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π-conjugated chromophore functionalized high-nuclearity titanium-oxo clusters containing structural unit of anatase for photocatalytic selective oxidation of sulfides

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Abstract

N-doping has significant influence in manipulating the properties of TiO2, and this has stimulated the development of N-donor-functionalized titanium-oxo clusters (TOCs) as molecular models to study the structure–property relationship. However, the structural type and photoresponsive application are still limited for such TOCs, especially regarding the high-nuclearity TOCs that contain structure unit of TiO2 for photocatalysis. Herein, we showed the synthesis of a series of high-nuclearity TOCs 1–3 compounds using π-conjugated 1,10-phenanthroline (phen) as chromophore and N-donor functional ligand. Compound 1 features cocrystal structure composed of one [Ti26]2+ and half [Ti22]2+, which renders it as the first cocrystallized TOC containing two positively charged species and phen-functionalized TOC showing the highest nuclearity up to 37 Ti centers. By adjusting the synthetic conditions, the individual {Ti22} and {Ti26} clusters can also be isolated as Compounds 2 and 3, respectively. The core structure of {Ti22} is mainly constructed from four lacunary {Ti4} derived from pentagonal {Ti(Ti)5} unit, while {Ti26} is built from four complete {Ti(Ti)5} unit. Notably, a {Ti8O14} structure unit of anatase TiO2 can be identified in {Ti26}. Based on the unique structural features and proper photophysical and photochemical properties of Compounds 1–3, they are applied for photocatalytic sulfoxidation. Owing to the presence of anatase structure unit in {Ti26} and the synergistic effect from {Ti22} and {Ti26}, the catalytic performance presents in the order of Compound 1 > Compound 3 > Compound 2. This work provides excellent models to understand the structure–property relationship from the perspective of cocrystallization and Ti–O binding model and will further promote the application of TOCs as functional catalysts for organic transformation.

Graphical abstract

摘要

氮掺杂对TiO2的性质调控有很重要的影响, 这也促进了以含氮配体修饰的钛氧簇(TOCs)作为分子模型研究其构效关系。然而, 对于此类TOCs的结构类型和光响应应用的报道非常有限, 尤其是将含有TiO2结构单元的高核TOCs用于光催化更是鲜有报道。本文以p-共轭1,10-邻菲啰啉作为生色团和含氮功能化配体构建得到了3例高核钛氧簇, 命名为化合物1-3。化合物1由1个[Ti26]2+和0.5个[Ti22]2+共晶构成, 是首例由两个阳离子型物种构成的共晶钛氧簇, 并且是邻菲啰啉修饰的钛氧簇中核数最高的。通过调控合成条件, {Ti22}、{Ti26}可以被独立合成出来, 即为化合物2和化合物3。化合物2的簇核结构由五边形{Ti(Ti)5}衍生的{Ti4}构建得到, 而化合物3则是由五边形{Ti(Ti)5}组装形成。更为重要的是, 从{Ti26}中可以分离出与锐钛矿型二氧化钛相同的构建单元{Ti8O14}。基于化合物1-3独特的结构及优异的光物理和光化学性质, 我们将其应用于硫醚的光催化氧化。基于光活性锐钛矿结构单元以及共晶组分间的协同作用, 化合物1显示出最佳催化性能, 其次是化合物3和化合物2。本工作从共结晶和Ti-O构建模式的角度为研究钛氧簇的构效关系提供了很好的分子模型, 并将进一步推动钛氧簇作为高效催化剂用于有机转化。

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Acknowledgements

This work was financially supported by the National Natural Science Foundation of China (Nos. 21901037, 21901038 and 92161111), the Program for Professor of Special Appointment (Eastern Scholar) at Shanghai Institutions of Higher Learning, the Fundamental Research Funds for the Central Universities (No. 2232019G-07) and the International Cooperation Fund of Science and Technology Commission of Shanghai Municipality (No. 21130750100). We also thank the staff from the BL17B1 beamline of the National Facility for Protein Science in Shanghai (NFPS) at Shanghai Synchrotron Radiation Facility, for assistance during data collection.

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Author notes

  1. Ling-Rong Liao, Dong-Chun Zheng and Pin-Xi Ou have contributed equally to this work.

Authors and Affiliations

  1. State Key Laboratory for Modification of Chemical Fibers and Polymer Materials & College of Materials Science and Engineering, Donghua University, Shanghai, 201620, China

    Ling-Rong Liao, Dong-Chun Zheng, Pin-Xi Ou & Qi Zheng

  2. State Key Laboratory for Modification of Chemical Fibers and Polymer Materials and College of Chemistry and Chemical Engineering, Donghua University, Shanghai, 201620, China

    Qi-Xin Zhao & Wei-Min Xuan

Authors
  1. Ling-Rong Liao
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  2. Dong-Chun Zheng
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  3. Pin-Xi Ou
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  4. Qi-Xin Zhao
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  5. Wei-Min Xuan
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  6. Qi Zheng
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Corresponding authors

Correspondence to Wei-Min Xuan or Qi Zheng.

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Liao, LR., Zheng, DC., Ou, PX. et al. π-conjugated chromophore functionalized high-nuclearity titanium-oxo clusters containing structural unit of anatase for photocatalytic selective oxidation of sulfides. Rare Met. 43, 1736–1746 (2024). https://doi.org/10.1007/s12598-023-02545-0

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  • DOI: https://doi.org/10.1007/s12598-023-02545-0

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