REMARK 2 REMARK 2 RESOLUTION. 2.30 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : BUSTER 2.8.0 REMARK 3 AUTHORS : BRICOGNE,BLANC,BRANDL,FLENSBURG,KELLER, REMARK 3 : PACIOREK,ROVERSI,SHARFF,SMART,VONRHEIN, REMARK 3 : WOMACK,MATTHEWS,TEN EYCK,TRONRUD REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS) : 2.30 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 28.23 REMARK 3 DATA CUTOFF (SIGMA(F)) : 0.000 REMARK 3 COMPLETENESS FOR RANGE (%) : 99.9 REMARK 3 NUMBER OF REFLECTIONS : 21224 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) : 0.171 REMARK 3 R VALUE (WORKING SET) : 0.169 REMARK 3 FREE R VALUE : 0.221 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 4.760 REMARK 3 FREE R VALUE TEST SET COUNT : 1010 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 : 11 REMARK 3 BIN RESOLUTION RANGE HIGH (ANGSTROMS) : 2.30 REMARK 3 BIN RESOLUTION RANGE LOW (ANGSTROMS) : 2.41 REMARK 3 BIN COMPLETENESS (WORKING+TEST) (%) : NULL REMARK 3 REFLECTIONS IN BIN (WORKING + TEST SET) : 2800 REMARK 3 BIN R VALUE (WORKING + TEST SET) : 0.2060 REMARK 3 REFLECTIONS IN BIN (WORKING SET) : 2663 REMARK 3 BIN R VALUE (WORKING SET) : 0.2023 REMARK 3 BIN FREE R VALUE : 0.2802 REMARK 3 BIN FREE R VALUE TEST SET SIZE (%) : 4.89 REMARK 3 BIN FREE R VALUE TEST SET COUNT : 137 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 : 3309 REMARK 3 NUCLEIC ACID ATOMS : 0 REMARK 3 HETEROGEN ATOMS : 12 REMARK 3 SOLVENT ATOMS : 227 REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : 40.76 REMARK 3 MEAN B VALUE (OVERALL, A**2) : 33.37 REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2) : 3.97610 REMARK 3 B22 (A**2) : -0.47970 REMARK 3 B33 (A**2) : -3.49640 REMARK 3 B12 (A**2) : 0.00000 REMARK 3 B13 (A**2) : -0.88790 REMARK 3 B23 (A**2) : 0.00000 REMARK 3 REMARK 3 ESTIMATED COORDINATE ERROR. REMARK 3 ESD FROM LUZZATI PLOT (A) : 0.26 REMARK 3 DPI (BLOW EQ-10) BASED ON R VALUE (A) : NULL REMARK 3 DPI (BLOW EQ-9) BASED ON FREE R VALUE (A) : NULL REMARK 3 DPI (CRUICKSHANK) BASED ON R VALUE (A) : NULL REMARK 3 DPI (CRUICKSHANK) BASED ON FREE R VALUE (A) : NULL 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 : 0.947 REMARK 3 CORRELATION COEFFICIENT FO-FC FREE : 0.908 REMARK 3 REMARK 3 NUMBER OF GEOMETRIC FUNCTION TERMS DEFINED : 15 REMARK 3 TERM COUNT WEIGHT FUNCTION. REMARK 3 BOND LENGTHS : 3388 ; 2.000 ; HARMONIC REMARK 3 BOND ANGLES : 4598 ; 2.000 ; HARMONIC REMARK 3 TORSION ANGLES : 1144 ; 2.000 ; SINUSOIDAL REMARK 3 TRIGONAL CARBON PLANES : 74 ; 2.000 ; HARMONIC REMARK 3 GENERAL PLANES : 495 ; 5.000 ; HARMONIC REMARK 3 ISOTROPIC THERMAL FACTORS : 3388 ; 20.000 ; 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 : 449 ; 5.000 ; 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 : 3890 ; 4.000 ; SEMIHARMONIC REMARK 3 REMARK 3 RMS DEVIATIONS FROM IDEAL VALUES. REMARK 3 BOND LENGTHS (A) : 0.010 REMARK 3 BOND ANGLES (DEGREES) : 1.28 REMARK 3 PEPTIDE OMEGA TORSION ANGLES (DEGREES) : 3.64 REMARK 3 OTHER TORSION ANGLES (DEGREES) : 20.34 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 4 REMARK 3 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: A 1 A 114 REMARK 3 ORIGIN FOR THE GROUP (A): 26.7536 -5.3230 12.7695 REMARK 3 T TENSOR REMARK 3 T11: -0.0553 T22: -0.0060 REMARK 3 T33: -0.0001 T12: 0.0371 REMARK 3 T13: 0.0044 T23: -0.0237 REMARK 3 L TENSOR REMARK 3 L11: 1.5444 L22: 0.2069 REMARK 3 