Name: preparation of sns cobalt(ii) pincer model complexes of liver alcohol dehydrogenase
Uploaded: 2020-03-19T13:00:00
Description: Watch this Scientific Journal Video about Preparation of SNS CobaltII Pincer Model Complexes of Liver Alcohol Dehydrogenase at JoVE.com

约翰·米奇尼科夫斯基获得以下项目的财政支助：康涅狄格州航天局空间赠款联盟（编号为P-1168），费尔菲尔德大学科学研究所，艺术与科学学院出版基金，费尔菲尔德大学教师暑期研究津贴，以及国家科学基金会-主要研究仪器计划（授予编号CHE-1827854），用于资金购买400兆赫NMR光谱仪。他还感谢特伦斯·吴（耶鲁大学）在获取电喷质谱方面给予的帮助。杰里·贾辛斯基承认国家科学基金会-主要研究仪器计划（授予编号CHE-1039027）用于购买X射线衍射仪的资金。希拉·博尼塔蒂布斯、埃米尔斯·阿尔曼扎、拉米·哈尔布赫和萨曼莎·齐格蒙特承认哈迪曼学者计划提供了他们的暑期研究津贴。

1. 合成氯（n33-S，S，N）-2，6-bis（N-isopropyl-N'-甲苯胺酮-2-硫酮）丙氨酸_钴（II）四氯钴酸盐[4]
<ol><li>要制备复合4，在100mL圆形底部烧瓶中加入0.121克（3.12 x 10-4 mol）2，6-bis（N-isopropyl-N'-甲苯甲酰胺）丙氨酸（C19H25N5S2）6至15 mL的醋酸酯。6接下来，在此解决方案中，添加0.0851克（3.58 x 10-4 mol）氯化钴（II）六甲?...

<ol>
	<li>Holm, R. H., Kennepohl, P., Solomon, E. I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+and+Functional+Aspects+of+Metal+Sites+in+Biology.">Structural and Functional Aspects of Metal Sites in Biology.</a> Chemical Reviews. 96 (7), 2239-2314 (1996).</li><li>Ibers, J. A., Holm, R. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modeling+coordination+sites+in+metallobiomolecules.">Modeling coordination sites in metallobiomolecules.</a> Science. 209 (4453), 223-235 (1980).</li><li>Kannan, K. 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A., 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=Copper(I)+SNS+Pincer+Complexes:+Impact+of+Ligand+Design+and+Solvent+Coordination+on+Conformer+Interconversion+from+Spectroscopic+and+Computational+Studies.">Copper(I) SNS Pincer Complexes: Impact of Ligand Design and Solvent Coordination on Conformer Interconversion from Spectroscopic and Computational Studies.</a> Inorganica Chimica Acta. 495, (2019).</li><li>. Web Elements Available from: <a target="_blank" href="https://www.webelements.com/zinc/atom_sizes.html">https://www.webelements.com/zinc/atom_sizes.html</a> (2019)</li><li>. Web Elements Available from: <a target="_blank" href="https://www.webelements.com/cobalt/atom_sizes.html">https://www.webelements.com/cobalt/atom_sizes.html</a> (2019)</li><li>Caballero, A., D&#237;ez-Barra, E., Jal&#243;n, F. A., Merino, S., Tejeda, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=1,1'-(pyridine-2,6-diyl)bis(3-benzyl-2,3-dihydro-1H-imidazol-2-ylidine),+a+new+multidentate+N-heterocyclic+bis-carbene+and+its+silver(I)+complex+derivative.">1,1'-(pyridine-2,6-diyl)bis(3-benzyl-2,3-dihydro-1H-imidazol-2-ylidine), a new multidentate N-heterocyclic bis-carbene and its silver(I) complex derivative.</a> Journal of Organometallic Chemistry. 617-618, 395-398 (2001).</li><li>Albrecht, M., van Koten, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Platinum+Group+Organometallics+Based+on+"Pincer"+Complexes:+Sensors,+Switches,+and+Catalysis.">Platinum Group Organometallics Based on "Pincer" Complexes: Sensors, Switches, and Catalysis.</a> Angewandte Chemie International Edition. 40 (20), 3750-3781 (2001).</li><li>Peris, E., Crabtree, R. 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D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Imidazole-2-Thiones:+Synthesis,+Structure,+Properties.">Imidazole-2-Thiones: Synthesis, Structure, Properties.</a> Sulfur Reports. 10 (4), 389 (1991).</li><li>Schneider, G., Eklund, H., Cedergren-Zeppezauer, E., Zeppezauer, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Crystal+structure+of+the+active+site+in+specifically+metal-depleted+and+cobalt+substituted+horse+liver+alcohol+dehydrogenase+derivatives.">Crystal structure of the active site in specifically metal-depleted and cobalt substituted horse liver alcohol dehydrogenase derivatives.</a> Proceedings of the National Academies of the Sciences of the United States of America. 80, 5289-5293 (1983).</li><li>Yang, L., Powell, D. R., Houser, R. 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复合体4和5的制备是方便的。关键步骤是将固体 CoCl2+6H2O 添加到包含相应配体前体的醋酸酯溶液中。在添加 CoCl2+6H2O 后，该解决方案在几秒钟内变为深绿色，形成复合4。加入 CoCl 2 +6H2O2后，该解决方案变为明亮的蓝色，形成复合5。为确保完全反应，溶液在回流上过夜。
要生长...

