REMARK 2 REMARK 2 RESOLUTION. 3.00 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.7.3_928) 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 : MLHL REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS) : 3.00 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 38.96 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 1.380 REMARK 3 COMPLETENESS FOR RANGE (%) : 99.9 REMARK 3 NUMBER OF REFLECTIONS : 9841 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.224 REMARK 3 R VALUE (WORKING SET) : 0.221 REMARK 3 FREE R VALUE : 0.290 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.020 REMARK 3 FREE R VALUE TEST SET COUNT : 494 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 38.9678 - 4.7602 1.00 2381 116 0.2155 0.2722 REMARK 3 2 4.7602 - 3.7793 1.00 2326 126 0.1937 0.2577 REMARK 3 3 3.7793 - 3.3019 1.00 2316 138 0.2297 0.3177 REMARK 3 4 3.3019 - 3.0000 1.00 2324 114 0.2673 0.3377 REMARK 3 REMARK 3 BULK SOLVENT MODELLING. REMARK 3 METHOD USED : FLAT BULK SOLVENT MODEL REMARK 3 SOLVENT RADIUS : 1.20 REMARK 3 SHRINKAGE RADIUS : 0.98 REMARK 3 K_SOL : 0.31 REMARK 3 B_SOL : 19.11 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.350 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 29.410 REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : NULL REMARK 3 MEAN B VALUE (OVERALL, A**2) : 47.29 REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2) : 6.49390 REMARK 3 B22 (A**2) : 6.49390 REMARK 3 B33 (A**2) : -12.98780 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 : 0.009 3342 REMARK 3 ANGLE : 1.293 4558 REMARK 3 CHIRALITY : 0.076 511 REMARK 3 PLANARITY : 0.007 584 REMARK 3 DIHEDRAL : 16.229 1175 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 5 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: chain 'J' and (resseq 1:126) REMARK 3 ORIGIN FOR THE GROUP (A): -31.5503 31.7490 -6.1874 REMARK 3 T TENSOR REMARK 3 T11: -0.7415 T22: -1.0875 REMARK 3 T33: -0.5182 T12: -0.9116 REMARK 3 T13: 0.7494 T23: 0.6837 REMARK 3 L TENSOR REMARK 3 L11: 0.2029 L22: 0.4477 REMARK 3 L33: 0.1877 L12: 0.2355 REMARK 3 L13: -0.0913 L23: -0.1928 REMARK 3 S TENSOR REMARK 3 S11: -0.3653 S12: 0.0489 S13: -0.0262 REMARK 3 S21: -0.4390 S22: -0.1142 S23: -0.5395 REMARK 3 S31: 0.1651 S32: 0.1599 S33: -0.7476 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: chain 'J' and (resseq 127:227) REMARK 3 ORIGIN FOR THE GROUP (A): -23.6575 7.0029 15.9286 REMARK 3 T TENSOR REMARK 3 T11: 1.0700 T22: 0.6299 REMARK 3 T33: 0.5881 T12: -0.0143 REMARK 3 T13: 0.5693 T23: 0.2671 REMARK 3 L TENSOR REMARK 3 L11: 0.0408 L22: 0.0271 REMARK 3 L33: 0.0522 L12: 0.0010 REMARK 3 L13: 0.0345 L23: 0.0319 REMARK 3 S TENSOR REMARK 3 S11: -0.0419 S12: 0.2611 S13: -0.1473 REMARK 3 S21: -0.1000 S22: -0.0693 S23: -0.0644 REMARK 3 S31: 0.0679 S32: 0.1442 S33: 0.0097 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: chain 'N' and (resseq 1:115) REMARK 3 ORIGIN FOR THE GROUP (A): -52.3293 24.7266 -2.7558 REMARK 3 T TENSOR REMARK 3 T11: -0.1419 T22: -0.1577 REMARK 3 T33: -0.3518 T12: -0.6472 REMARK 3 T13: 0.2962 T23: 0.4130 REMARK 3 L TENSOR REMARK 3 L11: 0.4225 L22: 0.0332 REMARK 3 L33: 0.4204 L12: -0.0198 REMARK 3 L13: -0.1464 L23: 0.0478 REMARK 3 S TENSOR REMARK 3 S11: -0.2008 S12: -0.4069 S13: -0.1290 REMARK 3 S21: 0.1267 S22: -0.1472 S23: 0.0712 REMARK 3 S31: 0.4966 S32: -0.3217 S33: -0.4691 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: chain 'N' and (resseq 116:152) REMARK 3 ORIGIN FOR THE GROUP (A): -32.6508 7.8000 26.4808 REMARK 3 T TENSOR REMARK 3 T11: 0.7538 T22: 0.4902 REMARK 3 T33: 0.5619 T12: 0.2967 REMARK 3 T13: 0.2903 T23: 0.1710 REMARK 3 L TENSOR REMARK 3 L11: 0.0080 L22: 0.2914 REMARK 3 L33: 0.1745 L12: -0.0292 REMARK 3 L13: 0.0063 L23: -0.1744 REMARK 3 S TENSOR REMARK 3 S11: -0.2210 S12: -0.0817 S13: -0.1358 REMARK 3 S21: -0.1955 S22: -0.1471 S23: -0.4074 REMARK 3 S31: -0.0060 S32: 0.1594 S33: -0.0079 REMARK 3 TLS GROUP : 5 REMARK 3 SELECTION: chain 'N' and (resseq 153:210) REMARK 3 ORIGIN FOR THE GROUP (A): -36.4623 9.1526 29.1341 REMARK 3 T TENSOR REMARK 3 T11: 0.6484 T22: 0.4067 REMARK 3 T33: 0.3937 T12: 0.2695 REMARK 3 T13: 0.2922 T23: 0.6641 REMARK 3 L TENSOR REMARK 3 L11: 0.0892 L22: 0.1163 REMARK 3 L33: 0.1452 L12: -0.0040 REMARK 3 L13: 0.0435 L23: 0.0494 REMARK 3 S TENSOR REMARK 3 S11: -0.1425 S12: -0.0249 S13: -0.0937 REMARK 3 S21: -0.3744 S22: -0.2156 S23: -0.2560 REMARK 3 S31: -0.0351 S32: -0.0074 S33: -0.3379 REMARK 3 REMARK 3 NCS DETAILS REMARK 3 NUMBER OF NCS GROUPS : NULL REMARK 3 REMARK 3 OTHER REFINEMENT REMARKS: NULL REMARK 4 REMARK 4 4HK3 COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 25-OCT-12. REMARK 100 THE RCSB ID CODE IS RCSB075564. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 29-MAY-12 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 : ALS REMARK 200 BEAMLINE : 8.2.2 REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 0.99997 REMARK 200 MONOCHROMATOR : DOUBLE CRYSTAL SI(111) REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : ADSC QUANTUM 315 REMARK 200 INTENSITY-INTEGRATION SOFTWARE : HKL-2000 REMARK 200 DATA SCALING SOFTWARE : HKL REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 16968 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.498 REMARK 200 RESOLUTION RANGE LOW (A) : 50.000 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : NULL REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 100.0 REMARK 200 DATA REDUNDANCY : 15.000 REMARK 200 R MERGE (I) : 0.06000 REMARK 200 R SYM (I) : NULL REMARK 200 FOR THE DATA SET : 8.4000 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 (%): 51.72 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.55 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 1.5 M SODIUM CITRATE, PH 5.0, VAPOR REMARK 280 DIFFUSION, HANGING DROP, TEMPERATURE 298K REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: P 64 REMARK 290 REMARK 290 SYMOP SYMMETRY REMARK 290 NNNMMM OPERATOR REMARK 290 1555 X,Y,Z REMARK 290 2555 -Y,X-Y,Z+1/3 REMARK 290 3555 -X+Y,-X,Z+2/3 REMARK 290 4555 -X,-Y,Z REMARK 290 5555 Y,-X+Y,Z+1/3 REMARK 