Reiser, Sara and Brunklaus, Gunther and Hong, Jung Hoon and Chan, Jerry C. C. and Eckert, Hellmut and Pfitzner, Arno (2002) (CuI)(3)P4S4: Preparation, structural, and NMR spectroscopic characterization of a copper(I) halide adduct with beta-P4S4. CHEMISTRY-A EUROPEAN JOURNAL, 8 (18). pp. 4228-4233. ISSN 0947-6539
Full text not available from this repository.Abstract
(CuI)(3)P4S4 is obtained by reaction of stoichiometric amounts of CuI, P, and S in evacuated silica ampoules. The yellow compound consists of monomeric beta-P4S4 cage molecules that are separated by hexagonal columns of CuI. (CuI)(3)P4S4 crystallizes isotypic to (CuI)(3)P4Se4 in the hexagonal system, space group P6(3)cm (no. 185) with a = 19.082(3), c = 6.691 (1) Angstrom, V = 2109.9(6) Angstrom(3), and Z=6. Three of the four phosphorus atoms are bonded to copper, whereas no bonds between copper and sulfur are observed. The two crystallographically distinct copper sites are clearly differentiated by Cu-65 magic-angle spinning (MAS) NMR spectroscopy. Furthermore, an unequivocal assignment of the P-31 MAS-NMR spectra is possible on the basis of homo- and heteronuclear dipole-dipole and scalar interactions. Dipolar coupling to the adjacent quadrupolar spins Cu-63 65 generates a clear multiplet structure of the peaks attributable to P1 and P2, respectively. Furthermore, the utility of a newly developed two-dimensional NMR technique is illustrated to reveal direct connectivity between P atoms based on (P-31-P-31) scalar interactions.
| Item Type: | Article |
|---|---|
| Uncontrolled Keywords: | NUCLEAR-MAGNETIC-RESONANCE; SOLID-STATE; PHOSPHORUS-SELENIUM; SYMMETRY PRINCIPLES; SEQUENCES; COMPLEXES; MOLECULES; SYSTEMS; SPECTRA; SULFUR; cage compounds; copper; dipole-dipole interactions; NMR spectroscopy; phosphorus; sulfur |
| Subjects: | 500 Science > 540 Chemistry & allied sciences |
| Divisions: | Chemistry and Pharmacy > Institut für Anorganische Chemie > Chair Prof. Dr. Arno Pfitzner |
| Depositing User: | Dr. Gernot Deinzer |
| Date Deposited: | 27 Aug 2021 07:50 |
| Last Modified: | 27 Aug 2021 07:50 |
| URI: | https://pred.uni-regensburg.de/id/eprint/39871 |
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