森3）2）20 4 -可以得到）16，17。 通过歧化反应合成途径因此最有生产力的，导致团簇直径在纳米范围内。然而，这种合成路线是唯一可能的，如果亚稳subhalide是在手该disproportionates在低温（通常远低于0℃）。再次，在基14的情况下，需要单卤化物，如subvalent二卤化物MX 2（M =锗，锡，铅）过于稳定，在远高于100℃的温度下不相称。亚稳态组14一卤化物解决方案的综合通过制备共缩聚技术是可能的。然而，在高得多的温度相对于获得该组13单卤化物，这是容易获得的作为在1000℃的气相物种组14单卤化物。因此，SnBr在最高产量在1250℃18获得的，而GEBR 19，以及的SiCl 2 20，以甚至更高的温度下得到的，高达1600℃。的单卤化物被"困"经由制备型共缩合技术（ 图1），从而导致亚稳态单卤化物的解决方案。从这些亚稳的解决方案开始，我们最近能合成各种Ø˚F锗和锡，即[李（THF）2] 3 [葛14脯氨酸（Hyp）5]脯氨酸（Hyp =硅（森）3）21，锡10脯氨酸（Hyp）6 22，以及新颖的准金属基14簇化合物{ [李（[12]冠4）2]} 2 [锡10（羟脯氨酸）4] 23。在这里，我们提出了一个亚稳态锡（I）Cl溶液合成的自制合作冷凝装置内，并描述其与LiHyp反应给金属簇[10锡（羟脯氨酸）4] 2 - 1高产。

<table><tbody><tr><td>Tin, 99.999%</td><td>ABCR</td><td>AB122397</td><td></td></tr><tr><td>Hydrogen chloride N28, 99.8%</td><td>Air Liquide</td><td>P0820S10R0A001</td><td>Toxic</td></tr><tr><td>Toluene anhydrous, 99.8%</td><td>Sigma Aldrich</td><td>244511</td><td></td></tr><tr><td>Tri-n-butylphosphine, &amp;#62;93.5%</td><td>Sigma Aldrich</td><td>90827</td><td>Toxic</td></tr><tr><td>TMEDA, &amp;#62;99.5%</td><td>Sigma Aldrich</td><td>411019</td><td></td></tr><tr><td>12-crown-4</td><td>Sigma Aldrich</td><td>194905</td><td>Toxic</td></tr><tr><td>THF anhydrous, &amp;#62;99.9%</td><td>Sigma Aldrich</td><td>401757</td><td></td></tr><tr><td>Sodium, 99.95%</td><td>Sigma Aldrich</td><td>262715</td><td></td></tr><tr><td>Benzophenone, &amp;#62;99%</td><td>Sigma Aldrich</td><td>427551</td><td></td></tr><tr><td>Differential pressure manometer</td><td>MKS</td><td>MKS Baratron 223B</td><td></td></tr><tr><td>Mass flow controller&amp;nbsp;</td><td>Bronckhorst&amp;nbsp;</td><td>Low &amp;Delta;p flow mass flow controller</td><td></td></tr><tr><td>High frequency generator</td><td>Trumpf H&amp;uuml;ttinger</td><td>TruHeat MF 5020</td><td></td></tr><tr><td>NMR spectrometer</td><td>Bruker</td><td>Bruker DRX-250</td><td></td></tr><tr><td>Glovebox</td><td>GS Systemtechnik</td><td></td><td></td></tr><tr><td>Argon 5.0</td><td>Westfalen</td><td></td><td></td></tr><tr><td>Nitrogen 4.8</td><td>Westfalen</td><td></td><td></td></tr><tr><td>Graphite</td><td>SGL</td><td></td><td></td></tr><tr><td>Quartz glass tube</td><td>Gebr. Rettberg GmbH</td><td></td><td></td></tr><tr><td>Steel transferring cannula</td><td>Rohre Ketterer</td><td></td><td></td></tr><tr><td>Balance</td><td>Kern</td><td>Kern PFB200-3</td><td></td></tr><tr><td>Oil diffusion pump</td><td>Balzers</td><td>Balzers Diff900</td><td></td></tr><tr><td>Rotary vane pump</td><td>Balzers</td><td>Balzers QK100L4D</td><td></td></tr><tr><td>Pyrometer</td><td>Sensotherm</td><td>6285</td><td></td></tr><tr><td>Schlenk tubes with glassy stopcocks</td><td>Gebr. Rettberg GmbH</td><td>J.-Young-type valve with glassy stopcock</td><td></td></tr></tbody></table>

the synthesis of [sn10(si(sime3)3)4]2- using a metastable sn(i) halide solution synthesized via a co-condensation technique

