We have approached the synthesis of discrete fulleride salts, through the use of strongly reducing organometallic species such as metallocenes, which allow precise control of stoichiometry for the production of C{sub 60}{sup n-} species. Decamethylnickelocene Ni(C{sub 5}Me{sub 5}){sub 2}, is a selective reductant for the production of C{sub 60} monoanion and yields a crystalline 1:1 salt when combined with C{sub 60} in CS{sub 2}. The structure of this salt [Ni(C{sub 5}Me{sub 5}) {sub 2}{sup +}][C{sub 60}{sup -}].CS{sub 2} (1), is highly ordered and is the first example of a non-disordered monoanionic C{sub 60} structure. We report here the synthesis and single-crystal X-ray structure of 1 and structural evidence for the expected Jahn-Teller distortion in the C{sub 60} monoanion. 16 refs., 3 figs.