A series of five new monofluoro complexes of chromium(III) of the type [Cr(en)2FX]n+ (en is ethylenediamine) has been pre¬pared and characterized. The complexes which contain Cl−, Br−, I−, or NCS− as the X− group all appear to involve a cis arrangement of the FX ligands. However, those complexes which contain ONO− or F− as the X− groups appear to have the FX ligands trans to each other. Structures were established via ultraviolet-visible spectral studies, by ion-exchange techniques, and in one case by the resolution of a complex into its optical antipodes. In addition, new synthetic methods are presented for some known complexes of chromium(III). © 1968, American Chemical Society. All rights reserved.