REMARK 2 REMARK 2 RESOLUTION. 2.80 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.6_289) 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) : 2.80 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 41.54 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 0.200 REMARK 3 COMPLETENESS FOR RANGE (%) : 95.0 REMARK 3 NUMBER OF REFLECTIONS : 21650 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.186 REMARK 3 R VALUE (WORKING SET) : 0.183 REMARK 3 FREE R VALUE : 0.243 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.010 REMARK 3 FREE R VALUE TEST SET COUNT : 1085 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 41.5444 - 5.5962 0.99 2748 145 0.1770 0.2122 REMARK 3 2 5.5962 - 4.4435 0.99 2668 141 0.1425 0.1969 REMARK 3 3 4.4435 - 3.8823 0.98 2672 143 0.1475 0.2193 REMARK 3 4 3.8823 - 3.5275 0.98 2638 138 0.1837 0.2606 REMARK 3 5 3.5275 - 3.2748 0.96 2569 139 0.1965 0.2452 REMARK 3 6 3.2748 - 3.0818 0.94 2512 135 0.2039 0.2594 REMARK 3 7 3.0818 - 2.9275 0.90 2421 118 0.2185 0.2917 REMARK 3 8 2.9275 - 2.8001 0.86 2337 126 0.2389 0.3096 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 : 0.31 REMARK 3 B_SOL : 42.37 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.360 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 25.580 REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : 37.19 REMARK 3 MEAN B VALUE (OVERALL, A**2) : 62.01 REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2) : -14.20590 REMARK 3 B22 (A**2) : -14.37910 REMARK 3 B33 (A**2) : -8.73820 REMARK 3 B12 (A**2) : -0.00000 REMARK 3 B13 (A**2) : -3.77680 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 : 0.012 5695 REMARK 3 ANGLE : 1.300 7702 REMARK 3 CHIRALITY : 0.105 852 REMARK 3 PLANARITY : 0.005 991 REMARK 3 DIHEDRAL : 19.833 2019 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 3UX9 COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY PDBJ ON 15-DEC-11. REMARK 100 THE RCSB ID CODE IS RCSB069323. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 07-AUG-10 REMARK 200 TEMPERATURE (KELVIN) : 100 REMARK 200 PH : 8.5 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : APS REMARK 200 BEAMLINE : 19-ID REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 0.9794 REMARK 200 MONOCHROMATOR : NULL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : ADSC QUANTUM 315 REMARK 200 INTENSITY-INTEGRATION SOFTWARE : HKL-2000 REMARK 200 DATA SCALING SOFTWARE : HKL-2000 REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 21650 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.750 REMARK 200 RESOLUTION RANGE LOW (A) : 50.000 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : 2.000 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 99.9 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) : 2.75 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 2.82 REMARK 200 COMPLETENESS FOR SHELL (%) : 99.6 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: BALBES REMARK 200 STARTING MODEL: NULL REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 50.49 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.48 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: MAGNESIUM ACETATE, 0.1M TRIS (PH 8.5), REMARK 280 12% PEG 8000, VAPOR DIFFUSION, HANGING DROP, TEMPERATURE 289K REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: