| Summary: | Reaction of <i>ortho</i>-carborane with anhydrous AlCl<sub>3</sub> in chloroform results in a mixture of 9-chloro, 9,12-dichloro, and 8,9,12-trichloro derivatives with 9,12-dichloro-<i>ortho</i>-carborane being the main product. Molecular crystal structure of 9,12-dichloro-<i>ortho</i>-carborane was determined by the single crystal X-ray diffraction. The crystal structure of 9,12-Cl<sub>2</sub>-1,2-C<sub>2</sub>B<sub>10</sub>H<sub>10</sub> appeared to be nearly isostructural to 9,12-dibromo-<i>ortho</i>-carborane: the crystal packing is built of layers in which molecules are connected via weak hydrogen and halogen bonds. A synthetic scheme for preparation of the hexachloro derivative of cobalt bis(dicarbollide) Cs[8,8′,9,9′,12,12′-Cl<sub>6</sub>-3,3′-Co(1,2-C<sub>2</sub>B<sub>9</sub>H<sub>8</sub>)<sub>2</sub>] from 9,12-dichloro-<i>ortho</i>-carborane has been proposed.
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