良好表征金属锡簇，通过施加在空间位苛刻的配体的存在下，亚稳定的Sn（I）的卤化物的歧化合成的数目，在最近几年已经增加。亚锡（I）卤化物在通过制备共缩聚技术"外太空条件"的合成。由此，subhalide是在高温烘箱合成，约1300℃，并在通过元素锡的卤化氢气体（例如 HCl）的反应减压。所述subhalide（例如氯化亚锡）在-196℃下被捕获的惰性溶剂的基质内，如甲苯。固体基质加热至-78℃，使subhalide的亚稳态溶液。亚稳subhalide溶液是高度反应性的，但可存储在-78℃下几个星期。上加热该溶液到室温时，发生歧化反应，导致元素锡和相应的二卤化物。通过采用大体积配体与Si（SIME 3）3，中间金属原子簇化合物可以完成歧化元素锡之前捕获。因此，亚稳的Sn（I）Cl溶液与锂硅（森3）3的反应得到[锡10（硅（森3）3）4] 2 - 1以高收率。1为黑色晶体经由包括盐复分解，歧化，和较大的簇降解的复杂反应顺序形成。此外，1可通过各种方法，如NMR或单晶X-射线结构分析来分析。

在与制备共缩合技术缀合基质隔离技术的原理示出（ 图1），以及作为助冷凝装置（ 图2）和石墨反应器的设置（ 图3）。 图4和图5显示的照片共缩聚装置的组装。在图6中 ，用质量流量控制器的气体供给部件被示出。 图7示出了前不久钢容器固定在主凸缘关闭共缩合装置的主装置。到?...

Watch this Scientific Journal Video about The Synthesis of [Sn10SiSiMe334]2- Using a Metastable SnI Halide Solution Synthesized via a Co-condensation Technique at JoVE.com

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 ...

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Research

JoVE Journal

Chemistry

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

8.4K 次观看.  University of Tübingen. 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.

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

Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand

A simple and effective method for selective sulfate separation from aqueous solutions by crystallization with a bis-guanidinium ligand, 1,4-benzene-bis(iminoguanidinium) (BBIG), is demonstrated. The ligand is synthesized as the chloride salt (BBIG-Cl) by in situ imine condensation of terephthalaldehyde with aminoguanidinium chloride in water, followed by crystallization as the sulfate salt (BBIG-SO4). Alternatively, BBIG-Cl is synthesized ex situ in larger scale from ethanol. The sulfate separation ability of the BBIG ligand is demonstrated by selective and quantitative crystallization of sulfate from seawater. The ligand can be recycled by neutralization of BBIG-SO4 with aqueous NaOH and crystallization of the neutral bis-iminoguanidine, which can be converted back into BBIG-Cl with aqueous HCl and reused in another separation cycle. Finally, 35S-labeled sulfate and &#946; liquid scintillation counting are employed for monitoring the sulfate concentration in solution. Overall, this protocol will instruct the user in the necessary skills to synthesize a ligand, employ it in the selective crystallization of sulfate from aqueous solutions, and quantify the separation efficiency.

A protocol for in situ aqueous synthesis of a bis(iminoguanidinium) ligand and its utilization in selective separation of sulfate is presented.

分离硫酸选择性结晶用双 -  iminoguanidinium配体

A simple and effective method for selective sulfate separation from aqueous solutions by crystallization with a bis-guanidinium ligand, ...

科研

化学

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of Chalcogenidoplumbates(II or 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 glass ampules). Reduction of such phases by elemental alkaline metals in amines affords crystalline chalcogenidoplumbate(II) salts comprised of [PbTe3]2- or [Pb2Ch3]2- anions, depending upon which sequestering agent for the cations is present: crown ethers, like 18-crown-6, or cryptands, like [2.2.2]crypt. Reactions of solutions of such anions with transition-metal compounds yield (poly-)chalcogenide anions or transition-metal chalcogenide clusters, including one with a &#181;-PbSe ligand (i.e., the heaviest-known CO homolog).
In contrast, the solid-state synthesis of a phase of the nominal composition &#34;K2PbSe2&#34; by successive reactions of the elements and by the subsequent solvothermal treatment in amines yields the first non-oxide/halide inorganic lead(IV) compound: a salt of the ortho-selenidoplumbate(IV) anion [PbSe4]4-. This was unexpected due to the redox potentials of Pb(IV) and Se(-II). Such methods can further be applied to other elemental combinations, leading to the formation of solutions with binary [HgTe2]2- or [BiSe3]3- anions, or to large-scale syntheses of K2Hg2Se3 or K3BiSe3 via the solid-state route.
All compounds are characterized by single-crystal X-ray diffraction and elemental analysis; solutions of plumbate salts can be investigated by 205Pb and 77Se or 127Te NMR techniques. Quantum chemical calculations using density functional theory methods enable energy comparisons. They further allow for insights into the electronic configuration and thus, the bonding situation. Molecular Rh-containing Chevrel-type compounds were found to exhibit delocalized mixed valence, whereas similar telluridopalladate anions are electron-precise; the cluster with the &#181;-PbSe ligand is energetically favored over a hypothetical CO analog, in line with the unsuccessful attempt at its synthesis. The stability of formal Pb(IV) within the [PbSe4]4- anion is mainly due to a suitable stabilization within the crystal lattice.

