Table 2.
Crystallization data collection and refinement statistics
| HAO N27A ligand-free | HAO N27A ClHAA-bound | HAO I142A ligand-free | HAO I142A ClHAA-bound | HAO I142A 3-HAA-bound | HAO I142P ligand-free | HAO I142P ClHAA-bound | HAO I142P 3-HAA-bound | |
|---|---|---|---|---|---|---|---|---|
| Data collection | ||||||||
| Space group | P6522 | P6522 | P6522 | P6522 | P6522 | P6522 | P6522 | P6522 |
| Cell dimensions a, b, c (Å) | 58.4, 58.4, 230.5 | 58.6, 58.6, 236.3 | 58.9, 58.9, 232.1 | 58.3, 58.3, 239.6 | 58.4, 58.4, 230.8 | 58.5, 58.5, 232.2 | 58.7, 58.7, 231.9 | 58.9, 58.9, 232.3 |
| Resolution | 50–1.90 (1.97–1.90)a | 50–2.10 (2.18–2.10) | 50–1.90 (1.93–1.90) | 50–2.31 (2.35–2.31) | 50–2.60 (2.64–2.60) | 50–2.22 (2.26–2.22) | 50–1.74 (1.77–1.74) | 50–1.77 (1.80–1.77) |
| No. of observed reflections | 19,292 (1816) | 14,268 (1466) | 20,024 (946) | 10,918 (519) | 7693 (350) | 12,593 (620) | 25,473 (1160) | 24,171 (1151) |
| Redundancy | 10.3 (5.7) | 28.7 (31.4) | 10.8 (8.2) | 17.6 (19.0) | 15.2 (7.5) | 22.5 (22.6) | 26.1 (21.2) | 9.9 (9.0) |
| Completeness (%) | 99.4 (97.3) | 100 (94.3) | 99.9 (99.3) | 99.9 (99.8) | 98.4 (87.1) | 99.8 (100) | 99.5 (92.9) | 98.6 (97.9) |
| I/σ(I) | 16.7 (1.6) | 8.8 (10.3) | 22.9 (3.6) | 17.9 (3.7) | 19.0 (2.2) | 21.9 (4.8) | 42 (3.2) | 30.2 (5.5) |
| Rmerge (%)b | 17.1 (52.2) | 23.6 (39.4) | 11.8 (38.2) | 21.1 (93.3) | 17.8 (43.9) | 18.4 (95.4) | 10.1 (90.9) | 8.2 (31.4) |
| CC1/2c | 0.99 (0.85) | 0.98 (0.98) | 1.00 (0.98) | 0.99 (0.97) | 1.00 (0.93) | 1.00 (0.98) | 1.00 (0.97) | 1.00 (0.99) |
| Refinementd | ||||||||
| Rwork | 19.2 | 22.8 | 19.2 | 20.5 | 19.2 | 20.8 | 19.9 | 18.7 |
| Rfree | 23.2 | 26.7 | 24.1 | 25.5 | 24.9 | 25.2 | 23.7 | 21.6 |
| RMSD bond length (Å)e | 0.007 | 0.011 | 0.007 | 0.009 | 0.007 | 0.008 | 0.006 | 0.006 |
| RMSD bond angles (°) | 0.830 | 0.935 | 0.896 | 0.901 | 0.974 | 1.174 | 0.802 | 0.848 |
| Ramachandran statisticsf | ||||||||
| Preferred (%) | 98.2 | 97.6 | 98.3 | 98.8 | 97.6 | 98.3 | 99.4 | 98.8 |
| Allowed (%) | 1.2 | 2.4 | 1.7 | 1.2 | 1.2 | 1.7 | 0.6 | 1.2 |
| Outliers (%) | 0 | 0 | 0 | 0 | 1.2 | 0 | 0 | 0 |
| Average B-factor (Å2) | ||||||||
| Protein/atoms | 38.7/1382 | 44.4/1377 | 40.0/1428 | 45.8/1401 | 31.3/1377 | 35.3/1408 | 27.5/1408 | 21.9/1414 |
| ClHAA or 3-HAA/atoms | NAg | 53.7/12 | NA | 62.8/12 | 38.0/11 | NA | 30.1/12 | 22.9/11 |
| Tris/atoms | 49.3/8 | 47.6/8 | 39.2/8 | 53.8/8 | NA | 39.0/8 | 31.0/8 | 30.6/8 |
| Iron/atoms | 42.4/2 | 58.4/2 | 36.6/2 | 59.6/2 | 26.2/2 | 48.8/2 | 33.4/2 | 28.8/2 |
| Solvent/atoms | 47.2/143 | 47.8/96 | 46.5/181 | 45.9/68 | 28.9/63 | 37.8/144 | 37.8/264 | 33.0/298 |
| PDB code | 6BVP | 6BVQ | 6BVR | 6BVS | 6CD3 | 6D60 | 6D61 | 6D62 |
a Values in parentheses are for the highest resolution shell.
b Rmerge = ΣhklΣi|Ii(hkl) − I(hkl)|/ΣhklΣiIi (hkl), in which the sum is over all the i measured reflections with equivalent Miller indices hkl, I(hkl) is the averaged intensity of these i reflections, and the grand sum is over all measured reflections in the data set.
c According to Karplus and Diederichs (28).
d All positive reflections were used in the refinement.
e According to Engh and Huber (29).
f Calculated by using MolProbity (30).
g NA, not applicable.