0000000000820296
AUTHOR
M. I. Rybinskaya
Cyclopentadienyl derivatives of octahedral carbonylcarbide hexaruthenium clusters: synthesis, NMR, IR and X-ray characterization
Abstract The reaction of hexanuclear carbonylcarbide cluster Ru6C(CO)17 (1) with pentamethylcyclopentadiene by reflux in heptane leads to a new chelate cluster Ru6C(μ-η1-η5-CH2C5Me4)(CO)14 (2). The compound 2 contains a CH2 group α-bonded to one of the Ru atoms in the Ru6 cluster and a C5Me4-ligand η5-coordinated by the adjacent Ru atom of the Ru6 cluster. Reflux of 1 in hexane with two molecular equivalents of nickelocene, Ni(C5H5)2 NiCp2, used as a source of cyclopentadiene yields the Ru6C(CO)12Cp2 (3) cluster. The compounds 2 and 3 have been characterized by NMR and IR spectroscopy and their crystal structures determined by X-ray diffraction studies.
Synthesis, crystal and molecular structure of η3-allylundecacarbonylosmium tetrafluoroborate
Abstract The η3-allylundecacarbonylosmium tetrafluoroborate has been synthesized in high yield by treatment of Os3(CO)11MeCN with allyl alcohol and subsequent protonation. It has been studied by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group Pna21 (no. 33) with a 17.933(2), b 11.440(2), c 11.797(2)A and Dc 2.76 g cm−3 for Z = 4. A final R value of 0.046 (Rw = 0.083) based on 2067 reflections was obtained. The presence of the positively charged allyl ligand in the triosmium cluster lengthens the Os1Os2 and Os2Os3 bonds (0.057A) and 0.074 A, respectively) relative to the OsOs bonds in Os3(CO)12.