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 ...

Atmospheric Pressure Fabrication of Large-Sized Single-Layer Rectangular SnSe Flakes

Tin selenide (SnSe) belongs to the family of layered metal chalcogenide materials with a buckled structure like phosphorene, and has shown potential for applications in two-dimensional nanoelectronics devices. Although many methods to synthesize SnSe nanocrystals have been developed, a simple way to fabricate large-sized single-layer SnSe flakes remains a great challenge. Herein, we show the experimental method to directly grow large-sized single-layer rectangular SnSe flakes on commonly used SiO2/Si insulating substrates using a straightforward two-step fabrication method in an atmospheric pressure quartz tube furnace system. The single-layer rectangular SnSe flakes with an average thickness of ~6.8 &#197; and lateral dimensions of about 30 &#181;m &#215; 50 &#181;m were fabricated by a combination of vapor transport deposition technique and nitrogen etching route. We characterized the morphology, microstructure, and electrical properties of the rectangular SnSe flakes and obtained excellent crystallinity and good electronic properties. This article about the two-step fabrication method can help researchers grow other similar two-dimensional, large-sized, single-layer materials using an atmospheric pressure system.

A protocol is presented demonstrating a two-step fabrication technique to grow large-sized single-layer rectangular shaped SnSe flakes on low-cost SiO2/Si dielectrics wafers in an atmospheric pressure quartz tube furnace system.

大型单层矩形 SnSe 片的常压制备

Tin selenide (SnSe) belongs to the family of layered metal chalcogenide materials with a buckled structure like phosphorene, and has shown potential for ...

工程学

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 Bimetallic Pt/Sn-based Nanoparticles in Ionic Liquids

We demonstrate a method for the synthesis of bimetallic nanoparticles consisting of Pt and Sn. A synthesis strategy is used in which the particular physico-chemical properties of ionic liquids (ILs) are exploited to control both nucleation and growth processes. The nanoparticles form colloidal sols of very high colloidal stability in the IL, which is particularly interesting in view of their use as quasi-homogeneous catalysts. Procedures for both nanoparticle extraction in conventional solvents and for nanoparticle precipitation are presented. The size, structure and composition of the synthesized nanocrystals are confirmed using inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray diffraction analysis (XRD) and transmission electron microscopy (TEM) with energy-dispersive X-ray spectroscopy (EDX). By this, we show that the nanocrystals are random-type alloy and of small (2-3 nm) size. The catalytic activity and selectivity in the hydrogenation of &#945;,&#946;-unsaturated aldehydes is tested in a semi-continuous batch-type reactor. In this context, the bimetallic Pt/Sn-based nanoparticles reveal a high selectivity towards the unsaturated alcohol.

A protocol for the synthesis of bimetallic nanoparticles in ionic liquids and the procedure of their catalytic testing in the selective hydrogenation of unsaturated aldehydes are described.

离子液体中双金属 Pt/锡基纳米粒子的合成

We demonstrate a method for the synthesis of bimetallic nanoparticles consisting of Pt and Sn. A synthesis strategy is used in which the particular ...

