Table 1. X-ray data collection and structure refinement statistics.
| Se-Met gp2C | gp2C | gp2C-K428A:Mg2+ | gp2C-K428A:Mn2+ | gp2C-K428A: Mn2+:BTPe | gp2C-K428A:Ca2+ | |
|---|---|---|---|---|---|---|
| Crystal ID | C1 | A10 | D8 | D1 | F12 | E8 |
| Radiation source | NSLS | APS 23ID-B | APS 23ID-B | APS 23ID-B | APS 23ID-D | APS 23ID-B |
| Wavelength (Å) | 0.97920 | 1.03316 | 1.03316 | 1.03316 | 1.03330 | 1.03319 |
| Resolution (Å) | 64.9–2.44 (2.57–2.44)a | 29.69–1.55 (1.57–1.55) | 29.54–1.52 (1.56–1.52) | 50–1.57 (1.60–1.57) | 28.79–1.86 (1.90–1.86) | 29.6–1.59 (1.59–1.62) |
| Completeness(%) | 98.7(97.2) | 97.7(90.8) | 93.1(97.6) | 97.6(84.5) | 95.4(85.2) | 98.6(90.7) |
| Rmergeb(%) | 14.9(80.4) | 3.3(49.7) | 7.3(38.5) | 4.1(77.6) | 4.1(52.9) | 5.2(81.4) |
| I/σ | 11.0(3.3) | 17.7(1.9) | 9.6(1.8) | 27.0(1.0) | 17.1(2.0) | 16.1(1.2) |
| Redundancy | 7.2 | 3.7 | 3.3 | 3.1 | 3.5 | 3.0 |
| Space group | C2 | C2 | C2 | C2 | P21 | C2 |
| Unit cell (a, b, c, β) | 131.82, 59.5, 46.61, 100.02° | 133.683, 57.734, 46.654, 98.865° | 132.645, 57.519, 46.598, 98.761° | 132.766, 57.365, 46.646, 98.710° | 46.59, 58.42, 53.38, 96.43° | 133.078, 57.437, 46.568, 98.993° |
| Refinement statistics | ||||||
| Rwork/Rfreec | - | 0.14/0.16 | 0.16/0.18 | 0.16/0.19 | 0.17/0.21 | 0.16/0.19 |
| Rmsd bond length/Å | - | 0.009 | 0.009 | 0.009 | 0.007 | 0.006 |
| Rmsd bond angle/° | - | 1.179 | 1.208 | 1.173 | 1.063 | 0.983 |
| Metal | - | 10 mM MgCl2 | 100 mM MgCl2 | 100 mM MnCl2 | 100 mM MnCl2 and 1mM BTP | 10 mM CaCl2 |
| Soaking time | - | 16 h | 5 min | 5 min | 2 h | 1.5 h |
| Metal ions/ligand in the active site | - | None | Two Mg2+ | Two Mn2+ | Two Mn2+ and one BTP | One Ca2+ |
| Metal ion(s) occupancy | - | - | 0.88/0.96 | 0.89/0.68 | 1.0/1.0d | 1.0d |
| B-factor(Å2) | - | - | 19.6/45.5 | 31.9/65.0 | 25.7/27.4 | 33.1 |
aValues in the parentheses are for the outermost resolution shells.
bRmerge = ΣhklΣi|Ii(hkl) − <I(hkl)>| / ΣhklΣiIi(hkl), where Ii(hkl) is the observed intensity of reflection hkl and <I(hkl)> is the averaged intensity of symmetry-equivalent measurements
cRwork = Σhkl∥Fobs| − |Fcalc∥ / Σhkl|Fobs|, where Fobs and Fcalc are structure factors of the observed reflections and those calculated from the refined model, respectively. Rfree has the same formula as Rwork, except that it was calculated against a test set of the data that was not included in the refinement.
dOccupancy not refined.
eBTP, β-thujaplicinol.