Oxidative addition of diphenyl disulfide across a Ta=Ta bond. Preparation and characterization of (TaCl/sub 3/(Me/sub 2/S))/sub 2/(. mu. -SPh)/sub 2/
Journal Article
·
· Inorg. Chem.; (United States)
The tantalum complex (SMe/sub 2/)Cl/sub 2/Ta(..mu..-Cl)/sub 2/(..mu..-SMe/sub 2/)TaCl/sub 2/(SMe/sub 2/), possessing a sigma/sup 2/..pi../sup 2/ Ta=Ta double bond, reacts readily with PhSSPh to give (SMe/sub 2/)Cl/sub 3/Ta(..mu..-SPh)/sub 2/TaCl/sub 2/(SMe/sub 2/). In this reaction, the starting material loses the bridging SMe/sub 2/ ligand and two chloride bridges are broken while only two new SPh bridges are formed in the final product. This oxidative-addition reaction of the S-S single bond to the Ta=Ta double bond converts the face-sharing bioctahedron structure of the starting compound to an edge-sharing bioctahedron structure in the final dimer, with concomitant change of the oxidation state of tantalum from III to IV. The product is the first example of a d/sup 1/-d/sup 1/ ditantalum thiolate-bridged dimer. Important structural data for (SMe/sub 2/)Cl/sub 3/Ta(..mu..-SPh)/sub 2/TaCl/sub 3/(SMe/sub 2/), which has an inversion center, are determined. The new compound crystallizes in the monoclinic space group C2/c with a = 17.934 (5) A, b = 12.445 (4) A, c = 11.705 (4) A, ..beta.. = 92.50 (3)/sup 0/, V = 2610 (2) A/sup 3/, and Z = 4. Solid-state /sup 13/C NMR spectroscopy with cross polarization and magic-angle spinning (CP/MAS) at 28 and -103 /sup 0/C provides evidence that this compound is diamagnetic. 12 references, 3 figures, 4 tables.
- Research Organization:
- Texas A and M Univ., College Station
- OSTI ID:
- 5908550
- Journal Information:
- Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 25:3; ISSN INOCA
- Country of Publication:
- United States
- Language:
- English
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OSTI ID:5145684
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Related Subjects
36 MATERIALS SCIENCE
360101 -- Metals & Alloys-- Preparation & Fabrication
360102* -- Metals & Alloys-- Structure & Phase Studies
CHEMICAL BONDS
CHEMICAL PREPARATION
CHEMICAL REACTIONS
CHLORINE COMPLEXES
COHERENT SCATTERING
COMPLEXES
CRYSTAL DEFECTS
CRYSTAL STRUCTURE
DATA
DIFFRACTION
DOUBLE BONDS
ELECTRONIC STRUCTURE
EXPERIMENTAL DATA
INFORMATION
INTERSTITIALS
LATTICE PARAMETERS
LIGANDS
MAGNETIC RESONANCE
MOLECULAR ORBITAL METHOD
NMR SPECTRA
NUCLEAR MAGNETIC RESONANCE
NUMERICAL DATA
OXIDATION
PHOSPHORUS COMPLEXES
POINT DEFECTS
RESONANCE
SCATTERING
SPACE GROUPS
SPECTRA
SULFUR COMPLEXES
SYNTHESIS
TANTALUM COMPLEXES
TRANSITION ELEMENT COMPLEXES
VALENCE
X-RAY DIFFRACTION
360101 -- Metals & Alloys-- Preparation & Fabrication
360102* -- Metals & Alloys-- Structure & Phase Studies
CHEMICAL BONDS
CHEMICAL PREPARATION
CHEMICAL REACTIONS
CHLORINE COMPLEXES
COHERENT SCATTERING
COMPLEXES
CRYSTAL DEFECTS
CRYSTAL STRUCTURE
DATA
DIFFRACTION
DOUBLE BONDS
ELECTRONIC STRUCTURE
EXPERIMENTAL DATA
INFORMATION
INTERSTITIALS
LATTICE PARAMETERS
LIGANDS
MAGNETIC RESONANCE
MOLECULAR ORBITAL METHOD
NMR SPECTRA
NUCLEAR MAGNETIC RESONANCE
NUMERICAL DATA
OXIDATION
PHOSPHORUS COMPLEXES
POINT DEFECTS
RESONANCE
SCATTERING
SPACE GROUPS
SPECTRA
SULFUR COMPLEXES
SYNTHESIS
TANTALUM COMPLEXES
TRANSITION ELEMENT COMPLEXES
VALENCE
X-RAY DIFFRACTION