REMARK 2 REMARK 2 RESOLUTION. 2.50 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) : 2.50 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 46.60 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 1.990 REMARK 3 COMPLETENESS FOR RANGE (%) : 98.8 REMARK 3 NUMBER OF REFLECTIONS : 30334 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.232 REMARK 3 R VALUE (WORKING SET) : 0.230 REMARK 3 FREE R VALUE : 0.265 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 6.580 REMARK 3 FREE R VALUE TEST SET COUNT : 1997 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 46.6048 - 6.0219 0.96 2142 152 0.2186 0.2486 REMARK 3 2 6.0219 - 4.7813 1.00 2095 148 0.1755 0.1833 REMARK 3 3 4.7813 - 4.1774 1.00 2058 144 0.1572 0.2162 REMARK 3 4 4.1774 - 3.7956 0.99 2034 144 0.2117 0.2296 REMARK 3 5 3.7956 - 3.5237 0.91 1885 132 0.2935 0.3423 REMARK 3 6 3.5237 - 3.3160 0.99 2018 142 0.2466 0.2615 REMARK 3 7 3.3160 - 3.1500 1.00 2035 143 0.2446 0.2867 REMARK 3 8 3.1500 - 3.0129 1.00 1993 141 0.2594 0.2868 REMARK 3 9 3.0129 - 2.8969 1.00 2040 144 0.2641 0.2959 REMARK 3 10 2.8969 - 2.7969 1.00 2013 142 0.2554 0.3355 REMARK 3 11 2.7969 - 2.7095 1.00 2013 142 0.2755 0.2876 REMARK 3 12 2.7095 - 2.6321 1.00 2014 141 0.3024 0.3887 REMARK 3 13 2.6321 - 2.5628 1.00 2001 141 0.3098 0.3624 REMARK 3 14 2.5628 - 2.5000 0.99 1996 141 0.3068 0.3794 REMARK 3 REMARK 3 BULK SOLVENT MODELLING. REMARK 3 METHOD USED : FLAT BULK SOLVENT MODEL REMARK 3 SOLVENT RADIUS : 1.20 REMARK 3 SHRINKAGE RADIUS : 0.98 REMARK 3 K_SOL : 0.35 REMARK 3 B_SOL : 43.97 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.790 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 25.710 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) : 2.48290 REMARK 3 B22 (A**2) : 0.10240 REMARK 3 B33 (A**2) : -2.58530 REMARK 3 B12 (A**2) : 0.00000 REMARK 3 B13 (A**2) : -0.00000 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 : 0.009 5793 REMARK 3 ANGLE : 1.287 7883 REMARK 3 CHIRALITY : 0.081 894 REMARK 3 PLANARITY : 0.006 997 REMARK 3 DIHEDRAL : 19.009 2120 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 5 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: chain A REMARK 3 ORIGIN FOR THE GROUP (A): -16.6282 14.3109 -18.3542 REMARK 3 T TENSOR REMARK 3 T11: 0.1748 T22: 0.3006 REMARK 3 T33: 0.3273 T12: 0.0126 REMARK 3 T13: 0.0083 T23: -0.0343 REMARK 3 L TENSOR REMARK 3 L11: 0.3672 L22: 1.1433 REMARK 3 L33: 2.5587 L12: 0.2143 REMARK 3 L13: 0.7616 L23: 0.6260 REMARK 3 S TENSOR REMARK 3 S11: -0.0268 S12: 0.0018 S13: 0.0211 REMARK 3 S21: 0.0403 S22: 0.0287 S23: 0.0079 REMARK 3 S31: -0.0575 S32: -0.1022 S33: 0.0129 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: chain H and resid 1:112 REMARK 3 ORIGIN FOR THE GROUP (A): -23.0912 -7.2195 1.9507 REMARK 3 T TENSOR REMARK 3 T11: 0.3150 T22: 0.3349 REMARK 3 T33: 0.2439 T12: -0.0130 REMARK 3 T13: 0.0641 T23: -0.0508 REMARK 3 L TENSOR REMARK 3 L11: 0.9073 L22: 2.2376 REMARK 3 L33: 1.5603 L12: 1.0123 REMARK 3 L13: 0.2602 L23: -0.5364 REMARK 3 S TENSOR REMARK 3 S11: -0.1152 S12: 0.0424 S13: -0.1178 REMARK 3 S21: -0.0321 S22: 0.0432 S23: 0.0388 REMARK 3 S31: 0.2305 S32: -0.3562 S33: 0.0531 