Table 1. Crystal data-collection and refinement statistics.
Values in parentheses are for the highest resolution shell.
| Form I | Form II | Form III | |
|---|---|---|---|
| Data collection | |||
| Beamline | BL-5C, PLS | BL-7A, PLS | I04, DLS |
| Wavelength (Å) | 0.98 | 0.98 | 0.98 |
| Resolution range (Å) | 40.0–2.1 | 40.0–3.2 | 77.0–3.4 |
| Space group | P212121 | P43212 | P3121 |
| a, b, c (Å) | 30.610, 89.955, 114.961 | 67.621, 67.621, 190.646 | 80.890, 80.890, 153.910 |
| α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 |
| Observations (total/unique) | 379872/20447 | 14009/7877 | 47017/9603 |
| Completeness (%) | 99.8 (99.7) | 100 (100) | 99.5 (99.2) |
| R merge † | 0.079 (0.261) | 0.105 (0.757) | 0.112 (2.663) |
| CC1/2 | 0.99 (0.98) | 0.98 (0.89) | 0.99 (0.51) |
| Multiplicity | 6.0 (6.2) | 7.4 (7.4) | 4.9 (5.1) |
| 〈I/σ(I)〉 | 29.0 (15.5) | 24.7 (7.0) | 7.9 (0.9) |
| Refinement | |||
| R work/R free ‡ (%) | 20.9/24.7 | 21.5/26.4 | 20.6/27.7 |
| Average B value (Å2) | 35.4 | 99.6 | 126.4 |
| R.m.s.d., bond lengths (Å) | 0.010 | 0.009 | 0.009 |
| R.m.s.d., angles (°) | 1.693 | 1.697 | 1.849 |
| Ramachandran plot (%) | |||
| Favoured | 98.88 | 89.32 | 82.74 |
| Allowed | 1.12 | 7.83 | 13.74 |
| Disallowed | 0 | 2.85 | 4.09 |
†
Rmerge = \textstyle \sum_{hkl}\sum_{i}|I_{i}(hkl)- \langle I(hkl)\rangle|/\textstyle \sum_{hkl}\sum_{i}I_{i}(hkl), where Ii (hkl) is the ith measured intensity of reflection hkl and 〈I(hkl)〉 is the mean of all measured intensities of reflection hkl.
‡
Rwork = \textstyle \sum_{hkl}\big ||F_{\rm obs}|-|F_{\rm calc}|\big |/ \textstyle \sum_{hkl}|F_{\rm obs}|, where F obs is the observed structure-factor amplitude and F calc is the structure factor calculated from the model. R free is computed in the same manner as R work but from a test set containing 5% of the data, which were excluded from the refinement calculation.