该方法的目的是制备LADH的小分子类似物，以进一步了解金属酶的催化活性。LADH是一种含共量结合域和含锌（II）金属催化域1的二聚基酶。LADH，在共同因子NADH的存在，可以减少酮和醛到各自的酒精衍生物2。在NAD+的存在下，LADH可以对酮和醛2的酒精氧化进行反向催化。LADH活性位点的晶体结构表明，其锌（II）金属中心与一个氮原子结合，由一个石氨酸侧链和两个硫原子提供，由两个半胱氨酸配体3提供。进一步研究表明，锌金属中心与一个阴唇水分子连接，导致金属中心周围出现伪四面体几何形状4。
我们之前已经报告和利用SNS针质配体前体，以及金属化的配体前体与ZnCl2形成Zn（II）复合体，其中包含三叉体配体前体5，6，7。6,75这些配体前体如图1所示。这些锌（II）复合物表现出对电子贫乏醛的化学测量还原活性，因此是LADH的模型复合物。随后，对一系列含有SNS配体前体的铜（I）和铜（II）复合体的合成和表征报告为8、9、10。,9,10
虽然LADH是一种锌（II）酶，但我们有兴趣制备LADH的钴（II）模型复合物，以便获得有关LADH钴（II）模拟物的更多光谱信息。钴（II）复合体为彩色，而锌（II）复合体为白色。由于钴（II）复合物是彩色的，因此可以获取复合物的紫外线可见光谱，从而还可以收集钴（II）复合物中配体场强度的信息。利用高斯计算资料和实验获得的紫紫可见光谱，可以推断出配体场强度的信息。钴（II）是锌（II）的良好替代品，因为两个离子具有相似的离子半径和类似的刘易斯酸度11，12。11,
该方法涉及对模型复合物进行合成和特征化，试图模仿LADH55、66的自然催化行为。此前，我们曾用ZnCl2对一系列配体前体进行金属化，形成LADH的锌（II）模型复合物，对LADH4中锌活性位点的结构及反应进行建模。通过多次实验，这些针脚配体已被证明在不同的环境条件下是健壮的，并且通过各种附加R组来保持稳定。5，6
三联配体比单体配体更可取，因为由于三叉体配体的强切酸作用，它们在金属化方面更为成功。这种观察是由于与单体配体13相比，三叉针配体形成更受青睐的熵。此外，三叉针固定体可能防止金属复合物的二化，这是值得青睐的，因为二氧化二化可能会减缓复合14的催化活性。因此，在制备催化活性强复合物方面，使用三叉针固定体配体已被证明在有机金属化学方面是成功的。SNS针尖复合物的研究比其他针尖系统少，因为针刺复合体通常包含第二排和第三排过渡金属15。
这种对金属酶的研究有助于进一步了解它们的酶活性，这可应用于生物学的其他领域。与替代方法（合成LADH的整个蛋白质）相比，这种合成模型复合物的方法有很多原因。第一个优点是模型复合物的分子质量低，仍然能够准确表示天然酶活性位点的催化活性和环境条件。其次，模型复合体更易于使用和生成可靠且可比较的数据。
本稿描述了LADH两个钴（II）针脚模型复合物的合成制备和表征。这两种复合物均具有含有硫、氮和硫供体原子的针质配体。第一个复合体 （4） 基于一种乙酰氨基酮前体，第二个 （5） 基于三甲酮前体。这些复合物显示了在氢体捐赠者存在的情况下减少电子贫乏醛的气动性反应。这些反应结果将在后续手稿中报告。

