Table 1

Crystallographic data and structure statistics.

Crystal form12
Data collection *
Space groupI222I222
Unit cell dimensions (Å)130.7 by 224.8 by 369.4122.7 by 223.0 by 376.1
Wavelength (Å)1.283 1.291
Resolution (Å)40–3.1 (3.2–3.1) 40–2.8 (2.9–2.8)
Unique reflections98,315 (9,073) 125,251 (12,023)
Completeness (%)99.2 (92.7) 99.0 (96.2)
Redundancy4.73.6
Mosaicity (°)0.440.36
Rsym(%)§8.4 (29.8) 5.8 (34.4)
Refinement
Nonhydrogen atoms28,17328,379
Protein residues35433559
Water molecules078
Metal ions8 Zn2+, 1 Mg2+ 8 Zn2+, 1 Mn2+
Anisotropic scaling (B 11,B 22, B 33)−7.9, 11.3, 6.7−14.2, 4.3, 9.9
rmsd bonds (Å)0.0080.007
rmsd angles (°)1.501.43
Reflections in test set (%)4,778 (4.8)3,800 (3.0)
Rcryst/Rfree|22.9/28.322.9/28.2
  • * Data for form 1 are from (9). Data collection for form 2 was carried out at 100 K as described (9) with an ADSC Quantum 4 charge-coupled device detector at beamline 9-2 of SSRL. Diffraction data were processed with DENZO and SCALEPACK (79).

  • Data for form 1 were collected at the Zn2+ anomalous peak to reveal native Zn2+sites. Data for form 2 were collected below the Zn2+anomalous peak energy to localize the Mn2+ ion at the active center.

  • Values in parentheses correspond to the highest resolution shells.

  • § Rsymi,h|I(i,h) − 〈I(h)〉|/Σi,h|I(i,h)|, where 〈I(h)〉 is the mean of the Iobservations of reflection h. Rsymwas calculated with anomalous pairs merged; no σ cut-off was applied.

  • | Rcryst/free = ΣhFobs(h)| − |Fcalc(h)∥/Σh|Fobs(h)|.Rcryst and Rfree were calculated from the working and test reflection set, respectively.