Imine Metathesis by Silica-Supported Catalysts Using the Methodology of Surface Organometallic Chemistry

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared according to the methodology developed by surface organometallic chemistry (SOMC). In this framework, catalytic cycles can be determined by isolating crucial intermediates. All air-sensitive materials are handled under inert atmosphere (using gloveboxes or a Schlenk line) or high vacuum lines (HVLs, &#60;10-5 mbar). The preparation of SiO2-700 (silica dehydroxylated at 700 &#176;C) and subsequent applications (the grafting of complexes and catalytic runs) requires the use of HVLs and double-Schlenk techniques. Several well-known characterization methods are used, such as Fourier-transform infrared spectroscopy (FTIR), elemental microanalysis, solid-state nuclear magnetic resonance spectroscopy (SSNMR), and state-of-the-art dynamic nuclear polarization surface enhanced NMR spectroscopy (DNP-SENS). FTIR and elemental microanalysis permit scientists to establish the grafting and its stoichiometry. 1H and 13C SSNMR allows the structural determination of the hydrocarbon ligands coordination sphere. DNP SENS is an emerging powerful technique in solid characterization for the detection of poorly sensitive nuclei (15N, in our case). SiO2-700 is treated with about one equivalent of the metal precursor compared to the amount of surface silanol (0.30 mmol&#183;g-1) in pentane at room temperature. Then, volatiles are removed, and the powder samples are dried under dynamic high vacuum to afford the desired materials [(&#8801;Si-O-)Hf(&#951;2&#960;-MeNCH2)(&#951;1-NMe2)(&#951;1-HNMe2)]. After a thermal treatment under high vacuum, the grafted complex is converted into metal imido silica complex [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)]. [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] effectively promotes the metathesis of imines, using the combination of two imine substrates, N-(4-phenylbenzylidene)benzylamine, or N-(4-fluorobenzylidene)-4-fluoroaniline, with N-benzylidenetert-butylamine as substrates. A significantly lower conversion is observed with the blank runs; thus, the presence of the imido group in [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is correlated to the catalytic performance.

A new group IV metal catalyst for imine metathesis is prepared by grafting amine metal complex onto dehydroxylated silica. Surface metal fragments are characterized using FT-IR, elemental microanalysis, and solid-state NMR spectroscopy. Further dynamic nuclear polarization surface enhanced NMR spectroscopy experiments complement the determination of the coordination sphere.

利用表面有机金属化学方法，利用硅支持的催化剂进行Imine金属分析

With this protocol, a well-defined singlesite silica-supported heterogeneous catalyst [(&#8801;Si-O-)Hf(=NMe)(&#951;1-NMe2)] is designed and prepared ...

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, ...

从固结 SnSe 颗粒生产 CdSe-SnSe 纳米复合材料

Solution&#45;Processed, Surface&#45;Engineered, Polycrystalline CdSe&#45;SnSe Exhibiting Low Thermal Conductivity

In recent years, solution processes have gained considerable traction as a cost-effective and scalable method to produce high-performance thermoelectric materials. The process entails a series of critical steps: synthesis, purification, thermal treatments, and consolidation, each playing a pivotal role in determining performance, stability, and reproducibility. We have noticed a need for more comprehensive details for each of the described steps in most published works. Recognizing the significance of detailed synthetic protocols, we describe here the approach used to synthesize and characterize one of the highest-performing polycrystalline p-type SnSe. In particular, we report the synthesis of SnSe particles in water and the subsequent surface treatment with CdSe molecular complexes that yields CdSe-SnSe nanocomposites upon consolidation. Moreover, the surface treatment inhibits grain growth through Zenner pinning of secondary phase CdSe nanoparticles and enhances defect formation at different length scales. The enhanced complexity in the CdSe-SnSe nanocomposite microstructure with respect to SnSe promotes phonon scattering and thereby significantly reduces the thermal conductivity. Such surface engineering provides opportunities in solution processing for introducing and controlling defects, making it possible to optimize the transport properties and attain a high thermoelectric figure of merit.

作者聚焦:使用纳米复合材料作为加工热电材料推进能源解决方案

CdSe-SnSe nanocomposites are produced by consolidating surface-engineered SnSe particles. A simple aqueous synthesis is employed to produce SnSe particles. Coating SnSe particles with CdSe molecular complexes allows for controlling grain size and increasing the number of defects present in the nanocomposite, thus lowering the thermal conductivity.

溶液处理、表面工程、多晶 CdSe-SnSe，具有低导热性

In recent years, solution processes have gained considerable traction as a cost-effective and scalable method to produce high-performance thermoelectric ...

的合成[锡

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分离硫酸选择性结晶用双 - iminoguanidinium配体

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

大型单层矩形 SnSe 片的常压制备

半导体回转金属硫框架结晶的硫醇构建块的合成

离子液体中双金属 Pt/锡基纳米粒子的合成

利用表面有机金属化学方法，利用硅支持的催化剂进行Imine金属分析

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

多位膦接头合成低价金属有机骨架的实验方法

溶液处理、表面工程、多晶 CdSe-SnSe，具有低导热性