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Barnes, Christopher M. ; Bohle, D. Scott ; Dinnebier, Robert E. ; Madsen, Sara K. ; Stephens, Peter W.:
Structural and Spectroscopic Studies of Two Phases of the Organometallic Chain Polymer [Ru₂{μ₂:μ₂:η²-O₂PMe₂}₂(CO)₄]n.
In: Inorganic Chemistry.
Bd. 36
(1997)
Heft 25
.
- S. 5793-5798.
ISSN 1520-510X
DOI: https://doi.org/10.1021/ic970265n
Abstract
The microcrystalline organometallic coordination polymer Ru2{μ2:μ2:η2-O2PMe2}2(CO)4n which results from the oxidative addition of dimethylphosphinic acid to triruthenium dodecacarbonyl has been structurally characterized by X-ray powder diffraction, λ = 1.149 49(1) Å, at 295 and 50 K. At room temperature the crystallites have a monoclinic unit cell with the space group C2/c with lattice constants a = 18.0792(3) Å, b = 9.0626(2) Å, c = 10.0372(2) Å, β = 112.107(1)°, and Z = 4; the final refinement of 52 variables converged to Rp, Rwp, RF, and RF2 of 8.2, 10.8, 4.6, and 8.3\%, respectively, for data collected between 4 and 60° (2θ). At 50 K the phase is described by a triclinic unit cell, space group P1̄, and is characterized by the lattice constants a = 9.8637(6) Å, b = 8.9290(6) Å, c = 9.8870(5) Å, α = 115.051(3)°, β = 108.587(5)°, γ = 92.015(5)°, and Z = 2; the final refinement of 102 variables converged to and Rp, Rwp, RF, and RF2 of 8.3, 11.4, 1.5, and 3.0\%, respectively, for data collected between 3 and 74° (2θ). The transition between the two crystalline phases has been determined by differential scanning calorimetry to occur at circa 220 K, and the most pronounced difference in the environment of the chains, as determined by variable-temperature IR spectroscopy, is in the ρ(PCH3) modes for the bridging dimethylphosphinate ligands.
Weitere Angaben
| Publikationsform: | Artikel in einer Zeitschrift |
|---|---|
| Begutachteter Beitrag: | Ja |
| Zusätzliche Informationen: | PMID: 11670201 |
| Institutionen der Universität: | Fakultäten > Fakultät für Mathematik, Physik und Informatik > Fachgruppe Materialwissenschaften > Lehrstuhl Kristallographie Fakultäten Fakultäten > Fakultät für Mathematik, Physik und Informatik Fakultäten > Fakultät für Mathematik, Physik und Informatik > Fachgruppe Materialwissenschaften |
| Titel an der UBT entstanden: | Ja |
| Themengebiete aus DDC: | 500 Naturwissenschaften und Mathematik > 530 Physik |
| Eingestellt am: | 15 Jun 2016 08:44 |
| Letzte Änderung: | 15 Jun 2016 08:44 |
| URI: | https://eref.uni-bayreuth.de/id/eprint/32680 |