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. Author manuscript; available in PMC: 2020 Apr 10.
Published in final edited form as: J Am Chem Soc. 2019 Apr 1;141(14):5681–5691. doi: 10.1021/jacs.8b09216

Table 1.

Summary of 19F and 1H signal enhancements in 14.1 T DNP MAS NMR spectra of 5F-Trp,U-13C,15N CA tubular assemblies under different experimental conditions.*

Biradical concentration (mM) T (K) MAS frequency (kHz) Microwave power (mA / W**) 19F DNP polarization buildup time, Tb (s) 19F DNP signal enhancement 1H DNP polarization buildup time, Tb (s) 1H DNP signal enhancement
integrated intensity (isotropic peak) integrated intensity (all side bands) integrated intensity
4.3 120 24 120 / 8.4 11.8 29 37 4.3 63
130 / 10.2 34 45 71
140 / 12.0 38 48 76
150 / 13.8 40 51 77
160 / 15.6 41 53 76
12 120 15 150 / 13.8 11.1 32 36
20 130 / 10.2 68 70
150 / 13.8 77 82
22 130 / 10.2 50 60
150 / 13.8 66 72
15 106 24 110 / 6.6 18.9 37 46
120 140 / 12.0 58.4 72 49
150 / 13.8 1.4 50
125 25 120 / 8.4 14.4 30 36
130 / 10.2 33 39
140 / 12.0 36 43
150 / 13.8 43 51
160 / 15.6 38 44
130 25 130 / 10.2 33 38
160 25 130 / 10.2 12.1 7 8
185 30 130 / 10.2 7 7
22.2 120 24 150 / 13.8 10.9 79 100 1.2 72
28.5 120 24 150 / 13.8 9.5 80 98.5 0.9 65
*

The DNP enhancement factors were calculated as ratios of the integrated peak intensities for maximum peak intensities with and without the microwave irradiation.

**

Microwave power at the end of the waveguide.