Data for Probing intermolecular interactions in a diethylcarbamazine citrate salt by fast MAS 1H solid-state NMR spectroscopy and GIPAW calculations

Specifically, a dihydrogen citrate salt that has improved thermal stability and solubility as compared to the free form is studied. One-dimensional 1H, 13C and 15N and two-dimensional 1H-13C and 14N-1H heteronuclear correlation NMR experiments under moderate and fast MAS together with GIPAW (CASTEP) calculations enable the assignment of the 1H, 13C and 14N/15N resonances.

A two-dimensional 1H-1H double-quantum (DQ) –single-quantum (SQ) MAS spectrum recorded with BaBa recoupling at 60 kHz MAS identifies specific proton-proton proximities associated with citrate-citrate and citrate-diethylcarbamazine intermolecular interactions.<br><br>1.Raw files for the solid-state NMR experiments as recorded by Tiago Venâncio. Figure 1a: 13C CP MAS (5 kHz, 500 MHz): 13C_CPMAS_Fig1a(recorded on 07.11.2016) Figure 1b: 1H single pulse (60 kHz, 600 MHz): 1H_singlepulse_Fig1b(recorded on 28.05.2016) Figure 1c: 15N CP MAS (5 kHz, 500 MHz): 15N_CPMAS_Fig1c (recorded on 26.11.2016) Figure 2a: 1H-1H-DQ-SQ_BABA (60 kHz, 600 MHz): DQ-SQ_BABA_Fig2a(recorded on 28.05.2016) Figures 2b, 3: 1H-13C HETCOR (12.5 kHz, 500 MHz, p15 = 200 µs): 1H-13C-HETCOR_Figs2b_3 (recorded on 02.05.2016) Figure 2c: 14N-1H-HMQC (60 kHz, 600 MHz, l6=4): 14N-1H_HMQC_Fig2c (recorded on 28.05.2016) 2.For the calculations, the initial CIF file, the CIF file after geometry optimization and the magres-file for the full crystal structure.