Time-controlled synthesis of the 3D coordination polymer U(1,2,3-Hbtc)2 followed by the formation of molecular poly-oxo cluster {U14} containing hemimellitate uranium(iv)

Maxime Dufaye; Nicolas P. Martin; Sylvain Duval; Christophe Volkringer; Atsushi Ikeda-Ohno; Thierry Loiseau

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Time-controlled synthesis of the 3D coordination polymer U(1,2,3-Hbtc)2 followed by the formation of molecular poly-oxo cluster {U14} containing hemimellitate uranium(iv)

机译：3D配位聚合物U（1,2,3-HBTC）2的时间控制合成，然后形成含有Hemimellite铀（IV）的分子聚氧代簇{U14}

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Two coordination compounds bearing tetravalent uranium were synthesized in the presence of tritopic hemimellitic acid in acetonitrile with a controlled amount of water (H _(2) O/U ≈ 8) and structurally characterized. Compound 1 , [U(1,2,3-Hbtc) _(2) ]·0.5CH _(3) CN is constructed around an eight-fold coordinated uranium cationic unit [UO _(8) ] linked by the poly-carboxylate ligands to form dimeric subunits, which are further connected to form infinite corrugated ribbons and a three-dimensional framework. Compound 2 , [U _(14) O _(8) (OH) _(4) Cl _(8) (H _(2) O) _(16) (1,2,3-Hbtc) _(8) (ox) _(4) (ac) _(4) ] ({U _(14) }) exhibits an unprecedented polynuclear {U _(14) } poly-oxo uranium cluster surrounded by O-donor and chloride ligands. It is based on a central core of [U _(6) O _(8) ] type surrounded by four dinuclear uranium-subunits {U _(2) }. Compound 1 was synthesized by a direct reaction of hemimellitic acid with uranium tetrachloride in acetonitrile (+H _(2) O), while the molecular species ({U _(14) } ( 2 )) crystallized from the supernatant solution after one month. The slow hydrolysis reaction together with the partial decomposition of the starting organic reactants into oxalate and acetate molecules induces the generation of such a large poly-oxo cluster with fourteen uranium centers. Structural comparisons with other closely related uranium-containing clusters, such as the {U _(12) } cluster based on the association of inner core [U _(6) O _(8) ] with three dinuclear sub-units {U _(2) }, were performed.

机译：携带四价铀的两种配位化合物在乙腈中的氚化学氧化酸存在下合成，具有受控量的水（H _（2）O /U≈8）和结构表征。化合物1，[u（1,2,3-HBTC）_（2）]·0.5CH _（3）CN由聚 - 连接的八倍的协调铀阳离子单元[UO _（8）]构建。羧酸盐配体形成二聚体亚基，其进一步连接以形成无限瓦楞丝带和三维框架。化合物2，[u _（14）O _（8）（OH）_（4）CL _（8）（H _（2）o）_（16）（1,2,3-HBTC）_（8 ）（OX）_（4）（AC）_（4）]（{u _（14）}）表现出由O-供体和氯配体包围的前所未有的多核{U _（14）}聚氧代铀簇。它基于[U _（6）o _（8）]类型的核心核心，由四个核心utanium-sub单元包围{u _（2）}。通过在乙腈（+ H _（2）O）中与四氯化铀的直接反应合成化合物1，而分子物种（{U _（14）}（2））在一个月后从上清液溶液中结晶。慢水解反应与原始有机反应物中的部分分解成草酸和乙酸盐分子，诱导与十四个铀中心的这种大型聚氧代群的产生。与其他密切相关的含铀集群的结构比较，例如基于内核的关联[u _（6）o _（8）]的{u _（12）}群），具有三个二核子单元{u _ （2）}进行。

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《RSC Advances》 |2019年第40期|共10页
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Maxime Dufaye; Nicolas P. Martin; Sylvain Duval; Christophe Volkringer; Atsushi Ikeda-Ohno; Thierry Loiseau;
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1. Time-controlled synthesis of the 3D coordination polymer U(1,2,3-Hbtc)(2) followed by the formation of molecular poly-oxo cluster {U-14} containing hemimellitate uranium(iv) [J] . Dufaye Maxime, Martin Nicolas P., Duval Sylvain, RSC Advances . 2019,第40期

机译：3D配位聚合物U（1,2,3-HBTC）（2）的时间控制合成，然后形成含有Hemimellite铀（IV）的分子聚烯烃簇{U-14}
2. Formation of a new type of uranium(iv) poly-oxo cluster {U38} based on a controlled release of water via esterification reaction [J] . Nicolas P. Martin, Christophe Volkringer, Natacha Henry, Chemical science . 2018,第22期

机译：通过酯化反应控制水的释放形成新型铀（iv）多氧代簇{U38}
3. 3D supramolecular array assembled by cross-like arrangement of 1D sandwich mixed molybdenum-vanadium polyoxometalate bridged coordination polymer chains: Hydrothermal synthesis and crystal structure of {[(Mo5Mo3V8O40)-Mo-VI-V-V-O-IV(PO4)][Ni(en)(2)]} [J] . Liu CM, Zhang DQ, Zhu DB Crystal growth & design . 2005,第4期

机译：一维夹层混合钼-钒-多金属氧酸盐桥联的配位聚合物链的交叉样排列组装的3D超分子阵列：{[（（Mo5Mo3V8O40）-Mo-VI-VVO-IV（PO4）] [Ni（en）的水热合成和晶体结构（2）]}
4. Synthesis and Crystal Structure of a Novel 3D Sm(lll) Coordination Polymer with Mixed Ligands [C] . Shu-ju Wang, Yan-wen Tian, Li-xin You International Conference on Advanced Engineering Materials and Technology . 2013

机译：用混合配体的新型3D SM（LLL）配位聚合物的合成与晶体结构
5. Octahedral metal clusters as molecular building blocks of coordination polymers: Synthesis, characterization, and study of their host-guest interactions. [D] . Chen, Lei. 2011

机译：八面体金属簇作为配位聚合物的分子构建基块：合成，表征和研究其主客体相互作用。
6. Formation of a new type of uranium(iv) poly-oxo cluster {U38} based on a controlled release of water via esterification reaction [O] . Nicolas P. Martin, Christophe Volkringer, Natacha Henry, 2018

机译：通过酯化反应控制水的释放形成新型铀（iv）多氧代簇{U38}
7. Time-controlled synthesis of the 3D coordination polymer U(1,2,3-Hbtc)2 followed by the formation of molecular poly-oxo cluster {U14} containing hemimellitate uranium(iv) [O] . Maxime Dufaye, Nicolas P. Martin, Sylvain Duval, 2019

机译：3D配位聚合物U（1,2,3-HBTC）2的时间控制合成，然后形成含有Hemimellite铀（IV）的分子聚氧代簇{U14}
8. Dioxouranium(VI) Dicarboxylate Polymers: Synthesis and Characterization of Tractable Coordination Polymers and Evidence for Rigid Rod Confirmation [R] . Hardiman, C. J., Archer, R. D. 1987

机译：二氧脲（VI）二羧酸酯聚合物：可转导配位聚合物的合成和表征以及刚性棒确认的证据

Time-controlled synthesis of the 3D coordination polymer U(1,2,3-Hbtc)2 followed by the formation of molecular poly-oxo cluster {U14} containing hemimellitate uranium(iv)

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