REMARK 2 REMARK 2 RESOLUTION. 2.91 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.7.2_869) 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) : 2.91 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 32.37 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 1.340 REMARK 3 COMPLETENESS FOR RANGE (%) : 82.4 REMARK 3 NUMBER OF REFLECTIONS : 22836 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.216 REMARK 3 R VALUE (WORKING SET) : 0.215 REMARK 3 FREE R VALUE : 0.245 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.150 REMARK 3 FREE R VALUE TEST SET COUNT : 1176 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 32.3752 - 5.8030 1.00 3455 200 0.1985 0.2168 REMARK 3 2 5.8030 - 4.6103 1.00 3294 198 0.1780 0.1879 REMARK 3 3 4.6103 - 4.0287 1.00 3305 157 0.1747 0.2347 REMARK 3 4 4.0287 - 3.6609 0.93 3032 168 0.2322 0.2619 REMARK 3 5 3.6609 - 3.3988 0.81 2621 145 0.2504 0.2705 REMARK 3 6 3.3988 - 3.1986 0.71 2305 110 0.2711 0.3149 REMARK 3 7 3.1986 - 3.0386 0.61 2001 90 0.3046 0.3952 REMARK 3 8 3.0386 - 2.9064 0.51 1647 108 0.3627 0.4298 REMARK 3 REMARK 3 BULK SOLVENT MODELLING. REMARK 3 METHOD USED : FLAT BULK SOLVENT MODEL REMARK 3 SOLVENT RADIUS : 1.10 REMARK 3 SHRINKAGE RADIUS : 0.86 REMARK 3 K_SOL : 0.30 REMARK 3 B_SOL : 42.84 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.830 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 26.610 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) : 37.07690 REMARK 3 B22 (A**2) : -20.49860 REMARK 3 B33 (A**2) : -16.57830 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 : 0.002 6936 REMARK 3 ANGLE : 0.582 9406 REMARK 3 CHIRALITY : 0.038 1017 REMARK 3 PLANARITY : 0.003 1225 REMARK 3 DIHEDRAL : 9.874 2474 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 8 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: chain L and resid 1:110 REMARK 3 ORIGIN FOR THE GROUP (A): -18.5709 34.7147 3.0723 REMARK 3 T TENSOR REMARK 3 T11: 0.1212 T22: 0.0521 REMARK 3 T33: 0.0727 T12: -0.0313 REMARK 3 T13: 0.1011 T23: 0.0401 REMARK 3 L TENSOR REMARK 3 L11: 2.2640 L22: 6.1742 REMARK 3 L33: 3.9616 L12: 1.3374 REMARK 3 L13: 0.4823 L23: 1.2887 REMARK 3 S TENSOR REMARK 3 S11: -0.0018 S12: -0.0913 S13: -0.3297 REMARK 3 S21: 0.1115 S22: 0.0014 S23: -0.2498 REMARK 3 S31: 0.3461 S32: -0.0978 S33: -0.0192 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: chain L and resid 111:214 REMARK 3 ORIGIN FOR THE GROUP (A): -9.7294 19.0577 -26.8495 REMARK 3 T TENSOR REMARK 3 T11: 1.0986 T22: 0.4693 REMARK 3 T33: 0.7017 T12: -0.1420 REMARK 3 T13: 0.5114 T23: -0.1672 REMARK 3 L TENSOR REMARK 3 L11: 1.2843 L22: 0.2512 REMARK 3 L33: 3.6052 L12: 0.3628 REMARK 3 L13: -0.5515 L23: -0.8637 REMARK 3 S TENSOR REMARK 3 S11: 0.0889 S12: 0.3718 S13: 0.0026 REMARK 3 S21: -0.8304 S22: 0.0663 S23: -0.7721 REMARK 3 S31: -0.0090 S32: 0.5634 S33: -0.0835 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: chain H and resid 1:134 REMARK 3 ORIGIN FOR THE GROUP (A): -14.8269 54.6042 -5.0953 REMARK 3 T TENSOR REMARK 3 T11: 0.4593 T22: 0.2750 REMARK 3 T33: 0.3556 T12: -0.0356 REMARK 3 T13: 0.0896 T23: -0.0044 REMARK 3 L TENSOR REMARK 3 L11: 2.9541 L22: 2.9910 REMARK 3 L33: 2.8171 L12: 0.1623 REMARK 3 L13: -1.6700 L23: 0.4177 REMARK 3 S TENSOR REMARK 3 S11: -0.2603 S12: 0.0979 S13: 0.0695 REMARK 3 S21: -0.3574 S22: -0.1022 S23: -0.3868 REMARK 3 