Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds: In Situ Ligand Synthesis versus Direct Assembly

Rowland CE; Belai N; Knope KE; Cahill CL

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Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds: In Situ Ligand Synthesis versus Direct Assembly

机译：含二硫键的铀酰化合物的水热合成：原位配体合成与直接组装

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Three disulfide-containing uranyl compounds, [UO2(C7H4O2S)(3)]center dot H2O (1), [UO2(C7H4O2S)(2)(C7H5O2S)] (2), and [UO2(C7H4O2S)(4)] (3) have been hydrothermally synthesized. Both in situ disulfide bond formation from 3- and 4-mercaptobenzoic acid (C7H5O2S, MBA) to yield 3,3'- and 4,4'-dithiobisbenzoic acid (C14H8O4S2, DTBA) and direct assembly with the presynthesized dimeric ligands have been explored. While the starting materials 4-MBA and 4,4'-DTBA both yield 2 via in situ ligand synthesis and direct assembly, respectively, we observe the formation of I from the starting material 3-MBA via in situ ligand synthesis and of 3 from the direct assembly of the uranyl cation with 3,3'-DTBA. Concurrently with the synthesis of I and 2, we have observed the in situ formation of the crystalline dimeric organic species, 3,3'-DTBA, [(C7H5O2S)(2)] (4) and 4,4'-DTBA, [(C7H5O2S)(2)] (5). Herein we report the synthesis and crystallographic characterization of 1-5, as well as observations regarding the utility of product formation via direct assembly and in situ ligand synthesis.

机译：三种含二硫键的铀酰化合物[UO2（C7H4O2S）（3）]中心点H2O（1），[UO2（C7H4O2S）（2）（C7H5O2S）]（2）和[UO2（C7H4O2S）（4）] [ 3）已经水热合成。已经研究了由3-和4-巯基苯甲酸（C7H5O2S，MBA）在原位形成二硫键以生成3,3'-和4,4'-二硫代双苯甲酸（C14H8O4S2，DTBA）以及与预先合成的二聚配体直接组装的方法。虽然原料4-MBA和4,4'-DTBA都分别通过原位配体合成和直接组装获得2，但我们观察到原料3-MBA通过原位配体合成形成I，而从原料3-MBA通过原位配体合成形成3。铀酰阳离子与3,3'-DTBA的直接组装。在合成I和2的同时，我们观察到了原位形成的结晶二聚有机物3,3'-DTBA，[（C7H5O2S）（2）]（4）和4,4'-DTBA，[ （C7H5O2S）（2）]（5）。在本文中，我们报道了1-5的合成和晶体学表征，以及有关通过直接组装和原位配体合成形成产品的效用的观察结果。

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《Crystal growth & design》 |2010年第3期|共9页
作者
Rowland CE; Belai N; Knope KE; Cahill CL;
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正文语种 eng
中图分类晶体学;
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Hydrothermal; Synthesis; Disulfide-Containing Uranyl Compounds;

机译：水热合成二硫化铀酰化合物;

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1. Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds: In Situ Ligand Synthesis versus Direct Assembly [J] . Rowland CE, Belai N, Knope KE, Crystal growth & design . 2010,第3期

机译：含二硫键的铀酰化合物的水热合成：原位配体合成与直接组装
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4. Metal-Controlled Assembly of Uranyl Diphosphonates towards the Synthesis of Functional Materials [C] . Yilin Wang, Kariem Diefenbach, Thomas Albrecht-Schmitt Plutonium futures: the science 2014 . 2014

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5. Three Assembly Modes of Hydrothermally Synthesized Inorganic Organic Hybrid Materials: Direct Metal-Ligand Coordination, Supramolecular Chemistry, and in situ Ligand Synthesis. [D] . Cantos, Paula M. 2014

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6. NN′N′′ versus NN′O imine-containing coordination motifs: ligand-directed synthesis of mononuclear and binuclear CuII compounds [O] . Raphael Enoque Ferraz de Paiva, Douglas Hideki Nakahata, Marcos Alberto de Carvalho, 2017

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Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds: In Situ Ligand Synthesis versus Direct Assembly

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