Table 4.
Chemical Shift Tensors of SeM in GB1 Variants Measured by Solid-State NMRa
| T (K) | MAS (kHz) | δiso (ppm) | δCSA (ppm) | ηCSA | δ11 (ppm) | δ22 (ppm) | δ33 (ppm) | FWHMb (Hz) | Int1:Int 2c | Δδiso/ΔT (ppm/K) |
|---|---|---|---|---|---|---|---|---|---|---|
| 77Se Selenomethionine | ||||||||||
| 299 | 3 (site 1) | 117.4 | −322 | 0.51 | 363 | 198 | −203 | 217 | 1.0:0.8 | 0.04 (site 1) |
| 299 | 3 (site 2) | 78.9 | −300 | 0.36 | 285 | 178 | −219 | 323 | ||
| 292 | 3 (site 1) | 117.4 | −321 | 0.58 | 371 | 184 | −203 | 148 | 1.0:0.7 | |
| 292 | 3 (site 2) | 76.0 | −304 | 0.41 | 291 | 165 | −228 | 207 | ||
| 267 | 3 (site 1) | 117.0 | −335 | 0.53 | 374 | 195 | −218 | 154 | 1.0:1.1 | 0.24 (site 2) |
| 267 | 3 (site 2) | 70.5 | −317 | 0.36 | 286 | 172 | −247 | 189 | ||
| 248 | 3 (site 1) | 115.2 | −336 | 0.55 | 375 | 191 | −220 | 178 | 1.0:1.0 | |
| 248 | 3 (site 2) | 66.3 | −334 | 0.42 | 304 | 163 | −268 | 193 | ||
| 77Se GB1 L5SeM | ||||||||||
| 293 | 5 (site 1) | 111.3 | −256 | 0.31 | 279 | 199 | −145 | 93d | 1.0:1.0 | −0.09 (site 1) |
| 293 | 5 (site 2) | 110.1 | −259 | 0.35 | 284 | 195 | −149 | 118d | ||
| 279 | 5 (site 1) | 111.8 | −251 | 0.40 | 287 | 187 | −139 | 82d | 1.0:1.1 | |
| 279 | 5 (site 2) | 110.9 | −260 | 0.33 | 283 | 199 | −149 | 84d | ||
| 270 | 5 | 112.2 | −268 | 0.37 | 295 | 197 | −155 | 118 | NA | |
| 260 | 5 | 112.8 | −273 | 0.38 | 301 | 198 | −161 | 239 | NA | |
| 249 | 5 | 114.7 | −283 | 0.38 | 310 | 203 | −168 | 867 | NA | |
| 77Se GB1 I6SeM | ||||||||||
| 293 | 5 (site 1)e | 79.1 | −149 | 0.00 | 154 | 154 | −70 | 357 | ~1.0:0e | 0.17 (site 1) |
| 279 | 5 (site 1) | 76.9 | −155 | 0.10 | 161 | 148 | −78 | 847 | 1.0:0.2 | |
| 279 | 5 (site 2)f | 90.8 | −97 | 0.10 | 147 | 132 | −6 | 1036 | ||
| 270 | 5 (site 1) | 75.8 | −161 | 0.35 | 184 | 128 | −85 | 1094 | 1.0:0.3 | |
| 270 | 5 (site 2)f | 88.2 | −114 | 0.40 | 167 | 123 | −25 | 759 | ||
| 77Se GB1 V29SeM | ||||||||||
| 293 | 5 (site 1) | 100.0 | −275 | 0.32 | 281 | 194 | −175 | 72d | 1.0:1.0 | −0.12 (site 1) |
| 293 | 5 (site 2) | 98.1 | −273 | 0.34 | 281 | 188 | −175 | 74d | ||
| 279 | 5 | 100.3 | −282 | 0.34 | 289 | 194 | −182 | 310 | NA | |
| 270 | 5 | 100.8 | −283 | 0.33 | 288 | 196 | −182 | 438 | NA | |
| 260 | 5 | 101.5 | −284 | 0.28 | 283 | 204 | −183 | 764 | NA | |
| 249 | 5f | 104.6 | −318 | 0.33 | 316 | 211 | −213 | 1881 | NA | |
| 77Se GB1 V39SeM | ||||||||||
| 293 | 5 (site 1) | 91.8 | −287 | 0.58 | 318 | 153 | −195 | 154d | 1.0:0.3 | 0.01 (site 1) |
| 293 | 5 (site 2) | 89.5 | −274 | 0.51 | 297 | 157 | −185 | 168d | ||
| 279 | 5 (site 1) | 91.1 | −291 | 0.56 | 318 | 155 | −200 | 163d | 1.0:0.2 | |
| 279 | 5 (site 2) | 88.7 | −266 | 0.60 | 302 | 142 | −177 | 185d | ||
| 270 | 5 | 90.4 | −294 | 0.57 | 321 | 154 | −204 | 191 | NA | |
| 260 | 5 | 90.3 | −296 | 0.58 | 324 | 153 | −206 | 263 | NA | |
| 249 | 5 | 90.0 | −309 | 0.59 | 336 | 154 | −219 | 617 | NA | |
a
The error for the chemical shift tensor parameters extracted by Topspin-SOLA is estimated to be ±3% based on signal-to-noise.
b
The FWHM is reported as natural line width (no line broadening parameter was applied).
c
“Int1:Int2” means (peak intensity of site 1):(peak intensity of site 2).
d
The overlapping peaks were deconvolved using Topspin-SOLA.
e
For GB1 I6SeM, 293 K, MAS of 5 kHz, site 2 was not fitted due to low signal-to-noise.
f
For GB1 I6SeM, 279 K, site 2, GB1 I6SeM, 270 K, site 2, and GB1 V29SeM, 249 K, the fitting is the least accurate because of the low signal-to-noise of these two resonances.