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Herein, we report a ternary core\u2013shell heterostructure, Cu\/Cu2O\/CuVO3@MOF(Cu-His-BDC)(CCVO@@MOF(Cu-His-BDC)), constructed via an in situ dual-ligand coordination strategy using histidine and terephthalic acid. This dual-ligand architecture enriches surface oxygen vacancies (33.86% \u2192 59.87%) and reshuffles valence equilibria (V4+: 10.75% \u2192 29.21%; Cu+: +10.21%), while creating a hierarchical porous network. Spectroscopic and electrochemical characterizations reveal that the enhanced oxidase-like activity stems from coupled ROS generation and interfacial electron transfer. Interestingly, Cr(VI) acts as a bifunctional regulator, triggering metal valence cycling (Cu+\/V4+ \u21cc Cu2+\/V5+) to amplify colorimetric signals while suppressing electrochemical responses. Leveraging this orthogonal promotion\u2013inhibition effect, a dual-mode platform covering pM to \u03bcM ranges is established with recoveries of 94\u2013107% in complex matrices. Combined with EDTA masking and alkaline persulfate oxidation, the platform enables reliable Cr(VI)\/Cr(III) speciation, validated by ICP-MS, while smartphone-based RGB readout offers field-deployable capability. This work establishes a design paradigm for intelligent nanozymes through synergistic ligand and defect modulation.<\/jats:p>","DOI":"10.1021\/acs.inorgchem.6c03375","type":"journal-article","created":{"date-parts":[[2026,8,31]],"date-time":"2026-08-31T15:44:19Z","timestamp":1788191059000},"page":"20613-20630","source":"Crossref","is-referenced-by-count":0,"title":["Ligand Synergy\nEnhances Oxygen Vacancies: A Heterostructured\nNanozyme for Ultra-Sensitive Dual-Mode Cr(VI) Speciation"],"prefix":"10.1021","volume":"65","author":[{"ORCID":"https:\/\/orcid.org\/0009-0001-8956-5002","authenticated-orcid":true,"given":"Yanhui","family":"Feng","sequence":"first","affiliation":[{"name":"Minnan Normal University , , ,","place":["Zhangzhou, China, 363000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Linghong","family":"Han","sequence":"additional","affiliation":[{"name":"Minnan Normal University , , ,","place":["Zhangzhou, China, 363000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"An","family":"Xu","sequence":"additional","affiliation":[{"name":"Minnan Normal University , , ,","place":["Zhangzhou, China, 363000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xueying","family":"Liang","sequence":"additional","affiliation":[{"name":"Minnan Normal University , , ,","place":["Zhangzhou, China, 363000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6843-2841","authenticated-orcid":true,"given":"Xiumei","family":"Lin","sequence":"additional","affiliation":[{"name":"Minnan Normal University , , ,","place":["Zhangzhou, China, 363000"]},{"name":"Minnan Normal University , , ,","place":["Zhangzhou, China, 363000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0374-5900","authenticated-orcid":true,"given":"Hongxu","family":"Guo","sequence":"additional","affiliation":[{"name":"Minnan Normal University , , ,","place":["Zhangzhou, China, 363000"]},{"name":"Minnan Normal University , , ,","place":["Zhangzhou, China, 363000"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,24]]},"reference":[{"issue":"22","key":"2026090707072051300_cit1","doi-asserted-by":"publisher","DOI":"10.3390\/s23229080","article-title":"Electrochemical and\nColorimetric Nanosensors for Detection of Heavy Metal Ions: A Review","volume":"23","author":"Fakayode","year":"2023","journal-title":"Sensors"},{"key":"2026090707072051300_cit2","doi-asserted-by":"publisher","first-page":"1","DOI":"10.1080\/10408347.2025.2603486","article-title":"The Application of Nanozymes in Colorimetric-Electrochemical\nDual-Mode Biosensors for Efficient and Advanced Detection: From Mechanism\nto Applications","author":"Hsu","year":"2026","journal-title":"Crit. 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