REMARK 2 REMARK 2 RESOLUTION. 2.93 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.8.1_1168) REMARK 3 AUTHORS : PAUL ADAMS,PAVEL AFONINE,VICENT CHEN,IAN REMARK 3 : DAVIS,KRESHNA GOPAL,RALF GROSSE- REMARK 3 : KUNSTLEVE,LI-WEI HUNG,ROBERT IMMORMINO, REMARK 3 : TOM IOERGER,AIRLIE MCCOY,ERIK MCKEE,NIGEL REMARK 3 : MORIARTY,REETAL PAI,RANDY READ,JANE REMARK 3 : RICHARDSON,DAVID RICHARDSON,TOD ROMO,JIM REMARK 3 : SACCHETTINI,NICHOLAS SAUTER,JACOB SMITH, REMARK 3 : LAURENT STORONI,TOM TERWILLIGER,PETER REMARK 3 : ZWART REMARK 3 REMARK 3 REFINEMENT TARGET : ML REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS) : 2.93 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 44.13 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 2.030 REMARK 3 COMPLETENESS FOR RANGE (%) : 98.6 REMARK 3 NUMBER OF REFLECTIONS : 21156 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.239 REMARK 3 R VALUE (WORKING SET) : 0.237 REMARK 3 FREE R VALUE : 0.269 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.010 REMARK 3 FREE R VALUE TEST SET COUNT : 1060 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT (IN BINS). REMARK 3 BIN RESOLUTION RANGE COMPL. NWORK NFREE RWORK RFREE REMARK 3 1 44.1378 - 5.8577 0.99 2682 142 0.2388 0.2431 REMARK 3 2 5.8577 - 4.6511 1.00 2579 135 0.2044 0.2630 REMARK 3 3 4.6511 - 4.0636 1.00 2545 134 0.1944 0.2171 REMARK 3 4 4.0636 - 3.6923 1.00 2524 133 0.2374 0.2856 REMARK 3 5 3.6923 - 3.4278 1.00 2507 133 0.2421 0.2584 REMARK 3 6 3.4278 - 3.2257 1.00 2515 133 0.2682 0.3173 REMARK 3 7 3.2257 - 3.0642 1.00 2497 131 0.2987 0.3762 REMARK 3 8 3.0642 - 2.9309 0.90 2247 119 0.3412 0.3437 REMARK 3 REMARK 3 BULK SOLVENT MODELLING. REMARK 3 METHOD USED : FLAT BULK SOLVENT MODEL REMARK 3 SOLVENT RADIUS : 1.11 REMARK 3 SHRINKAGE RADIUS : 0.90 REMARK 3 K_SOL : NULL REMARK 3 B_SOL : NULL REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.420 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 32.010 REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : NULL REMARK 3 MEAN B VALUE (OVERALL, A**2) : NULL REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2) : 6.80850 REMARK 3 B22 (A**2) : -9.01010 REMARK 3 B33 (A**2) : 2.20160 REMARK 3 B12 (A**2) : 0.00000 REMARK 3 B13 (A**2) : 0.00000 REMARK 3 B23 (A**2) : 0.00000 REMARK 3 REMARK 3 TWINNING INFORMATION. REMARK 3 FRACTION: NULL REMARK 3 OPERATOR: NULL REMARK 3 REMARK 3 DEVIATIONS FROM IDEAL VALUES. REMARK 3 RMSD COUNT REMARK 3 BOND : 0.003 6914 REMARK 3 ANGLE : 0.863 9412 REMARK 3 CHIRALITY : 0.058 1038 REMARK 3 PLANARITY : 0.004 1214 REMARK 3 DIHEDRAL : 13.916 2453 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : NULL REMARK 3 REMARK 3 NCS DETAILS REMARK 3 NUMBER OF NCS GROUPS : 2 REMARK 3 NCS GROUP : 1 REMARK 3 NCS OPERATOR : 1 REMARK 3 REFERENCE SELECTION: chain H and (resseq 1:232 ) and (not REMARK 3 element H) and (not element D) REMARK 3 SELECTION : chain A and (resseq 1:232 ) and (not REMARK 3 element H) and (not element D) REMARK 3 ATOM PAIRS NUMBER : 1792 REMARK 3 RMSD : 0.085 REMARK 3 NCS GROUP : 2 REMARK 3 NCS OPERATOR : 1 REMARK 3 REFERENCE SELECTION: chain L and (resseq 2:210 ) and (not REMARK 3 element H) and (not element D) REMARK 3 SELECTION : chain B and (resseq 2:210 ) and (not REMARK 3 element H) and (not element D) REMARK 3 ATOM PAIRS NUMBER : 1531 REMARK 3 RMSD : 0.071 REMARK 3 REMARK 3 OTHER REFINEMENT REMARKS: NULL REMARK 4 REMARK 4 4IML COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 09-JAN-13. REMARK 100 THE RCSB ID CODE IS RCSB076941. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : NULL REMARK 200 TEMPERATURE (KELVIN) : 100 REMARK 200 PH : 5.0 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : SLS REMARK 200 BEAMLINE : X06SA REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : NULL REMARK 200 MONOCHROMATOR : NULL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : MARMOSAIC 225 MM CCD REMARK 200 INTENSITY-INTEGRATION SOFTWARE : XDS REMARK 200 DATA SCALING SOFTWARE : XDS REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 24225 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.795 REMARK 200 RESOLUTION RANGE LOW (A) : 44.133 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : NULL REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : NULL REMARK 200 DATA REDUNDANCY : NULL REMARK 200 R MERGE (I) : NULL REMARK 200 R SYM (I) : NULL REMARK 200 FOR THE DATA SET : NULL REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : NULL REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : NULL REMARK 200 COMPLETENESS FOR SHELL (%) : NULL REMARK 200 DATA REDUNDANCY IN SHELL : NULL REMARK 200 R MERGE FOR SHELL (I) : NULL REMARK 200 R SYM FOR SHELL (I) : NULL REMARK 200 FOR SHELL : NULL REMARK 200 REMARK 200 DIFFRACTION PROTOCOL: SINGLE WAVELENGTH REMARK 200 METHOD USED TO DETERMINE THE STRUCTURE: MOLECULAR REPLACEMENT REMARK 200 SOFTWARE USED: PHASER REMARK 200 STARTING MODEL: NULL REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 49.75 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.45 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 17.5-20 %(W/V) PEG6000, 0.1 M CITRIC REMARK 280 ACID, 0.2 M NDSB-221, PH 5.0, VAPOR DIFFUSION, HANGING DROP, REMARK 280 TEMPERATURE 293K REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: P 21 21 21 REMARK 290 REMARK 290 SYMOP SYMMETRY REMARK 290 NNNMMM OPERATOR REMARK 290 1555 X,Y,Z REMARK 290 2555 -X+1/2,-Y,Z+1/2 REMARK 290 3555 -X,Y+1/2,-Z+1/2 REMARK 290 4555 X+1/2,-Y+1/2,-Z REMARK 290 REMARK 290 WHERE NNN -> OPERATOR NUMBER REMARK 290 MMM -> TRANSLATION VECTOR REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY TRANSFORMATIONS REMARK 290 THE FOLLOWING TRANSFORMATIONS OPERATE ON THE ATOM/HETATM REMARK 290 RECORDS IN THIS ENTRY TO PRODUCE CRYSTALLOGRAPHICALLY REMARK 290 RELATED MOLECULES. REMARK 290 SMTRY1 1 1.000000 0.000000 0.000000 0.00000 REMARK 290 SMTRY2 1 0.000000 1.000000 0.000000 0.00000 REMARK 290 SMTRY3 1 0.000000 0.000000 1.000000 0.00000 REMARK 290 SMTRY1 2 -1.000000 0.000000 0.000000 37.87750 REMARK 290 SMTRY2 2 0.000000 -1.000000 0.000000 0.00000 REMARK 290 SMTRY3 2 0.000000 0.000000 1.000000 79.13300 REMARK 290 SMTRY1 3 -1.000000 0.000000 0.000000 0.00000 REMARK 290 SMTRY2 3 0.000000 1.000000 0.000000 40.27600 REMARK 290 SMTRY3 3 0.000000 0.000000 -1.000000 79.13300 REMARK 290 SMTRY1 4 1.000000 0.000000 0.000000 37.87750 REMARK 290 SMTRY2 4 