REMARK 2 REMARK 2 RESOLUTION. 1.90 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 : ML REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS) : 1.90 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 36.31 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 1.350 REMARK 3 COMPLETENESS FOR RANGE (%) : 95.5 REMARK 3 NUMBER OF REFLECTIONS : 31363 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.189 REMARK 3 R VALUE (WORKING SET) : 0.187 REMARK 3 FREE R VALUE : 0.223 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 4.720 REMARK 3 FREE R VALUE TEST SET COUNT : 1479 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 36.3198 - 4.2236 0.91 2704 134 0.1651 0.1777 REMARK 3 2 4.2236 - 3.3531 0.94 2699 134 0.1615 0.2015 REMARK 3 3 3.3531 - 2.9295 0.94 2685 132 0.1817 0.2147 REMARK 3 4 2.9295 - 2.6617 0.95 2701 134 0.1996 0.2763 REMARK 3 5 2.6617 - 2.4710 0.97 2776 137 0.2065 0.2619 REMARK 3 6 2.4710 - 2.3253 0.95 2694 134 0.2050 0.2209 REMARK 3 7 2.3253 - 2.2089 0.96 2706 134 0.2033 0.2429 REMARK 3 8 2.2089 - 2.1128 0.97 2735 134 0.1958 0.2360 REMARK 3 9 2.1128 - 2.0314 0.98 2743 137 0.2106 0.2406 REMARK 3 10 2.0314 - 1.9613 0.95 2722 134 0.2183 0.2522 REMARK 3 11 1.9613 - 1.9000 0.97 2719 135 0.2414 0.2916 REMARK 3 REMARK 3 BULK SOLVENT MODELLING. REMARK 3 METHOD USED : FLAT BULK SOLVENT MODEL REMARK 3 SOLVENT RADIUS : 1.00 REMARK 3 SHRINKAGE RADIUS : 0.73 REMARK 3 K_SOL : 0.38 REMARK 3 B_SOL : 43.37 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.230 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 21.490 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) : -6.16530 REMARK 3 B22 (A**2) : 2.18450 REMARK 3 B33 (A**2) : 3.98080 REMARK 3 B12 (A**2) : 0.00000 REMARK 3 B13 (A**2) : -2.77810 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 : 0.007 3466 REMARK 3 ANGLE : 1.234 4715 REMARK 3 CHIRALITY : 0.079 529 REMARK 3 PLANARITY : 0.005 601 REMARK 3 DIHEDRAL : 15.379 1236 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 5 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: (CHAIN H AND RESID 1:90 ) REMARK 3 ORIGIN FOR THE GROUP (A): -10.9370 4.0689 188.2397 REMARK 3 T TENSOR REMARK 3 T11: 0.1046 T22: 0.1747 REMARK 3 T33: 0.1520 T12: -0.0383 REMARK 3 T13: 0.0184 T23: 0.0179 REMARK 3 L TENSOR REMARK 3 L11: 3.1711 L22: 3.8756 REMARK 3 L33: 3.4874 L12: -0.8469 REMARK 3 L13: 0.7590 L23: -0.9016 REMARK 3 S TENSOR REMARK 3 S11: -0.0041 S12: -0.3207 S13: -0.1324 REMARK 3 S21: 0.2058 S22: -0.0224 S23: -0.0714 REMARK 3 S31: -0.0480 S32: -0.0461 S33: 0.0280 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: (CHAIN H AND RESID 91:138 ) REMARK 3 ORIGIN FOR THE GROUP (A): -2.7193 7.1390 183.3925 REMARK 3 T TENSOR REMARK 3 T11: 0.1480 T22: 0.1680 REMARK 3 T33: 0.1538 T12: -0.0259 REMARK 3 T13: 0.0646 T23: 0.0367 REMARK 3 L TENSOR REMARK 3 L11: 1.8703 L22: 0.9707 REMARK 3 L33: 1.8914 L12: 0.1357 REMARK 3 L13: 1.0620 L23: 0.1709 REMARK 3 S TENSOR REMARK 3 S11: -0.0466 S12: -0.4920 S13: -0.0908 REMARK 3 S21: 0.0732 S22: 0.0548 S23: 0.0922 REMARK 3 S31: -0.1729 S32: -0.3138 S33: -0.0022 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: (CHAIN H AND RESID 139:216 ) REMARK 3 ORIGIN FOR THE GROUP (A): 16.1647 8.3065 200.9326 REMARK 3 T TENSOR REMARK 3 T11: 0.2473 T22: 0.3531 REMARK 3 T33: 0.1527 T12: 0.0287 REMARK 3 T13: -0.0381 T23: 0.0244 REMARK 3 L TENSOR REMARK 3 L11: 4.7185 L22: 5.0445 REMARK 3 L33: 3.8069 L12: 1.7566 REMARK 3 L13: 0.5474 L23: 0.5632 REMARK 3 S TENSOR REMARK 3 S11: 0.0219 S12: -0.6887 S13: 0.1785 REMARK 3 S21: 0.3916 S22: -0.0673 S23: 0.0621 REMARK 3 S31: -0.3649 S32: -0.3608 S33: 0.0129 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: (CHAIN L AND RESID 8:105 ) REMARK 3 ORIGIN FOR THE GROUP (A): 0.4892 7.3113 166.9493 REMARK 3 T TENSOR REMARK 3 T11: 0.1276 T22: 0.0833 REMARK 3 T33: 0.1096 T12: 0.0079 REMARK 3 T13: 0.0145 T23: -0.0125 REMARK 3 L TENSOR REMARK 3 L11: 5.6214 L22: 2.3821 REMARK 3 L33: 0.6439 L12: 1.0296 REMARK 3 L13: -0.4234 L23: -0.3707 REMARK 3 S TENSOR REMARK 3 S11: -0.1044 S12: 