MULTINUCLEAR COMPLEXES DERIVED FROM FERROCENYLPHOSPHINES AND TRIRUTHENIUM DODECACARBONYL

Pyrolysis of Ru-3(CO)(1)1(PFc(2)Ph) in hexanes for 15 h gave the trinu clear cluster Ru-3(CO)(8)(mu )[mu-eta(3)-(eta(5)-C(5)H(3)PFcPh)Fe(eta( 5)-C5H5)] (11) in 20% yield. Pyrolysis of Ru-3(CO)(12) with PFc(2)Ph i n octane for 3.5 h gave the tetranuclear cluster RU(4)(CO)(11)(mu(3)-P Fc)(mu-eta(1):eta(5)-C5H4) (12) in 12% yield and the previously known 8, RU(4)(CO)(10)(mu-CO)mu(4)-PFc)(mu(4)-C6H4), in 10 yield: the mild c onditions are noteworthy. Pyrolysis of Ru-3(CO)(12) With PEt(2)Fc in o ctane for 18 h gave the hexanuclear cluster complexes RU(6)C(CO)(14)(m u-PEt(2))(2) (13) and RU(6)C(CO)(13)(mu-PEt(2))(eta(5)-C5H5) (14) in 1 5% and 25% yields, respectively, and the pentanuclear derivative Ru-5( CO)(9)(mu-CO)(eta(6)-C6H6)(2)(mu(4)-PEt) (15) (low yield). Pyrolysis O f Ru-3(CO)(12) with PEtFc(2) in toluene for 10 h gave the pentanuclear cluster RU(5)(CO)(12)(mu(4)-PEt)(eta(6)-C7H8) (16) in similar to 5% y ield. Crystal data: 8, monoclinic, space group P2(1)/c, a = 14.725(3) Angstrom, b = 9.024(2) Angstrom, c = 22.719(1) Angstrom, beta = 92.078 (8)degrees, Z = 4; 11, triclinic, <P(1)over bar>, a = 12.7671(9) Angst rom, b = 13.284(1) Angstrom, c = 10.2212(8) Angstrom, alpha = 93.006(6 )degrees, beta = 98.561(6)degrees, gamma = 83.665(6)degrees, Z = 2; 12 , monoclinic, space group P2(1)/c, a = 10.463(2) Angstrom, b = 16.412( 1) Angstrom, c = 17.903(2) Angstrom, beta = 103.85(1)degrees, Z = 4; 1 3, monoclinic, space group C2/c, a = 12.566(2) Angstrom, b = 16.326(2) Angstrom, c = 17.001(2) Angstrom, beta = 105.43(1)degrees Z = 4; 14, monoclinic, space group P2(1)/c,a = 12.638(2) Angstrom, b = 9.911(3) A ngstrom, c = 24.743(5) Angstrom, beta = 91.33(2)degrees, Z = 4; 15, or thorhombic, space group Cmc=2(1), a = 16.239(1) Angstrom, b = 13.754(2 ) Angstrom, c = 11.895(2) Angstrom, Z = 4; 16, monoclinic, space group C2/c, a = 31.831(3) Angstrom, b = 9.904(2) Angstrom, c = 17.536(2) An gstrom, beta = 99.36(1)degrees, Z = 8. The structures were solved by d irect or Patterson methods and were refined by full-matrix least-squar es procedures to R = 0.042, 0.024, 0.027, 0.024, 0.028, 0.032, and 0.0 26 for 4943, 8583, 5279, 3650, 6357, 1302, and 5711 reflections with I greater than or equal to 3 sigma(I), respectively.