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: chain H and resid 113:216 REMARK 3 ORIGIN FOR THE GROUP (A): -29.8382 -40.4012 24.4912 REMARK 3 T TENSOR REMARK 3 T11: 0.2497 T22: 0.2662 REMARK 3 T33: 0.3327 T12: 0.0036 REMARK 3 T13: -0.0324 T23: -0.0292 REMARK 3 L TENSOR REMARK 3 L11: 1.6413 L22: 2.3354 REMARK 3 L33: 2.3165 L12: 0.2796 REMARK 3 L13: 0.0848 L23: -0.2600 REMARK 3 S TENSOR REMARK 3 S11: 0.0909 S12: 0.0667 S13: 0.0143 REMARK 3 S21: 0.0982 S22: -0.2327 S23: 0.0808 REMARK 3 S31: -0.2044 S32: 0.0991 S33: 0.1406 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: chain L and resid 1:107 REMARK 3 ORIGIN FOR THE GROUP (A): -16.9168 -2.7279 22.5847 REMARK 3 T TENSOR REMARK 3 T11: 0.5391 T22: 0.3316 REMARK 3 T33: 0.3371 T12: 0.0237 REMARK 3 T13: -0.0699 T23: -0.0510 REMARK 3 L TENSOR REMARK 3 L11: 1.4274 L22: 0.8914 REMARK 3 L33: 1.9462 L12: 0.2945 REMARK 3 L13: -0.0942 L23: -1.0691 REMARK 3 S TENSOR REMARK 3 S11: 0.0109 S12: -0.1720 S13: 0.0077 REMARK 3 S21: 0.2234 S22: -0.0496 S23: -0.0297 REMARK 3 S31: -0.3210 S32: -0.1100 S33: 0.0875 REMARK 3 TLS GROUP : 5 REMARK 3 SELECTION: chain L and resid 108:211 REMARK 3 ORIGIN FOR THE GROUP (A): -15.2637 -33.2866 27.2927 REMARK 3 T TENSOR REMARK 3 T11: 0.3051 T22: 0.3793 REMARK 3 T33: 0.4264 T12: -0.0527 REMARK 3 T13: -0.0372 T23: -0.0510 REMARK 3 L TENSOR REMARK 3 L11: 1.8613 L22: 2.6937 REMARK 3 L33: 2.0939 L12: 0.3714 REMARK 3 L13: 0.4105 L23: 0.5983 REMARK 3 S TENSOR REMARK 3 S11: -0.1708 S12: 0.0355 S13: 0.1707 REMARK 3 S21: -0.0790 S22: 0.0777 S23: -0.0860 REMARK 3 S31: -0.2725 S32: 0.1649 S33: 0.1348 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 4FQJ 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 RCSB073229. 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 : 8.0 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : SSRL REMARK 200 BEAMLINE : BL11-1 REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 0.9795 REMARK 200 MONOCHROMATOR : DOUBLE CRYSTAL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : MARMOSAIC 325 MM CCD REMARK 200 INTENSITY-INTEGRATION SOFTWARE : XDS REMARK 200 DATA SCALING SOFTWARE : XSCALE REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 30377 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.500 REMARK 200 RESOLUTION RANGE LOW (A) : 47.000 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : -3.000 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 98.9 REMARK 200 DATA REDUNDANCY : 5.600 REMARK 200 R MERGE (I) : NULL REMARK 200 R SYM (I) : 0.08000 REMARK 200 FOR THE DATA SET : 15.6000 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 2.50 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 2.60 REMARK 200 COMPLETENESS FOR SHELL (%) : 99.2 REMARK 200 DATA REDUNDANCY IN SHELL : 6.30 REMARK 200 R MERGE FOR SHELL (I) : NULL REMARK 200 R SYM FOR SHELL (I) : 0.69000 REMARK 200 FOR SHELL : 2.400 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 ENTRIES 2RFT AND 3N9G REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 53.17 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.63 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 20% PEG3350, 200 MM SODIUM SULFATE, PH REMARK 280 