TABLE 1.
Data collection and crystallographic refinement statistics
| AGAOPEA | AGAOHTA | AGAOETA/HCl | AGAOPEA/NaBr | AGAOPEA/NaCl | AGAONaBr | |
|---|---|---|---|---|---|---|
| Soaking conditions | 4 mm 2-PEA, anaerobic | 10 mm histamine, anaerobic | 50 mm ethylamine-HCl, anaerobic | 4 mm 2-PEA, 300 mm NaBr, anaerobic | 4 mm 2-PEA, 100 mm NaCl, anaerobic | 300 mm NaBr, aerobic |
| Protein Data Bank code | 3X3X | 3X3Y | 3X3Z | 3X41 | 3X40 | 3X42 |
| Data collection | ||||||
| Temperature (K) | 100 | 100 | 100 | 100 | 100 | 100 |
| Wavelength (Å) | 0.9 | 0.9 | 0.9 | 0.919 | 0.9 | 0.919 |
| Space group | C2 | C2 | C2 | C2 | C2 | C2 |
| Unit-cell dimensions | ||||||
| a, b, c (Å) | 191.66, 62.89, 158.01 | 193.47, 63.25, 157.91 | 192.55, 62.73, 157.65 | 191.62, 63.29, 157.85 | 191.81, 63.02, 158.11 | 192.68, 63.51, 158.10 |
| β (degrees) | 117.48 | 117.73 | 117.62 | 117.21 | 117.29 | 117.55 |
| Resolution limit (Å) | 38.5–1.57 (1.65–1.57) | 50.0–1.50 (1.53–1.50) | 38.5–1.51 (1.59–1.51) | 47.3–1.87 (1.97–1.87) | 26.5–1.85 (1.95–1.85) | 100–1.89 (1.96–1.89) |
| No. of observations | 1,511,400 | 1,700,730 | 1,862,064 | 503,626 | 520,004 | 935,217 |
| No. of unique reflections | 228,324 | 264,870 | 260,515 | 137,175 | 142,096 | 267,101 |
| I/σ (I)a | 5.3 (1.9) | 26.1 (19.1) | 17.3 (4.0) | 13.0 (2.6) | 10.1 (3.5) | 6.6 (1.7) |
| Redundancya | 6.6 (6.2) | 6.4 (6.0) | 7.1 (6.9) | 3.7 (3.5) | 3.7 (3.8) | 3.5 (3.2) |
| Overall completeness (%)a | 98.1 (96.0) | 98.1 (97.4) | 99.8 (99.8) | 98.7 (97.2) | 99.2 (98.8) | 99.3 (98.7) |
| Overall Rmerge (%)a,b | 9.3 (39.2) | 8.8 (42.5) | 9.2 (40.4) | 9.1 (35.1) | 11.2 (38.2) | 5.6 (34.7) |
| Wilson B factor (Å2) | 13.85 | 13.84 | 11.87 | 16.52 | 16.85 | 19.81 |
| No. of molecules/asymmetric unit | 2 | 2 | 2 | 2 | 2 | 2 |
| Refinement statistics | ||||||
| Resolution limit (Å) | 20.4–1.57 (1.59–1.57) | 36.5–1.50 (1.52–1.50) | 22.3–1.51 (1.53–1.51) | 37.1–1.87 (1.89–1.87) | 26.2–1.85 (1.87–1.85) | 24.7–1.89 (1.90–1.88) |
| Residues in the core φψ region (%) | 96.4 | 96.7 | 96.3 | 96.4 | 96.2 | 96.5 |
| No. of atoms/asymmetric unit | 11,032 | 11,413 | 11,677 | 11,201 | 11,118 | 11,191 |
| No. of solvent atoms | 1170 | 1236 | 1527 | 1134 | 1239 | 1198 |
| Average temperature factors | ||||||
| Protein | 18.5 | 17.5 | 17.5 | 21.5 | 24.0 | 23.2 |
| Ligand/ion | 29.1 | 35.0 | 33.2 | 38.9 | 37.3 | 48.2 |
| Solvent | 29.2 | 29.2 | 31.8 | 34.7 | 33.3 | 34.5 |
| Root mean square deviation from ideal values | ||||||
| Bond lengths (Å) | 0.011 | 0.012 | 0.011 | 0.014 | 0.013 | 0.009 |
| Bond angles (degrees) | 1.049 | 1.078 | 1.153 | 1.112 | 1.077 | 1.083 |
| Rwork (%)a,c | 21.5 (26.2) | 16.2 (22.4) | 16.1 (20.3) | 15.2 (20.5) | 21.2 (28.1) | 15.8 (22.6) |
| Rfree (%)a,d | 24.3 (30.5) | 17.7 (25.7) | 17.8 (21.9) | 18.0 (23.7) | 26.4 (34.1) | 19.0 (27.9) |
| Ramachandran plot statistics (%) | ||||||
| Residues in favored regions | 96.4 | 96.7 | 96.3 | 96.3 | 96.1 | 96.6 |
| Residues in allowed regions | 3.6 | 3.3 | 3.5 | 3.7 | 3.7 | 3.4 |
| Outliers | 0 | 0 | 0.2 | 0 | 0.2 | 0 |
a Values in parentheses refer to data for the highest resolution shells.
b Rmerge = ΣhΣi|Ih,1 − 〈Ih〉|/ΣhΣi Ih,1, where Ih,1 is the intensity value of the ith measurement of h, and 〈Ih〉 is the corresponding mean value of Ih for all i measurements.
c Rwork = Σ‖Fo| − |Fc‖/Σ|Fo|.
d Rfree is an R factor of the refinement evaluated for 5% of reflections that were excluded from the refinement.