REMARK 2 REMARK 2 RESOLUTION. 2.20 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.8.1_1168) 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) : 2.20 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 46.76 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 2.000 REMARK 3 COMPLETENESS FOR RANGE (%) : 99.8 REMARK 3 NUMBER OF REFLECTIONS : 60561 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.200 REMARK 3 R VALUE (WORKING SET) : 0.199 REMARK 3 FREE R VALUE : 0.226 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.000 REMARK 3 FREE R VALUE TEST SET COUNT : 3029 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 46.7711 - 6.1643 1.00 2838 150 0.1847 0.2014 REMARK 3 2 6.1643 - 4.8944 1.00 2697 142 0.1755 0.2054 REMARK 3 3 4.8944 - 4.2762 1.00 2679 141 0.1486 0.1636 REMARK 3 4 4.2762 - 3.8855 1.00 2624 138 0.1703 0.1956 REMARK 3 5 3.8855 - 3.6071 1.00 2644 139 0.1880 0.1965 REMARK 3 6 3.6071 - 3.3945 1.00 2642 139 0.1944 0.2179 REMARK 3 7 3.3945 - 3.2245 1.00 2617 138 0.2134 0.2212 REMARK 3 8 3.2245 - 3.0842 1.00 2630 138 0.2215 0.2659 REMARK 3 9 3.0842 - 2.9655 1.00 2611 138 0.2297 0.2533 REMARK 3 10 2.9655 - 2.8632 1.00 2575 135 0.2313 0.2597 REMARK 3 11 2.8632 - 2.7737 1.00 2604 137 0.2365 0.2694 REMARK 3 12 2.7737 - 2.6944 1.00 2638 139 0.2325 0.2745 REMARK 3 13 2.6944 - 2.6235 1.00 2576 136 0.2463 0.2894 REMARK 3 14 2.6235 - 2.5595 1.00 2607 137 0.2417 0.2782 REMARK 3 15 2.5595 - 2.5013 1.00 2602 137 0.2424 0.3377 REMARK 3 16 2.5013 - 2.4480 1.00 2555 134 0.2574 0.3049 REMARK 3 17 2.4480 - 2.3991 1.00 2596 137 0.2487 0.2941 REMARK 3 18 2.3991 - 2.3538 1.00 2563 135 0.2662 0.3148 REMARK 3 19 2.3538 - 2.3118 1.00 2631 139 0.2603 0.2960 REMARK 3 20 2.3118 - 2.2726 1.00 2534 133 0.2655 0.3153 REMARK 3 21 2.2726 - 2.2359 1.00 2615 137 0.2811 0.3684 REMARK 3 22 2.2359 - 2.2015 0.96 2454 130 0.3130 0.3274 REMARK 3 REMARK 3 BULK SOLVENT MODELLING. REMARK 3 METHOD USED : FLAT BULK SOLVENT MODEL REMARK 3 SOLVENT RADIUS : 1.11 REMARK 3 SHRINKAGE RADIUS : 0.90 REMARK 3 K_SOL : NULL REMARK 3 B_SOL : NULL REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.280 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 26.130 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) : NULL REMARK 3 B22 (A**2) : NULL REMARK 3 B33 (A**2) : NULL REMARK 3 B12 (A**2) : NULL REMARK 3 B13 (A**2) : NULL REMARK 3 B23 (A**2) : NULL 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 : 0.003 6882 REMARK 3 ANGLE : 0.824 9368 REMARK 3 CHIRALITY : 0.056 1033 REMARK 3 PLANARITY : 0.004 1207 REMARK 3 DIHEDRAL : 13.732 2444 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : NULL 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 4IMK COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 09-JAN-13. REMARK 100 THE RCSB ID CODE IS RCSB076940. 