Table 2.
Data collection and Refinement Statistics for inhibitor-complexed CDOsa
| CDO form | Wild-type | C93A | Y157F | Wild-type | C93A |
|---|---|---|---|---|---|
| soak | Hcy | Hcy | Hcy | azide | D-Cys |
| nominal pH | 8.0 | 8.0 | 8.0 | 6.2 | pH 8.0 |
| Data collection | |||||
| Resolution (Å) | 41-1.35 (1.37-1.35) |
34-1.30 (1.32-1.30) |
33-1.65 (1.68-1.65) |
34-1.50 (1.58-1.50) |
42-1.35 (1.37-1.35) |
| Unique Obs. | 43919 (1521) |
43282 (896) |
25597 (1236) |
33827 (4812) |
46343 (2257) |
| Multiplicity | 23.8 (10.3) | 26.7 (17.9) | 27.4 (22.8) | 11.8 (11.9) | 53.5 (36.7) |
| Completeness | 94.9 (68) | 84.2 (36.2) | 98.9 (95.2) | 100 (100) | 100 (100) |
| <I/ρ> | 23.7 (1.0) | 21.3 (1.2) | 26.3 (2.0) | 8.6 (0.6) | 17.4 (0.8) |
| Rmeasc (%) | 8.0 (245) | 10.5 (251) | 9.1 (199) | 18.2 (538) | 25.0 (614) |
| CC1/2d | 1.0 (0.26) | 1.0 (0.33) | 1.0 (0.60) | 1.0 (0.17) | 1.0 (0.22) |
| Refinement | |||||
| Rcryst / Rfree (%) | 16.2/19.1 | 15.7/18.6 | 16.9/21.0 | 17.2/21.0 | 16.9/20.0 |
| No. Obs | 43838 | 43245 | 25071 | 33667 | 46118 |
| No. residues | 186 | 186 | 186 | 186 | 186 |
| No. waters | 280 | 302 | 182 | 214 | 321 |
| No. atoms | 1914 | 1907 | 1749 | 1785 | 1914 |
| rmsd angles (°) | 1.36 | 1.27 | 1.33 | 1.31 | 1.01 |
| rmsd lengths (Å) | 0.011 | 0.010 | 0.013 | 0.012 | 0.008 |
| φ,ψ-favored (%)e | 99.0 | 99.0 | 99.5 | 99.5 | 99.0 |
| <B> protein (Å2) | 23 | 20 | 40 | 28 | 23 |
| <B> ligand (Å2) | 40 | 33 | 30 | 47 | 16 |
| PDB code | 4XF4 | 4XF9 | 4XFA | 4PJY | 5I0R |
a
All refinements used space group P43212 with a=b=57.60 Å and c= 122.40 Å. Numbers in parentheses refer to the highest resolution bin.
b
Soak solution at pH 8, but pH sensitive loop conformation indicates pH ~ 7 (see27 and methods)
c
Rmeas is the multiplicity-weighted merging R-factor65
d
CC1/2 is the correlation between two datasets each based on half of the data as defined in Karplus & Diederichs.62
e
Ramachandran statistics as defined by Molprobity64, no φ,ψ-outliers in any structures