REMARK 2 REMARK 2 RESOLUTION. 1.70 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.6.1_357) 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) : 1.70 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 30.56 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 0.070 REMARK 3 COMPLETENESS FOR RANGE (%) : 98.0 REMARK 3 NUMBER OF REFLECTIONS : 54885 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.179 REMARK 3 R VALUE (WORKING SET) : 0.178 REMARK 3 FREE R VALUE : 0.200 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.080 REMARK 3 FREE R VALUE TEST SET COUNT : 2788 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 30.5636 - 4.6095 0.85 2329 114 0.1880 0.2124 REMARK 3 2 4.6095 - 3.6607 0.97 2585 142 0.1427 0.1417 REMARK 3 3 3.6607 - 3.1985 1.00 2666 140 0.1472 0.1703 REMARK 3 4 3.1985 - 2.9063 1.00 2681 140 0.1632 0.1696 REMARK 3 5 2.9063 - 2.6981 1.00 2660 138 0.1729 0.2084 REMARK 3 6 2.6981 - 2.5391 1.00 2668 142 0.1696 0.2007 REMARK 3 7 2.5391 - 2.4120 1.00 2658 120 0.1697 0.2236 REMARK 3 8 2.4120 - 2.3071 1.00 2640 166 0.1752 0.2104 REMARK 3 9 2.3071 - 2.2183 1.00 2663 162 0.1711 0.2056 REMARK 3 10 2.2183 - 2.1417 1.00 2630 130 0.1694 0.1858 REMARK 3 11 2.1417 - 2.0748 0.99 2635 145 0.1707 0.2291 REMARK 3 12 2.0748 - 2.0155 1.00 2597 160 0.1765 0.1879 REMARK 3 13 2.0155 - 1.9624 0.99 2643 135 0.1887 0.2184 REMARK 3 14 1.9624 - 1.9146 0.99 2611 147 0.2040 0.2267 REMARK 3 15 1.9146 - 1.8711 0.99 2637 139 0.2153 0.2234 REMARK 3 16 1.8711 - 1.8312 0.99 2625 145 0.2191 0.2577 REMARK 3 17 1.8312 - 1.7946 0.98 2614 122 0.2242 0.2661 REMARK 3 18 1.7946 - 1.7608 0.98 2570 127 0.2395 0.2476 REMARK 3 19 1.7608 - 1.7293 0.97 2583 131 0.2512 0.2753 REMARK 3 20 1.7293 - 1.7000 0.92 2402 143 0.2641 0.2762 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 : 0.40 REMARK 3 B_SOL : 59.57 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.210 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : NULL REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : 28.70 REMARK 3 MEAN B VALUE (OVERALL, A**2) : NULL REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2) : -3.91870 REMARK 3 B22 (A**2) : 3.29560 REMARK 3 B33 (A**2) : 0.62310 REMARK 3 B12 (A**2) : -0.00000 REMARK 3 B13 (A**2) : -4.08680 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 : 0.006 3494 REMARK 3 ANGLE : 1.094 4753 REMARK 3 CHIRALITY : 0.078 532 REMARK 3 PLANARITY : 0.004 606 REMARK 3 DIHEDRAL : 13.089 1252 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 4 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: CHAIN L AND RESSEQ 1:109 REMARK 3 ORIGIN FOR THE GROUP (A): 36.4283 5.4409 24.3594 REMARK 3 T TENSOR REMARK 3 T11: 0.2303 T22: 0.2042 REMARK 3 T33: 0.1983 T12: -0.0054 REMARK 3 T13: -0.0166 T23: -0.0084 REMARK 3 L TENSOR REMARK 3 L11: 1.7868 L22: 0.7649 REMARK 3 L33: 1.6397 L12: 0.2076 REMARK 3 L13: -0.2461 L23: -0.7631 REMARK 3 S TENSOR REMARK 3 S11: -0.0058 S12: -0.2636 S13: 0.0998 REMARK 3 S21: 0.2618 S22: -0.0085 S23: -0.0993 REMARK 3 S31: -0.1167 S32: -0.0028 S33: -0.0000 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: CHAIN L AND RESSEQ 110:214 REMARK 3 ORIGIN FOR THE GROUP (A): 9.0360 8.9132 