TABLE 1.
Data collection and refinement statistics
The following abbreviations are used: APS, advanced photon source; r.m.s., root mean square; ASU, asymmetric unit.
| Crystal form | I, ligand-free | II, CRF-(22-41)-NH2-bound | III, CRF-(27-41)-NH2-bound |
|---|---|---|---|
| Data collection | |||
| Beamline | APS 21-ID-D | APS 21-ID-F | APS 21-ID-D |
| Space group | P41212 | P1 | P41212 |
| a, b, c | 112.02, 112.02, 145.79 Å | 49.20, 63.48, 85.88 Å | 112.92, 112.92, 158.17 Å |
| α, β, γ | 90.0, 90.0, 90.0° | 99.75, 106.28, 101.67° | 90.0, 90.0, 90.0° |
| Resolution range | 50.00-2.75 Å (2.85-2.75 Å)a | 50.00-1.96 Å (2.03-1.96 Å) | 50.00-3.40 Å (3.52-3.40 Å) |
| Wavelength | 0.97872 Å | 0.97872 Å | 0.99999 Å |
| No. of observations | 335,781 | 217,545 | 100,651 |
| Unique reflections | 24,253 | 64,919 | 14,697 |
| Completeness | 98.4% (90.2%) | 94.7% (75.2%) | 99.4% (97.2%) |
| Redundancy | 13.8 | 3.4 | 6.8 |
| I/σ | 33.26 (2.99) | 13.49 (2.32) | 20.81 (1.88) |
| Rmergeb | 5.9% (57.3%) | 11.3% (33.7%) | 8.5% (73.9%) |
| Mosaicity | 0.441° | 0.909° | 0.623° |
| Refinement | |||
| Resolution range | 50.00-2.76 | 39.50-1.96 | 50.00-3.40 |
| No. of reflections (total/test) | 22,995/1238 | 61,357/3254 | 13,897/739 |
| Rcrystc/Rfreed | 20.7%/24.0% | 20.9%/25.6% | 21.8%/25.2% |
| MBP-ECD molecules/ASU | 1 | 2 | 1 |
| No. of TLS groups | 2 | 6 | 1 |
| Mean B value | 111.60 Å2 | 32.13 Å2 | 156.49 Å2 |
| No. of protein atoms | 3539 | 7044 | 3586 |
| No. of water atoms | 6 | 450 | 0 |
| No. of heterogen atoms | 23 (1 maltose molecule) | 90 (2 maltose, 2 calcium, 2 Bis Tris, and 2 PEG molecules) | 23 (1 maltose molecule) |
| r.m.s. bond length deviation | 0.011 Å | 0.012 Å | 0.006 Å |
| r.m.s. bond angle deviation | 1.233° | 1.285° | 0.997° |
| Ramachandran plot, % residues ine | |||
| Most favored | 91.9 | 92.2 | 89.7 |
| Additional allowed | 7.6 | 7.6 | 9.5 |
| Generously allowed | 0.5 | 0.3 | 0.8 |
| Disallowed | 0 | 0 | 0 |
a
Values in parentheses are for the highest resolution shell.
b
Rmerge = ∑|I - 〈I〉| > |/∑|I|, where I is the intensity measurement for a given reflection, and <I> is the average intensity for multiple measurements of the reflection.
c
Rcryst = ∑(|Fo| - K|Fc|)/∑|Fo|.
d
Rfree was calculated using a randomly selected 5% test set of the total reflections that was omitted from the refinement.
e
Data were as defined in Procheck (42).