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 : X06SA REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : NULL REMARK 200 MONOCHROMATOR : NULL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : MARMOSAIC 225 MM CCD REMARK 200 INTENSITY-INTEGRATION SOFTWARE : XDS REMARK 200 DATA SCALING SOFTWARE : XDS REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 60561 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.200 REMARK 200 RESOLUTION RANGE LOW (A) : 46.761 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) : 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 (%): 59.00 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 3.00 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 15%(W/V) PEG4000, 0.1 M TRI-NA- REMARK 280 CITRATE, 15%(V/V) ISOPROPANOL, PH 7.0, VAPOR DIFFUSION, HANGING REMARK 280 DROP, TEMPERATURE 293K REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: P 21 21 21 REMARK 290 REMARK 290 SYMOP SYMMETRY REMARK 290 NNNMMM OPERATOR REMARK 290 1555 X,Y,Z REMARK 290 2555 -X+1/2,-Y,Z+1/2 REMARK 290 3555 -X,Y+1/2,-Z+1/2 REMARK 290 4555 X+1/2,-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 32.98450 REMARK 290 SMTRY2 2 0.000000 -1.000000 0.000000 0.00000 REMARK 290 SMTRY3 2 0.000000 0.000000 1.000000 102.90650 REMARK 290 SMTRY1 3 -1.000000 0.000000 0.000000 0.00000 REMARK 290 SMTRY2 3 0.000000 1.000000 0.000000 43.33500 REMARK 290 SMTRY3 3 0.000000 0.000000 -1.000000 102.90650 REMARK 290 SMTRY1 4 1.000000 0.000000 0.000000 32.98450 REMARK 290 SMTRY2 4 0.000000 -1.000000 0.000000 43.33500 REMARK 290 SMTRY3 4 0.000000 0.000000 -1.000000 0.00000 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: 3850 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 19250 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -36.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: A, D 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: 4070 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 19770 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -34.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: 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 LYS A 230 REMARK 465 GLN C 1 REMARK 465 PRO C 2 REMARK 465 GLY C 216 REMARK 465 SER C 217 REMARK 465 GLY C 218 REMARK 465 HIS C 219 REMARK 465 HIS C 220 REMARK 465 HIS C 221 REMARK 465 HIS C 222 REMARK 465 HIS C 223 REMARK 465 HIS C 224 REMARK 465 GLN D 1 REMARK 465 PRO D 2 REMARK 465 GLY D 213 REMARK 465 GLU D 214 REMARK 465 CYS D 215 REMARK 465 GLY D 216 REMARK 465 SER D 217 REMARK 465 GLY D 218 REMARK 465 HIS D 219 REMARK 465 HIS D 220 REMARK 465 HIS D 221 REMARK 465 HIS D 222 REMARK 465 HIS D 223 REMARK 465 HIS D 224 REMARK 475 REMARK 475 ZERO OCCUPANCY RESIDUES REMARK 475 THE FOLLOWING RESIDUES WERE MODELED WITH ZERO OCCUPANCY. REMARK 475 THE LOCATION AND PROPERTIES OF THESE RESIDUES MAY NOT REMARK 475 BE RELIABLE. (M=MODEL NUMBER; RES=RESIDUE NAME; REMARK 475 C=CHAIN IDENTIFIER; SSEQ=SEQUENCE NUMBER; I=INSERTION CODE) REMARK 475 M RES C SSEQI REMARK 475 SER B 107 REMARK 480 REMARK 480 ZERO OCCUPANCY ATOM REMARK 480 THE FOLLOWING RESIDUES HAVE ATOMS MODELED WITH ZERO REMARK 480 OCCUPANCY. THE LOCATION AND PROPERTIES OF THESE ATOMS REMARK 480 MAY NOT BE RELIABLE. (M=MODEL NUMBER; RES=RESIDUE NAME; REMARK 480 C=CHAIN IDENTIFIER; SSEQ=SEQUENCE NUMBER; I=INSERTION CODE): REMARK 480 M RES C SSEQI ATOMS REMARK 480 GLN A 1 CG CD OE1 NE2 REMARK 480 LYS A 23 CE NZ REMARK 480 GLN A 62 