Table 3. Data collection and processing.
Values in parentheses are for the outer shell.
| Native | Osmate derivative | |
|---|---|---|
| Diffraction source | Beamline ID29, ESRF | Beamline ID29, ESRF |
| Wavelength (Å) | 1.03320 | 1.13937 |
| Temperature (K) | 100 | 100 |
| Detector | PILATUS 6M, Dectris | PILATUS 6M, Dectris |
| Crystal-to-detector distance (mm) | 454.54 | 484.71 |
| Rotation range per image (°) | 0.05 | 0.15 |
| Total rotation range (°) | 100 | 3 × 360† |
| Exposure time per image (s) | 0.04 | 0.04 |
| Space group | H32 | H32 |
| a, b, c (Å) | 140.82, 140.82, 205.71 | 141.26, 141.26, 206.22 |
| α, β, γ (°) | 90, 90, 120 | 90, 90, 120 |
| Mosaicity (°) | 0.111 | 0.166 |
| Resolution range (Å) | 49.12–2.40 (2.49–2.40) | 49.33–2.77 (2.92–2.77) |
| Total No. of reflections | 171405 (18652) | 1062487 (68326) |
| No. of unique reflections | 30873 (3223) | 20468 (2938) |
| Completeness (%) | 99.6 (100) | 100 (100) |
| Multiplicity | 5.6 (5.8) | 51.9 (23.3) |
| 〈I/σ(I)〉 | 12.0 (1.3)‡ | 17.4 (1.7)§ |
| R r.i.m. ¶ | 0.081 (1.561) | 0.228 (2.517) |
| R p.i.m. †† | 0.034 (0.646) | 0.030 (0.502) |
| Overall B factor from Wilson plot (Å2) | 62.7 | 75.0 |
†
Recorded at κ = 0, 20 and 40°.
‡
The crystal exhibited anisotropic X-ray diffraction, with resolutions of 2.71 and 2.4 Å in the hk plane and along the l axis, respectively (according to the CC1/2 > 0.5 criterion of AIMLESS). The mean I/σ(I) in the outer shell falls below 2.0 at 2.57 Å resolution.
§
The crystal exhibited anisotropic X-ray diffraction, with resolutions of 2.85 and 2.77 Å in the hk plane and along the l axis, respectively (according to the CC1/2 > 0.5 criterion of AIMLESS). The mean I/σ(I) in the outer shell falls below 2.0 at 2.87 Å resolution.
¶
R
r.i.m. = 
, where 〈I(hkl)〉 is the mean of the observations Ii(hkl) of reflection hkl.
††
R
p.i.m. = 
.