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The bond lengths Co–C(CO), Co–N(NO) and angles L–Co–C(CO), L–Co–N(NO) in six tetrahedral complexes, determined by X‐ray crystallography, were analysed and compared with the calculated compound Co(CO)2(NO)PH3. Distinct differences were found which allow a differentiation of the two similar ligands CO and NO. These differences are used to assign CO and NO ligands in cases where this has not been possible before including a structure in which the two independent molecules in the unit cell are diastereomers. The relationship seems to hold not only for tetrahedral compounds but also for other polyhedral coordination types.