REMARK 2 REMARK 2 RESOLUTION. 2.80 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.6.4_486) 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) : 44.79 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 1.350 REMARK 3 COMPLETENESS FOR RANGE (%) : 97.8 REMARK 3 NUMBER OF REFLECTIONS : 17490 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.224 REMARK 3 R VALUE (WORKING SET) : 0.222 REMARK 3 FREE R VALUE : 0.268 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.100 REMARK 3 FREE R VALUE TEST SET COUNT : 939 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 44.7964 - 5.3534 1.00 2609 152 0.2680 0.3060 REMARK 3 2 5.3534 - 4.2502 1.00 2539 129 0.1986 0.2463 REMARK 3 3 4.2502 - 3.7132 1.00 2595 123 0.2031 0.2210 REMARK 3 4 3.7132 - 3.3739 1.00 2515 155 0.1990 0.2836 REMARK 3 5 3.3739 - 3.1321 1.00 2548 127 0.2127 0.2604 REMARK 3 6 3.1321 - 2.9475 0.98 2487 145 0.2357 0.2781 REMARK 3 7 2.9475 - 2.8000 0.86 2194 108 0.2634 0.3078 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 : 0.33 REMARK 3 B_SOL : 31.48 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.400 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : NULL REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : 55.69 REMARK 3 MEAN B VALUE (OVERALL, A**2) : NULL REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2) : 6.77210 REMARK 3 B22 (A**2) : -5.48230 REMARK 3 B33 (A**2) : -1.28990 REMARK 3 B12 (A**2) : 0.00000 REMARK 3 B13 (A**2) : -8.68640 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 : NULL NULL REMARK 3 ANGLE : NULL NULL REMARK 3 CHIRALITY : NULL NULL REMARK 3 PLANARITY : NULL NULL REMARK 3 DIHEDRAL : NULL NULL REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 5 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: CHAIN L AND RESID 1:110 REMARK 3 ORIGIN FOR THE GROUP (A): 38.5945 62.8801 49.2642 REMARK 3 T TENSOR REMARK 3 T11: 0.1527 T22: 0.4046 REMARK 3 T33: 0.1846 T12: 0.0001 REMARK 3 T13: -0.0105 T23: 0.0014 REMARK 3 L TENSOR REMARK 3 L11: 0.1443 L22: 0.1503 REMARK 3 L33: 0.1807 L12: 0.0931 REMARK 3 L13: -0.0808 L23: -0.1741 REMARK 3 S TENSOR REMARK 3 S11: -0.0955 S12: -0.0971 S13: 0.1228 REMARK 3 S21: 0.1388 S22: 0.0694 S23: 0.0918 REMARK 3 S31: 0.0097 S32: 0.4361 S33: 0.0000 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: CHAIN L AND RESID 111:214 REMARK 3 ORIGIN FOR THE GROUP (A): 25.3412 50.8494 16.2620 REMARK 3 T TENSOR REMARK 3 T11: 0.1361 T22: 0.0978 REMARK 3 T33: 0.1145 T12: -0.0167 REMARK 3 T13: -0.0238 T23: -0.0505 REMARK 3 L TENSOR REMARK 3 L11: 0.3069 L22: 0.0098 REMARK 3 L33: 0.2877 L12: -0.0410 REMARK 3 L13: -0.0135 L23: -0.1090 REMARK 3 S TENSOR REMARK 3 S11: -0.2120 S12: 0.0644 S13: -0.0459 REMARK 3 S21: 0.0523 S22: 0.0808 S23: 0.1056 REMARK 3 S31: -0.0311 S32: 0.1574 S33: -0.0546 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: CHAIN H AND RESID 1:114 REMARK 3 ORIGIN FOR THE GROUP (A): 16.8658 67.3834 52.3019 REMARK 3 T TENSOR REMARK 3 T11: 0.2166 T22: 0.1267 REMARK 3 T33: 0.1252 T12: 0.0839 REMARK 3 T13: -0.0758 T23: -0.0450 REMARK 3 L TENSOR REMARK 3 L11: 0.1997 L22: 0.2164 REMARK 3 L33: 0.3355 L12: -0.0267 REMARK 3 L13: 0.1010 L23: 0.2842 REMARK 3 S TENSOR REMARK 3 S11: -0.1714 S12: -0.2171 S13: 0.0618 REMARK 3 S21: -0.1413 S22: 0.0495 S23: 0.0548 REMARK 3 S31: -0.1371 S32: -0.1216 S33: 0.0002 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: CHAIN H AND RESID 115:218 REMARK 3 ORIGIN FOR THE GROUP (A): 15.1662 49.3585 28.8807 REMARK 3 T TENSOR REMARK 3 T11: 0.1905 T22: 0.1426 REMARK 3 T33: 0.2294 T12: 0.0656 REMARK 3 T13: 0.0232 T23: -0.0254 REMARK 3 L TENSOR REMARK 3 L11: 0.0386 L22: 0.0654 REMARK 3 L33: 0.1200 L12: 0.0273 REMARK 3 L13: -0.0646 L23: -0.0397 REMARK 3 S TENSOR REMARK 3 S11: -0.0161 S12: -0.0928 S13: -0.1187 REMARK 3 S21: -0.2262 S22: -0.0379 S23: 0.2244 REMARK 3 S31: 0.0280 S32: -0.0430 S33: 0.0000 REMARK 3 TLS GROUP : 5 REMARK 3 SELECTION: CHAIN B REMARK 3 ORIGIN FOR THE GROUP (A): 27.8660 51.6992 92.4359 REMARK 3 T TENSOR REMARK 3 T11: 0.0492 T22: 0.0065 REMARK 3 T33: 0.0745 T12: 0.0093 REMARK 3 T13: -0.0268 T23: -0.0240 REMARK 3 L TENSOR REMARK 3 L11: 0.4495 L22: 0.8363 REMARK 3 L33: 0.8744 L12: 0.1125 REMARK 3 L13: 0.0182 L23: -0.3291 REMARK 3 S TENSOR REMARK 3 S11: -0.0067 S12: 0.0561 S13: -0.0138 REMARK 3 S21: 0.0191 S22: 0.0136 S23: -0.0118 REMARK 3 S31: -0.0212 S32: -0.0120 S33: 0.0001 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 3R1G COMPLIES WITH FORMAT V. 3.20, 01-DEC-08 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 15-MAR-11. REMARK 100 THE RCSB ID CODE IS RCSB064369. