CRYSTAL AND MOLECULAR-STRUCTURES OF 2 TRIOSMIUM CARBONYL CLUSTER COMPLEXES CONTAINING ORTHO-METALATED PHENYLPHOSPHINES (MU-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(eta-C5H5)2 affords (mu-H)Os3(CO)9[PFcPh(C6H4)], 5, and (mu-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 mu3-PFcPh(C6H4) moiety resulting from the ortho-metalation of one phenyl group and subsequent formation of a eta2-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) angstrom, alpha = 92.82(1)-degrees, beta = 100.32(1)-degrees, gamma = 71.55(1)-degrees, Z = 2, space group P1BAR, and those of 6.CH2Cl2, are also triclinic, a = 13.151(3), b = 17.177(4), c = 12.619(3) angstrom, alpha = 91.98(2)-degrees, beta = 104.18(2)-degrees, gamma = 67.72(2)-degrees, Z = 2, space group P1BAR. 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 greater-than-or-equal-to 3sigma(I), respectively.