290 6555 X-Y,X,Z+2/3 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 -0.500000 -0.866025 0.000000 0.00000 REMARK 290 SMTRY2 2 0.866025 -0.500000 0.000000 0.00000 REMARK 290 SMTRY3 2 0.000000 0.000000 1.000000 27.16400 REMARK 290 SMTRY1 3 -0.500000 0.866025 0.000000 0.00000 REMARK 290 SMTRY2 3 -0.866025 -0.500000 0.000000 0.00000 REMARK 290 SMTRY3 3 0.000000 0.000000 1.000000 54.32800 REMARK 290 SMTRY1 4 -1.000000 0.000000 0.000000 0.00000 REMARK 290 SMTRY2 4 0.000000 -1.000000 0.000000 0.00000 REMARK 290 SMTRY3 4 0.000000 0.000000 1.000000 0.00000 REMARK 290 SMTRY1 5 0.500000 0.866025 0.000000 0.00000 REMARK 290 SMTRY2 5 -0.866025 0.500000 0.000000 0.00000 REMARK 290 SMTRY3 5 0.000000 0.000000 1.000000 27.16400 REMARK 290 SMTRY1 6 0.500000 -0.866025 0.000000 0.00000 REMARK 290 SMTRY2 6 0.866025 0.500000 0.000000 0.00000 REMARK 290 SMTRY3 6 0.000000 0.000000 1.000000 54.32800 REMARK 290 REMARK 290 REMARK: NULL REMARK 300 REMARK 300 BIOMOLECULE: 1 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: 3160 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 19950 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -24.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: J, N 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 LYS J 142 REMARK 465 SER J 143 REMARK 465 THR J 144 REMARK 465 SER J 145 REMARK 465 GLY J 146 REMARK 465 SER J 201 REMARK 465 LEU J 202 REMARK 465 GLY J 203 REMARK 465 THR J 204 REMARK 465 SER J 228 REMARK 465 CYS J 229 REMARK 465 ASP J 230 REMARK 465 LYS J 231 REMARK 465 HIS J 232 REMARK 465 HIS J 233 REMARK 465 HIS J 234 REMARK 465 HIS J 235 REMARK 465 HIS J 236 REMARK 465 HIS J 237 REMARK 465 THR N 211 REMARK 465 GLU N 212 REMARK 465 CYS N 213 REMARK 465 SER N 214 REMARK 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: CLOSE CONTACTS IN SAME ASYMMETRIC UNIT REMARK 500 REMARK 500 THE FOLLOWING ATOMS ARE IN CLOSE CONTACT. REMARK 500 REMARK 500 ATM1 RES C SSEQI ATM2 RES C SSEQI DISTANCE REMARK 500 O GLY J 147 OG SER J 199 1.61 REMARK 500 CD1 LEU J 151 CG1 VAL J 224 2.11 REMARK 500 O PRO J 136 OG SER N 123 2.17 REMARK 500 REMARK 500 REMARK: NULL 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 ALA J 16 -163.29 -71.38 REMARK 500 THR J 71 -159.36 -129.35 REMARK 500 ARG J 72 156.06 177.31 REMARK 500 ARG J 104 -75.04 -49.08 REMARK 500 SER J 105 144.32 78.78 REMARK 500 LEU J 137 75.94 -118.59 REMARK 500 ALA J 150 -98.88 -88.10 REMARK 500 LEU J 151 135.74 66.09 REMARK 500 THR J 173 -71.95 -111.27 REMARK 500 HIS J 213 78.99 -111.99 REMARK 500 GLN N 16 -164.95 -77.55 REMARK 500 SER N 31 107.55 73.93 REMARK 500 ASP N 50 -55.35 81.33 REMARK 500 SER N 51 24.34 -154.59 REMARK 500 ALA N 83 -178.79 -176.41 REMARK 500 VAL N 107 79.08 -111.85 REMARK 500 PRO N 143 -179.47 -67.86 REMARK 500 ASN N 171 26.68 -79.49 REMARK 500 GLU N 200 42.35 38.90 REMARK 500 REMARK 500 REMARK: NULL REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 4HK0 RELATED DB: PDB REMARK 900 RELATED ID: 4HKB RELATED DB: PDB REMARK 900 RELATED ID: 4HKX RELATED DB: PDB