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Data for An NMR crystallography investigation of furosemide Miri Zilka (8275890) Jonathan R. Yates (1920148) Steven P. Brown (1296819) Furosemide -- Research Nuclear magnetic resonance Crystallography -- Computer programs Migrated from ePrints This paper presents an NMR crystallography study of three polymorphs of furosemide. Experimental magic-angle spinning (MAS) solid-state NMR spectra are reported for formI of furosemide, and these are assigned using DFT-based GIPAWcalculations. Focusing on the three known polymorphs we examine the changes to theNMRparameters due to crystal packing effects.We use a recently developed formalism to visualise which regions are responsible for the chemical shielding of particular sites, and hence understand the variation inNMRparameters between the three polymorphs.<br><br>Data folders are specified in the readme file for the following: Figure 2 A 13C CP MAS spectrum of furosemide (form I) (black) with the GIPAW calculated chemical shifts for 13C FURSEM01 overlaid in red. Figure 3 Plot of the experimental 13C chemical shifts of furosemide (form I) against the GIPAW calculated absolute isotropic shielding for the twelve carbon atoms in the two distinct furosemide molecules in the asymmetric unit cell (FURSEM01). Figure 4 A 1H (500 MHz)-13C refocused INEPT (12.5 kHz MAS, eDUMBO-122 1H homonuclear decoupling) spectrum, together with skyline projections, of furosemide form I. 256 transients were co-added for each of 26 t1 FIDs, corresponding to a total experimental time of 4 days and 15 hours. The base contour level is at 15%. Crosses (in red) correspond to the GIPAW calculated 13C and 1H chemical shifts for directly bonded CH moieties, using σref = 29.6 ppm for 1H and σref = 168.4 ppm for 13C for the geometry optimised Figure 5 A 1H (500 MHz) DQ MAS (30 kHz) NMR spectrum, together with skyline projections, of furosemide from I, recorded using one rotor period of BABA recoupling. 64 transients were co-added for each of 256 t1 FIDs, corresponding to a total experimental time of 13.8 h. The base contour level is at 7% of the maximum peak height. The F1 = 2F2. diagonal is shown as a dashed line. Horizontal lines (in light blue) indicate pairs of DQ peaks corresponding to close (<3.5 Å) H –H proximities. Crosses represent the GIPAW calculated shift with a dipolar coupling weighting. A partial assignment of the peaks is presented on the spectrum. The number refers to the label of the hydrogen (see Scheme 1) and the superscript to the structures data Figure 6 Decomposition maps visualizing the effect of aromatic ring currents on the NMR chemical shifts of (a) hydrogen 9 in molecule a in FURSEM01 (a) hydrogen 3 in molecule b in FURSEM01 (c) hydrogen 3 in FURSEM14 (d) hydrogen 7 in FURSEM16. 2018-08-16T00:00:00Z Dataset Dataset 10.82444/warw.34014969.v1 https://figshare.com/articles/dataset/Data_for_An_NMR_crystallography_investigation_of_furosemide/34014969 CC BY 4.0