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In conventional poly(heptazine imide) (PHI), alkali cations are incorporated through molten\u2010salt\u2010mediated equilibration, producing statistically distributed ionic environments with little spatial correlation. Here, we demonstrate that organic\u2010inorganic ionic cocrystals (ICCs) serve as molecularly preorganized precursors that promote spatially correlated ionic environments during framework formation, enabling controlled incorporation of Li\n                    <jats:sup>+<\/jats:sup>\n                    into imide\u2010bridged N sites. This ICC\u2010programmed architecture decouples composition from photocatalytic function, demonstrating that photocatalytic activity is governed by the ion incorporation pathway and the resulting spatial ionic organization, rather than cation identity or content alone. The resulting ionic carbon nitride, CALiK, achieves an apparent quantum yield of 58% at 410\u00a0nm, the highest among the benchmarked state\u2010of\u2010the\u2010art photocatalysts, while requiring substantially lower inorganic salt loading than conventional ionothermal synthesis. Operando\u2010relevant spectroscopic and electrochemical analyses reveal directional charge migration driven by internal electrostatic polarization and enhanced accumulation of long\u2010lived photogenerated electrons. Representative density functional theory models suggest that spatially correlated ionic motifs and cyano\u2010derived electron\u2010accepting domains generate polarized charge landscapes that lower the energetic barrier for the two\u2010electron oxygen reduction pathway.\n                  <\/jats:p>","DOI":"10.1002\/adma.75258","type":"journal-article","created":{"date-parts":[[2026,10,1]],"date-time":"2026-10-01T10:09:17Z","timestamp":1790849357000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Ionic Cocrystal Programming of Spatial Ionic Organization in Carbon Nitrides Enables Highly Efficient H\n                    <sub>2<\/sub>\n                    O\n                    <sub>2<\/sub>\n                    Photosynthesis"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0006-0541-2268","authenticated-orcid":false,"given":"Anna Lo","family":"Presti","sequence":"first","affiliation":[{"name":"Department of Colloid Chemistry Max Planck Institute of Colloids and Interfaces  Potsdam Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6774-9137","authenticated-orcid":false,"given":"Zahra","family":"Hajiahmadi","sequence":"additional","affiliation":[{"name":"CASUS\u2010Center For Advanced Systems Understanding Helmholtz\u2010Zentrum Dresden\u2010Rossendorf e.V. (HZDR)  G\u00f6rlitz Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2619-2859","authenticated-orcid":false,"given":"Sam A. J.","family":"Hillman","sequence":"additional","affiliation":[{"name":"Department of Chemistry Imperial College London Molecular Sciences Research Hub  London UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2132-340X","authenticated-orcid":false,"given":"Mu","family":"Xiao","sequence":"additional","affiliation":[{"name":"School of Chemical Engineering The University of Queensland  St Lucia Australia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8353-7345","authenticated-orcid":false,"given":"James R.","family":"Durrant","sequence":"additional","affiliation":[{"name":"Department of Chemistry Imperial College London Molecular Sciences Research Hub  London UK"},{"name":"Department of Chemistry University of Oxford  Oxford UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5471-2407","authenticated-orcid":false,"given":"Thomas D.","family":"K\u00fchne","sequence":"additional","affiliation":[{"name":"CASUS\u2010Center For Advanced Systems Understanding Helmholtz\u2010Zentrum Dresden\u2010Rossendorf e.V. (HZDR)  G\u00f6rlitz Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4119-2523","authenticated-orcid":false,"given":"Christian Mark","family":"Pelicano","sequence":"additional","affiliation":[{"name":"Department of Colloid Chemistry Max Planck Institute of Colloids and Interfaces  Potsdam Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2026,10,1]]},"reference":[{"issue":"6276","key":"e_1_2_8_2_1","doi-asserted-by":"crossref","first-page":"965","DOI":"10.1126\/science.aad5705","article-title":"Palladium\u2010Tin Catalysts for the Direct Synthesis of H2O2 With High Selectivity","volume":"351","author":"Freakley S. 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W.