REMARK 2 REMARK 2 RESOLUTION. 2.37 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : BUSTER 2.11.4 REMARK 3 AUTHORS : BRICOGNE,BLANC,BRANDL,FLENSBURG,KELLER, REMARK 3 : PACIOREK,ROVERSI,SHARFF,SMART,VONRHEIN,WOMACK; REMARK 3 : MATTHEWS,TEN EYCK,TRONRUD REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS) : 2.37 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 34.70 REMARK 3 DATA CUTOFF (SIGMA(F)) : 0.0 REMARK 3 COMPLETENESS FOR RANGE (%) : 99.59 REMARK 3 NUMBER OF REFLECTIONS : 49387 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 CROSS-VALIDATION METHOD : THROUGHOUT REMARK 3 FREE R VALUE TEST SET SELECTION : RANDOM REMARK 3 R VALUE (WORKING + TEST SET) : 0.1861 REMARK 3 R VALUE (WORKING SET) : 0.1849 REMARK 3 FREE R VALUE : 0.2085 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.07 REMARK 3 FREE R VALUE TEST SET COUNT : 2502 REMARK 3 ESTIMATED ERROR OF FREE R VALUE : NULL REMARK 3 REMARK 3 FIT IN THE HIGHEST RESOLUTION BIN. REMARK 3 TOTAL NUMBER OF BINS USED : 20 REMARK 3 BIN RESOLUTION RANGE HIGH (ANGSTROMS) : 2.37 REMARK 3 BIN RESOLUTION RANGE LOW (ANGSTROMS) : 2.43 REMARK 3 BIN COMPLETENESS (WORKING+TEST) (%) : 99.59 REMARK 3 REFLECTIONS IN BIN (WORKING + TEST SET) : 3565 REMARK 3 BIN R VALUE (WORKING + TEST SET) : 0.2684 REMARK 3 REFLECTIONS IN BIN (WORKING SET) : 3382 REMARK 3 BIN R VALUE (WORKING SET) : 0.2682 REMARK 3 BIN FREE R VALUE : 0.2720 REMARK 3 BIN FREE R VALUE TEST SET SIZE (%) : 5.13 REMARK 3 BIN FREE R VALUE TEST SET COUNT : 183 REMARK 3 ESTIMATED ERROR OF BIN FREE R VALUE : NULL REMARK 3 REMARK 3 NUMBER OF NON-HYDROGEN ATOMS USED IN REFINEMENT. REMARK 3 PROTEIN ATOMS : 4541 REMARK 3 NUCLEIC ACID ATOMS : 0 REMARK 3 HETEROGEN ATOMS : 5 REMARK 3 SOLVENT ATOMS : 311 REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : 67.97 REMARK 3 MEAN B VALUE (OVERALL, A**2) : 66.58 REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2) : 9.9482 REMARK 3 B22 (A**2) : -15.4095 REMARK 3 B33 (A**2) : 5.4613 REMARK 3 B12 (A**2) : 0.0000 REMARK 3 B13 (A**2) : 0.0000 REMARK 3 B23 (A**2) : 0.0000 REMARK 3 REMARK 3 ESTIMATED COORDINATE ERROR. REMARK 3 ESD FROM LUZZATI PLOT (A) : 0.359 REMARK 3 DPI (BLOW EQ-10) BASED ON R VALUE (A) : 0.181 REMARK 3 DPI (BLOW EQ-9) BASED ON FREE R VALUE (A) : 0.156 REMARK 3 DPI (CRUICKSHANK) BASED ON R VALUE (A) : 0.176 REMARK 3 DPI (CRUICKSHANK) BASED ON FREE R VALUE (A) : 0.155 REMARK 3 REMARK 3 REFERENCES: BLOW, D. (2002) ACTA CRYST D58, 792-797 REMARK 3 CRUICKSHANK, D.W.J. (1999) ACTA CRYST D55, 583-601 REMARK 3 REMARK 3 CORRELATION COEFFICIENTS. REMARK 3 CORRELATION COEFFICIENT FO-FC : 0.9416 REMARK 3 CORRELATION COEFFICIENT FO-FC FREE : 0.9389 REMARK 3 REMARK 3 NUMBER OF GEOMETRIC FUNCTION TERMS DEFINED : 15 REMARK 3 TERM COUNT WEIGHT FUNCTION. REMARK 3 BOND LENGTHS : 4651 ; 2.00 ; HARMONIC REMARK 3 BOND ANGLES : 6313 ; 2.00 ; HARMONIC REMARK 3 TORSION ANGLES : 1547 ; 2.00 ; SINUSOIDAL REMARK 3 TRIGONAL CARBON PLANES : 101 ; 2.00 ; HARMONIC REMARK 3 GENERAL PLANES : 689 ; 5.00 ; HARMONIC REMARK 3 ISOTROPIC THERMAL FACTORS : 4651 ; 20.00 ; HARMONIC REMARK 3 BAD NON-BONDED CONTACTS : NULL ; NULL ; NULL REMARK 3 IMPROPER TORSIONS : NULL ; NULL ; NULL REMARK 3 PSEUDOROTATION ANGLES : NULL ; NULL ; NULL REMARK 3 CHIRAL IMPROPER TORSION : 605 ; 5.00 ; SEMIHARMONIC REMARK 3 SUM OF OCCUPANCIES : NULL ; NULL ; NULL REMARK 3 UTILITY DISTANCES : NULL ; NULL ; NULL REMARK 3 UTILITY ANGLES : NULL ; NULL ; NULL REMARK 3 UTILITY TORSION : NULL ; NULL ; NULL REMARK 3 IDEAL-DIST CONTACT TERM : 5028 ; 4.00 ; SEMIHARMONIC REMARK 3 REMARK 