Table 1. X-ray Crystallographic Data Collection and Refinement Statistics for Macrocyclic β-Sheet Peptide 3.
| Crystal parameters | |
| space group | C2 |
| a, b, c (Å) | 32.174, 62.852, 20.094 |
| α, β, γ (deg) | 90.00, 89.98, 90.00 |
| molecules per asymmetric unit | 2 |
| Data collection | |
| synchrotron beamline | SSRL beamline 7–1 |
| wavelength (Å) | 1.00 |
| resolution (Å) | 17.56–1.75 (1.81–1.75) |
| total reflectionsa | 14845 (1450) |
| unique reflectionsa | 4060 (398) |
| completeness (%)a | 99.2 (97.1) |
| multiplicitya | 3.7 (3.6) |
| Rmerge (%)a,b | 3.6 (6.3) |
| CC1/2 (%)a | 99.8 (99.6) |
| CC* (%)a | 100 (99.9) |
| I/σ(I)a | 25.4 (13.4) |
| Refinement | |
| resolution (Å) | 1.75 |
| Rwork (%)c | 17.9 |
| Rfree (%)d | 22.0 |
| RMS bond lengths (Å) | 0.010 |
| RMS bond angles (deg) | 1.52 |
| ligands | 2-methyl-2,4-pentanediol (2) |
| water | 43 |
| Ramachandran favored (%) | 100 |
| Ramachandran outliers (%) | 0 |
| Wilson B-factor (Å2) | 18.5 |
| average B-factor (Å2) | 22.6 |
| twinning | –h, −k, l (α = 0.49) |
a
Statistics for the highest resolution shell are shown in parentheses.
b
Rmerge = ∑|I – ⟨I⟩|/∑I.
c
Rwork = ∑|Fobs – Fcalc|/∑Fobs.
d
Rfree was computed as Rwork using a cross-validation set of 10% nonredundant data.