C 1 2 1 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+1/2,Z 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 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 118.11250 REMARK 290 SMTRY2 3 0.000000 1.000000 0.000000 45.97250 REMARK 290 SMTRY3 3 0.000000 0.000000 1.000000 0.00000 REMARK 290 SMTRY1 4 -1.000000 0.000000 0.000000 118.11250 REMARK 290 SMTRY2 4 0.000000 1.000000 0.000000 45.97250 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: 1760 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 15970 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -4.0 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 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: 1750 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 15680 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -4.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: C, 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 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 A -2 REMARK 465 ASN A -1 REMARK 465 ALA A 0 REMARK 465 CYS A 1 REMARK 465 ASP A 2 REMARK 465 LEU A 3 REMARK 465 PRO A 4 REMARK 465 GLU A 5 REMARK 465 THR A 6 REMARK 465 HIS A 7 REMARK 465 SER A 8 REMARK 465 GLY A 45 REMARK 465 ASN A 46 REMARK 465 GLN A 47 REMARK 465 PHE A 48 REMARK 465 GLN A 49 REMARK 465 LYS A 50 REMARK 465 GLU A 103 REMARK 465 GLU A 104 REMARK 465 ARG A 105 REMARK 465 VAL A 106 REMARK 465 GLY A 107 REMARK 465 GLU A 108 REMARK 465 THR A 109 REMARK 465 PRO A 110 REMARK 465 LEU A 111 REMARK 465 MET A 112 REMARK 465 ASN A 157 REMARK 465 LEU A 158 REMARK 465 GLN A 159 REMARK 465 GLU A 160 REMARK 465 ARG A 161 REMARK 465 LEU A 162 REMARK 465 ARG A 163 REMARK 465 ARG A 164 REMARK 465 LYS A 165 REMARK 465 GLU A 166 REMARK 465 MET B 1 REMARK 465 ALA B 2 REMARK 465 ASP B 3 REMARK 465 GLY B 113 REMARK 465 SER B 114 REMARK 465 GLY B 115 REMARK 465 GLY B 116 REMARK 465 SER B 117 REMARK 465 THR B 118 REMARK 465 ILE B 119 REMARK 465 THR B 120 REMARK 465 SER B 121 REMARK 465 TYR B 122 REMARK 465 ASN B 123 REMARK 465 VAL B 124 REMARK 465 TYR B 125 REMARK 465 TYR B 126 REMARK 465 THR B 127 REMARK 465 LYS B 128 REMARK 465 LEU B 129 REMARK 465 SER B 130 REMARK 465 SER B 131 REMARK 465 SER B 132 REMARK 465 GLY B 133 REMARK 465 SER B 134 REMARK 465 GLU B 255 REMARK 465 HIS B 256 REMARK 465 SER C -2 REMARK 465 ASN C -1 REMARK 465 ALA C 0 REMARK 465 CYS C 1 REMARK 465 ASP C 2 REMARK 465 LEU C 3 REMARK 465 PRO C 4 REMARK 465 GLU C 5 REMARK 465 THR C 6 REMARK 465 HIS C 7 REMARK 465 SER C 8 REMARK 465 ASP C 44 REMARK 465 GLY C 45 REMARK 465 ASN C 46 REMARK 465 GLN C 47 REMARK 465 PHE C 48 REMARK 465 GLN C 49 REMARK 465 LYS C 50 REMARK 465 ALA C 51 REMARK 465 GLN C 102 REMARK 465 GLU C 103 REMARK 465 GLU C 104 REMARK 465 ARG C 105 REMARK 465 VAL C 106 REMARK 465 GLY C 107 REMARK 465 GLU C 108 REMARK 465 THR C 109 REMARK 465 PRO C 110 REMARK 465 LEU C 111 REMARK 465 MET C 112 REMARK 465 ASN C 157 REMARK 465 LEU C 158 REMARK 465 GLN C 159 REMARK 465 GLU C 160 REMARK 465 ARG C 161 REMARK 465 LEU C 162 REMARK 465 ARG C 163 REMARK 465 ARG C 164 REMARK 465 LYS C 165 REMARK 465 GLU C 166 REMARK 465 MET D 1 REMARK 465 ALA D 2 REMARK 465 ASP D 3 REMARK 465 GLY D 113 REMARK 465 SER D 114 REMARK 465 GLY D 115 REMARK 465 GLY D 116 REMARK 465 SER D 