3 RMS DEVIATIONS FROM IDEAL VALUES. REMARK 3 BOND LENGTHS (A) : 0.010 REMARK 3 BOND ANGLES (DEGREES) : 1.16 REMARK 3 PEPTIDE OMEGA TORSION ANGLES (DEGREES) : 3.38 REMARK 3 OTHER TORSION ANGLES (DEGREES) : 18.44 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 3 REMARK 3 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: CHAIN A REMARK 3 ORIGIN FOR THE GROUP (A): -24.5760 -24.1114 34.8618 REMARK 3 T TENSOR REMARK 3 T11: -0.0178 T22: -0.0378 REMARK 3 T33: -0.0609 T12: 0.0096 REMARK 3 T13: 0.0370 T23: 0.1858 REMARK 3 L TENSOR REMARK 3 L11: 0.8988 L22: 0.6146 REMARK 3 L33: 2.1618 L12: -0.4493 REMARK 3 L13: 1.0925 L23: -0.7424 REMARK 3 S TENSOR REMARK 3 S11: -0.0378 S12: -0.1349 S13: -0.1532 REMARK 3 S21: -0.0517 S22: -0.0324 S23: -0.1111 REMARK 3 S31: -0.0866 S32: 0.1647 S33: 0.0701 REMARK 3 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: CHAIN B REMARK 3 ORIGIN FOR THE GROUP (A): -16.5003 -39.1687 66.7277 REMARK 3 T TENSOR REMARK 3 T11: -0.1724 T22: 0.0975 REMARK 3 T33: -0.0474 T12: 0.0154 REMARK 3 T13: -0.0186 T23: 0.3014 REMARK 3 L TENSOR REMARK 3 L11: 3.1443 L22: 2.2400 REMARK 3 L33: 3.5588 L12: -1.1742 REMARK 3 L13: -0.1023 L23: -1.4181 REMARK 3 S TENSOR REMARK 3 S11: -0.0861 S12: 0.0406 S13: -0.0938 REMARK 3 S21: 0.1538 S22: 0.1050 S23: 0.0990 REMARK 3 S31: -0.0491 S32: -0.1575 S33: -0.0189 REMARK 3 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: CHAIN C REMARK 3 ORIGIN FOR THE GROUP (A): -12.6534 -11.5714 -7.8228 REMARK 3 T TENSOR REMARK 3 T11: -0.0089 T22: -0.1296 REMARK 3 T33: -0.1125 T12: -0.0011 REMARK 3 T13: -0.0220 T23: -0.0402 REMARK 3 L TENSOR REMARK 3 L11: 4.4718 L22: 3.9115 REMARK 3 L33: 2.9267 L12: 1.0763 REMARK 3 L13: -1.0305 L23: -0.0002 REMARK 3 S TENSOR REMARK 3 S11: -0.1364 S12: -0.2594 S13: -0.2559 REMARK 3 S21: 0.1384 S22: 0.0272 S23: -0.3259 REMARK 3 S31: -0.0478 S32: 0.3868 S33: 0.1093 REMARK 3 REMARK 3 OTHER REFINEMENT REMARKS: NULL REMARK 4 REMARK 4 3ZKX COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY PDBE ON 25-JAN-13. REMARK 100 THE PDBE ID CODE IS EBI-55643. 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 : 7.0 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : SLS REMARK 200 BEAMLINE : X10SA REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 1.0 REMARK 200 MONOCHROMATOR : NULL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : PIXEL (PILATUS 6M) REMARK 200 DETECTOR MANUFACTURER : DECTRIS REMARK 200 INTENSITY-INTEGRATION SOFTWARE : XDS REMARK 200 DATA SCALING SOFTWARE : SCALA REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 49549 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.37 REMARK 200 RESOLUTION RANGE LOW (A) : 34.70 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : -3.0 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 99.9 REMARK 200 DATA REDUNDANCY : 6.6 REMARK 200 R MERGE (I) : 0.09 REMARK 200 R SYM (I) : NULL REMARK 200 FOR THE DATA SET : 13.40 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 2.37 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 2.50 REMARK 200 COMPLETENESS FOR SHELL (%) : 99.8 REMARK 200 DATA REDUNDANCY IN SHELL : 6.7 REMARK 200 R MERGE FOR SHELL (I) : 0.88 REMARK 200 R SYM FOR SHELL (I) : NULL REMARK 200 FOR SHELL : 1.20 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: PDB ENTRY 3ZKQ REMARK 200 REMARK 200 REMARK: NONE REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 71.96 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 4.39 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 0.2M SODIUM MALONATE, 20% REMARK 280 PEG3350 REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: I 2 2 2 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,Y,-Z REMARK 290 4555 X,-Y,-Z REMARK 290 5555 X+1/2,Y+1/2,Z+1/2 REMARK 290 6555 -X+1/2,-Y+1/2,Z+1/2 REMARK 290 7555 -X+1/2,Y+1/2,-Z+1/2 REMARK 290 8555 X+1/2,-Y+1/2,-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 0.00000 REMARK 290 SMTRY2 3 0.000000 1.000000 0.000000 0.00000 REMARK 290 SMTRY3 3 0.000000 0.000000 -1.000000 0.00000 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 1.000000 0.000000 0.000000 31.68350 REMARK 290 SMTRY2 5 0.000000 1.000000 0.000000 76.91450 REMARK 290 SMTRY3 5 0.000000 0.000000 1.000000 123.58900 REMARK 290 SMTRY1 6 -1.000000 0.000000 0.000000 31.68350 REMARK 290 SMTRY2 6 0.000000 -1.000000 0.000000 76.91450 REMARK 290 SMTRY3 6 0.000000 0.000000 1.000000 123.58900 REMARK 290 SMTRY1 7 -1.000000 0.000000 0.000000 31.68350 REMARK 290 SMTRY2 7 0.000000 1.000000 0.000000 76.91450 REMARK 290 SMTRY3 7 0.000000 0.000000 -1.000000 123.58900 REMARK 290 SMTRY1 8 1.000000 0.000000 0.000000 31.68350 REMARK 290 SMTRY2 8 0.000000 -1.000000 0.000000 76.91450 REMARK 290 SMTRY3 8 0.000000 0.000000 -1.000000 123.58900 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: TRIMERIC REMARK 350 SOFTWARE DETERMINED QUATERNARY STRUCTURE: TRIMERIC REMARK 350 SOFTWARE USED: PISA REMARK 350 TOTAL BURIED SURFACE AREA: 3140 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 25200 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -19.6 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: A, C, 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 ALA A 13 REMARK 465 ASN A 14 REMARK 465 PHE A 15 REMARK 465 PRO A 176 REMARK 465 VAL A 177 REMARK 465 ALA A 178 REMARK 465 GLY A 179 REMARK 465 SER A 180 REMARK 465 GLY A 181 REMARK 465 THR A 182 REMARK 465 ASN A 183 REMARK 465 MET A 323 REMARK 465 GLY A 324 REMARK 465 ALA A 325 REMARK 465 GLY A 326 REMARK 465 ALA A 398 REMARK 465 SER B 271 REMARK 465 HIS B 272 REMARK 465 HIS B 273 REMARK 465 HIS B 274 REMARK 465 HIS B 275 REMARK 465 HIS B 276 REMARK 465 HIS B 277 REMARK 465 GLU B 278 REMARK 465 PRO B 279 REMARK 465 GLU B 280 REMARK 465 ALA B 281 REMARK 465 GLN C 160 REMARK 465 VAL C 161 REMARK 465 GLN C 162 REMARK 465 HIS C 274 REMARK 465 HIS C 275 REMARK 465 HIS C 276 REMARK 465 HIS C 277 REMARK 465 GLU C 278 REMARK 465 PRO C 279 REMARK 465 GLU C 280 REMARK 465 ALA C 281 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 TRP A 210 -80.01 -142.82 REMARK 500 ASN A 285 -146.26 64.77 REMARK 500 VAL B 207 -61.04 -105.10 REMARK 500 GLU C 201 -48.88 77.71 REMARK 500 ASN C 258 76.22 9.21 REMARK 500 REMARK 500 REMARK: NULL REMARK 525 REMARK 525 SOLVENT REMARK 525 REMARK 525 THE SOLVENT MOLECULES HAVE CHAIN IDENTIFIERS THAT REMARK 525 INDICATE THE POLYMER CHAIN WITH WHICH THEY ARE MOST REMARK 525 CLOSELY ASSOCIATED. THE REMARK LISTS ALL THE SOLVENT REMARK 525 MOLECULES WHICH ARE MORE THAN 5A AWAY FROM THE REMARK 525 NEAREST POLYMER CHAIN (M = MODEL NUMBER; REMARK 525 RES=RESIDUE NAME; C=CHAIN IDENTIFIER; SSEQ=SEQUENCE REMARK 525 NUMBER; I=INSERTION CODE): REMARK 525 REMARK 525 M RES CSSEQI REMARK 525 HOH A2092 DISTANCE = 5.55 ANGSTROMS REMARK 525 HOH A2200 DISTANCE = 5.05 ANGSTROMS REMARK 525 HOH B2053 DISTANCE = 5.05 ANGSTROMS REMARK 525 HOH C2056 DISTANCE = 8.62 ANGSTROMS REMARK 800 REMARK 800 SITE REMARK 800 SITE_IDENTIFIER: AC1 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE CL B1271 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC2 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE DMS B1272