Crystal and molecular structures of two triosmium carbonyl cluster complexes containing ortho-metalated phenylphosphines (μ-H)Os3(CO)8L[PFcPh(C6H4)] (L = PFcPh2 or CO)
Pyrolysis of Os3(CO)11(PFcPh2), 7, and Os3(CO)10(PFcPh2)2, 8, (FcH = (Fe(η-C5H5)2 affords (μ-H)Os3(CO)9[PFcPh(C6H4)], 5, and (μ-H)Os3(CO)8(FcPPh2)[PFcPh(C6H4)], 6, respectively. The structures of 5 and 6 are analogous; they both contain a bridging hydride and a μ3-PFcPh(C6H4) moiety resulting from the ortho-metalation of one phenyl group and subsequent formation of a η2-bond from that metalated phenyl to the third osmium atom. Crystals of 5, are triclinic, a = 11.380(2), b = 15.930(3), c = 9.467(1) Å, α = 92.82(1)°, β = 100.32(1)°, 7 = 71.55(1)°, Z = 2, space group [Formula: see text], and those of 6•CH2Cl2, are also triclinic, a = 13.151(3), b = 17.177(4), c = 12.619(3) Å, α = 91.98(2)°, β = 104.18(2)°, γ = 67.72(2)°, Z = 2, space group [Formula: see text]. The structures were solved by heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.028 and 0.026 by using 8080 and 9336 reflections with I ≥ 3σ(I), respectively.