0.000000 -1.000000 0.000000 40.27600 REMARK 290 SMTRY3 4 0.000000 0.000000 -1.000000 0.00000 REMARK 290 REMARK 290 REMARK: NULL REMARK 300 REMARK 300 BIOMOLECULE: 1, 2 REMARK 300 SEE REMARK 350 FOR THE AUTHOR PROVIDED AND/OR PROGRAM REMARK 300 GENERATED ASSEMBLY INFORMATION FOR THE STRUCTURE IN REMARK 300 THIS ENTRY. THE REMARK MAY ALSO PROVIDE INFORMATION ON REMARK 300 BURIED SURFACE AREA. REMARK 350 REMARK 350 COORDINATES FOR A COMPLETE MULTIMER REPRESENTING THE KNOWN REMARK 350 BIOLOGICALLY SIGNIFICANT OLIGOMERIZATION STATE OF THE REMARK 350 MOLECULE CAN BE GENERATED BY APPLYING BIOMT TRANSFORMATIONS REMARK 350 GIVEN BELOW. BOTH NON-CRYSTALLOGRAPHIC AND REMARK 350 CRYSTALLOGRAPHIC OPERATIONS ARE GIVEN. REMARK 350 REMARK 350 BIOMOLECULE: 1 REMARK 350 AUTHOR DETERMINED BIOLOGICAL UNIT: DIMERIC REMARK 350 SOFTWARE DETERMINED QUATERNARY STRUCTURE: DIMERIC REMARK 350 SOFTWARE USED: PISA REMARK 350 TOTAL BURIED SURFACE AREA: 3520 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 20250 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -24.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: H, L REMARK 350 BIOMT1 1 1.000000 0.000000 0.000000 0.00000 REMARK 350 BIOMT2 1 0.000000 1.000000 0.000000 0.00000 REMARK 350 BIOMT3 1 0.000000 0.000000 1.000000 0.00000 REMARK 350 REMARK 350 BIOMOLECULE: 2 REMARK 350 AUTHOR DETERMINED BIOLOGICAL UNIT: DIMERIC REMARK 350 SOFTWARE DETERMINED QUATERNARY STRUCTURE: DIMERIC REMARK 350 SOFTWARE USED: PISA REMARK 350 TOTAL BURIED SURFACE AREA: 3510 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 20270 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -25.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: A, B REMARK 350 BIOMT1 1 1.000000 0.000000 0.000000 0.00000 REMARK 350 BIOMT2 1 0.000000 1.000000 0.000000 0.00000 REMARK 350 BIOMT3 1 0.000000 0.000000 1.000000 0.00000 REMARK 465 REMARK 465 MISSING RESIDUES REMARK 465 THE FOLLOWING RESIDUES WERE NOT LOCATED IN THE REMARK 465 EXPERIMENT. (M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN REMARK 465 IDENTIFIER; SSSEQ=SEQUENCE NUMBER; I=INSERTION CODE.) REMARK 465 REMARK 465 M RES C SSSEQI REMARK 465 GLU H 235 REMARK 465 CYS H 236 REMARK 465 GLY H 237 REMARK 465 SER H 238 REMARK 465 GLY H 239 REMARK 465 HIS H 240 REMARK 465 HIS H 241 REMARK 465 HIS H 242 REMARK 465 HIS H 243 REMARK 465 HIS H 244 REMARK 465 HIS H 245 REMARK 465 LYS L 211 REMARK 465 SER L 212 REMARK 465 CYS L 213 REMARK 465 GLU A 235 REMARK 465 CYS A 236 REMARK 465 GLY A 237 REMARK 465 SER A 238 REMARK 465 GLY A 239 REMARK 465 HIS A 240 REMARK 465 HIS A 241 REMARK 465 HIS A 242 REMARK 465 HIS A 243 REMARK 465 HIS A 244 REMARK 465 HIS A 245 REMARK 465 GLN B 1 REMARK 480 REMARK 480 ZERO OCCUPANCY ATOM REMARK 480 THE FOLLOWING RESIDUES HAVE ATOMS MODELED WITH ZERO REMARK 480 OCCUPANCY. THE LOCATION AND PROPERTIES OF THESE ATOMS REMARK 480 MAY NOT BE RELIABLE. (M=MODEL NUMBER; RES=RESIDUE NAME; REMARK 480 C=CHAIN IDENTIFIER; SSEQ=SEQUENCE NUMBER; I=INSERTION CODE): REMARK 480 M RES C SSEQI ATOMS REMARK 480 LYS H 13 CG CD CE NZ REMARK 480 LYS H 19 CG CD CE NZ REMARK 480 LYS H 63 CG CD CE NZ REMARK 480 GLU H 82 CG CD OE1 OE2 REMARK 480 ARG H 87 NE CZ NH1 NH2 REMARK 