Table 1.
Crystallographic data and refinement parameters
| Data set | Space group* | Cell dimensions, Å | Resolution, Å | Reflections (no.)
|
Completeness,† % | Rsym (I),‡ % | I/σ | Rcryst,§ % | Rfree,¶ % | rms deviation bond lengths, Å | rms deviation bond angles, deg | |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| Overall | Unique | |||||||||||
| Native | I213 | a = 131.17 | 10 − 1.75 | 104,019 | 36,586 | 96.7 (91.6) | 4.9 (33.8) | 20.5 (4.0) | 19.8 | 24.4 | 0.010 | 2.30 |
| C146 tethered N-tosyl-d-proline | P63 | a = 126.22 c = 67.02 | 10 − 2.00 | 97,445 | 41,001 | 98.8 (94.5) | 4.4 (26.0) | 14.7 (4.1) | 19.8 | 26.8 | 0.010 | 2.59 |
| L143C tethered N-tosyl-d-proline | P63 | a = 126.33 c = 67.12 | 10 − 2.15 | 78,793 | 32,045 | 96.7 (92.1) | 8.1 (28.6) | 12.8 (4.5) | 19.6 | 26.7 | 0.014 | 3.06 |
| Noncovalent N-tosyl-d-proline | I213 | a = 131.88 | 10 − 1.90 | 202,300 | 31,422 | 100 (100) | 7.4 (28.2) | 19.7 (3.8) | 19.2 | 23.8 | 0.011 | 2.49 |
| Glu-TP | P63 | a = 126.14 c = 66.81 | 10 − 2.00 | 143,599 | 40,497 | 99.4 (96.9) | 8.5 (31.9) | 13.9 (4.0) | 19.4 | 25.1 | 0.007 | 2.15 |
| Glu-TP-β-Ala | P63 | a = 126.03 c = 66.84 | 10 − 1.75 | 142,016 | 58,487 | 95.8 (85.2) | 4.0 (22.5) | 17.1 (4.9) | 18.0 | 21.4 | 0.007 | 2.00 |
This is not a “true” free R factor because the starting model was a fully refined structure. However, the free R factor set of reflections was kept constant for each of the above refinements.
The I213 crystal contains one monomer per asymmetric unit. The P63 form contains the biologically relevant homodimer.
Values in parentheses are for the highest resolution bin.
Rsym (I) = Σhkl|Ihkl〈Ihkl〉|/ΣhklIhkl, where Ihkl is the intensity of reflection hkl.
Rcryst = Σhkl||Fobs| − |Fcalc||/|Fobs|, where Fobs and Fcalc are the observed and calculated structure factors, respectively, for the data used in refinement.
Rfree = Σhkl||Fobs| − |Fcalc||/|Fobs|, where Fobs and Fcalc are the observed and calculated structure factors, respectively, for 10% of the data omitted from refinement.