0.3307 REMARK 3 T TENSOR REMARK 3 T11: 0.1497 T22: 0.1248 REMARK 3 T33: 0.1564 T12: -0.0039 REMARK 3 T13: 0.0091 T23: 0.0045 REMARK 3 L TENSOR REMARK 3 L11: 1.8663 L22: 1.0467 REMARK 3 L33: 0.6939 L12: -0.5630 REMARK 3 L13: 0.3306 L23: -0.4818 REMARK 3 S TENSOR REMARK 3 S11: -0.0731 S12: 0.0608 S13: 0.1628 REMARK 3 S21: -0.0231 S22: 0.0374 S23: 0.0034 REMARK 3 S31: -0.0349 S32: 0.1069 S33: 0.0000 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: CHAIN H AND RESSEQ 1:112 REMARK 3 ORIGIN FOR THE GROUP (A): 22.5773 -6.9638 36.3886 REMARK 3 T TENSOR REMARK 3 T11: 0.3063 T22: 0.4199 REMARK 3 T33: 0.2409 T12: -0.0261 REMARK 3 T13: -0.0092 T23: 0.1074 REMARK 3 L TENSOR REMARK 3 L11: 2.4105 L22: 0.5181 REMARK 3 L33: 1.1765 L12: 1.1112 REMARK 3 L13: 0.9047 L23: 0.3511 REMARK 3 S TENSOR REMARK 3 S11: 0.1592 S12: -0.7145 S13: -0.3329 REMARK 3 S21: 0.2482 S22: -0.0608 S23: -0.1294 REMARK 3 S31: 0.2393 S32: -0.2102 S33: 0.0000 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: CHAIN H AND RESSEQ 113:225 REMARK 3 ORIGIN FOR THE GROUP (A): 7.5481 -6.2996 1.1594 REMARK 3 T TENSOR REMARK 3 T11: 0.0908 T22: 0.0410 REMARK 3 T33: 0.1031 T12: -0.0046 REMARK 3 T13: -0.0060 T23: -0.0127 REMARK 3 L TENSOR REMARK 3 L11: 2.4409 L22: 2.3394 REMARK 3 L33: 1.0659 L12: 0.3066 REMARK 3 L13: -0.1072 L23: 0.0914 REMARK 3 S TENSOR REMARK 3 S11: 0.0128 S12: 0.2300 S13: -0.1278 REMARK 3 S21: -0.2855 S22: 0.0296 S23: 0.0491 REMARK 3 S31: 0.0606 S32: -0.0475 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 3NAA COMPLIES WITH FORMAT V. 3.20, 01-DEC-08 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 08-JUN-10. REMARK 100 THE RCSB ID CODE IS RCSB059577. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 17-MAR-10 REMARK 200 TEMPERATURE (KELVIN) : 100 REMARK 200 PH : NULL REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : APS REMARK 200 BEAMLINE : 17-ID REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 1.0000 REMARK 200 MONOCHROMATOR : ACCEL SI (111) DOUBLE CRYSTAL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : ADSC QUANTUM 210 REMARK 200 INTENSITY-INTEGRATION SOFTWARE : D*TREK REMARK 200 DATA SCALING SOFTWARE : D*TREK REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 55410 REMARK 200 RESOLUTION RANGE HIGH (A) : 1.700 REMARK 200 RESOLUTION RANGE LOW (A) : 30.559 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : -3.000 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 98.9 REMARK 200 DATA REDUNDANCY : 3.610 REMARK 200 R MERGE (I) : 0.07300 REMARK 200 R SYM (I) : NULL REMARK 200 FOR THE DATA SET : 8.7000 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 1.70 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 1.76 REMARK 200 COMPLETENESS FOR SHELL (%) : 98.3 REMARK 200 DATA REDUNDANCY IN SHELL : 3.01 REMARK 200 R MERGE FOR SHELL (I) : 0.42300 REMARK 200 R SYM FOR SHELL (I) : NULL REMARK 200 FOR SHELL : 1.800 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 3NA9 REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 54.58 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.71 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: NULL 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 37.39200 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: DIMERIC REMARK 350 SOFTWARE DETERMINED QUATERNARY STRUCTURE: DIMERIC REMARK 350 SOFTWARE USED: PISA REMARK 350 TOTAL BURIED SURFACE AREA: 4920 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 19550 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -115.