8.0, VAPOR DIFFUSION, SITTING DROP, TEMPERATURE 295K 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 22.78500 REMARK 290 SMTRY2 2 0.000000 -1.000000 0.000000 0.00000 REMARK 290 SMTRY3 2 0.000000 0.000000 1.000000 84.13000 REMARK 290 SMTRY1 3 -1.000000 0.000000 0.000000 0.00000 REMARK 290 SMTRY2 3 0.000000 1.000000 0.000000 55.96500 REMARK 290 SMTRY3 3 0.000000 0.000000 -1.000000 84.13000 REMARK 290 SMTRY1 4 1.000000 0.000000 0.000000 22.78500 REMARK 290 SMTRY2 4 0.000000 -1.000000 0.000000 55.96500 REMARK 290 SMTRY3 4 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: 6920 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 32740 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -14.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: A, 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 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 PRO A 31 REMARK 465 LEU A 32 REMARK 465 PRO A 325 REMARK 465 LEU A 326 REMARK 465 HIS A 327 REMARK 465 HIS A 328 REMARK 465 HIS A 329 REMARK 465 HIS A 330 REMARK 465 HIS A 331 REMARK 465 HIS A 332 REMARK 465 SER L 212 REMARK 465 SER H 128 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 ND2 ASN A 59 C2 NAG A 701 2.13 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 ASP A 56 -21.59 99.23 REMARK 500 MET A 71 3.66 84.53 REMARK 500 VAL A 73 74.74 -105.74 REMARK 500 SER A 92 41.49 -143.99 REMARK 500 CYS A 94 -169.88 61.53 REMARK 500 LYS A 103 30.50 -89.60 REMARK 500 ASN A 145 -126.84 -95.45 REMARK 500 ASN A 163A 0.63 171.25 REMARK 500 LYS A 164 95.55 -57.13 REMARK 500 ILE A 177 -11.55 69.23 REMARK 500 GLU A 180 -144.83 44.99 REMARK 500 GLN A 261 -132.98 -116.43 REMARK 500 GLN A 268 -89.53 -133.82 REMARK 500 LYS A 302 39.18 -87.54 REMARK 500 ALA A 312 -169.55 -64.02 REMARK 500 ASN L 27B -94.00 -107.04 REMARK 500 SER L 51 -43.76 68.97 REMARK 500 ALA L 84 -167.88 -169.74 REMARK 500 ASP L 151 -106.49 50.01 REMARK 500 GLN L 167 -160.86 -115.68 REMARK 500 GLN H 43 -167.52 -129.15 REMARK 500 THR H 76 60.46 36.99 REMARK 500 TYR H 100F -161.74 -101.41 REMARK 500 ASP H 101 -88.56 -100.91 REMARK 500 SER H 115 49.74 -145.24 REMARK 500 THR H 116 101.36 51.60 REMARK 500 ASP H 144 74.58 61.45 REMARK 500 THR H 160 -32.91 -132.13 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 NAG A 701 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC2 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE NAG A 702 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC3 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE NAG A 703 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC4 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE NAG A 704 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC5 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE BMA A 705 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC6 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE NAG A 706 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC7 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE NAG A 707 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: 4FQK RELATED DB: PDB REMARK 900 RELATED ID: 4FQL 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