REMARK 2 REMARK 2 RESOLUTION. 1.90 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.7.2_869) 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 : MLHL REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS) : 1.90 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 40.24 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 1.990 REMARK 3 COMPLETENESS FOR RANGE (%) : 98.6 REMARK 3 NUMBER OF REFLECTIONS : 40102 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.196 REMARK 3 R VALUE (WORKING SET) : 0.194 REMARK 3 FREE R VALUE : 0.231 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 4.980 REMARK 3 FREE R VALUE TEST SET COUNT : 1999 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 40.2537 - 4.5732 0.99 2822 148 0.2003 0.2261 REMARK 3 2 4.5732 - 3.6307 0.99 2767 146 0.1669 0.2064 REMARK 3 3 3.6307 - 3.1719 0.99 2735 143 0.1877 0.2189 REMARK 3 4 3.1719 - 2.8820 0.99 2734 143 0.1971 0.2166 REMARK 3 5 2.8820 - 2.6755 0.99 2750 145 0.2081 0.2639 REMARK 3 6 2.6755 - 2.5178 0.99 2707 142 0.2036 0.2421 REMARK 3 7 2.5178 - 2.3917 0.99 2723 143 0.2009 0.2681 REMARK 3 8 2.3917 - 2.2876 0.99 2732 142 0.1961 0.2140 REMARK 3 9 2.2876 - 2.1995 0.99 2725 144 0.1934 0.2445 REMARK 3 10 2.1995 - 2.1236 0.99 2705 142 0.1913 0.2517 REMARK 3 11 2.1236 - 2.0572 0.99 2708 142 0.2024 0.2290 REMARK 3 12 2.0572 - 1.9984 0.99 2717 142 0.2012 0.2166 REMARK 3 13 1.9984 - 1.9458 0.99 2667 139 0.2134 0.2651 REMARK 3 14 1.9458 - 1.8984 0.94 2611 138 0.2419 0.3046 REMARK 3 REMARK 3 BULK SOLVENT MODELLING. REMARK 3 METHOD USED : FLAT BULK SOLVENT MODEL REMARK 3 SOLVENT RADIUS : 1.30 REMARK 3 SHRINKAGE RADIUS : 1.11 REMARK 3 K_SOL : 0.33 REMARK 3 B_SOL : 32.35 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.510 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 23.100 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) : -5.79200 REMARK 3 B22 (A**2) : 7.35070 REMARK 3 B33 (A**2) : -1.55870 REMARK 3 B12 (A**2) : 0.00000 REMARK 3 B13 (A**2) : 7.01180 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 3413 REMARK 3 ANGLE : 1.177 4629 REMARK 3 CHIRALITY : 0.077 517 REMARK 3 PLANARITY : 0.005 596 REMARK 3 DIHEDRAL : 14.327 1224 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 4 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: chain L and resid 1:108 REMARK 3 ORIGIN FOR THE GROUP (A): -5.6420 -13.1799 25.1769 REMARK 3 T TENSOR REMARK 3 T11: 0.1818 T22: 0.1678 REMARK 3 T33: 0.2211 T12: -0.0034 REMARK 3 T13: -0.0137 T23: 0.0124 REMARK 3 L TENSOR REMARK 3 L11: 0.3901 L22: 0.9351 REMARK 3 L33: 0.7047 L12: -0.4366 REMARK 3 L13: 0.2718 L23: 0.0027 REMARK 3 S TENSOR REMARK 3 S11: -0.0215 S12: 0.0879 S13: 0.1240 REMARK 3 S21: 0.0161 S22: 0.0357 S23: -0.1075 REMARK 3 S31: -0.0121 S32: -0.0619 S33: -0.0000 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: chain L and resid 109:213 REMARK 3 ORIGIN FOR THE GROUP (A): 0.4152 -35.6513 52.9828 REMARK 3 T TENSOR REMARK 3 T11: 0.2335 T22: 0.2795 REMARK 3 T33: 0.2413 T12: 0.0738 REMARK 3 T13: 0.0342 T23: 0.0617 REMARK 3 L TENSOR REMARK 3 L11: 0.8122 L22: 0.5237 REMARK 3 L33: 0.6942 L12: 0.1907 REMARK 3 L13: 0.0533 L23: -0.0749 REMARK 3 S TENSOR REMARK 3 S11: -0.0560 S12: -0.2624 S13: -0.0905 REMARK 3 S21: -0.0134 S22: 0.0337 S23: -0.0117 REMARK 3 S31: 0.0347 S32: 0.1289 S33: -0.0004 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: chain H and resid 1:118 REMARK 3 ORIGIN FOR THE GROUP (A): -6.2311 -31.8114 11.6180 REMARK 3 T TENSOR REMARK 3 T11: 0.1913 T22: 0.2255 REMARK 3 T33: 0.1616 T12: -0.0039 REMARK 3 T13: -0.0222 T23: -0.0083 REMARK 3 L TENSOR REMARK 3 L11: 0.5398 L22: 0.4573 REMARK 3 L33: 1.1614 L12: -0.2216 REMARK 3 L13: -0.6297 L23: -0.0453 REMARK 3 S TENSOR REMARK 3 S11: -0.0605 S12: 0.1112 S13: -0.0146 REMARK 3 S21: 0.0845 S22: -0.0104 S23: 0.0357 REMARK 3 S31: 0.0659 S32: -0.0927 S33: -0.0000 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: chain H and resid 119:216 REMARK 3 ORIGIN FOR THE GROUP (A): -10.4769 -43.8580 44.6486 REMARK 3 T TENSOR REMARK 3 T11: 0.2732 T22: 0.2067 REMARK 3 T33: 0.3386 T12: 0.0430 REMARK 3 T13: 0.0648 T23: 0.0438 REMARK 3 L TENSOR REMARK 3 L11: 0.4825 L22: 0.6740 REMARK 3 L33: 0.6564 L12: -0.1666 REMARK 3 L13: 0.4341 L23: 0.4836 REMARK 3 S TENSOR REMARK 3 S11: -0.1265 S12: -0.1851 S13: -0.2252 REMARK 3 S21: 0.0644 S22: -0.0308 S23: 0.2035 REMARK 3 S31: 0.1564 S32: -0.0152 S33: 0.0000 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 4FQL COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 11-JUL-12. REMARK 100 THE RCSB ID CODE IS RCSB073231. