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Here, we break this trade\u2010off through dimensional competition between halogen bonding and\n                    <jats:italic>\u03c0<\/jats:italic>\n                    \u2013\n                    <jats:italic>\u03c0<\/jats:italic>\n                    stacking in two nitroazole\u2010based organic frameworks. The parent (IClPzNO\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    \u00b7H\n                    <jats:sub>2<\/jats:sub>\n                    O forms a centrosymmetric two\u2010dimensional framework with coplanar chromophores and a birefringence of 0.705 at 546\u00a0nm. Combined skeletal and halogen substitutional editing, from pyrazole (Pz) to imidazole (Im) and from an ortho\u2010I\/Cl to a meta\u2010I\/I substitution pattern, redirects in\u2010plane hydrogen\u2010bonding aggregation via relocating the N\u2500H donor, and then extends C\u2500I\u00b7\u00b7\u00b7O connectivity from two to three dimensions. The resulting halogen\u2010bonded network governs chromophore orientation and produces a twofold\u2010interpenetrated polar framework, (I\n                    <jats:sub>2<\/jats:sub>\n                    ImNO\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>2<\/jats:sub>\n                    \u00b7H\n                    <jats:sub>2<\/jats:sub>\n                    O (\n                    <jats:italic>Pna<\/jats:italic>\n                    2\n                    <jats:sub>1<\/jats:sub>\n                    ). The crystal exhibits a phase\u2010matchable powder SHG response 20 times that of KDP (KH\n                    <jats:sub>2<\/jats:sub>\n                    PO\n                    <jats:sub>4<\/jats:sub>\n                    ), the largest value among five\u2010membered\u2010ring and nitro\/nitrate NLO crystals, as well as a giant birefringence of 0.554 at 546\u00a0nm. To the best of our knowledge, this combination occupies a previously unreported performance regime. These results identify interaction dimensionality as a practical design parameter for aligning polar\n                    <jats:italic>\u03c0<\/jats:italic>\n                    \u2010conjugated molecules and combining strong SHG with giant optical anisotropy.\n                  <\/jats:p>","DOI":"10.1002\/smll.76103","type":"journal-article","created":{"date-parts":[[2026,10,4]],"date-time":"2026-10-04T14:03:03Z","timestamp":1791122583000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Halogen\u2010Bond Dimensionality Controls\n                    <i>\u03c0\u2013\u03c0<\/i>\n                    Packing to Unlock Ultrahigh Second\u2010Harmonic Generation and Giant Birefringence"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-2439-7535","authenticated-orcid":false,"given":"Jin","family":"Chen","sequence":"first","affiliation":[{"name":"Fujian Provincial Key Laboratory of Advanced Materials Oriented Chemical Engineering College of Chemistry and Material Science Fujian Normal University  Fuzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yun\u2010Xia","family":"Hu","sequence":"additional","affiliation":[{"name":"Fujian Provincial Key Laboratory of Advanced Materials Oriented Chemical Engineering College of Chemistry and Material Science Fujian Normal University  Fuzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0007-3609-3236","authenticated-orcid":false,"given":"Huai\u2010Yu","family":"Wu","sequence":"additional","affiliation":[{"name":"School of Chemistry Sun Yat\u2010Sen University  Guangzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jia\u2010Min","family":"Lian","sequence":"additional","affiliation":[{"name":"Fujian Provincial Key Laboratory of Advanced Materials Oriented Chemical Engineering College of Chemistry and Material Science Fujian Normal University  Fuzhou P. R. 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