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Updated: May 1, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
Solid-state NMR studies for the determination of 11B electric field-gradient tensor orientations in P/B Frustrated
Thomas Wiegand1, Melanie Siedow1, Olga Ekkert2
1Institut für Physikalische Chemie and Graduate School of Chemistry, WWU Münster, Corrensstrasse 30, D 48149 Münster, Germany.
Abstract:
A solid state NMR method is described for measuring the angle Θ specifying the orientation of the principal component of the (11)B electric field gradient tensor relative to the (11)B(…31)P internuclear vector of (11)B-(31)P spin pairs. It is based on the anisotropic dephasing of (11)B spins in the dipolar field of (31)P nuclei via (11)B{(31)P} Rotational Echo DOuble Resonance (REDOR) experiments. The method is applied to four solid borane-phosphane compounds related to Frustrated Lewis Pair (FLP) chemistry. Results determined by numerical line shape simulations are found in excellent agreement with theoretically calculated values using advanced DFT methods. The angle Θ, which can be measured with an estimated precision of ±5°, offers a clear spectroscopic distinction between classical Lewis-acid/base adducts and active Frustrated Lewis pairs (FLPs).
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