Table 3. Data-collection and processing statistics (trigonal crystal form).
Values in parentheses are for the highest resolution shell.
| Compound | Apo | Vanadate | S1 | 2 | 4 | 5 | 7 | 10 |
|---|---|---|---|---|---|---|---|---|
| Source | † | ‡ | † | † | † | † | † | † |
| Wavelength | 1.54178 | 1.0 | 1.54178 | 1.54178 | 1.54178 | 1.54178 | 1.54178 | 1.54178 |
| Detector | Rigaku R-AXIS IV++ | ADSC Q210 | Rigaku R-AXIS IV++ | Rigaku R-AXIS IV++ | Rigaku R-AXIS IV++ | Rigaku R-AXIS IV++ | Rigaku R-AXIS IV++ | Rigaku R-AXIS IV++ |
| Crystal-to-detector distance (mm) | 180 | 170 | 150 | 175 | 175 | 175 | 120 | 180 |
| Rotation range/image (°) | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Total rotation range (°) | 180 | 180 | 120 | 180 | 180 | 180 | 120 | 180 |
| Exposure time per image (min) | 4 | 5 s | 3 | 3 | 3 | 8 | 4 | 4 |
| Space group | P3221 | P3221 | P3221 | P3221 | P3221 | P3221 | P3221 | P3221 |
| Unit-cell parameters (Å, °) | a = b = 75.2, c = 152.3 | a = b = 75.4, c = 151.0 | a = b = 75.5, c = 152.1 | a = b = 75.5, c = 152.9 | a = b = 75.4, c = 153.8 | a = b = 75.7, c = 152.2 | a = b = 75.5, c = 152.6 | a = b = 75.5, c = 151.8 |
| Mosaicity range (°) | 1.3–2.0 | 0.5–0.6 | 0.4 | 0.8–1.4 | 0.7–1.1 | 0.7–0.9 | 1.0–1.1 | 0.4–0.9 |
| Resolution range (Å) | 50–2.41 (2.5–2.41) | 50–1.8 (1.86–1.80) | 50–2.05 (2.12–2.05) | 50–2.40 (2.49–2.4) | 50–2.26 (2.34–2.26) | 50–2.26 (2.34–2.26) | 50–2.05 (2.12–2.05) | 50–2.40 (2.49–2.4) |
| Total No. of measured reflections§ | 169546 (≥13336) | 494573 (≥35913) | 215486 (≥1681) | 163183 (≥14661) | 227584 (≥18692) | 213656 (≥18020) | 217352 (≥19837) | 164368 (≥15531) |
| Unique reflections | 19097 (1795) | 45117 (4250) | 30938 (2844) | 20534 (2008) | 24039 (2373) | 23970 (2282) | 32729 (3202) | 20275 (1989) |
| Multiplicity | 8.9 (8.6) | 11.0 (10.5) | 7.0 (7.2) | 7.9 (7.9) | 9.5 (9.0) | 8.9 (8.7) | 6.6 (6.7) | 8.1 (8.6) |
| Completeness (%) | 96.0 (92.0) | 96.6 (92.1) | 95.6 (89.9) | 99.8 (100) | 99.7 (99.7) | 98.2 (96.2) | 99.7 (99.7) | 99.5 (99.4) |
| Rmerge¶ (%) | 18.6 (53.7) | 7.3 (61.4) | 4.0 (13.9) | 18.6 (65.1) | 9.8 (52.1) | 10.9 (41.6) | 7.3 (67.8) | 20.7 (78.1) |
| Mean I/σ(I) | 8.0 (4.3) | 24.1 (4.1) | 37.6 (14.4) | 9.0 (3.5) | 16.4 (4.7) | 14.5 (5.4) | 18.0 (3.2) | 9.2 (4.6) |
| Overall B from Wilson plot (Å2) | 58 | 32 | 31 | 58 | 50 | 49 | 42 | 54 |
†
Rigaku FR-E running at 45 kV and 45 mA and equipped with Rigaku VariMaxHR confocal optics.
‡
Beamline 17-ID (IMCA-CAT) at the Advanced Photon Source at Argonne National Laboratory, Argonne, Illinois, USA as configured in 2005–2006.
§
If any reflections are measured more than four times then one cannot extract from HKL-2000 output the total number of measured reflections in a shell but merely a lower limit, hence the use of the ≥ sign.
¶
R
merge = 
, where I
i(hkl) is the ith observation of reflection hkl and 〈I(hkl)〉 is the weighted average intensity for all observations i of reflection hkl.