Nuclear Magnetic Resonance (NMR) Spectroscopy of Inorganic/Organometallic Molecules

Abstract

NMR spectroscopy is an indispensable spectroscopic tool for the characterization of inorganic compounds. This contribution provides a guide to the application of recent advances in high‐resolution, solid‐state, and high‐pressure NMR spectroscopic methods to organometallic/inorganic molecules and solids. The topics covered include methods for the determination of structure, intermolecular interactions, solid‐state organization, reaction kinetics, and diffusion.

The Aromatization of C5 Rings on a Heteronuclear Cluster

“…The cyclopentenyl ligand bridges one of the metal-metal edges in a µ,η 1 :η 2 manner. This bonding mode has been previously encountered, for example, in Os 4 (µ-H) 3 (CO) 11 -(µ,η 1 :η 2 -C 6 H 9 ), [2b,18] Os 4 (µ-H) 3 (CO) 11 (µ,η 1 :η 2 -CHCHPh), [19] Os 3 (µ-H)(CO) 10 (µ,η 1 :η 2 -CHCHCH 2 CH 3 ), Os 3 (µ-H)(CO) 10 (µ,η 1 :η 2 -CHCH 2 ), and Os 3 (µ-H)(CO) 10 (µ,η 1 :η 2 -CHCHPh).…”

“…Furthermore, a comparison of the hydride chemical shift for 2d (δ = -18.34 ppm) with that reported for the tetraosmium analogue, Os 4 (µ-H)(CO) 9 (µ-CO) 2 (η 5 -Cp*) (δ = -20.71 ppm), [9] shows that replacement of the osmium atom at the apex of the tetrahedron with the relatively more electronegative ruthenium atom results in a decrease in electron density at the hydride. [10] Some of the reactions with the C 5 carbocyclic rings also afforded other minor products other than 2. The reaction of 1 with propylcyclopentane afforded, after TLC separation, unreacted 1, Os 3 (µ-H) 2 (CO) 10 (a decomposition product of 1), 2c, and another novel cluster Ru 2 Os 3 (µ-H) 2 (CO) 13 (µ-CO)(µ 3 ,η 5 :σ 2 -C 5 H 3 C 3 H 7 ) (3).…”

“…[10] Some of the reactions with the C 5 carbocyclic rings also afforded other minor products other than 2. The reaction of 1 with propylcyclopentane afforded, after TLC separation, unreacted 1, Os 3 (µ-H) 2 (CO) 10 (a decomposition product of 1), 2c, and another novel cluster Ru 2 Os 3 (µ-H) 2 (CO) 13 (µ-CO)(µ 3 ,η 5 :σ 2 -C 5 H 3 C 3 H 7 ) (3). Clusters 2c and 3 could not be separated by chromatographic methods although NMR integration suggested that they were present in a ratio of 5:2.…”

Synthesis and antimicrobial activities of sulfonohydrazide‐substituted 8‐hydroxyquinoline derivative and its oxinates

“…[43,44] Disappearance of this signal in the spectrum of Zn(II) complex suggested that this proton had been lost due to coordination of oxygen atom to the metal ion. [45] The signal due to H 2 of Zn(II) complex appeared at very low magnetic field compared with that of ligand, suggesting the involvement of N 1 in the formation of complex. The protons of N (1) and N (2) in AHQMBSH and its Zn(II) complex resonated as a singlet at δ 10.74, δ 12.48 and δ 10.71, δ 12.47 ppm respectively.…”

“…All the quinoline protons shifted slightly downfield, except H 7 , which shifted slightly upfield. [45,46] a Zone of inhibition (mm) obtained upon subtraction of control (DMSO) ≈11.…”