| Summary: | The solvothermal reaction of Zn(NO<sub>3</sub>)<sub>2</sub>·4H<sub>2</sub>O, 1-OH-2-naphthaldehyde, and 2-methylalanine (<i>mAla</i>) in MeOH leads to the formation of complex {[ZnL<sub>1</sub>]}<sub>2n</sub> (<b>1</b>) (H<sub>2</sub>L<sub>1</sub> = the Schiff-base resulting from the reaction of 1-OH-2-naphthaldehyde and <i>mAla</i>) in good yields. The structure of the neutral species, as determined by single-crystal crystallography, describes a two-dimensional coordination polymer, with repeating {Zn<sub>2</sub>} units bridged by <i>syn, anti</i>-carboxylate groups of the Schiff-base ligands. Repeating the same reaction using glycine (<i>gly</i>) instead of <i>mAla</i> leads to the formation of complex {[ZnL<sub>2</sub>]·0.33MeOH}<sub>3n</sub> (<b>2</b>.0.33MeOH) (H<sub>2</sub>L<sub>2</sub> = the Schiff-base resulting from the reaction of 1-OH-2-naphthaldehyde and <i>gly</i>), again in good yields. Complex <b>2</b> describes a three-dimensional coordination polymer based on {Zn<sub>2</sub>} building blocks, arranged by <i>anti, anti</i>-carboxylate groups in a 3D motif. Complexes <b>1</b> and <b>2</b> were found to strongly emit at ~435 nm (λ<sub>exc</sub> = 317 nm) both in solution and solid state, with complex <b>2</b> displaying a slightly longer lifetime of <i>τ</i><sub>av</sub> = 2.45 ns vs. <i>τ</i><sub>av</sub> = 2.02 ns for <b>1</b>.
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