Synthesis, characterization, and x-ray structure of bis(/mu/-acetato dicarbonyl(di-tert-butylphosphine) ruthenium (I))
Ru/sub 3/(CO)/sub 12/ reacts with d-tert-butylphosphine and acetic acid in di-n-butylether under reflux to form bis(/mu/-acetatodicarbonyl(di-tert-butylphosphine)ruthenium (I)) in 80% yield. The crystal structure of 1 has been determined by single crystal X-ray diffraction methods. Crystal data for 1: C/sub 24/H/sub 42/O/sub 8/P/sub 2/Ru/sub 2/, M = 722.7, orthorhombic, space group Pbca, a = 12.955 (2), b = 17.347 (2), c = 28.638 (4) /angstrom/, U = 6435.8 (5) /angstrom//sup 3/, D/sub c/ = 1.492 gcm/sup /minus/3/, /lambda/(Mo K/alpha/) = 0.71073 /angstrom/, graphite monochromator, /mu/ = 10.56 cm/sup /minus/1/. Methods MULTAN, difference Fourier, full-matrix least-squares. All non-hydrogen atoms were refined with anisotropic thermal parameters. Hydrogen atoms were not located. Data/parameter ratio = 7.07, shift to error ratio = 0.38, highest peak in the final difference Fourier = 0.70 /angstrom//sup /minus/3/. Data were collected on an Enraf-Nonius CAD-4 diffractometer at 23 /plus minus/2/degree/C. The complex has a Ru-Ru bond of 2.735 (1) /angstrom/ which is bridged by two cis acetate groups. The CO groups also occupy cis acetate groups. The CO groups also occupy cis locations on each Ru, while the two t-Bu/sub 2/PH ligands occupy axial positions trans to the metal-metal bond. The coordination geometry about each Ru atom is roughly octahedral. The overall geometry of the molecule can be described as that of a sawhorse-like structure.
- Research Organization:
- Univ. of Texas, Austin (USA)
- OSTI ID:
- 5914225
- Journal Information:
- J. Coord. Chem.; (United States), Vol. 18:4
- Country of Publication:
- United States
- Language:
- English
Similar Records
Interaction of iodine with a hydridotriosmium cluster containing a carboxamido ligand: Crystal and molecular structure of a dinuclear carboxamido complex and a mononuclear amine complex
Di-tert-butylphosphinic iodide
Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ACETATES
CRYSTAL STRUCTURE
ACETIC ACID
CHEMICAL REACTIONS
CARBONYLS
PHOSPHINES
RUTHENIUM COMPLEXES
RUTHENIUM COMPOUNDS
CHEMICAL REACTION YIELD
EXPERIMENTAL DATA
SPACE GROUPS
X-RAY DIFFRACTION
CARBOXYLIC ACID SALTS
CARBOXYLIC ACIDS
COHERENT SCATTERING
COMPLEXES
DATA
DIFFRACTION
INFORMATION
MONOCARBOXYLIC ACIDS
NUMERICAL DATA
ORGANIC ACIDS
ORGANIC COMPOUNDS
PHOSPHORUS COMPOUNDS
REFRACTORY METAL COMPOUNDS
SCATTERING
TRANSITION ELEMENT COMPLEXES
TRANSITION ELEMENT COMPOUNDS
YIELDS
400201* - Chemical & Physicochemical Properties