4.14. Structure determination by the MAD method and refinement of the structure (III)

The MAD datasets collected at the peak and remote wavelengths were scaled to the dataset collected at the inflection point wavelength with SCALEIT (Collaborative Computational Project Number 4 1994). The initial heavy-atom positions were located with RSPS (Collaborative Computational Project Number 4 1994) and SOLVE (Terwilliger & Berendzen 1999). The two heavy-atom positions found were refined and the phases to 2.5 Å resolution were calculated with the program MLPHARE (Collaborative Computational Project Number 4 1994). The initial maps were improved by solvent-flattening calculations and the phases were extended to 2.15 Å resolution with the DM program (Cowtan & Main 1996), after which the maps were easily interpretable with the O program (Jones et al. 1991). The model of Eci1p monomer was built manually in O. Subsequently, the model was subjected to restrained refinement, using the maximum-likelihood target, with REFMAC (Murshudov et al. 1997). Water molecules were added automatically by the solvent-building mode of the program ARP/wARP (Perrakis et al. 1999). Ethylene glycol and perrhenate molecules were also added into the refinement. The pdb entry code for the perrhenate-complexed yeast enoyl-CoA isomerase is 1HNU.

The unliganded structure (not soaked in perrhenate) of the yeast enoyl-CoA isomerase was solved by rigid body refinement with REFMAC using the perrhenate-complexed structure as the starting model. Further restrained refinement to 2.5 Å resolution was also carried out with REFMAC. The pdb entry code is 1HNO.