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 10-DEC-09 REMARK 200 TEMPERATURE (KELVIN) : 93 REMARK 200 PH : 8.5 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : SSRL REMARK 200 BEAMLINE : BL7-1 REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 0.98057 REMARK 200 MONOCHROMATOR : SIDE SCATTERING I-BEAM BENT REMARK 200 SINGLE CRYSTAL, ASYMMETRIC CUT REMARK 200 4.9650 DEG 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 : 17490 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.800 REMARK 200 RESOLUTION RANGE LOW (A) : 45.000 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : 1.000 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 97.9 REMARK 200 DATA REDUNDANCY : 3.500 REMARK 200 R MERGE (I) : NULL REMARK 200 R SYM (I) : 0.11200 REMARK 200 FOR THE DATA SET : 10.8000 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 2.80 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 2.90 REMARK 200 COMPLETENESS FOR SHELL (%) : 84.4 REMARK 200 DATA REDUNDANCY IN SHELL : 2.50 REMARK 200 R MERGE FOR SHELL (I) : NULL REMARK 200 R SYM FOR SHELL (I) : 0.36600 REMARK 200 FOR SHELL : 2.000 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 (%): 41.59 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.11 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 1 UL OF THE BACE1/FAB COMPLEX SOLUTION REMARK 280 MIXED WITH 1 UL OF WELL SOLUTION CONTAINING 20% PEG 4000, 0.1M REMARK 280 TRIS, 0.2 M SODIUM ACETATE, PH 8.5, VAPOR DIFFUSION, SITTING REMARK 280 DROP, TEMPERATURE 292K 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 37.76850 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: TRIMERIC REMARK 350 SOFTWARE DETERMINED QUATERNARY STRUCTURE: TRIMERIC REMARK 350 SOFTWARE USED: PISA REMARK 350 TOTAL BURIED SURFACE AREA: 5340 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 33440 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -36.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: B, 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 GLY B 55 REMARK 465 GLY B 219 REMARK 465 PHE B 220 REMARK 465 PRO B 221 REMARK 465 LEU B 222 REMARK 465 ASN B 223 REMARK 465 GLN B 224 REMARK 465 SER B 225 REMARK 465 GLU B 226 REMARK 465 VAL B 227 REMARK 465 GLU B 371 REMARK 465 ASP B 372 REMARK 465 PRO B 448 REMARK 465 GLN B 449 REMARK 465 THR B 450 REMARK 465 ASP B 451 REMARK 465 GLU B 452 REMARK 465 SER B 453 REMARK 465 GLY B 454 REMARK 465 ASN B 455 REMARK 465 SER B 456 REMARK 465 SER H 129 REMARK 465 SER H 130 REMARK 465 LYS H 131 REMARK 465 SER H 132 REMARK 465 THR H 133 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 B 65 38.15 70.44 REMARK 500 ARG B 125 43.59 39.37 REMARK 500 HIS B 150 54.22 -96.42 REMARK 500 PHE B 169 -69.13 -96.34 REMARK 500 ASN B 172 100.77 -50.72 REMARK 500 HIS B 206 30.66 -96.18 REMARK 500 ASN B 209 75.35 -68.76 REMARK 500 LEU B 210 144.08 -170.26 REMARK 500 TRP B 258 -71.75 -128.05 REMARK 500 ASN B 282 51.46 -114.00 REMARK 500 THR B 315 45.68 -143.56 REMARK 500 GLU B 326 -31.69 -130.39 REMARK 500 ALA B 333 125.60 -38.97 REMARK 500 ASN B 354 -9.29 70.78 REMARK 500 SER B 376 -55.59 -25.53 REMARK 500 ALA B 384 32.05 -81.86 REMARK 500 PHE B 426 -52.60 -146.32 REMARK 500 MET B 440 -129.97 52.33 REMARK 500 PHE H 29 -72.97 -38.25 REMARK 500 PRO H 52A 18.78 -62.28 REMARK 500 ALA H 53 58.46 -158.64 REMARK 500 ALA H 116 -179.96 -66.82 REMARK 500 PHE H 148 137.77 -174.19 REMARK 500 ASP L 28 108.33 -59.82 REMARK 500 SER L 30 -115.93 50.89 REMARK 500 ALA L 51 -44.92 82.10 REMARK 500 PRO L 59 156.73 -46.00 REMARK 500 ALA L 84 178.78 176.69 REMARK 500 PHE L 91 35.27 -158.82 REMARK 500 ASN L 138 79.97 53.48 REMARK 500 PRO L 141 -166.64 -77.57 REMARK 500 GLU L 213 -154.38 -104.03 REMARK 500 REMARK 500 REMARK: NULL