TABLE 1.
Data collection and refinement statistics
Values in parentheses are for the highest resolution shell. r.m.s.d., root mean square deviation.
| PaaK1 ATP | PaaK1 intermediate | PaaK2 intermediate | |
|---|---|---|---|
| Data collection | |||
| Space group | P1 | P1 | P21 |
| a, b, c (Å) | 56.71, 62.47, 78.49 | 57.26, 62.38, 76.60 | 69.15, 81.97, 80.89 |
| α, β, γ | 90.97, 109.81, and 106.51° | 91.14, 108.35, and 106.28° | 90.00, 97.27, and 90.00° |
| Wavelength (Å) | 0.9792 | 1.5418 | 0.97884 |
| Resolution (Å) | 40.00-1.60 (1.69-1.60) | 27.01-1.92 (2.02-1.92) | 30.00-1.90 (2.0-1.90) |
| Measured reflections | 482,646 (69,360) | 262,037 (36,580) | 28,3830 (31,225) |
| Unique reflections | 121,839 (17,505) | 68,731 (9729) | 69,914 (9527) |
| Redundancy | 4.0 (4.0) | 3.8 (3.8) | 4.1 (3.1) |
| Completeness (%) | 95.8 (94.1) | 93.8 (90.8) | 96.0 (92.9) |
| I/σ(I) | 8.6 (2.2) | 15.2 (2.7) | 9.2 (3.1) |
| Rmergea | 0.084 (0.497) | 0.056 (0.444) | 0.094 (0.327) |
| Refinement statistics | |||
| Resolution range (Å) | 29.98–1.60 (1.64–1.60) | 27.01–1.92 (1.97–1.92) | 40.99–1.90 (1.95–1.90) |
| Rcrystb | 0.166 (0.302) | 0.1806 (0.327) | 0.168 (0.232) |
| Rfreec | 0.193 (0.331) | 0.2319 (0.433) | 0.214 (0.289) |
| No. of atoms | |||
| Protein (chain A, B) | 3344, 3366 | 3317, 3312 | 3339, 3327 |
| Solvent | 952 | 664 | 860 |
| ATP | 62 | N/A | N/A |
| Phenylacetyl Adenylate | N/A | 64 | 64 |
| Phenylacetate | N/A | 10 | N/A |
| Glycerol | 30 | N/A | N/A |
| Thiocyanate | 27 | N/A | N/A |
| β-mercaptoethanol | 20 | 12 | 4 |
| PEG | 12 | 17 | 32 |
| Mg | 6 | 4 | 2 |
| B-values (Å2) | |||
| Protein (chain A, B) | 21.33, 18.55 | 26.63, 32.98 | 19.74, 19.54 |
| Solvent | 34.34 | 38.45 | 31.12 |
| ATP | 14.14 | N/A | N/A |
| Phenylacetyl adenylate | N/A | 21.74 | 12.52 |
| Phenylacetate | N/A | 63.95 | N/A |
| Glycerol | 34.20 | N/A | N/A |
| Thiocyanate | 44.56 | N/A | N/A |
| β-mercaptoethanol | 55.46 | 47.31 | 44.40 |
| PEG | 45.17 | 51.53 | 48.34 |
| Mg | 19.78 | 38.46 | 22.12 |
| R.m.s.d. from ideality | |||
| Bond lengths (Å) | 0.009 | 0.005 | 0.007 |
| Bond angles | 1.199° | 0.798° | 0.962° |
| Ramachandran statistics (%) | |||
| Most favored | 92.7 | 91.4 | 92.1 |
| Allowed | 7.1 | 8.5 | 7.5 |
| Disallowed | 0.0 | 0.0 | 0.0 |
a Rmerge = ΣhklΣi|Ihkl,i − [Ihkl]|/ΣhklΣiIhkl,i, where [Ihkl] is the average of symmetry related observations of a unique reflection.
b Rcryst = Σ|Fobs − Fcalc/ΣFfobs, where Fobs and Fcalc are the observed and the calculated structure factors, respectively.
c Rfree is R using 5% of reflections randomly chosen and omitted from refinement.