The reaction of [CpCr(CO)(3)](2) with P-4 in toluene at 90 degreesC for 5 h
affords the triple-decker sandwich complex [CpCr(CO)(eta (3)-P-3)(CpCr)(2)
(mu,eta (1):eta (5):eta (5)-P-5)] (1) as a new product, along with the prev
iously described products with P-2, P-3, and P-10 units. The structure of t
he paramagnetic complex 1 has been established by single-crystal X-ray diff
raction methods. A novel complex [{CpCr(CO)(2)}(2)(mu,eta (1):eta (1):eta P
-2(2)){Mo(CO)(4)}(2){(mu,eta (1):eta (1):eta (5):eta (5)-P-5)(CpCr)(2)}] (2
) has been obtained from the reaction of [{CpCr(CO)(2)}(2)(mu,eta (2)-P-2)]
With [Mo-(CO)(4)(NBD)] (NBD = norbornadiene). The X-ray structure of 2 rev
eals a six-membered Mo2P4 ring combining a Cr2P2 tetrahedral core and a tri
ple-decker sandwich Cr2P5 moiety. The EPR spectra of the paramagnetic (S' =
1/2) complexes 1 and 2 are reported. A noticeable hyperfine interaction wi
th two P-31 nuclei is observed for 2.