TABLE 1.
Data collection and refinement statistics
| A. Data collection | |||
| Data set | EMTS peak | Csd6-unbound | Csd6-Ala |
| Beamline sourcea | PLS BL-4A | PF BL-1A | PLS BL-5C |
| Space group | P212121 | P212121 | P212121 |
| a, b, c (Å) | 61.8, 89.6, 128.7 | 63.0, 91.0, 127.8 | 63.4, 90.6, 127.9 |
| X-ray wavelength (Å) | 1.0048 | 1.0000 | 0.9796 |
| Resolution rangeb (Å) | 50.0–2.90 (2.95–2.90) | 50.0–2.03 (2.07–2.03) | 50.0–2.04 (2.08–2.04) |
| No. of total reflectionsb | 373,689 (18,354) | 229,193 (11,715) | 227,623 (11,074) |
| No. of unique reflectionsb | 30,311 (1,515)c | 47,555 (2,343) | 47,575 (2,307) |
| Completeness (%)b | 99.9 (100)c | 98.3 (98.1) | 99.9 (100) |
| 〈I〉/〈σI〉b | 35.0 (4.7)c | 25.0 (3.0) | 29.3 (3.4) |
| Wilson B factor (Å2) | 53.1 | 34.2 | 30.5 |
| Rmergeb,d (%) | 11.0 (73.1)c | 9.5 (47.0) | 8.6 (53.7) |
| B. SAD phasing | Figure of merit (before/after density modification) 0.34/0.66 | ||
| C. Model refinement | |||
| PDB ID code | 4XZZ | 4Y4V | |
| Resolution range (Å) | 30.0–2.03 | 20.0–2.04 | |
| Rwork/Rfreee (%) | 19.6/24.8 | 19.1/24.2 | |
| No. of non-hydrogen atoms/average B-factor (Å2) | |||
| Total | 5,589/40.6 | 5,606/37.8 | |
| Protein | 5,248/40.4 | 5,249/38.7 | |
| Water oxygen | 323/41.5 | 315/40.5 | |
| Glycerol | 18/63.4 | 24/58.9 | |
| d-Ala | −/− | 18/44.6 | |
| R.m.s. deviations from ideal geometry | |||
| Bond lengths (Å)/angles (°) | 0.009/1.33 | 0.010/1.39 | |
| R.m.s. Z-scores | |||
| Bond lengths (Å)/angles (°) | 0.46/0.61 | 0.49/0.65 | |
| Ramachandran (%)f | |||
| Favored/outliers | 98.6/0.00 | 98.4/0.00 | |
| Poor rotamers (%)f | 0.00 | 0.70 | |
a PF and PLS stand for Photon Factory, Japan, and Pohang Light Source, Korea, respectively.
b Values in parentheses refer to the highest resolution shell.
c Friedel pairs were treated as separate observations.
d Rmerge = ΣhΣi|I(h)i − 〈I(h)〉|/ΣhΣiI(h)i, where I(h) is the intensity of reflection h; Σh is the sum over all reflections, and Σi is the sum over i measurements of reflection h.
e Rwork = Σ‖Fobs| − |Fcalc‖/Σ|Fobs|, where Rfree is calculated for a randomly chosen 5% of reflections, which were not used for structure refinement, and Rwork is calculated for the remaining reflections.
f Values were obtained using MolProbity.