\u2010H.","year":"2016","journal-title":"Nature Communications"},{"issue":"49","key":"e_1_2_8_26_1","doi-asserted-by":"crossref","first-page":"45712","DOI":"10.1021\/jacs.5c17982","article-title":"Unraveling the Correlation Between Crystallographic Structure and Charge Transport in Metal Poly(heptazine imides)","volume":"147","author":"Liang X.","year":"2025","journal-title":"Journal of the American Chemical Society"},{"issue":"30","key":"e_1_2_8_27_1","doi-asserted-by":"crossref","first-page":"9372","DOI":"10.1002\/anie.201804702","article-title":"Ionothermal Synthesis of Triazine\u2013Heptazine\u2010Based Copolymers with Apparent Quantum Yields of 60\u2009% at 420\u2005Nm for Solar Hydrogen Production from \u201cSea Water\u201d","volume":"57","author":"Zhang G.","year":"2018","journal-title":"Angewandte Chemie International Edition"},{"issue":"10","key":"e_1_2_8_28_1","doi-asserted-by":"crossref","first-page":"1366","DOI":"10.1039\/C7CE00037E","article-title":"Anhydrous Ionic co\u2010Crystals of Cyanuric Acid with LiCl and NaCl","volume":"19","author":"Shemchuk O.","year":"2017","journal-title":"CrystEngComm"},{"issue":"16","key":"e_1_2_8_29_1","doi-asserted-by":"crossref","first-page":"2212","DOI":"10.1039\/C8CE00304A","article-title":"Organic\u2013Inorganic Ionic co\u2010Crystals: A New Class of Multipurpose Compounds","volume":"20","author":"Braga D.","year":"2018","journal-title":"CrystEngComm"},{"issue":"2026","key":"e_1_2_8_30_1","doi-asserted-by":"crossref","first-page":"966","DOI":"10.1016\/j.jechem.2026.03.023","article-title":"Topotactic\u2010Templated Conversion of Ionic\u2010Cocrystal Unlocking Atomic\u2010Layered Poly(heptazine imide) for Pt\u2010Assisted Hydrogen Photocatalysis","volume":"118","author":"Dai L.","year":"2026","journal-title":"Journal of Energy Chemistry"},{"issue":"11","key":"e_1_2_8_31_1","doi-asserted-by":"crossref","first-page":"7230","DOI":"10.1021\/acs.cgd.0c00899","article-title":"Mechanochemical Preparation and Solid\u2010State Characterization of 1:1 and 2:1 Ionic Cocrystals of Cyanuric Acid with Alkali Halides","volume":"20","author":"Shemchuk O.","year":"2020","journal-title":"Crystal Growth & Design"},{"issue":"16","key":"e_1_2_8_32_1","doi-asserted-by":"crossref","DOI":"10.1002\/anie.2543286","article-title":"Atomically Dispersed Cobalt on Ionic Carbon Nitrides for Selective and Efficient Nitrate Electroreduction to Ammonia","volume":"65","author":"Gao N.","year":"2026","journal-title":"Angewandte Chemie International Edition"},{"issue":"13","key":"e_1_2_8_33_1","doi-asserted-by":"crossref","first-page":"1517","DOI":"10.1002\/asia.201700209","article-title":"Towards Organic Zeolites and Inclusion Catalysts: Heptazine Imide Salts Can Exchange Metal Cations in the Solid State","volume":"12","author":"Savateev A.","year":"2017","journal-title":"Chemistry\u2014An Asian Journal"},{"issue":"37","key":"e_1_2_8_34_1","doi-asserted-by":"crossref","DOI":"10.1002\/anie.202511459","article-title":"Ordered Copper Triangular Atomic Sites for Industrial\u2010Grade Electromethanation of CO2 via Self\u2010Regulated Adsorption of Reactants","volume":"64","author":"Yao F.","year":"2025","journal-title":"Angewandte Chemie International Edition"},{"issue":"12","key":"e_1_2_8_35_1","doi-asserted-by":"crossref","first-page":"5511","DOI":"10.1021\/acs.chemmater.2c00528","article-title":"Enhanced H2O2 Production via Photocatalytic O2 Reduction Over Structurally\u2010Modified Poly(heptazine imide)","volume":"34","author":"Sharma P.","year":"2022","journal-title":"Chemistry of Materials"},{"issue":"42","key":"e_1_2_8_36_1","doi-asserted-by":"crossref","first-page":"5641","DOI":"10.1039\/D0CC01338B","article-title":"Controlling Defects in Crystalline Carbon Nitride to Optimize Photocatalytic CO2 Reduction","volume":"56","author":"Li H.","year":"2020","journal-title":"Chemical Communications"},{"issue":"34","key":"e_1_2_8_37_1","doi-asserted-by":"crossref","first-page":"17668","DOI":"10.1039\/D2TA04213D","article-title":"NH\u2010Rich Red Poly(heptazine imide) Nanoparticles with Simultaneously Promoted Exciton Dissociation and Activated n\u2192\u03c0* Electronic Transition for Boosted Photocatalytic H2 Generation","volume":"10","author":"Zhao Z.","year":"2022","journal-title":"Journal of Materials Chemistry A"},{"issue":"3","key":"e_1_2_8_38_1","doi-asserted-by":"crossref","first-page":"1283","DOI":"10.1021\/acs.chemmater.2c03325","article-title":"Influence of Ion Exchange on Photoresponsive Properties of Potassium Poly(heptazine imide)","volume":"35","author":"Hattori M.","year":"2023","journal-title":"Chemistry of Materials"},{"issue":"15","key":"e_1_2_8_39_1","doi-asserted-by":"crossref","first-page":"4878","DOI":"10.1039\/D2CS00806H","article-title":"Carbon Nitride Based Materials: More than Just a Support for Single\u2010Atom Catalysis","volume":"52","author":"Rocha G. 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