<table>
	<tbody>
		<tr>
			<td>100 mL Round Bottomed Flask</td>
			<td>Chem Glass</td>
			<td>CG150691</td>
			<td>100mL Single Neck Round Bottomed Flask, 19/22 Outer Joint</td>
		</tr>
		<tr>
			<td>Acetonitrile</td>
			<td>Fisher</td>
			<td>HB9823-4</td>
			<td>HPLC Grade</td>
		</tr>
		<tr>
			<td>Chiller for roto-vap</td>
			<td>Lauda</td>
			<td>L000638</td>
			<td>Alpha RA 8</td>
		</tr>
		<tr>
			<td>Cobalt Chloride hexahydrate</td>
			<td>Acros Organics</td>
			<td>AC423571000</td>
			<td>Acros Organics</td>
		</tr>
		<tr>
			<td>Diethyl Ether</td>
			<td>Fisher</td>
			<td>E-138-1</td>
			<td>Diethyl Ether Anhydorus</td>
		</tr>
		<tr>
			<td>graduated cylinder</td>
			<td>Fisher</td>
			<td>S63456</td>
			<td>25 mL graduated cylinder</td>
		</tr>
		<tr>
			<td>hotplate</td>
			<td>Fisher</td>
			<td>11-100-49SH</td>
			<td>Isotemp Basic Stirring Hotplate</td>
		</tr>
		<tr>
			<td>jars</td>
			<td>Fisher</td>
			<td>05-719-481</td>
			<td>250 mL jars</td>
		</tr>
		<tr>
			<td>Ligand</td>
			<td>-----</td>
			<td>-----</td>
			<td>Synthezied previously by Professor Miecznikowski</td>
		</tr>
		<tr>
			<td>medium cotton balls</td>
			<td>Fisher</td>
			<td>22-456-80</td>
			<td>medium cotton balls</td>
		</tr>
		<tr>
			<td>one dram vials</td>
			<td>Fisher</td>
			<td>03-339</td>
			<td>one dram vials with TFE Lined Cap</td>
		</tr>
		<tr>
			<td>pipet</td>
			<td>Fisher</td>
			<td>13-678-20B</td>
			<td>5.75 inch pipets</td>
		</tr>
		<tr>
			<td>pipet bulbs</td>
			<td>Fisher</td>
			<td>03-448-21</td>
			<td>Fisher Brand Latex Bulb for pipet</td>
		</tr>
		<tr>
			<td>recrystallizing dish for sand bath</td>
			<td>Fisher</td>
			<td>08-741 D</td>
			<td>325 mL recrystallizing dish for sand bath</td>
		</tr>
		<tr>
			<td>reflux condensor</td>
			<td>Chem Glass</td>
			<td>CG-1218-A-22</td>
			<td>Condenser with 19/22 inner joint</td>
		</tr>
		<tr>
			<td>Rotovap</td>
			<td>Heidolph Collegiate</td>
			<td>36000090</td>
			<td>Brinkmann; Heidolph Collegiate Rotary Evaporator with Heidolph WB eco bath Heidolph Rotary Evaporator</td>
		</tr>
		<tr>
			<td>sea sand for sandbath</td>
			<td>Acros Organics</td>
			<td>612355000</td>
			<td>washed sea sand for sand bath</td>
		</tr>
		<tr>
			<td>Stir bar</td>
			<td>Fisher</td>
			<td>07-910-23</td>
			<td>Egg-Shaped Magnetic Stir Bar</td>
		</tr>
		<tr>
			<td>Vacum grease</td>
			<td>Fisher</td>
			<td>14-635-5D</td>
			<td>Dow Corning High Vacuum Grease</td>
		</tr>
		<tr>
			<td>vacuum pump for rotovap</td>
			<td>Heidolph Collegiate</td>
			<td>36302830</td>
			<td>Heidolph Rotovac Valve Control</td>
		</tr>
	</tbody>
</table>

preparation of sns cobalt(ii) pincer model complexes of liver alcohol dehydrogenase