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: L, H 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 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 CYS L 134 CA CB SG 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 HOH H 242 O HOH H 362 1.89 REMARK 500 O HOH L 289 O HOH H 291 1.89 REMARK 500 OE2 GLU H 133 O HOH H 338 2.00 REMARK 500 O HOH H 269 O HOH H 306 2.00 REMARK 500 O HOH H 424 O HOH H 439 2.00 REMARK 500 O HOH H 230 O HOH H 418 2.01 REMARK 500 O HOH H 283 O HOH H 459 2.01 REMARK 500 O HOH H 353 O HOH H 436 2.04 REMARK 500 O HOH H 272 O HOH H 317 2.05 REMARK 500 O HOH L 380 O HOH H 354 2.08 REMARK 500 O HOH L 228 O HOH L 451 2.08 REMARK 500 O HOH H 392 O HOH H 476 2.10 REMARK 500 OG SER L 127 O HOH L 241 2.10 REMARK 500 O HOH L 268 O HOH L 439 2.11 REMARK 500 OE1 GLU L 123 O HOH L 228 2.12 REMARK 500 O HOH H 261 O HOH H 369 2.14 REMARK 500 O HOH L 357 O HOH L 470 2.14 REMARK 500 NZ LYS H 117 O HOH H 249 2.15 REMARK 500 O HOH H 300 O HOH H 411 2.19 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 L 51 -42.57 74.56 REMARK 500 ALA L 84 -179.94 -179.20 REMARK 500 ALA H 88 169.17 177.46 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 ZN L 215 ZN REMARK 620 N RES CSSEQI ATOM REMARK 620 1 ASP L 151 OD2 REMARK 620 2 ACT L 216 OXT 103.4 REMARK 620 3 HIS L 189 ND1 105.0 112.0 REMARK 620 N 1 2 REMARK 620 REMARK 620 COORDINATION ANGLES FOR: M RES CSSEQI METAL REMARK 620 ZN H 218 ZN REMARK 620 N RES CSSEQI ATOM REMARK 620 1 CYS L 214 O REMARK 620 2 HIS H 213 NE2 105.5 REMARK 620 3 HIS H 217 NE2 97.1 102.2 REMARK 620 4 ACT H 220 O 120.1 103.5 125.9 REMARK 620 5 ACT H 220 OXT 90.0 157.2 92.1 53.8 REMARK 620 N 1 2 3 4 REMARK 620 REMARK 620 COORDINATION ANGLES FOR: M RES CSSEQI METAL REMARK 620 ZN H 219 ZN REMARK 620 N RES CSSEQI ATOM REMARK 620 1 ASP H 54 OD2 REMARK 620 2 ASP H 52 OD2 116.5 REMARK 620 N 1 REMARK 800 REMARK 800 SITE REMARK 800 SITE_IDENTIFIER: AC1 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE ZN L 215 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC2 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE ACT L 216 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC3 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE GOL L 217 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC4 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE ZN H 218 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC5 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE ZN H 219 REMARK 800 REMARK 800 SITE_IDENTIFIER: AC6 REMARK 800 EVIDENCE_CODE: SOFTWARE REMARK 800 SITE_DESCRIPTION: BINDING SITE FOR RESIDUE ACT H 220 REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 3NA9 RELATED DB: PDB REMARK 900 RELATED ID: 3NCJ RELATED DB: PDB REMARK 900 RELATED ID: 3NAB RELATED DB: PDB REMARK 900 RELATED ID: 3NAC RELATED DB: PDB