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : NULL REMARK 200 TEMPERATURE (KELVIN) : NULL REMARK 200 PH : 6.0 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : ALS REMARK 200 BEAMLINE : 5.0.2 REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 1.00000 REMARK 200 MONOCHROMATOR : DOUBLE CRYSTAL SI(111) REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : ADSC QUANTUM 315 REMARK 200 INTENSITY-INTEGRATION SOFTWARE : XDS REMARK 200 DATA SCALING SOFTWARE : XSCALE REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 40203 REMARK 200 RESOLUTION RANGE HIGH (A) : 1.898 REMARK 200 RESOLUTION RANGE LOW (A) : 69.113 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : -3.000 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 98.0 REMARK 200 DATA REDUNDANCY : 3.800 REMARK 200 R MERGE (I) : NULL REMARK 200 R SYM (I) : 0.13000 REMARK 200 FOR THE DATA SET : 6.9000 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 1.90 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 2.00 REMARK 200 COMPLETENESS FOR SHELL (%) : 98.2 REMARK 200 DATA REDUNDANCY IN SHELL : 3.80 REMARK 200 R MERGE FOR SHELL (I) : NULL REMARK 200 R SYM FOR SHELL (I) : 0.63000 REMARK 200 FOR SHELL : 2.600 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 3N9G REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 53.66 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.65 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 200 MM ZINC ACETATE, 10% PEG8000, 100 REMARK 280 MM MES, PH 6.0, VAPOR DIFFUSION, SITTING DROP, TEMPERATURE 295K 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 68.10000 REMARK 290 SMTRY2 3 0.000000 1.000000 0.000000 27.50000 REMARK 290 SMTRY3 3 0.000000 0.000000 1.000000 0.00000 REMARK 290 SMTRY1 4 -1.000000 0.000000 0.000000 68.10000 REMARK 290 SMTRY2 4 0.000000 1.000000 0.000000 27.50000 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: 3290 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 20070 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -27.0 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 350 REMARK 350 BIOMOLECULE: 2 REMARK 350 SOFTWARE DETERMINED QUATERNARY STRUCTURE: TETRAMERIC REMARK 350 SOFTWARE USED: PISA REMARK 350 TOTAL BURIED SURFACE AREA: 8130 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 38590 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -63.0 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 350 BIOMT1 2 -1.000000 0.000000 0.000000 0.00000 REMARK 350 BIOMT2 2 0.000000 1.000000 0.000000 0.00000 REMARK 350 BIOMT3 2 0.000000 0.000000 -1.000000 0.00000 REMARK 375 REMARK 375 SPECIAL POSITION REMARK 375 THE FOLLOWING ATOMS ARE FOUND TO BE WITHIN 0.15 ANGSTROMS REMARK 375 OF A SYMMETRY RELATED ATOM AND ARE ASSUMED TO BE ON SPECIAL REMARK 375 POSITIONS. REMARK 375 REMARK 375 ATOM RES CSSEQI REMARK 375 HOH H 310 LIES ON A SPECIAL POSITION. 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 H 129 REMARK 465 SER H 130 REMARK 465 THR H 131 REMARK 465 SER H 132 REMARK 465 GLY H 133 REMARK 465 HIS H 217 REMARK 465 HIS H 218 REMARK 465 HIS H 219 REMARK 465 HIS H 220 REMARK 465 HIS H 221 REMARK 465 HIS H 222 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 SG CYS H 216 CB CYS L 214 1.79 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 ALA H 100A -122.80 64.59 REMARK 500 MET H 100B 22.55 46.85 REMARK 500 ASP H 100C 83.85 46.24 REMARK 500 ASP H 144 64.03 64.89 REMARK 500 ALA L 51 -31.95 64.25 REMARK 500 ASN L 138 61.89 61.21 REMARK 500 LYS L 190 -60.20 -107.98 REMARK 500 REMARK 500 REMARK: NULL REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 4FNK RELATED DB: PDB REMARK 900 RELATED ID: 4FQH RELATED DB: PDB REMARK 900 RELATED ID: 4FQI RELATED DB: PDB REMARK 900 RELATED ID: 4FQJ RELATED DB: PDB REMARK 900 RELATED ID: 4FQK RELATED DB: PDB REMARK 900 RELATED ID: 4FQM RELATED DB: PDB REMARK 900 RELATED ID: 4FQV RELATED DB: PDB REMARK 900 RELATED ID: 4FQY RELATED DB: PDB