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Noncovalent assembly of the [Au(CN)\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sup>\u2212<\/jats:sup>\n                    anions tended to occur via Au\u00b7\u00b7\u00b7N\n                    <jats:sub>cyano<\/jats:sub>\n                    interactions; however, rare Au(III)\u00b7\u00b7\u00b7Au(III) contacts between the [Au(CN)\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sup>\u2212<\/jats:sup>\n                    groups \u2014 suggesting aurophilicity \u2014 could be induced when certain cation shape requirements were met. Specifically, cations with shape, size, and symmetry that allowed for packing in a complementary fashion with Au(III)\u00b7\u00b7\u00b7Au(III) aligned [Au(CN)\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sup>\u2212<\/jats:sup>\n                    dimers or trimers \u2014 providing efficiently close\u2010packed layers \u2014 were found to be sufficient for manifesting Au(III)\u00b7\u00b7\u00b7Au(III) contacts. Modifying the [RE(bipyO\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sup>3+<\/jats:sup>\n                    cation with peripheral methyl groups (the [Ln(dmbipyO\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sup>3+<\/jats:sup>\n                    cation) caused isoreticular replacement of a {[Au(CN)\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sub>3<\/jats:sub>\n                    }\n                    <jats:sup>3\u2212<\/jats:sup>\n                    trimer with a dumbbell\u2010shaped {[Au(CN)\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sub>2<\/jats:sub>\n                    Cl}\n                    <jats:sup>3\u2212<\/jats:sup>\n                    tri\u2010anion featuring an unusual Au\u00b7\u00b7\u00b7Cl\u00b7\u00b7\u00b7Au bridge \u2014 illustrating that the assembly of the anionic groups will adapt to conserve the same close packing. Au(III) aurophilicity between the [Au(CN)\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sup>\u2212<\/jats:sup>\n                    groups was studied using computational methods, crystal packing of the structures was probed using Hirshfeld surface analysis, and the emission properties of compounds containing the [Eu(dmbipyO\n                    <jats:sub>2<\/jats:sub>\n                    )\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sup>3+<\/jats:sup>\n                    luminophore were investigated, showing high quantum yields of\n                    <jats:italic>ca<\/jats:italic>\n                    . 50%.\n                  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