X-ray Crystal Structure and Homonuclear 31P-31P δ/J-Resolved NMR Spectroscopic Studies of [AgIr2(dimen)4(PPh3)2](PF6)3. Observation of a Statistical Mixture of “Head/Tail” Isomers

Andrew G. Sykes, Kent R. Mann

Research output: Contribution to journalArticlepeer-review

21 Scopus citations

Abstract

The reaction of [AgIr2(dimen)4(PF6)3(dimen = 1,8-diisocyanomenthane) with 2 equiv of triphenylphosphine results in the coordination of triphenylphosphine to the iridium atoms and forms a linear P-Ir-Ag-Ir-P unit. Recrystallization of the compound from acetone/hexane solutions afforded crystals of [AgIr2(dimen)4(PPh3)2](PF6)3(AgIr2C84H102Fl8N8P5) that were the subject of X-ray structural characterization. The complex crystallizes in the monoclinic space group C2/c (No. 15) with Z = 4, a = 26.6 (1) Å, b = 4.67 (1) Å, c = 27.49 (6) Å, β = 117.8 (3)°, and V= 9496 Å3. At convergence, R = 0.108 and Rw= 0.123 for 1251observed reflections. The structure features an encapsulated two-coordinate Ag+ion with Ir+−Ag+distances of 2.642 (1) Å. The dimen ligands are disordered in a “head to tail” fashion about the iridium metal centers. Homonuclear 31P{1H) δ/J-resolved NMR data for solutions of the [AgIr2(dimen)4(PPh3)2]3+cation show that a statistical distribution of four different geometrical isomers with different “head to tail” orientations of the dimen ligand occurs in the complex.

Original languageEnglish (US)
Pages (from-to)4449-4453
Number of pages5
JournalInorganic chemistry
Volume29
Issue number22
DOIs
StatePublished - 1990

Fingerprint

Dive into the research topics of 'X-ray Crystal Structure and Homonuclear <sup>31</sup>P-<sup>31</sup>P δ/J-Resolved NMR Spectroscopic Studies of [AgIr<sub>2</sub>(dimen)<sub>4</sub>(PPh<sub>3</sub>)<sub>2</sub>](PF<sub>6</sub>)3. Observation of a Statistical Mixture of “Head/Tail” Isomers'. Together they form a unique fingerprint.

Cite this