OE1 REMARK 480 TYR A 104 O CB CG CD1 CD2 CE1 CE2 REMARK 480 TYR A 104 CZ OH REMARK 480 TYR A 105 O CB CG CD1 CD2 CE1 CE2 REMARK 480 TYR A 105 CZ OH REMARK 480 ASP A 106 O CB CG OD1 OD2 REMARK 480 SER A 107 OG REMARK 480 LYS A 145 CB CG CD CE NZ REMARK 480 GLY A 149 C O REMARK 480 THR A 176 CB OG1 CG2 REMARK 480 LEU A 205 CD1 CD2 REMARK 480 GLY A 206 C REMARK 480 THR A 207 OG1 CG2 REMARK 480 ILE A 211 CD1 REMARK 480 ASN A 220 ND2 REMARK 480 LYS A 222 CG CD CE NZ REMARK 480 LYS A 226 CD CE NZ REMARK 480 GLU A 228 OE1 OE2 REMARK 480 GLN B 1 CB CG CD OE1 NE2 REMARK 480 GLN B 3 OE1 NE2 REMARK 480 LYS B 13 CG CD CE NZ REMARK 480 LYS B 19 CD CE NZ REMARK 480 LYS B 23 CG CD CE NZ REMARK 480 GLN B 62 CG CD OE1 NE2 REMARK 480 LYS B 63 CE REMARK 480 GLN B 65 CG CD OE1 NE2 REMARK 480 THR B 69 OG1 CG2 REMARK 480 ARG B 72 CG CD NE CZ NH1 NH2 REMARK 480 ASP B 73 CG OD1 OD2 REMARK 480 GLU B 82 CG CD OE1 OE2 REMARK 480 SER B 84 OG REMARK 480 ARG B 85 CD NE CZ NH1 NH2 REMARK 480 TYR B 103 CE1 CE2 CZ OH REMARK 480 TYR B 104 CG CD1 CD2 CE1 CE2 CZ OH REMARK 480 SER B 108 CB OG REMARK 480 LYS B 133 CE NZ REMARK 480 LYS B 145 CD CE NZ REMARK 480 LYS B 217 CD CE NZ REMARK 480 LYS B 222 CD CE NZ REMARK 480 LYS B 230 CG CD CE NZ REMARK 480 GLU C 59 CG CD OE1 OE2 REMARK 480 ARG C 76 CD NE CZ NH1 NH2 REMARK 480 SER C 93 OG REMARK 480 LYS C 127 CD CE NZ REMARK 480 ARG C 143 CZ NH1 NH2 REMARK 480 GLU C 144 CD OE1 OE2 REMARK 480 LYS C 146 CD CE NZ REMARK 480 LEU C 155 CD1 REMARK 480 LYS C 170 CE NZ REMARK 480 GLU C 188 OE2 REMARK 480 LYS C 189 NZ REMARK 480 LYS C 191 CE NZ REMARK 480 GLN D 16 CD OE1 NE2 REMARK 480 GLU D 59 OE2 REMARK 480 ASP D 123 CG OD1 OD2 REMARK 480 LYS D 127 CB CG CD CE NZ REMARK 480 GLU D 144 CD OE1 OE2 REMARK 480 LYS D 146 CE NZ REMARK 480 GLN D 148 OE1 NE2 REMARK 480 LYS D 184 CG CD CE NZ REMARK 480 LYS D 191 CD CE NZ 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 TYR A 103 41.50 -96.33 REMARK 500 ASP C 50 -55.35 74.69 REMARK 500 SER C 51 -1.45 -140.24 REMARK 500 LYS C 191 -62.82 -109.80 REMARK 500 ASP D 50 -52.78 68.44 REMARK 500 SER D 51 -3.94 -141.34 REMARK 500 ASN D 153 -3.08 73.67 REMARK 500 REMARK 500 REMARK: NULL REMARK 620 REMARK 620 METAL COORDINATION REMARK 620 (M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN IDENTIFIER; REMARK 620 SSEQ=SEQUENCE NUMBER; I=INSERTION CODE): REMARK 620 REMARK 620 COORDINATION ANGLES FOR: M RES CSSEQI METAL REMARK 620 NA A 301 NA REMARK 620 N RES CSSEQI ATOM REMARK 620 1 SER A 7 OG REMARK 620 2 GLY A 8 O 113.6 REMARK 620 3 GLU A 10 OE2 132.4 97.5 REMARK 620 N 1 2 REMARK 800 REMARK 800 SITE REMARK 800 SITE_IDENTIFIER: AC1 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE NA A 301 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC2 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE GOL C 301 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC3 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE SO4 C 302 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC4 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE GOL D 301 REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 4IML RELATED DB: PDB