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oai:figshare.com:article/33844702 2026-09-16T11:47:14Z portal_1197 item_type_3 month_year_09_2026

Data for Combining heteronuclear correlation NMR with spin-diffusion to detect relayed Cl–H–H and N–H–H proximities in molecular solids Parth Raval (11173179) Julien Trébosc (2690671) Tomasz Pawlak (1475584) Yusuke Nishiyama (719611) Steven P. Brown (1296819) G. N. Manjunatha Reddy (11428211) Nuclear magnetic resonance Nuclear magnetic resonance spectroscopy Crystallography Solid state chemistry Molecular crystals Migrated from ePrints Analysis of short-to-intermediate range intermolecular interactions offers a great way of characterizing the solid-state organization of small molecules and materials. This can be achieved by two-dimensional (2D) homo- and heteronuclear correlation NMR spectroscopy, for example, by carrying out experiments at high magnetic fields in conjunction with fast magic-angle spinning (MAS) techniques. But, detecting 2D peaks for the heteronuclear dipolar coupled spin pairs separated by greater than 3 Å is not always straightforward, particularly when low-gamma quadrupolar nuclei are involved. Here, we present a 2D correlation NMR experiment that combines the advantages of heteronuclear-multiple quantum coherence (HMQC) and proton-based spin-diffusion (SD) pulse sequences using radio-frequency-driven-recouping (RFDR) to probe inter and intramolecular 1H-X (X = 14N, 35Cl) interactions. This experiment can be used to acquire 2D 1H{X}-HMQC filtered 1H–1H correlation as well as 2D 1H-X HMQC spectra. Powder forms of dopamine·HCl and l-histidine·HCl·H2O are characterized at high fields (21.1 T and 18.8 T) with fast MAS (60 kHz) using the 2D HMQC-SD-RFDR approach. Solid-state NMR results are complemented with NMR crystallography analyses using the gauge-including projector augmented wave (GIPAW) approach. For histidine·HCl·H2O, 2D peaks associated with 14N–1H–1H and 35Cl–1H–1H distances of up to 4.4 and 3.9 Å have been detected. This is further corroborated by the observation of 2D peaks corresponding to 14N–1H–1H and 35Cl–1H–1H distances of up to 4.2 and 3.7 Å in dopamine·HCl, indicating the suitability of the HMQC-SD-RFDR experiments for detecting medium-range proximities in molecular solids.<br><br>Dataset for following figures: Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure S1 Figure S2 Figure S3 Figure S4 Figure S8 Figure S9 Figure S10 2022-06-21T00:00:00Z Dataset Dataset 10.82444/warw.33844702.v1 https://figshare.com/articles/dataset/Data_for_Combining_heteronuclear_correlation_NMR_with_spin-diffusion_to_detect_relayed_Cl_H_H_and_N_H_H_proximities_in_molecular_solids/33844702 CC BY 4.0