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Organic \u03c0\u2010conjugated molecules possess high intrinsic polarizability favorable for birefringent materials design, although this potential is often hindered by dense, cofacial \u03c0\u2013\u03c0 stacking, which induces strong interlayer electronic coupling and severely limits optical anisotropy. Metal\u2010organic frameworks (MOFs) offer a solution that utilizes coordination bonds to modulate the packing configuration of ligands. However, a dimensionality dilemma remains: 3D MOFs often possess high symmetry that cancels optical anisotropy, while 2D MOFs typically inherit eclipsed stacking of conjugated ligands, locking birefringence at low levels. Herein, we propose an anion\u2010induced coordination competition strategy (AICCS) to disrupt dense stacking. By steering inorganic anions (\n                    <jats:italic>T<\/jats:italic>\n                    <jats:sub>d<\/jats:sub>\n                    of SO\n                    <jats:sub>4<\/jats:sub>\n                    <jats:sup>2\u2212<\/jats:sup>\n                    and\n                    <jats:italic>D<\/jats:italic>\n                    <jats:sub>3h<\/jats:sub>\n                    of NO\n                    <jats:sub>3<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    ) and \u03c0\u2010conjugated 2,3,6,7,10,11\u2010hexahydroxytriphenylene (HHTP) ligands to competitively coordinate with La\n                    <jats:sup>3+<\/jats:sup>\n                    , we successfully force in\u2010plane slip of adjacent HHTP layers in resulted MOFs. This precisely engineered slip\u2010stacking decouples interlayer electronic states and liberates the latent polarizability of the \u03c0\u2010system. Consequently, we achieved a dramatic birefringence enhancement from the suppressed state in the parent LaHHTP (\u0394\n                    <jats:italic>n<\/jats:italic>\n                    = 0.12) to record\u2010high values of \u0394\n                    <jats:italic>n<\/jats:italic>\n                    = 1.1 in LaHHTP\u2010SO\n                    <jats:sub>4<\/jats:sub>\n                    and \u0394\n                    <jats:italic>n<\/jats:italic>\n                    = 1.3 in LaHHTP\u2010NO\n                    <jats:sub>3<\/jats:sub>\n                    , providing a versatile route to design next\u2010generation anisotropic optical crystals.\n                  <\/jats:p>","DOI":"10.1002\/adma.73757","type":"journal-article","created":{"date-parts":[[2026,6,19]],"date-time":"2026-06-19T06:14:26Z","timestamp":1781849666000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Interlayer Electronic Decoupling Unlocks Giant Birefringence in \u03c0\u2010Conjugated Metal\u2010Organic Frameworks"],"prefix":"10.1002","volume":"38","author":[{"ORCID":"https:\/\/orcid.org\/0009-0009-0424-7522","authenticated-orcid":false,"given":"Jia\u2010Xiang","family":"Zhang","sequence":"first","affiliation":[{"name":"National Key Laboratory of Advanced Micro and Nano Manufacture Technology School of Materials Science and Engineering Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xinyan","family":"Wu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Quantum Functional Materials, School of Physical Science and Technology ShanghaiTech University Shanghai China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Weishan","family":"Li","sequence":"additional","affiliation":[{"name":"National Key Laboratory of Advanced Micro and Nano Manufacture Technology School of Materials Science and Engineering Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0001-6898-980X","authenticated-orcid":false,"given":"Haolin","family":"Zhong","sequence":"additional","affiliation":[{"name":"National Key Laboratory of Advanced Micro and Nano Manufacture Technology School of Materials Science and Engineering Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jinkun","family":"Guo","sequence":"additional","affiliation":[{"name":"National Key Laboratory of Advanced Micro and Nano Manufacture Technology School of Materials Science and Engineering Peking University  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qingsheng","family":"Zeng","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Quantum Functional Materials, School of Physical Science and Technology ShanghaiTech University Shanghai 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