Related Experiment Video
Updated: Aug 13, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
Solid state 13C NMR of 30-crown-10 ether and 30-crown-10.4H2O
1Ottawa-Carleton Chemistry Institute, Department of Chemistry, Carleton University, Canada.
Abstract:
The 13C NMR solution spectra of 30-crown-10 ether and its tetrahydrate show only one resonance at all accessible temperatures. In contrast, the solid state 13C NMR spectrum of the 30-crown-10.4H2O shows two resonances in the ratio of 4:1, separated by 1.2 ppm. In the case of 30-crown-10 itself, six resolvable 13C resonances in the ratio of 4:1:1:2:1:1 are observed in the solid with an overall chemical shift dispersion of 5 ppm. The remarkably different spectral behavior of these two systems in the solid state is discussed in terms of the torsional environments of the crystallographically unique carbons and the results of GIAO calculations of isotropic 13C shieldings for simpler model compounds. Results of dipolar dephased 13C CPMAS spectra indicate that 30-crown-10 does not undergo a large amplitude molecular motion, in contrast to earlier results for 18-crown-6. Only a small amount of residual intensity is found in the dipolar dephased spectrum of 30-crown-10.4H2O, indicating that it also is relatively rigid in the solid.
More Related Videos
09:37Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR
Published on: February 12, 2019
11:38In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework
Published on: February 1, 2020
Related Concept Videos
Crown Ethers
¹H NMR of Labile Protons: Deuterium (²H) Substitution
Carbon-13 (¹³C) NMR: Overview
¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)
2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)
¹³C NMR: ¹H–¹³C Decoupling
A broadband decoupling technique is used to simplify these complex, sometimes overlapping, signals. Broadband decoupling relies on a...