L33: 1.9264 L12: 0.2928 REMARK 3 L13: 0.1945 L23: -0.4523 REMARK 3 S TENSOR REMARK 3 S11: 0.0569 S12: 0.0377 S13: -0.0245 REMARK 3 S21: -0.0565 S22: -0.1247 S23: 0.0236 REMARK 3 S31: 0.1001 S32: 0.1938 S33: 0.0679 REMARK 3 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: A 115 A 219 REMARK 3 ORIGIN FOR THE GROUP (A): -0.0625 -4.5187 39.5541 REMARK 3 T TENSOR REMARK 3 T11: -0.0374 T22: -0.0166 REMARK 3 T33: -0.0520 T12: -0.0196 REMARK 3 T13: 0.0024 T23: 0.0198 REMARK 3 L TENSOR REMARK 3 L11: 2.1495 L22: 1.5072 REMARK 3 L33: 0.8664 L12: 0.0619 REMARK 3 L13: -0.5783 L23: 0.2591 REMARK 3 S TENSOR REMARK 3 S11: 0.0191 S12: -0.0654 S13: -0.1134 REMARK 3 S21: 0.1383 S22: -0.0351 S23: -0.0782 REMARK 3 S31: 0.0321 S32: 0.0279 S33: 0.0160 REMARK 3 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: B 1 B 119 REMARK 3 ORIGIN FOR THE GROUP (A): 9.0152 2.0859 0.5751 REMARK 3 T TENSOR REMARK 3 T11: -0.0777 T22: 0.0140 REMARK 3 T33: -0.0061 T12: -0.0146 REMARK 3 T13: -0.0317 T23: 0.0272 REMARK 3 L TENSOR REMARK 3 L11: 1.4699 L22: 1.1738 REMARK 3 L33: 1.6916 L12: -0.3044 REMARK 3 L13: -0.8785 L23: -0.0782 REMARK 3 S TENSOR REMARK 3 S11: -0.0052 S12: 0.2466 S13: 0.2015 REMARK 3 S21: -0.1090 S22: -0.0045 S23: -0.0758 REMARK 3 S31: 0.0552 S32: -0.0455 S33: 0.0097 REMARK 3 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: B 120 B 220 REMARK 3 ORIGIN FOR THE GROUP (A): -1.5371 8.0183 30.0162 REMARK 3 T TENSOR REMARK 3 T11: -0.0338 T22: -0.0604 REMARK 3 T33: -0.0205 T12: -0.0110 REMARK 3 T13: 0.0113 T23: 0.0278 REMARK 3 L TENSOR REMARK 3 L11: 1.5531 L22: 1.1503 REMARK 3 L33: 1.9380 L12: 0.2906 REMARK 3 L13: 0.6603 L23: 0.6347 REMARK 3 S TENSOR REMARK 3 S11: 0.0183 S12: -0.1139 S13: -0.0219 REMARK 3 S21: 0.0393 S22: -0.0500 S23: -0.0999 REMARK 3 S31: -0.1435 S32: -0.1023 S33: 0.0316 REMARK 3 REMARK 3 OTHER REFINEMENT REMARKS: TLS REFINEMENT WAS PERFORMED REMARK 4 REMARK 4 3QO0 COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY PDBJ ON 21-FEB-11. REMARK 100 THE RCSB ID CODE IS RCSB063885. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 04-DEC-09 REMARK 200 TEMPERATURE (KELVIN) : 108 REMARK 200 PH : 6.1 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : N REMARK 200 RADIATION SOURCE : ROTATING ANODE REMARK 200 BEAMLINE : NULL REMARK 200 X-RAY GENERATOR MODEL : RIGAKU MICROMAX-007 HF REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 1.5418 REMARK 200 MONOCHROMATOR : VARIMAX-HF MULTILAYER MIRRORS REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : IMAGE PLATE REMARK 200 DETECTOR MANUFACTURER : MAR SCANNER 345 MM PLATE REMARK 200 INTENSITY-INTEGRATION SOFTWARE : XDS REMARK 200 DATA SCALING SOFTWARE : SCALA REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 21241 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.300 REMARK 200 RESOLUTION RANGE LOW (A) : 28.232 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : 0.000 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 99.9 REMARK 200 DATA REDUNDANCY : 3.700 REMARK 200 R MERGE (I) : NULL REMARK 200 R SYM (I) : 0.09700 REMARK 200 FOR THE DATA SET : 12.4000 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 2.30 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 2.42 REMARK 200 COMPLETENESS FOR SHELL (%) : 100.0 REMARK 200 DATA REDUNDANCY IN SHELL : 3.60 REMARK 200 R MERGE FOR SHELL (I) : 0.57200 REMARK 200 R SYM FOR SHELL (I) : 0.57200 REMARK 200 FOR SHELL : 1.400 REMARK 200 REMARK 200 DIFFRACTION PROTOCOL: SINGLE WAVELENGTH REMARK 200 METHOD USED TO DETERMINE THE STRUCTURE: FOURIER SYNTHESIS REMARK 200 SOFTWARE USED: FFT REMARK 200 STARTING MODEL: NULL REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 49.30 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.43 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 0.1M NA CITRATE, 20% ISOPROPANOL, 16% REMARK 280 PEG 4000, PH 6.1, VAPOR DIFFUSION, SITTING DROP, TEMPERATURE 293K 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 33.63500 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: TRIMERIC REMARK 350 SOFTWARE DETERMINED QUATERNARY STRUCTURE: TRIMERIC REMARK 350 SOFTWARE USED: PISA REMARK 350 TOTAL BURIED SURFACE AREA: 4460 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 19360 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -22.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: A, B, C 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 TYR C -16 REMARK 465 GLN C -15 REMARK 465 GLN C -14 REMARK 465 TYR C -13 REMARK 465 GLN C -12 REMARK 465 ASP C -11 REMARK 465 ALA C -10 REMARK 465 THR C -9 REMARK 465 ALA C -8 REMARK 465 GLU C -7 REMARK 465 GLU C -6 REMARK 465 GLU C -5 REMARK 465 GLU C -4 REMARK 465 ASP C -3 REMARK 465 PHE C -2 REMARK 465 GLY C -1 REMARK 465 GLU C 0 REMARK 465 GLU C 3 REMARK 470 REMARK 470 MISSING ATOM REMARK 470 THE FOLLOWING RESIDUES HAVE MISSING ATOMS (M=MODEL NUMBER; REMARK 470 RES=RESIDUE NAME; C=CHAIN IDENTIFIER; SSEQ=SEQUENCE NUMBER; REMARK 470 I=INSERTION CODE): REMARK 470 M RES CSSEQI ATOMS REMARK 470 SER A 61 OG REMARK 470 CYS A 219 SG REMARK 470 GLU B 1 CG CD OE1 OE2 REMARK 470 SER B 25 OG REMARK 470 ASN B 54 CG OD1 ND2 REMARK 470 ARG B 67 CG CD NE CZ NH1 NH2 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 LEU A 52 -51.87 -120.17 REMARK 500 SER A 57 -4.18 -144.32 REMARK 500 GLU A 218 5.37 51.66 REMARK 500 LYS B 43 -169.18 -107.75 REMARK 500 ARG B 67 95.87 -55.49 REMARK 500 ALA B 94 166.83 177.92 REMARK 500 ARG B 107 18.97 59.79 REMARK 500 PRO B 219 170.36 -58.39 REMARK 500 REMARK 500 REMARK: NULL REMARK 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: CHIRAL CENTERS REMARK 500 REMARK 500 UNEXPECTED CONFIGURATION OF THE FOLLOWING CHIRAL REMARK 500 CENTER(S) USING IMPROPER CA--C--CB--N CHIRALITY REMARK 500 FOR AMINO ACIDS AND C1'--O4'--N1(N9)--C2' FOR REMARK 500 NUCLEIC ACIDS OR EQUIVALENT ANGLE REMARK 500 M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN REMARK 500 IDENTIFIER; SSEQ=SEQUENCE NUMBER; I=INSERTION CODE REMARK 500 REMARK 500 STANDARD TABLE: REMARK 500 FORMAT: (10X,I3,1X,A3,1X,A1,I4,A1,6X,F5.1,6X,A1,10X,A1,3X,A16) REMARK 500 REMARK 500 M RES CSSEQI IMPROPER EXPECTED FOUND DETAILS REMARK 500 ILE A 81 24.4 L L OUTSIDE RANGE REMARK 500 GLU A 128 24.3 L L OUTSIDE RANGE REMARK 500 VAL A 151 21.2 L L OUTSIDE RANGE REMARK 500 LEU B 195 24.9 L L OUTSIDE RANGE 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 A 220 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC2 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE GOL A 221 REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 3M8O RELATED DB: PDB REMARK 900 RELATED ID: 3QNX RELATED DB: PDB REMARK 900 RELATED ID: 3QNY RELATED DB: PDB REMARK 900 RELATED ID: 3QOZ RELATED DB: PDB REMARK 900 RELATED ID: 3QO1 RELATED DB: PDB