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Despite these developments, constructing diverse COP structures using identical structural motifs to investigate the variations in their performance remains a significant but challenging task. In this paper, we introduce a strategy aimed at reducing the symmetry of structural units to achieve this target. By employing the 3\u2010pyridyl\u2010based tetrathiafulvalene motif (labeled as TTF\u2010(3\u2010py)\n                    <jats:sub>4<\/jats:sub>\n                    ), a series of single\u2010crystal COP structures sharing the same motifs, including one\u2010dimensional (1D) zigzag chains (\n                    <jats:bold>CityU\u201061<\/jats:bold>\n                    ), 1D nanobelt (\n                    <jats:bold>CityU\u201062<\/jats:bold>\n                    ), and 2D layer (\n                    <jats:bold>CityU\u201063<\/jats:bold>\n                    ) structures, are constructed under different solvent conditions. The rotatability of the carbon\u2010carbon single bond, coupled with the deviation of nitrogen in pyridine from the symmetry axis, endows TTF\u2010(3\u2010py)\n                    <jats:sub>4<\/jats:sub>\n                    with a diverse range of configurations. These COP compounds exhibit excellent light absorption properties and redox activities, facilitating efficient photocatalytic synthesis of hydrogen peroxide (H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    ) from water and air. Notably,\n                    <jats:bold>CityU\u201063<\/jats:bold>\n                    exhibits the highest catalytic activity, with an H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production rate of 10\u00a0488.9\u00a0\u00b5mol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    , positioning it among the most effective photocatalysts currently employed for H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    photosynthesis.\n                  <\/jats:p>","DOI":"10.1002\/anie.6579208","type":"journal-article","created":{"date-parts":[[2026,4,9]],"date-time":"2026-04-09T04:20:02Z","timestamp":1775708402000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":9,"title":["Diversifying Single\u2010Crystal Structures of Covalent Organic Polymers Through a Symmetry\u2010Broken Strategy"],"prefix":"10.1002","volume":"65","author":[{"given":"Lei","family":"Zhang","sequence":"first","affiliation":[{"name":"Department of Materials Science and Engineering City University of Hong Kong  Hong Kong SAR P. 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