Malberg, Jennifer and Wiegand, Thomas and Eckert, Hellmut and Bodensteiner, Michael and Wolf, Robert (2013) Gold(I) and Silver(I) Complexes of Diphosphacyclobutadiene Cobaltate Sandwich Anions. CHEMISTRY-A EUROPEAN JOURNAL, 19 (7). pp. 2356-2369. ISSN 0947-6539, 1521-3765
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The synthesis and structural characterization of the first coordination compounds of bis(diphosphacyclobutadiene) cobaltate anions [M(P2C2R2)2] is described. Reactions of the new potassium salts [K(thf)3{Co(4-P2C2tPent2)2}] (1) and [K(thf)4{Co(4-P2C2Ad2)2}] (2) with [AuCl(tht)] (tht=tetrahydrothiophene), [AuCl(PPh3)] and Ag[SbF6] afforded the complexes [Au{Co(P2C2tPent2)2}(PMe3)2] (3), [Au{Co(P2C2Ad2)2}]x (4), [Ag{Co(P2C2Ad2)2}]x (5), [Au(PMe3)4][Au{Co(P2C2Ad2)2}2] (6), [K([18]crown-6)(thf)2][Au{Co(P2C2Ad2)2}2] (7), and [K([18]crown-6)(thf)2][M{Co(P2C2Ad2)2}2] (8: M=Au 9: M=Ag) in moderate yields. The molecular structures of 2 and 3, and 69 were elucidated by X-ray crystallography. Complexes 49 were thoroughly characterized by 31P and 13C solid state NMR spectroscopy. The complexes [Au{Co(P2C2Ad2)2}]x (4) and [Ag{Co(P2C2Ad2)2}]x (5) exist as coordination polymers in the solid state. The linking mode between the monomeric units in the polymers is deduced. The soluble complexes 13, 6, and 7 were studied by multinuclear 1H-, 31P{1H}-, and 13C{1H} NMR spectroscopy in solution. Variable temperature NMR measurements of 3 and 6 in deuterated THF reveal the formation of equilibria between the ionic species [Au(PMe3)4]+, [Au(PMe3)2]+, [Co(P2C2R2)2], and [Au{Co(P2C2R2)2}2] (R=tPent and Ad).
| Item Type: | Article |
|---|---|
| Uncontrolled Keywords: | APPROXIMATE COULOMB POTENTIALS; REGULAR TETRAHEDRAL GEOMETRY; NUCLEAR MAGNETIC-RESONANCE; ZETA VALENCE QUALITY; AUXILIARY BASIS-SETS; GAUSSIAN-BASIS SETS; P-31 MAS-NMR; CRYSTAL-STRUCTURES; MOLECULAR-STRUCTURE; STRUCTURAL-CHARACTERIZATION; cobalt; gold; phosphorus; sandwich complexes; silver; solid-state NMR spectroscopy |
| Subjects: | 500 Science > 540 Chemistry & allied sciences |
| Divisions: | Chemistry and Pharmacy > Institut für Anorganische Chemie Chemistry and Pharmacy > Institut für Anorganische Chemie > Arbeitskreis Prof. Dr. Robert Wolf |
| Depositing User: | Dr. Gernot Deinzer |
| Date Deposited: | 27 Apr 2020 06:16 |
| Last Modified: | 27 Apr 2020 06:16 |
| URI: | https://pred.uni-regensburg.de/id/eprint/17221 |
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