4-(Pyren-1-yl)pyridine　(L)　with　luminescence　properties　was　self-assembled　with　beta-diketone-based　transition　metal　compounds　to　produce　five　new　hexacoordinated　metal　complexes:　[Zn(acac)(2)L-2]　(1),　[Zn(hfacac)(2)L-2]　(2),　[Ni(hfacac)(2)L-2]　(3),　[Cu(hfacac)(2)L-2]　(4),　and　[Co(acac)(2)L-2]　(5)　[L　=　4-(pyren-1-yl)pyridine,　acac　=　acetylacetone,　and　hfacac　=　hexafluoroacetylacetone].　The　structures　of　these　complexes　were　characterized　by　single-crystal　and　powder　X-ray　diffractometry;　elemental　analysis;　electrospray　ionization　masss　pectrometry;　and　nuclear　magnetic　resonance,　infrared,　and　fluorescence　spectroscopies.　The　beta-diketone　ancillary　ligands　and　pyrenylpyridine　functional　ligands　were　bonded　to　Zn(II)/Ni(II)　/Cu(II)/Co(II)　metal　ions　in　an　O＜^＞O　and　two　N　chelating　fashion,　leading　to　the　formation　of　mononuclear　coordination　complexes　where　one-dimensional　chains　and　two-dimensional　sheet　structures　were　formed　via　pi　center　dot　center　dot　center　dot　pi　stacking　and　hydrogen　bonding　interactions.　In　addition,　the　solid　state　photoluminescence　properties　of　these　new　crystalline　materials　were　examined,　with　obvious　differences　observed　between　the　metal　complexes.　(C)　2022　Elsevier　B.V.　All　rights　reserved.