Table 2. X-ray and neutron data collection and processing.
Values in parentheses are for the outer shell.
| Neutron | X-ray | |
|---|---|---|
| Diffraction source | MaNDi, ORNL | Rigaku MicroMax-007 HF rotating-anode generator, ORNL |
| Wavelength (Å) | 2–4 | 1.5417 |
| Temperature (K) | 293 | 293 |
| Detector | 32 Anger cameras | R-AXIS IV |
| Crystal-to-detector distance (mm) | 420–450 | 120 |
| Rotation range per image (°) | 0† | 0.25 |
| Total rotation range (°) | 90 | 132 |
| Exposure time per image (s) | 48 h | 30 s |
| Space group | H3 | H3 |
| a, b, c ‡ (Å) | 83.16, 83.16, 294.32 | 83.64, 83.64, 294.78 |
| Resolution range (Å) | 14.63–2.20 (2.28–2.20) | 19.65–1.74 |
| Total No. of reflections | 29653 | 73470 |
| No. of unique reflections | 2344 | 3850 |
| Completeness (%) | 76.1 (60.3) | 93.3 (49.2) |
| Multiplicity | 2.5 (1.6) | 3.6 (3.3) |
| 〈I/σ(I)〉 | 5.7 (2.1) | 10.8 (2.4) |
| R merge | 0.173 (0.223) | 0.061 (0.409) |
| Overall B factor from Wilson plot (Å2) | 18.2 |
†
Still quasi-Laue diffraction images were collected at 10° steps in φ rotation at three unique crystal orientations and were combined into a single data set.
‡
The absolute unit-cell parameters determined from X-ray monochromatic data were used in refinement. The axial ratios from Laue refinement scale to the absolute cell.