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However, the stability of the adjacent ligands in alkaline environments and their influence on energy storage behavior remain inadequately understood. In this study, two nickel\u2010based MHOFs, namely NiHOF\u2010BPDC and NiHOF\u2010NDC, have been prepared using electron\u2010withdrawing 4,4\u2032\u2010biphenyldicarboxylic acid (BPDC) and 2,6\u2010naphthalenedicarboxylic acid (NDC) as building linkers. The impact of the ligand chain length on the structural development and electrochemical performance of the materials was comprehensively investigated. The results revealed that the longer BPDC ligand constructs a more open confined space within the layered framework, manifested as enlarged interlayer spacing and increased accessible surface area, thereby significantly enhancing its charge\u2010storage capacity. In contrast, the shorter NDC ligand resulted in a denser stacked framework, which improved the cycling stability. In situ Raman spectroscopy and X\u2010ray photoelectron spectroscopy (XPS) analyses demonstrated that the Ni\u2500O\/Ni\u2500OH coordination environment undergoes reversible changes during the electrochemical process, and that the linker\u2010layer created \u201cconfined space\u201d is crucial for maintaining the stability and cycling reversibility of the material.<\/jats:p>","DOI":"10.1002\/smll.73318","type":"journal-article","created":{"date-parts":[[2026,4,6]],"date-time":"2026-04-06T03:24:08Z","timestamp":1775445848000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Ligand\u2010Engineered Confined Spaces of Nickel Hydroxide\u2013Organic Frameworks Boost Their Electrochemical Performance in Alkaline Condition"],"prefix":"10.1002","volume":"22","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-1807-9661","authenticated-orcid":false,"given":"Kuaibing","family":"Wang","sequence":"first","affiliation":[{"name":"Jiangsu Key Laboratory of Zero\u2010Carbon Energy Development and System Integration Key Laboratory of Advanced Functional Materials of Nanjing School of Environmental Science Nanjing Xiaozhuang University  Nanjing P. 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