0.1537 S13: -0.3107 REMARK 3 S21: -0.1140 S22: 0.0808 S23: 0.0542 REMARK 3 S31: 0.0894 S32: -0.0371 S33: 0.0202 REMARK 3 TLS GROUP : 5 REMARK 3 SELECTION: (CHAIN L AND RESID 106:210 ) REMARK 3 ORIGIN FOR THE GROUP (A): 28.7559 -0.5033 193.1756 REMARK 3 T TENSOR REMARK 3 T11: 0.1253 T22: 0.1467 REMARK 3 T33: 0.1618 T12: -0.0387 REMARK 3 T13: -0.0022 T23: 0.0195 REMARK 3 L TENSOR REMARK 3 L11: 1.6568 L22: 1.8251 REMARK 3 L33: 6.8674 L12: 0.0913 REMARK 3 L13: 0.4806 L23: -1.1184 REMARK 3 S TENSOR REMARK 3 S11: 0.0840 S12: -0.3261 S13: -0.1632 REMARK 3 S21: 0.2137 S22: -0.0264 S23: -0.0470 REMARK 3 S31: 0.1056 S32: -0.1400 S33: -0.0486 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 4FQ2 COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 28-JUN-12. REMARK 100 THE RCSB ID CODE IS RCSB073212. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 28-JAN-12 REMARK 200 TEMPERATURE (KELVIN) : 100 REMARK 200 PH : 5.5 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : SSRL REMARK 200 BEAMLINE : BL12-2 REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 1.033 REMARK 200 MONOCHROMATOR : LIQUID NITROGEN-COOLED DOUBLE REMARK 200 CRYSTAL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : PIXEL REMARK 200 DETECTOR MANUFACTURER : DECTRIS PILATUS 6M REMARK 200 INTENSITY-INTEGRATION SOFTWARE : XSCALE REMARK 200 DATA SCALING SOFTWARE : SCALA REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 42465 REMARK 200 RESOLUTION RANGE HIGH (A) : 1.704 REMARK 200 RESOLUTION RANGE LOW (A) : 36.313 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : -3.000 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 94.0 REMARK 200 DATA REDUNDANCY : 2.700 REMARK 200 R MERGE (I) : NULL REMARK 200 R SYM (I) : 0.07500 REMARK 200 FOR THE DATA SET : 8.7000 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 1.70 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 1.80 REMARK 200 COMPLETENESS FOR SHELL (%) : 80.6 REMARK 200 DATA REDUNDANCY IN SHELL : 2.30 REMARK 200 R MERGE FOR SHELL (I) : 0.84900 REMARK 200 R SYM FOR SHELL (I) : 0.84900 REMARK 200 FOR SHELL : 0.900 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 (%): 41.20 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.09 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: PEG 3350, BIS-TRIS HCL, NACL, PH 5.5, REMARK 280 VAPOR DIFFUSION, TEMPERATURE 298K REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: P 1 21 1 REMARK 290 REMARK 290 SYMOP SYMMETRY REMARK 290 NNNMMM OPERATOR REMARK 290 1555 X,Y,Z REMARK 290 2555 -X,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 0.00000 REMARK 290 SMTRY2 2 0.000000 1.000000 0.000000 20.13050 REMARK 290 SMTRY3 2 0.000000 0.000000 -1.000000 0.00000 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: 4480 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 20770 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -25.0 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 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 SER H 130 REMARK 465 THR H 131 REMARK 465 SER H 132 REMARK 465 GLY H 133 REMARK 465 GLY H 134 REMARK 465 ASP H 217 REMARK 465 LYS H 218 REMARK 465 THR H 219 REMARK 465 HIS H 220 REMARK 465 HIS H 221 REMARK 465 HIS H 222 REMARK 465 HIS H 223 REMARK 465 HIS H 224 REMARK 465 HIS H 225 REMARK 465 SER L 6 REMARK 465 TYR L 7 REMARK 465 SER L 213 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 ASN L 51 -55.18 74.45 REMARK 500 ASP L 152 -123.58 54.51 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 144 H 301 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC2 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE EDO L 301 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC3 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE EDO L 302 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC4 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE EDO L 303 REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 4FQ1 RELATED DB: PDB REMARK 900 RELATED ID: 4FQC RELATED DB: PDB REMARK 900 RELATED ID: 4FQQ RELATED DB: PDB