SOME CHEMISTRY WITH A CHIRAL PHOSPHINE GENERATED FROM FENCHONE-PINACOLONE MIXED AZINE - CRYSTAL-STRUCTURE OF Z,E-PH2PCH2C(BU(T))=N-N=C10H16

Treatment of fenchone hydrazone with tert-butyl methyl ketone gave the mixed azine MeC(Bu(t))=N-N=C10H16 which on treatment with LiBu(n) fol lowed by PClPh2 gave the mixed azine monophosphine Z,E-Ph2PCH2C(Bu(t)) =N-N=C10H16. This was converted into the corresponding phosphine oxide or phosphine sulfide. The azine monophosphine with [Mo(CO)4(nbd)] (nb d = norbornadiene) gave the chelate complex [Mo(CO)4{PPh2CH2C(Bu(t))=N -N=C10H16}] which with L undergoes ring-opening to give [Mo(CO)4L{PPh2 CH2C(Bu(t))=N-N+C10H16}] (L = CO, CNBu(t) or CNMe) with monodentate ph osphine. Corresponding tungsten complexes [W(CO)4{PPh2CH2C(Bu(t))=N-N= C10H16}] and [W(CO)4L{PPh2CH2C(Bu(t))=N-N=C10H16}] (L=CNBu(t) or CNMe) were also prepared. Crystals of Z,E-Ph2PCH2C(Bu(t))=N-N-C10H16 are mo noclinic, space group P2(1) with a = 11.0737(8), b = 11.0377(9), c = 1 1,1072(7) angstrom, beta = 110.60(5)-degrees and Z = 2 for 3492 observ ed reflections. Proton, P-31-{H-1}, C-13-{H-1} NMR, IR and mass spectr al data are given.