$[(C_2B_9H_{11})Mo(CO)_3]_2PPN_2$ $(2{cdot}PPN_2)$, a new precursor for the oxidative decarbonylation reaction, was synthesized in high yield by the one-electron oxidation reaction of $[(C_2B_9H_{11})Mo(CO)_3]PPN_2$. $2{cdot}PPN_2$ was structurally characterized, showing a dimeric nature with long (3.321 ${AA}$) Mo-Mo bonding. Reaction of $2{cdot}PPN_2$ with sulfur gave the completely decarbonylated product $[(C_2B_9H_{11})Mo({mu}-S)(S)]_2PPN_2$ ($3{cdot}PPN_2$). The ligand substitution of the terminal sulfur ligands in $3{cdot}PPN_2$ to oxygen ligands was carried out with the use of PhIO to give $[(C_2B_9H_{11})Mo({mu}-S)(O)]_2PPN_2$ ($4{cdot}PPN_2$). The structures of $3{cdot}PPN_2$ and $4{cdot}PPN_2$ were also studied.