化学模型复合物准备代表酶的活性位点。在此协议中，一系列三叉针粘结剂配体前体（每个具有两硫和一个氮体供体原子功能 （SNS）， 并基于二乙二氮-乙酰氨基酮或二分三氮化合物） 用 CoCl2[6H2O] 金属化，以提供三叉星 SNS 针质钴 （II） 复合物。制备肝酒精脱氢酶的钴（II）模型复合物是容易的。基于将 CoCl2+6H2O 添加到含有配体前体的醋酸酯溶液时的快速颜色变化，复杂形状迅速。金属复合物的形成在允许溶液通宵回流后完成。这些钴（II）复合物作为肝酒精脱氢酶（LADH）中锌活性位点的模型。该复合物采用单晶X射线衍射、电喷质谱、紫外线可见光谱和元素分析进行特征分析。为了准确确定复合物的结构，必须确定其单晶结构。然后，通过二甲醚的缓慢蒸汽扩散，将适合X射线衍射的复合物的单晶体生长成含有钴（II）复合物的醋酸酯溶液。对于高品质的晶体，重新结晶通常发生在 1 周或更长时间内。该方法可应用于其他模型协调复合物的制备，并可用于本科教学实验室。最后，相信其他人可能会发现这种再结晶方法，以获得单晶有利于他们的研究。

合成 复合物4和5的合成通过反应含有二氧二体二体体素的前体与钴（II）氯化物六氧水合物（图2）的乙酰二醇溶液得以成功实施。这种反应发生在空气的回流温度下。一般来说，复合物4和5被观察到可溶于乙酰甲酸酯、二甲基亚硫酸盐、二氯甲烷和甲醇。复合4的颜色为绿色，复合5为?...

Watch this Scientific Journal Video about Preparation of SNS CobaltII Pincer Model Complexes of Liver Alcohol Dehydrogenase at JoVE.com

Preparation of SNS CobaltII Pincer Model Complexes of Liver Alcohol Dehydrogenase

介绍了肝酒精脱氢酶SNS针质钴（II）模型复合物的制备情况。复合物可以通过用CoCl2+6H2O对配体前体进行反应来制备，然后通过允许二苯醚缓慢扩散到含有钴复合物的醋酸酯溶液中来重新结晶。

制备SNS钴（II）针质模型复合物肝酒精脱氢酶

Chemical model complexes are prepared to represent the active site of an enzyme. In this protocol, a family of tridentate pincer ligand precursors (each ...

该方法可用于准备一种酶肝醇脱氢酶的化学模型复合物，并生长单晶。该技术的优点是复杂地层是简单的，再结晶法可以应用于其他协调复合物的制备。该方法可对无机协调化合物的制备和再结晶提供见解，并可应用于任何感兴趣的化合物中，以生长单晶。种植单晶需要实践。关键是使含有金属复合物的乙酰三叶酸溶液尽可能浓缩。要准备复合物四，将0.121克2、6-BIS-N-异丙基-N'甲基苯二甲酸酯-2-硫酮-丙胺和0.0851克钴二氯化六水合物加入含有15毫升乙酰乙酰三酯的100毫升圆形底瓶中。添加钴二氯化物六水合物后，反应应立即从浅黄色更改为祖母绿。然后回流并搅拌反应20小时，以确保完全反应，然后在压力下使用轮盘去除溶剂。对于氯-N3-S、S、N-2、6-BIS-N-异丙基-N'甲基苯二甲酸酯-2-硫化-丙烯酸酯II二四氯钴酸盐通过缓慢蒸汽扩散再结晶，将溶质溶解在10毫升乙酰胺中，将溶液化，然后在一个 dram 小瓶之间均匀地溶解溶液。在每个小瓶中加入1.5毫升的新鲜乙酰酸虫溶液，用棉花紧贴小瓶。将小瓶放在一个240毫升的罐子里，里面装着50毫升的二乙醚，然后用盖子把罐子关上。然后让晶体生长长达一周。要准备复合物五，在100毫升圆形底瓶中加入0.183克2、6-BIS-N-异丙基-N'甲基三甲苯胺-2-硫酮-丙胺和0.223克钴二氯化二氯化六氢水合物至15毫升乙酰酸盐。添加钴二氯化物六水合物后，反应应立即从浅黄色更改为皇家蓝色。然后回流并搅拌反应20小时，以确保完全的反应，然后使用在压力下的旋转剂去除溶剂。对于氯-N3-S、S、N-2、6-BIS-N-异丙基-N'甲基二甲酸酯-2-硫化-丙烯酸酯II二四氯钴酸盐通过缓慢蒸汽扩散再结晶，将溶质溶解在10毫升乙酰酸盐中，并在溶液均匀化后过滤溶液。将每瓶填充1.5毫升的醋酸石溶液，并用棉花紧贴小瓶。要种植高质量的单晶，棉质插头必须紧贴在一个 dram 小瓶内。我们用不到一个棉球每瓶。然后将小瓶放在一个装有50毫升二乙醚的罐子里，用帽子盖住罐子，让晶体长一个星期。复合物四和五的合成可以通过与钴二氯化物六水合物反应含有双硫体配体前体，成功地进行。通过慢蒸汽扩散获得四和五复合物的单晶是生长难以结晶样品的单晶的极好方法。对再结晶复合物进行元素分析表明，复合物4和5是纯的，因为计算出的碳、氢和氮的百分比与发现的碳、氢和氮的百分比非常一致。此外，四、五综合体的紫外可见光谱显示，复合物四个在可见区域呈现出680、632和589纳米的三个峰，而复数五的光谱显示可见区域的四个峰在682、613、588和573纳米。最重要的是要记住的是，当您准备复合物时，您必须在含有配体前体的乙酮三酯溶液中加入氯化钴六水合物。再结晶法可应用于任何难以再结晶的有机或无机化合物。我们目前正在准备在反年对中不含钴的钴II复合物，并筛选复合物的活性。请务必在烟罩中执行所有反应。