S31: -0.3544 S32: 0.1819 S33: 0.3160 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: chain H and resid 135:233 REMARK 3 ORIGIN FOR THE GROUP (A): -20.7734 29.7835 -33.4647 REMARK 3 T TENSOR REMARK 3 T11: 1.2652 T22: 0.4537 REMARK 3 T33: 0.4535 T12: -0.1930 REMARK 3 T13: 0.3738 T23: -0.0363 REMARK 3 L TENSOR REMARK 3 L11: 1.5694 L22: 1.5827 REMARK 3 L33: 4.5237 L12: 0.2374 REMARK 3 L13: -1.1972 L23: -2.4281 REMARK 3 S TENSOR REMARK 3 S11: 0.0988 S12: 0.2044 S13: 0.1829 REMARK 3 S21: -0.8422 S22: 0.2594 S23: -0.1205 REMARK 3 S31: -0.0335 S32: -0.2641 S33: 0.1438 REMARK 3 TLS GROUP : 5 REMARK 3 SELECTION: chain B and resid 1:110 REMARK 3 ORIGIN FOR THE GROUP (A): 4.6093 18.4262 -64.8966 REMARK 3 T TENSOR REMARK 3 T11: 0.6154 T22: 0.3325 REMARK 3 T33: 0.3369 T12: 0.1774 REMARK 3 T13: -0.0429 T23: -0.0399 REMARK 3 L TENSOR REMARK 3 L11: 4.6327 L22: 7.9926 REMARK 3 L33: 1.1276 L12: -2.5251 REMARK 3 L13: -0.2686 L23: -0.5562 REMARK 3 S TENSOR REMARK 3 S11: 0.0995 S12: 0.0109 S13: 0.5413 REMARK 3 S21: -0.0901 S22: -0.0618 S23: -0.6676 REMARK 3 S31: -0.4634 S32: 0.0464 S33: 0.0082 REMARK 3 TLS GROUP : 6 REMARK 3 SELECTION: chain B and resid 111:214 REMARK 3 ORIGIN FOR THE GROUP (A): -25.5597 34.2555 -57.1967 REMARK 3 T TENSOR REMARK 3 T11: 0.7468 T22: 0.2718 REMARK 3 T33: 0.2912 T12: 0.0543 REMARK 3 T13: 0.1962 T23: 0.1144 REMARK 3 L TENSOR REMARK 3 L11: 3.4905 L22: 2.4061 REMARK 3 L33: 5.8762 L12: 1.1246 REMARK 3 L13: -1.9428 L23: -1.0507 REMARK 3 S TENSOR REMARK 3 S11: 0.2251 S12: -0.1614 S13: 0.2935 REMARK 3 S21: 1.0100 S22: -0.0279 S23: 0.6820 REMARK 3 S31: -0.1114 S32: -0.5437 S33: -0.1330 REMARK 3 TLS GROUP : 7 REMARK 3 SELECTION: chain A and resid 1:134 REMARK 3 ORIGIN FOR THE GROUP (A): -3.5055 -1.2299 -60.2756 REMARK 3 T TENSOR REMARK 3 T11: 0.8576 T22: 0.3167 REMARK 3 T33: 0.5676 T12: 0.1951 REMARK 3 T13: -0.0831 T23: 0.0564 REMARK 3 L TENSOR REMARK 3 L11: 5.8183 L22: 2.4733 REMARK 3 L33: 1.3975 L12: -0.6211 REMARK 3 L13: -1.5332 L23: 0.5851 REMARK 3 S TENSOR REMARK 3 S11: 0.1825 S12: -0.3083 S13: -0.9619 REMARK 3 S21: 0.4875 S22: 0.0344 S23: 0.2785 REMARK 3 S31: 0.2694 S32: 0.1301 S33: -0.2015 REMARK 3 TLS GROUP : 8 REMARK 3 SELECTION: chain A and resid 135:233 REMARK 3 ORIGIN FOR THE GROUP (A): -32.1542 22.5157 -67.2865 REMARK 3 T TENSOR REMARK 3 T11: 0.4128 T22: 0.7406 REMARK 3 T33: 0.3284 T12: 0.0277 REMARK 3 T13: 0.0495 T23: 0.1260 REMARK 3 L TENSOR REMARK 3 L11: 4.6058 L22: 7.4527 REMARK 3 L33: 6.0449 L12: 0.7233 REMARK 3 L13: 0.4569 L23: 0.4716 REMARK 3 S TENSOR REMARK 3 S11: 0.1732 S12: 1.2591 S13: 0.0353 REMARK 3 S21: -0.6644 S22: 0.4529 S23: 0.7861 REMARK 3 S31: -0.0099 S32: -1.0650 S33: -0.4872 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 3U46 COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 17-OCT-11. REMARK 100 THE RCSB ID CODE IS RCSB068283. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 22-JUL-11 REMARK 200 TEMPERATURE (KELVIN) : 100 REMARK 200 PH : 4.5 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : APS REMARK 200 BEAMLINE : 22-ID REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 1.00 REMARK 200 MONOCHROMATOR : SI 111 REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : MAR SCANNER 345 MM PLATE REMARK 200 INTENSITY-INTEGRATION SOFTWARE : HKL-2000 REMARK 200 DATA SCALING SOFTWARE : HKL-2000 REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 22893 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.900 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 (%) : 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) : 2.90 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 3.00 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: PHASES REMARK 200 STARTING MODEL: NULL REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 60.36 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 3.10 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 16% PEG 400, 8% PEG 8000, 0.1M REMARK 280 ACETATE PH 4.5, VAPOR DIFFUSION, HANGING DROP, TEMPERATURE 293K REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: P 21 2 21 REMARK 290 REMARK 290 SYMOP SYMMETRY REMARK 290 NNNMMM OPERATOR REMARK 290 1555 X,Y,Z REMARK 290 2555 -X,Y,-Z REMARK 290 3555 X+1/2,-Y,-Z+1/2 REMARK 290 4555 -X+1/2,-Y,Z+1/2 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 0.00000 REMARK 290 SMTRY2 2 0.000000 1.000000 0.000000 0.00000 REMARK 290 SMTRY3 2 0.000000 0.000000 -1.000000 0.00000 REMARK 290 SMTRY1 3 1.000000 0.000000 0.000000 35.30350 REMARK 290 SMTRY2 3 0.000000 -1.000000 0.000000 0.00000 REMARK 290 SMTRY3 3 0.000000 0.000000 -1.000000 81.98800 REMARK 290 SMTRY1 4 -1.000000 0.000000 0.000000 35.30350 REMARK 290 SMTRY2 4 0.000000 -1.000000 0.000000 0.00000 REMARK 290 SMTRY3 4 0.000000 0.000000 1.000000 81.98800 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: 3330 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 20500 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -23.0 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: 3470 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 20170 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -24.0 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 LYS H 129 REMARK 465 SER H 130 REMARK 465 THR H 131 REMARK 465 SER H 132 REMARK 465 GLY H 133 REMARK 465 LYS H 214 REMARK 465 SER H 215 REMARK 465 CYS H 216 REMARK 465 ASP H 217 REMARK 465 LYS H 218 REMARK 465 CYS L 214 REMARK 465 LYS A 129 REMARK 465 SER A 130 REMARK 465 THR A 131 REMARK 465 SER A 132 REMARK 465 GLY A 133 REMARK 465 GLY A 134 REMARK 465 THR A 135 REMARK 465 ALA A 136 REMARK 465 LYS A 214 REMARK 465 SER A 215 REMARK 465 CYS A 216 REMARK 465 ASP A 217 REMARK 465 LYS A 218 REMARK 465 CYS B 214 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 PRO H 41 95.66 -61.26 REMARK 500 VAL H 48 -63.16 -103.10 REMARK 500 TRP H 100N -70.31 -61.77 REMARK 500 THR H 135 -165.48 -125.79 REMARK 500 ASP H 144 72.26 59.59 REMARK 500 SER H 156 -117.30 59.09 REMARK 500 THR H 160 -39.73 -135.61 REMARK 500 TYR L 32 65.94 -116.44 REMARK 500 SER L 52 37.91 -145.62 REMARK 500 THR L 76 -72.71 -53.53 REMARK 500 TYR L 91 34.05 -147.61 REMARK 500 LYS L 190 -52.96 -121.23 REMARK 500 PRO A 41 97.60 -57.46 REMARK 500 VAL A 48 -66.00 -98.28 REMARK 500 TRP A 100N -71.19 -61.99 REMARK 500 ASP A 144 65.75 61.00 REMARK 500 THR A 160 -38.85 -133.22 REMARK 500 TYR B 32 60.72 -117.29 REMARK 500 SER B 52 41.73 -145.38 REMARK 500 THR B 76 -76.43 -54.96 REMARK 500 TYR B 91 36.68 -146.19 REMARK 500 LYS B 190 -53.79 -124.79 REMARK 500 REMARK 500 REMARK: NULL REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 3TCL RELATED DB: PDB REMARK 900 RELATED ID: 3U4B RELATED DB: PDB REMARK 900 RELATED ID: 3U4E RELATED DB: PDB