117 REMARK 465 THR D 118 REMARK 465 ILE D 119 REMARK 465 THR D 120 REMARK 465 SER D 121 REMARK 465 TYR D 122 REMARK 465 ASN D 123 REMARK 465 VAL D 124 REMARK 465 TYR D 125 REMARK 465 TYR D 126 REMARK 465 THR D 127 REMARK 465 LYS D 128 REMARK 465 LEU D 129 REMARK 465 SER D 130 REMARK 465 SER D 131 REMARK 465 SER D 132 REMARK 465 GLY D 133 REMARK 465 SER D 134 REMARK 465 HIS D 256 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 GLN A 102 CG CD OE1 NE2 REMARK 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: CLOSE CONTACTS IN SAME ASYMMETRIC UNIT REMARK 500 REMARK 500 THE FOLLOWING ATOMS ARE IN CLOSE CONTACT. REMARK 500 REMARK 500 ATM1 RES C SSEQI ATM2 RES C SSEQI DISTANCE REMARK 500 O ASP C 10 O HOH C 176 1.55 REMARK 500 OD1 ASN A 11 CD2 LEU A 152 2.04 REMARK 500 OD1 ASP D 196 O HOH D 272 2.13 REMARK 500 O PHE A 36 NH1 ARG A 126 2.15 REMARK 500 OE2 GLU D 100 O HOH D 272 2.15 REMARK 500 O VAL C 143 O HOH C 175 2.17 REMARK 500 OD2 ASP C 10 NE ARG C 12 2.18 REMARK 500 N GLY B 60 O HOH B 259 2.19 REMARK 500 REMARK 500 REMARK: NULL REMARK 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: CLOSE CONTACTS REMARK 500 REMARK 500 THE FOLLOWING ATOMS THAT ARE RELATED BY CRYSTALLOGRAPHIC REMARK 500 SYMMETRY ARE IN CLOSE CONTACT. AN ATOM LOCATED WITHIN 0.15 REMARK 500 ANGSTROMS OF A SYMMETRY RELATED ATOM IS ASSUMED TO BE ON A REMARK 500 SPECIAL POSITION AND IS, THEREFORE, LISTED IN REMARK 375 REMARK 500 INSTEAD OF REMARK 500. ATOMS WITH NON-BLANK ALTERNATE REMARK 500 LOCATION INDICATORS ARE NOT INCLUDED IN THE CALCULATIONS. REMARK 500 REMARK 500 DISTANCE CUTOFF: REMARK 500 2.2 ANGSTROMS FOR CONTACTS NOT INVOLVING HYDROGEN ATOMS REMARK 500 1.6 ANGSTROMS FOR CONTACTS INVOLVING HYDROGEN ATOMS REMARK 500 REMARK 500 ATM1 RES C SSEQI ATM2 RES C SSEQI SSYMOP DISTANCE REMARK 500 OE2 GLU A 97 NH2 ARG C 125 4556 1.63 REMARK 500 C LEU B 254 NH2 ARG C 13 4546 1.98 REMARK 500 REMARK 500 REMARK: NULL REMARK 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: COVALENT BOND ANGLES REMARK 500 REMARK 500 THE STEREOCHEMICAL PARAMETERS OF THE FOLLOWING RESIDUES REMARK 500 HAVE VALUES WHICH DEVIATE FROM EXPECTED VALUES BY MORE REMARK 500 THAN 6*RMSD (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,A1,3(1X,A4,2X),12X,F5.1) REMARK 500 REMARK 500 EXPECTED VALUES PROTEIN: ENGH AND HUBER, 1999 REMARK 500 EXPECTED VALUES NUCLEIC ACID: CLOWNEY ET AL 1996 REMARK 500 REMARK 500 M RES CSSEQI ATM1 ATM2 ATM3 REMARK 500 ARG C 13 NE - CZ - NH1 ANGL. DEV. = 3.9 DEGREES REMARK 500 ARG C 13 NE - CZ - NH2 ANGL. DEV. = -3.9 DEGREES REMARK 500 REMARK 500 REMARK: NULL 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 CYS A 29 57.66 -112.44 REMARK 500 ASN B 30 -84.17 -113.96 REMARK 500 ASP B 53 56.90 39.02 REMARK 500 ASN B 54 -54.90 69.49 REMARK 500 SER B 59 -81.83 -16.64 REMARK 500 SER B 197 -52.16 -18.39 REMARK 500 ALA B 226 160.01 171.46 REMARK 500 ASP B 235 -110.90 58.72 REMARK 500 CYS C 29 60.03 -115.66 REMARK 500 ASN D 30 -85.39 -115.38 REMARK 500 ASN D 54 -53.64 70.38 REMARK 500 SER D 59 -100.21 -11.14 REMARK 500 PRO D 62 163.48 -48.72 REMARK 500 VAL D 182 -56.66 -121.15 REMARK 500 SER D 197 -52.19 -16.28 REMARK 500 ALA D 226 161.23 169.27 REMARK 500 ASP D 235 -109.34 60.74 REMARK 500 LEU D 254 -179.10 -68.68 REMARK 500 REMARK 500 REMARK: NULL