Metallacrowns are a versatile class of inorganic compounds with uses in several areas of chemistry. Students engage in a multiweek, upper-division inorganic laboratory that explores four different metallacrown compounds: Fe[superscript III](O[subscript 2]CCH[subscript 3])[subscript 3][9-MC[subscript Fe][superscript III][subscript (N)shi]-3](CH[subscript 3]OH)[subscript 3][dot]3CH[subscript 3]OH, Mn[superscript II](O[subscript 2]CCH[subscript 3])[subscript 2][12-MC[subscript Mn[superscript III](N)shi]-4](C[subscript 3]H[subscript 7]NO)[subscript 6][dot]2C[subscript 3]H[subscript 7]NO, [(CH[subscript 3])[subscript 4]N][subscript 2]{Cu[superscript II][12-MC[subscript Cu[superscript II](N)shi]-4]}[dot]C[subscript 3]H[subscript 7]NO, and Mn[superscript II](O[subscript 2]CCH[subscript 3])[subscript 2][15-MC[subscript Mn[super script III](N)shi]-5](C[subscript 5]H[subscript 5]N)[subscript 6][dot]CH[subscript 3]OH. The syntheses are straightforward, and the compounds are characterized by cyclic voltammetry, solid-state magnetic susceptibility, FT-IR, UV-vis, and paramagnetically shifted [superscript 1]H NMR. Students are provided with a research-like experience in which they can successfully synthesize a metallacrown, conduct a literature search, develop characterization parameters based on departmental resources, interpret experimental results and compare them to the primary literature, analyze the crystallographic structures of the compounds, and finally present an oral seminar detailing their results and analysis.