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Ongoing efforts to improve the stability of halide perovskites in ambient air has yielded promising results. However, the presence of toxic heavy element lead (Pb) remains a major concern requiring further attention. Herein, we report three new Pb\u2010free hybrid organic\u2013inorganic perovskite\u2010type halides based on gold (Au), (CH<jats:sub>3<\/jats:sub>NH<jats:sub>3<\/jats:sub>)AuBr<jats:sub>4<\/jats:sub>\u22c5H<jats:sub>2<\/jats:sub>O (<jats:bold>1<\/jats:bold>), (CH<jats:sub>3<\/jats:sub>NH<jats:sub>3<\/jats:sub>)AuCl<jats:sub>4<\/jats:sub>\u22c5H<jats:sub>2<\/jats:sub>O (<jats:bold>2<\/jats:bold>), and (CH<jats:sub>3<\/jats:sub>NH<jats:sub>3<\/jats:sub>)AuCl<jats:sub>4<\/jats:sub> (<jats:bold>3<\/jats:bold>). Hydrated compounds <jats:bold>1<\/jats:bold> and <jats:bold>2<\/jats:bold> crystallize in a brand\u2010new structure type featuring perovskite\u2010derived 2D layers and 1D chains based on pseudo\u2010octahedral AuX<jats:sub>6<\/jats:sub> building blocks. In contrast, the novel crystal structure of the solvent\u2010free compound <jats:bold>3<\/jats:bold> shows an exotic non\u2010perovskite quasi\u20102D layered structure containing edge\u2010 and corner\u2010shared AuCl<jats:sub>6<\/jats:sub> octahedra. The use of Au metal instead of Pb results in unprecedented low band gaps below 2.5\u2005eV for single\u2010layered metal chlorides and bromides. Moreover, at room temperature the three compounds show a weak blue emission due to the electronic transition between Au\u20106s and Au\u20105d, in agreement with the density function theory (DFT) calculation results. These findings are discussed in the context of viability of Au\u2010based halides as alternatives for Pb\u2010based halides for optoelectronic applications.<\/jats:p>","DOI":"10.1002\/chem.201901112","type":"journal-article","created":{"date-parts":[[2019,5,14]],"date-time":"2019-05-14T14:48:21Z","timestamp":1557845301000},"page":"9875-9884","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":23,"title":["(CH<sub>3<\/sub>NH<sub>3<\/sub>)AuX<sub>4<\/sub>\u22c5H<sub>2<\/sub>O (X=Cl, Br) and (CH<sub>3<\/sub>NH<sub>3<\/sub>)AuCl<sub>4<\/sub>: Low\u2010Band Gap Lead\u2010Free Layered Gold Halide Perovskite Materials"],"prefix":"10.1002","volume":"25","author":[{"given":"Chris","family":"Worley","sequence":"first","affiliation":[{"name":"Department of Chemistry and Biochemistry University of Oklahoma  101 Stephenson Parkway Norman OK 73019 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