TABLE 2.
Statistics of data collection and refinement
| Crystal form/PDB code | H77_X1/2XI2 | H77_X2/2XI3 | J4_02/2XHU | J4*_02/2XHV | J4_T/2XHW |
|---|---|---|---|---|---|
| Soaking conditions (immediately before cryocooling) | 80 μm CUGGC, 0.9 mm GTP, 0.14 m AmSO4, 25% PEG 5000 MME,d MES 0.1 m pH 6.5, 18% glycerol | 100 μm CUGGC, 10 mm GTP, 10 mm MgCl2, 25% PEG 5000 MME, MES 0.05 m pH 6.5, 20% glycerol | 0.2 m MgSO4, 25% PEG 2000 MME, 0.05 m HEPES pH 7.0, 15% glycerol | 0.2 m MgSO4, 25% PEG 2000 MME, 0.05 m HEPES pH 7.0, 15% glycerol | 0.2 m NaF, 8% PEG 3350, 0.05 m HEPES pH 7.0, 30% glycerol |
| Space group and cell parameters (Å, °) | P21 53.3 272.4 61.0 90 98.75 90 | P1 54.0 91.9 61.1 89.6 99.7 92.9 | P212121 106.5 107.8 133.8 90 90 90 | P212121 105.7 107.7 133.8 90 90 90 | P 32 2 1 125.4 125.4 140.1 90 90 120 |
| Number of molecules in the asymmetric unit | 3 | 2 | 2 | 2 | 1 |
| Resolution range (Å)a | 43.1-1.8 (1.85–1.8) | 30–1.7 (1.73-1.70) | 48.1-2.3 (2.37-2.29) | 34.7-1.9 (1.97-1.9) | 19.7–2.6 (2.72-2.66) |
| Rsymb | 0.082 (0.353) | 0.044 (0.348) | 0.15 (0.546) | 0.069 (0.359) | 0.20 (0.73) |
| I/σI | 13.2 (1.9) | 14.5 (2.0) | 12.90 (2.36) | 16.72 (3.21) | 8.59 (2.55) |
| Completeness (%) | 91.9 (81.6) | 95.5 (94.0) | 98.2 (97.1) | 98.5 (88.6) | 99.2 (92.4) |
| Unique reflections measured | 144,615 | 12,1329 | 69,005 | 118,899 | 36,792 |
| Average multiplicity | 2.9 (1.9) | 1.9 (1.8) | 5.5 (3.7) | 4.5 (2.9) | 9.1 (6.4) |
| Root mean square deviation bonds(Å)/angles(°) | 0.006/1.009 | 0.009/1.036 | 0.007/1.013 | 0.008/1.025 | 0.008/1.139 |
| R/Rfree (%)c | 16.6/20.7 (19.5/25.0) | 17.0/19.8 (27.3/32.0) | 16.5/21.6 (20.9/27.2) | 17.1/19.9 (22.3/27.2) | 17.2/22.0 (24.5/32.0) |
a In parentheses, statistics for the highest resolution shell.
b Rsym was determined by the equation R = ΣhklΣj|Ihkl,j − 〈Ihkl〉|/ΣhklΣjIhkl, where h, k, and l are the unique indices of all reflections measured more than once, and j the index for symmetry-redundant reflections.
c R and Rfree were determined by the equation R = Σhkl‖Fobs| − k |Fcalc‖/Σhkl|Fob‖, where h, k, and l are the indices of the reflections used in refinement (R) or of 5% of the reflections set aside and not used in refinement (Rfree). The same set of reflections was used for Rfree in all structures. Fobs is the structure factor deduced from the measured intensities, and Fcalc is the structure factor calculated from the model. k is a scale factor to put the Fcalc on the same scale as the Fobs.
d MME, monomethyl-ether.