Research

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JoVE Journal

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Chemistry

Preparation of SNS Cobalt(II) Pincer Model Complexes of Liver Alcohol Dehydrogenase

Transition Metals and Coordination Complexes

SCIENTISTS IN ACTION

Production of Disulfide-stabilized Transmembrane Peptide Complexes for Structural Studies

生产二硫键稳定的跨膜肽复合物的结构研究

Physical  interactions among the lipid-embedded alpha-helical domains of membrane  proteins play a crucial role in folding and assembly of membrane ...

科研

化学

Structure and Coordination Determination of Peptide-metal Complexes Using 1D and 2D 1H NMR

Structure and Coordination Determination of Peptide-metal Complexes Using 1D and 2D 1H NMR

Copper (I) binding by metallochaperone transport proteins prevents copper oxidation and release of the toxic ions that may participate in harmful redox ...

Anticancer Metal Complexes: Synthesis and Cytotoxicity Evaluation by the MTT Assay

抗癌金属配合物的合成与细胞毒性评价MTT法

Titanium (IV) and vanadium (V) complexes are highly potent anticancer agents. A challenge in their synthesis refers to their hydrolytic instability; ...

The Use of Gas Chromatography to Analyze Compositional Changes of Fatty Acids in Rat Liver Tissue during Pregnancy

使用气相色谱怀孕期间分析脂肪酸组成的变化在大鼠肝组织

Gas chromatography (GC) is a highly sensitive method used to identify and quantify the fatty acid content of lipids from tissues, cells, and plasma/serum, ...

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 ...

Preparation of Carbon Nanosheets at Room Temperature

碳纳米片在室温下准备

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into ...

Facile Preparation of 4-Substituted Quinazoline Derivatives

的4-取代喹唑啉衍生物简便制备

Reported in this paper is a very simple method for direct preparation of 4-substituted quinazoline derivatives from a reaction between substituted ...

Preparation of Biopolymer Aerogels Using Green Solvents

生物聚合物气凝胶制备使用绿色溶剂

Although the first reports on aerogels made by Kistler1 in the 1930s dealt with aerogels from both inorganic oxides (silica and others) and biopolymers ...

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

Controlled Photoredox Ring-Opening Polymerization of O-Carboxyanhydrides Mediated by Ni/Zn Complexes

镍/锌配合物介导的O-Carboxyanhydrides 的控制 Photoredox 环开聚合

Here, we describe an effective protocol that combines photoredox Ni/Ir catalysis with the use of a Zn-alkoxide for efficient ring-opening polymerization, ...

Microfluidic Preparation of Liquid Crystalline Elastomer Actuators

液晶弹性体致动器的微流控制备

This paper focuses on the microfluidic process (and its parameters) to prepare actuating particles from liquid crystalline elastomers. The preparation ...