Investigations On The Reaction Of Molybdenum Pentaobiloride And Chloroxtomolylbdenum Cohplexes With Sodium Azide

The reaction of MoC15 with NaNrn3rnin acetonitrilernfollowed by addition of OPPh3 resulted in the formationrnof impure MOOC1rn3rn(OPFh)2 rather than the expectedrnnitrido analogue. NaNrn3rnacts here as a;reducing agentrngenerating a molybdenum(IV) chloride derivative whichrnwas trapped as impure MoC14(Py)2~rnThe reaction of MoOC14 with acetonitrile or NaN3rnproduced a green solution containing an MOOC13(MeCN)2rnCOl'1plex which could not be isolated but trapped withrnOPPhrn3rnand identified as MOOC13(OPPh3)2'. Addition ofrnNaNrn3rnto the green molybdenum oxotrichloride intermediate,rnMOOC1rn3rn(MeCN)2 produced a deep violet solution, Thernviole product could not be isolated but was inferredrnto consist of [NaHMoOC13(N3)(MeCN)J, a loose adductrnof MoOC13(MeCN)2 and NaNrn3rn, Thus, addition of OPPhrn3rntornthe violet solution resulted in the formation of impurernMOOC1rn3rn(OPPhrn3rn)2' The violet intermediate obtained fromrnMOOC13(MeCN)2 and NaN3 is stable in acetonitrile butrndecomposes in CH2C12 under evolution of N2 and reductionrnyielding MOOC12(MeCN)3 as a brown crystalline productrnwhich is sensitive to; 'hytirolyoiB. ~13(OPPh3)2 itselfr.eactsrnslower Vii th NaN" in acetonitrile Hi thrn:Jrnexchange yielding MOOC12(Nrn3rn)(OPPhrn3rn)2'

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