480 ARG H 164 CG CD NE CZ NH1 NH2 REMARK 480 LYS H 167 CG CD CE NZ REMARK 480 GLN H 169 CD OE1 NE2 REMARK 480 LYS H 171 CG CD CE NZ REMARK 480 ASN H 174 CG OD1 ND2 REMARK 480 LEU H 176 CG CD1 CD2 REMARK 480 GLN H 188 CG CD OE1 NE2 REMARK 480 ASP H 189 CG OD1 OD2 REMARK 480 LYS H 191 CG CD CE NZ REMARK 480 ASP H 192 CG OD1 OD2 REMARK 480 LEU H 203 CG CD1 CD2 REMARK 480 LYS H 205 CG CD CE NZ REMARK 480 GLU H 209 CG CD OE1 OE2 REMARK 480 LYS H 210 CG CD CE NZ REMARK 480 LYS H 229 CD CE NZ REMARK 480 PHE H 231 CG CD1 CD2 CE1 CE2 CZ REMARK 480 LYS L 126 CG CD CE NZ REMARK 480 LEU L 186 CG CD1 CD2 REMARK 480 GLN L 189 CG CD OE1 NE2 REMARK 480 LYS L 206 CD CE NZ REMARK 480 LYS L 207 CG CD CE NZ REMARK 480 ARG A 87 CD NE CZ NH1 NH2 REMARK 480 ASP A 144 CG OD1 OD2 REMARK 480 LYS A 148 CG CD CE NZ REMARK 480 ARG A 164 CG CD NE CZ NH1 NH2 REMARK 480 LYS A 167 CG CD CE NZ REMARK 480 GLN A 169 CG CD OE1 NE2 REMARK 480 LYS A 171 CG CD CE NZ REMARK 480 ASP A 173 CG OD1 OD2 REMARK 480 ASN A 174 CG OD1 ND2 REMARK 480 GLN A 177 CG CD OE1 NE2 REMARK 480 GLU A 183 CG CD OE1 OE2 REMARK 480 ASP A 189 CG OD1 OD2 REMARK 480 SER A 190 CB OG REMARK 480 LYS A 191 CG CD CE NZ REMARK 480 LEU A 201 CG CD1 CD2 REMARK 480 LEU A 203 CG CD1 CD2 REMARK 480 LYS A 205 CG CD CE NZ REMARK 480 LYS A 212 CB CG CD CE NZ REMARK 480 GLU A 217 CG CD OE1 OE2 REMARK 480 GLN A 221 CG CD OE1 NE2 REMARK 480 LEU A 223 CG CD1 CD2 REMARK 480 LYS A 229 CG CD CE NZ REMARK 480 PHE A 231 CG CD1 CD2 CE1 CE2 CZ REMARK 480 ARG A 233 CG CD NE CZ NH1 NH2 REMARK 480 LYS B 140 CG CD CE NZ REMARK 480 LYS B 207 CG CD CE NZ REMARK 480 GLU B 209 CG CD OE1 OE2 REMARK 480 LYS B 211 CG CD CE NZ REMARK 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: TORSION ANGLES REMARK 500 REMARK 500 TORSION ANGLES OUTSIDE THE EXPECTED RAMACHANDRAN REGIONS: REMARK 500 (M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN IDENTIFIER; REMARK 500 SSEQ=SEQUENCE NUMBER; I=INSERTION CODE). REMARK 500 REMARK 500 STANDARD TABLE: REMARK 500 FORMAT:(10X,I3,1X,A3,1X,A1,I4,A1,4X,F7.2,3X,F7.2) REMARK 500 REMARK 500 EXPECTED VALUES: GJ KLEYWEGT AND TA JONES (1996). PHI/PSI- REMARK 500 CHOLOGY: RAMACHANDRAN REVISITED. STRUCTURE 4, 1395 - 1400 REMARK 500 REMARK 500 M RES CSSEQI PSI PHI REMARK 500 SER H 128 -74.05 -93.71 REMARK 500 ASN H 180 -49.11 -133.59 REMARK 500 LYS H 191 -75.97 -106.95 REMARK 500 LYS H 212 -0.94 78.66 REMARK 500 ASP L 50 -118.78 54.74 REMARK 500 SER L 124 -71.74 -142.82 REMARK 500 SER A 128 -76.79 -109.51 REMARK 500 ASN A 160 70.17 46.41 REMARK 500 ASP A 173 15.00 55.08 REMARK 500 LYS A 191 -58.07 -127.76 REMARK 500 ASP B 50 -113.73 53.24 REMARK 500 SER B 110 -2.16 64.82 REMARK 500 SER B 124 -72.45 -142.77 REMARK 500 ASP B 141 69.85 62.79 REMARK 500 PRO B 144 -156.61 -92.70 REMARK 500 THR B 157 -39.62 -134.00 REMARK 500 REMARK 500 REMARK: NULL REMARK 800 REMARK 800 SITE REMARK 800 SITE_IDENTIFIER: AC1 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE GOL H 301 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC2 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE GOL B 301 REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 4IMK RELATED DB: PDB REMARK 900 UNCROSSED FAB FRAGMENT