Synthesis and characterization of the trimetaphosphate molybdenum tricarbonyl anion as its tris(bis(triphenylphosphine)iminium) salt

Treatment of ( CH 3 CN ) 3 Mo ( CO ) 3 with the trimetaphosphate salt [ PPN ] 3 [ P 3 O 9 ] · H 2 O ( [ PPN ] + = [ Ph 3 PN- PPh 3 ] + ) (acetonitrile, 25 ° C ) gave the trimetaphosphate-molybdenum complex [ ( P 3 O 9 ) Mo ( CO ) 3 ] 3 - in 91% isolated yield. [ PPN ] 3 [ ( P 3 O 9 ) Mo ( CO ) 3 ] was also obtained in 77% isolated yield by directly treating Mo ( CO ) 6 with [ PPN ] 3 [ P 3 O 9 ] · H 2 O in refluxing acetonitrile, presumably by generating ( CH 3 CN ) 3 Mo ( CO ) 3 in situ. Reported herein is the full characterization and structural determination of [ PPN ] 3 [ ( P 3 O 9 ) Mo ( CO ) 3 ] and comparison to synthesized and calculated [ ( P 3 O 9 ) M ( CO ) 3 ] n - (M = group 6–9) complexes.