David A. T. Young

Synthesis and structure of FeRu3(CO)13(μ-PPh2)2; A “64-electron” cluster complex with a planar triangulated rhomboidal array of metal atoms

The species FeRu3(CO)13(μ-PPH2)2, synthesized from Ru3(CO)12 and Fe(CO)4(Ph2PPPh2),has been characterized both spectroscopically and via a single-crystal X-ray structural analysis. This complex crystallizes in the centrosymmetric triclinic space group P1 [No. 2, Ci1] with a  10.066(3), b  12.899(3), c  17.003(4) A, α  111.89(2), β  91.02(2), γ  102.00(2)°, V  1992.7(9) A3, Z  2, ϱ(obsd)  1.79(2) g cm-3 and ϱ(calcd)  1.82 cm-3. Diffraction data were collected with a Syntex P21 automated four-circle diffractometer and the structure was refined to RF  6.0% and RWF  3.6% for all 5213 reflections (RF  3.8%, RWF  3.6% for those 4140 reflections with |Fo|> 3σ(|Fo|). The metal atoms define a planar triangulated rhombus, with atoms Ru(1) and Ru(2) at the bridgehead, and Fe(1) and Ru(3) at the acute apices. Fe(1) is linked to four terminal carbonyl ligands and is associated with the heteronuclear bonds Fe(1)Ru(1)  2.861(1) A and Fe(1)Ru(2)  2.868(1) A. The ruthenium atoms are each bonded to three terminal carbonyl groups. The retheniumruthenium distances are Ru(1)Ru(2)  3.098(1), Ru(1)Ru(3)  3.147(1), and Ru(2)Ru(3)  3.171(1) A. The structure is completed by Ph2P bridges across the Ru(1)Ru(3) and Ru(2)(ru(3) vectors (

An insertion and Cycloaddition reaction of Dimethylketene with di-π-cyclopentadienylnickel

Abstract The complex (π-cyclopentadienyl)[σ-α,α-dimethyl-α-{2-3-π-[7,7-dimethyl-6-oxobicyclo[3.2.0]hept-2-en-4-yl]}acetyl]nickel (II) has been identified as the principal product of the reaction of two moles of dimethylketene with di-π-cyclopentadienylnickel. Degradation of II in methanol solution yielded methyl α,α,7,7-tetramethyl-6-oxobicyclo[3.2.0]hept-2-ene-4-acetate (III); and reduction of II gave the 6-hydroxy nickel complex (VI). Complex II is a result of 1,2-cycloaddition of one ketene function to a cyclopentadienyl ring and insertion of a second ketene function into a nickelcarbon bond.

X-Ray crystallographic determination of the molecular structure of B9C2H12AlMe2, a non-rigid aluminio-carborane derivative

Determination of the molecular structure of B9C2H12AlMe2 by single-crystal X-ray diffraction techniques, shows that the aluminium atom is involved in bonding only to two boron atoms of the B9C2H12 icosahedral fragment: 11B n.m.r. studies suggest that, in solution, the molecule undergoes rapid intramolecular rearrangements.