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Abstract By employing the solvothermal in situ N -alkylation of organic bases with alcohol molecules, four new organically templated iodometallates as [L1][Ag 2 I 4 ] (L12+ = 1,1,4,4-tetramethyl-1λ4,4λ4-piperazinium) 1 , [L2] 1.5 [AgI 4 ] (L22+ = 1,4-dibenzyl-1λ4,4λ4-diazabicyclo[2.2.2]octanium) 2 , [L2] 1.5 [CuI 4 ] 3 and [L3][CuI 3 ] (L32+ = 4,4′-bis(3-methyl-1H-3λ4-imidazol-1-yl)-1,1′-biphenylium) 4 were obtained. In 1 , the in situ substitution and N-alkylation of 1,4-bis(pyridin-4-ylmethyl)piperazine (L1') with CH 3 OH has occurred, producing L12+. Templated by L12+, Ag+ and I- aggregate into a chained iodoargentate, which can be described as a linear arrangement of AgI 4 tedrahedra by sharing the edges. 2 and 3 are isostructural. In 2 and 3 , the in situ N -alkylation of 1,4-diazabicyclo[2,2,2]octane (L2') with phenylmethanol has occurred, generating L22+. Templated by L22+, Ag+ (or Cu+) and I- aggregate into a mononuclear iodometallate with a tetrahedral structure. In 4 , the in situ N -alkylation of 4,4′-di(1H-imidazol-1-yl)-1,1′-biphenyl (L3') with CH 3 OH has occurred, creating L32+. Templating by L32+, Cu+ and I- aggregate into a mononuclear iodocuprate(I) with a planar trigonal structure. The photoluminescence analysis reveals that (i) at the room temperature, only 1 emits light (λ em = 550 nm); (ii) at the low temperature, 4 is found to possess the photoluminescence property (λ em = 546 nm at 77 K) with a ms-grade lifetime (τ = 4.915 ms). Graphical abstract By employing solvothermal in situ N -alkylation of organic bases with alcohol molecules, four new organically templated iodometallate(I) were obtained, and their photoluminescence properties were investigated. fx1 Highlights • Four new organically templated iodometallates(I) (M+ = Ag+, Cu+) are reported; • In situ N -alkylation of 1,4-diazabicyclo[2,2,2]octane with phenylmethanol is investigated for the first time; • In situ N -alkylation of 4,4′-di(1H-imidazol-1-yl)-1,1′-biphenyl with alcohol molecules is investigated for the first time; • Their photoluminescence properties at different temperature are investigated. [ABSTRACT FROM AUTHOR]