Table 1. Summary of data-collection and analysis statistics.
| Laue neutron diffraction | Monochromatic neutron diffraction | X-ray diffraction | |
|---|---|---|---|
| Data collection | |||
| Beamline | LADI-III at ILL | D19 at ILL | ID23-1 at ESRF |
| Temperature (K) | 293 | 293 | 293 |
| Wavelength () | 3.244.18 | 2.42 | 0.9791 |
| Resolution () | 43.682.00 (2.112.00) | 52.212.30 (2.422.30) | 52.281.85 (1.951.85) |
| No. reflections measured | 69034 (6128) | 40015 (4199) | 76578 (10682) |
| No. unique reflections | 13480 (1524) | 11358 (1613) | 21718 (3060) |
| Completeness (%) | 78.3 (62.1) | 99.3 (98.7) | 99.4 (97.9) |
| No. of images | 23 | N/A | 180 |
| Oscillation angle () | Step angle = 7 | Scan step 0.07 | 0.5 |
| Exposure time per image (s) | 18470 (5.13hours per image) | 87 or 173 | 0.1 (beam attenuated to 0.74%) |
| Space group | P21212 | P21212 | P21212 |
| Unit-cell parameters ()† | a = 43.68, b = 86.26, c = 65.72 | a = 43.68, b = 86.26, c = 65.72 | a = 43.68, b = 86.26, c = 65.72 |
| R merge | 0.182 (0.337) | 0.152 (0.645) | 0.093 (0.420) |
| R p.i.m. | 0.078 (0.162) | 0.096 (0.470) | 0.057 (0.254) |
| Multiplicity | 5.1 (4.0) | 3.5 (2.6) | 3.5 (3.5) |
| Mean I/(I) | 7.3 (3.4) | 7.7 (1.6) | 7.4 (2.6) |
| Wilson B factor (2) | 15.7 | 14.9 | 19.8 |
| Refinement | Joint NX | Joint NX | X only |
| Resolution range () | N: 36.382.00 (2.072.00) | N: 52.282.30 (2.532.30) | 43.131.95 (2.001.95) |
| X: 43.131.95 (2.001.95) | X: 43.131.95 (2.051.95) | ||
| PDB code | 4pvm | 4pvn | 4pvl |
| No. reflections N | 13391 (923) | 11395 (2630) | |
| No. reflections X | 18655 (1274) | 18655 (2512) | 18656 (1274) |
| Completeness (%) N | 76.9 (60.0) | 98.6 (98.0) | |
| Completeness (%) X | 99.4 (100.0) | 99.4 (100.0) | 99.5 (100.0) |
| R work N | 0.209 (0.280) | 0.209 (0.258) | |
| R work X | 0.153 (0.173) | 0.156 (0.185) | 0.152 (0.175) |
| R free N | 0.271 (0.320) | 0.262 (0.322) | |
| R free X | 0.203 (0.220) | 0.185 (0.226) | 0.201 (0.198) |
| No. protein atoms | 3630 | 3680 | 1815 (no H or D) |
| No. main-chain amide-H atoms with Hocc > 0.5 | 29 | 34 | 0 |
| No. D2O, DO, O-only molecules | 36, 12, 41 | 30, 18, 36 | 148 |
| R.m.s.d. bond length () | 0.013 | 0.012 | 0.011 |
| R.m.s.d. bond angles () | 1.354 | 1.309 | 1.282 |
| Average B factors (2) | |||
| Main chain (A/B) | 18.5/23.4 | 23.1/29.1 | 20.7/25.4 |
| Side chain (A/B) | 23.7/28.6 | 29.3/35.7 | 28.7/33.2 |
| Solvent | 26.8 | 46.4 | 40.9 |
| Ramachandran statistics (%) | |||
| Favoured | 98.3 | 98.3 | 97.8 |
| Allowed | 1.3 | 1.3 | 2.2 |
†
X-ray cell dimensions were used for both neutron structures.