Table 1. Data-collection and refinement statistics.
Values in parentheses are for the outer shell.
| X-ray/neutron analysis† | Neutron analysis | X-ray (1.72 Å)/neutron analysis | |||
|---|---|---|---|---|---|
| PDB entry 6l9c † | PDB entry 7wno | PDB entry 7wnp | |||
| X-ray | Neutron | Neutron | X-ray | Neutron | |
| Data collection | |||||
| Beamline | BL5A, PF | BL03, J-PARC | BL5A, PF | ||
| Wavelength (Å) | 1.0 | 3.0–5.7 | 1.0 | ||
| Space group | C2 | C2 | |||
| a, b, c (Å) | 157.55, 61.78, 92.23 | 157.21, 61.98, 92.45 | |||
| α, β, γ (°) | 90, 112.13, 90 | 90, 112.13, 90 | |||
| Resolution range (Å) | 50.00–1.14 (1.16–1.14) | 20.94–1.72 (1.78–1.72) | 44.55–1.72 (1.82–1.72) | ||
| R int | 0.069 (0.801) | 0.188 (0.596) | 0.053 (0.240) | ||
| 〈I/σ(I)〉 | 46.6 (2.00) | 4.99 (1.03) | 9.27 (2.54) | ||
| Completeness (%) | 99.4 (99.9) | 87.4 (66.6) | 93.1‡ (91.3) | ||
| Multiplicity | 5.2 (3.5) | 2.66 (1.62) | 1.91‡ (1.90) | ||
| Observed reflections | 1526790 | 203270 | 308652 | ||
| Unique reflections | 296297 (14901) | 76306 (5748) | 161381 (25556) | ||
| Refinement | |||||
| Resolution range (Å) | 45.03–1.14 (1.15–1.14) | 20.95–1.72 (1.74–1.72) | 20.95–1.72 (1.74–1.72) | 32.06–1.72 (1.73–1.72) | 21.00–1.72 (1.74–1.72) |
| R work | 0.1678 (0.3071) | 0.1865 (0.3215) | 0.1632 (0.2639) | 0.1569 (0.2475) | 0.1912 (0.3194) |
| R free | 0.1821 (0.3207) | 0.2146 (0.3428) | 0.2568 (0.3386) | 0.1894 (0.3100) | 0.2348 (0.3595) |
| Average B factors (Å2) | |||||
| Protein | 24.63 | 20.37 | 20.06 | ||
| Ligands (TPQ/Cu2+) | 23.33 | 18.21 | 17.72 | ||
| Waters | 39.77 | 41.08 | 35.54 | ||
| R.m.s. deviations | |||||
| Bond lengths (Å) | 0.028 | 0.006 | 0.010 | ||
| Bond angles (°) | 1.026 | 1.141 | 1.265 | ||
| No. of solvent atoms | 1063 | 1115 [719§] | 960 [806§] | ||
| No. of multiple conformers | 55 | 21 | 4 | ||
| Ramachandran plot (%) | |||||
| Favoured regions | 96.2 | 96.7 | 96.8 | ||
| Allowed regions | 3.7 | 3.1 | 3.0 | ||
| Outliers | 0.1 | 0.2 | 0.2 | ||
†
Data from Murakawa et al. (2020 ▸).
‡
The low values of completeness and multiplicity are due to the elimination of some reflection spots with an elliptical shape (presumably derived from a distorted portion of the crystal) in the integration process.
§
Number of water molecules detected at approximately the same location (within 1.0 Å) as those detected by X-ray/neutron analysis.