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12. trans-BIS-(TRIPHENYHOSPHINE)CI-ILORONITROSYLIRIDIUM(1+) TETRAFLUOROBORATE NOBF [I~X(NO)[P(CGH~)~]Z]BFI(X = C1, Br) Submitted by R. J. FITZGERALDT and H. -M. W. LINT Checked by B. L. 2 tDepartment of Chemistry, Illinois Institute of Technology, Chicago, Ill. 60616. t Department of Chemistry, Northwestern University, Evanston, Ill. 60201. * The sealed reaction mixture is then heated to 100" for 24 hr with magnetic stirring. Upon cooling, a solid [largely unreacted OS~(CO)IZ] precipitates. After flushing with argon, the mixture is filtered to give a pale-green solution.
FELTHAMT Compounds of the type CoXz(NO)(PR3)2 were briefly described by Booth and Chatt,l who noted the presence of two NO bands in the infrared spectrum. 2 suggested that these two NO bands were due to the presence of two different hybridization isomers. The ~ preparation of both forms of COCIZ(NO)[P(CH~)(C~H~)Z]Z is described below. General Procedure Because the nitrosyl complexes are extremely air-sensitive in solution, air must be rigorously excluded. The Schlenk-tube techniques described by Shriver4 are suitable for the synthesis of these compounds.
DICARBONYL-q-CYCLOPENTADIENYLNITROSYLMOLYBDENUM + MO(CO)~ NaCsH5 - Na[Mo(CO)&-GH5)] + 3CO + CH~COZH THF [ ( ~ - C ~ H ~ ) M O ( C O+ ) ~NaOzCCH3 H] (~-C~H~)MO(CO +)P~-HC H ~ C ~ H ~ S O Z N ( N O ) CTHF H~ (~-CSHS)MO(NO)(CO)~ + CO + P - C H ~ C ~ H ~ S O ~ N H C H ~ Na[Mo(C0)3(q-C5H5)] - Procedure rn Caution. AN reactions and operations must be carried out under nitrogen, *Department of Chemistry, Sheffield University, Sheffield S3 7HF, England. 'Department of Chemistry, University of Georgia, Athens, Ga.