Ph,AsCH,CH,AsPh, (dpae) ; cis-Ph,PCH=CHPPh, (dppen) ; cis-Ph,AsCH=CHAsPh, (dpaen) ; Ph,AsCH,-CH,PPh, (dadpn) ; cis-Ph,AsCH=CHPPh, (dadpen) ; and C,H,(AsPh,-o) (PPh,-o) (pdadp)] has led to the isolation of [MoCI,O(L-L)] complexes. Refluxing these complexes in methanol leads to partial reduction to form [MoxVCIO(L-L),][MoVCI,O], but reflux in methanol in the presence of L-L and Na[BPh,] results in complete reduction to [MoCIO(L-L),] [BPha]. These complexes have been characterised by the use of i.r.. electronic-absorption, and e.p.r. spectroscopy. E.p.r. spectra suggest that the [MoCI,O (L-L)] (L-L = dppe or dppen) species have a fac structure in dichloromethane. Considerable hyperfine structure, and g values ca. 1.97, have been observed for the e.p.r.-active species. C6H,(PPh2-o), (pdpp) ; * This complex has previously been prepared from [MoCl,O-(thf),] (thf = tetrahydrofuran) .6