REMARK 1 REMARK 2 REMARK 2 RESOLUTION. 1.50 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE) 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) : 1.50 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 58.70 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 1.420 REMARK 3 COMPLETENESS FOR RANGE (%) : 98.2 REMARK 3 NUMBER OF REFLECTIONS : 67712 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.188 REMARK 3 R VALUE (WORKING SET) : 0.187 REMARK 3 FREE R VALUE : 0.212 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.080 REMARK 3 FREE R VALUE TEST SET COUNT : 3440 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 58.7395 - 4.3855 0.99 2648 155 0.1491 0.1660 REMARK 3 2 4.3855 - 3.4810 0.99 2629 133 0.1558 0.1824 REMARK 3 3 3.4810 - 3.0410 1.00 2649 133 0.1817 0.1858 REMARK 3 4 3.0410 - 2.7630 1.00 2634 135 0.1981 0.2089 REMARK 3 5 2.7630 - 2.5649 1.00 2592 142 0.1985 0.2073 REMARK 3 6 2.5649 - 2.4137 1.00 2632 133 0.1922 0.2227 REMARK 3 7 2.4137 - 2.2928 0.99 2580 175 0.1976 0.2033 REMARK 3 8 2.2928 - 2.1930 0.99 2591 137 0.1918 0.2150 REMARK 3 9 2.1930 - 2.1086 0.99 2591 121 0.1895 0.2517 REMARK 3 10 2.1086 - 2.0358 0.98 2585 138 0.1868 0.2386 REMARK 3 11 2.0358 - 1.9722 0.99 2564 139 0.1928 0.2387 REMARK 3 12 1.9722 - 1.9158 0.98 2588 140 0.1908 0.2165 REMARK 3 13 1.9158 - 1.8653 0.98 2556 142 0.1854 0.2053 REMARK 3 14 1.8653 - 1.8198 0.98 2568 137 0.1830 0.2318 REMARK 3 15 1.8198 - 1.7785 0.98 2547 139 0.1809 0.2120 REMARK 3 16 1.7785 - 1.7406 0.98 2575 140 0.1808 0.2170 REMARK 3 17 1.7406 - 1.7058 0.98 2563 135 0.1793 0.2151 REMARK 3 18 1.7058 - 1.6736 0.98 2580 114 0.1763 0.2264 REMARK 3 19 1.6736 - 1.6437 0.98 2580 112 0.1820 0.2086 REMARK 3 20 1.6437 - 1.6158 0.98 2570 159 0.1811 0.2235 REMARK 3 21 1.6158 - 1.5898 0.98 2512 129 0.1884 0.2326 REMARK 3 22 1.5898 - 1.5653 0.98 2603 139 0.1924 0.2205 REMARK 3 23 1.5653 - 1.5423 0.98 2555 121 0.1969 0.2393 REMARK 3 24 1.5423 - 1.5206 0.95 2511 142 0.2077 0.2552 REMARK 3 25 1.5206 - 1.5000 0.89 2269 150 0.2043 0.2406 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 : 0.32 REMARK 3 B_SOL : 28.95 REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.220 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : NULL REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : NULL REMARK 3 MEAN B VALUE (OVERALL, A**2) : 20.93 REMARK 3 OVERALL ANISOTROPIC B VALUE. REMARK 3 B11 (A**2) : -0.32000 REMARK 3 B22 (A**2) : 5.13500 REMARK 3 B33 (A**2) : -4.81500 REMARK 3 B12 (A**2) : 0.00000 REMARK 3 B13 (A**2) : 0.12300 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 : 0.005 3678 REMARK 3 ANGLE : 0.994 5061 REMARK 3 CHIRALITY : 0.063 583 REMARK 3 PLANARITY : 0.004 644 REMARK 3 DIHEDRAL : 15.639 1347 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 5 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: CHAIN H AND RESID 1-120 REMARK 3 ORIGIN FOR THE GROUP (A): 9.6508 67.6863 39.2134 REMARK 3 T TENSOR REMARK 3 T11: 0.1090 T22: 0.0851 REMARK 3 T33: 0.0955 T12: 0.0022 REMARK 3 T13: -0.0154 T23: -0.0022 REMARK 3 L TENSOR REMARK 3 L11: 0.3414 L22: 0.5489 REMARK 3 L33: 1.6948 L12: 0.2041 REMARK 3 L13: -0.0323 L23: 0.2375 REMARK 3 S TENSOR REMARK 3 S11: -0.0126 S12: 0.0316 S13: -0.0585 REMARK 3 S21: -0.0898 S22: -0.0041 S23: -0.0120 REMARK 3 S31: -0.0918 S32: -0.1238 S33: 0.0173 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: CHAIN H AND RESID 121-222 REMARK 3 ORIGIN FOR THE GROUP (A): 30.5678 89.6032 63.2003 REMARK 3 T TENSOR REMARK 3 T11: -0.0003 T22: 0.0372 REMARK 3 T33: 0.0835 T12: -0.0050 REMARK 3 T13: 0.0146 T23: -0.0423 REMARK 3 L TENSOR REMARK 3 L11: 0.9904 L22: 0.7857 REMARK 3 L33: 0.6869 L12: 0.4540 REMARK 3 L13: -0.2207 L23: 0.2093 REMARK 3 S TENSOR REMARK 3 S11: 0.1558 S12: -0.1891 S13: 0.0709 REMARK 3 S21: 0.0376 S22: -0.0874 S23: -0.0776 REMARK 3 S31: -0.0999 S32: -0.0218 S33: -0.0388 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: CHAIN L AND RESID 1-112 REMARK 3 ORIGIN FOR THE GROUP (A): 23.4456 79.0992 25.9316 REMARK 3 T TENSOR REMARK 3 T11: 0.1577 T22: 0.0529 REMARK 3 T33: 0.0827 T12: 0.0107 REMARK 3 T13: 0.0201 T23: 0.0008 REMARK 3 L TENSOR REMARK 3 L11: 0.7823 L22: 0.4545 REMARK 3 L33: 0.3265 L12: 0.2139 REMARK 3 L13: -0.0085 L23: 0.2300 REMARK 3 S TENSOR REMARK 3 S11: 0.0346 S12: 0.0562 S13: 0.0291 REMARK 3 S21: -0.0618 S22: -0.0064 S23: -0.1040 REMARK 3 S31: -0.1208 S32: 0.0449 S33: -0.0276 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: CHAIN L AND RESID 113-219 REMARK 3 ORIGIN FOR THE GROUP (A): 44.0921 84.5801 55.3393 REMARK 3 T TENSOR REMARK 3 T11: 0.0646 T22: 0.1044 REMARK 3 T33: 0.0953 T12: 0.0159 REMARK 3 T13: -0.0049 T23: 0.0086 REMARK 3 L TENSOR REMARK 3 L11: 0.5249 L22: 0.7970 REMARK 3 L33: 0.2159 L12: -0.3950 REMARK 3 L13: 0.3266 L23: -0.0691 REMARK 3 S TENSOR REMARK 3 S11: 0.0498 S12: -0.0416 S13: 0.0323 REMARK 3 S21: -0.0776 S22: -0.0216 S23: 0.0076 REMARK 3 S31: 0.0224 S32: 0.0025 S33: -0.0147 REMARK 3 TLS GROUP : 5 REMARK 3 SELECTION: CHAIN P AND RESID 2-7 REMARK 3 ORIGIN FOR THE GROUP (A): 12.3196 62.1874 22.4043 REMARK 3 T TENSOR REMARK 3 T11: 0.2157 T22: 0.1552 REMARK 3 T33: 0.1815 T12: -0.0266 REMARK 3 T13: 0.0180 T23: -0.0014 REMARK 3 L TENSOR REMARK 3 L11: 2.4131 L22: 3.7367 REMARK 3 L33: 2.3834 L12: -0.2046 REMARK 3 L13: -2.7759 L23: -0.3909 REMARK 3 S TENSOR REMARK 3 S11: -0.2969 S12: 0.2821 S13: -0.1565 REMARK 3 S21: 0.0682 S22: -0.0116 S23: -0.3326 REMARK 3 S31: 0.4386 S32: -0.2667 S33: 0.2738 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 3IFN COMPLIES WITH FORMAT V. 3.20, 01-DEC-08 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 17-AUG-09. REMARK 100 THE RCSB ID CODE IS RCSB054350. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 27-AUG-07 REMARK 200 TEMPERATURE (KELVIN) : 100 REMARK 200 PH : 7.5 REMARK 200 NUMBER OF CRYSTALS USED : 1 REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : Y REMARK 200 RADIATION SOURCE : ALS REMARK 200 BEAMLINE : 8.2.2 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 : NULL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : ADSC QUANTUM 315 REMARK 200 INTENSITY-INTEGRATION SOFTWARE : NULL REMARK 200 DATA SCALING SOFTWARE : NULL REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 67740 REMARK 200 RESOLUTION RANGE HIGH (A) : 1.500 REMARK 200 RESOLUTION RANGE LOW (A) : 58.695 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : NULL REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : NULL REMARK 200 DATA REDUNDANCY : NULL REMARK 200 R MERGE (I) : 0.04000 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) : NULL REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : NULL REMARK 200 COMPLETENESS FOR SHELL (%) : NULL 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: NULL REMARK 200 STARTING MODEL: NULL REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 41.21 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.09 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: PROTEIN: 5.3 MG/ML, 10 MM HEPES, PH REMARK 280 7.5, 75 MM NACL. PROTEIN:PEPTIDE MOLAR RATIO: 1:4.5. REMARK 280 RESERVOIR: 0.2M NACL, 25% PEG 4K, 0.1M HEPES PH 7.5, VAPOR REMARK 280 DIFFUSION, SITTING DROP, TEMPERATURE 295K 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 43.50500 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 SOFTWARE DETERMINED QUATERNARY STRUCTURE: TRIMERIC REMARK 350 SOFTWARE USED: PISA REMARK 350 TOTAL BURIED SURFACE AREA: 4710 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 19850 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -28.0 KCAL/MOL REMARK 350 APPLY THE FOLLOWING TO CHAINS: P, 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 H 134 REMARK 465 SER H 135 REMARK 465 ALA H 136 REMARK 465 ALA H 137 REMARK 465 GLN H 138 REMARK 465 THR H 139 REMARK 465 ASN H 140 REMARK 465 ASP P 1 REMARK 465 SER P 8 REMARK 465 GLY P 9 REMARK 465 TYR P 10 REMARK 465 GLU P 11 REMARK 465 VAL P 12 REMARK 465 HIS P 13 REMARK 465 HIS P 14 REMARK 465 GLN P 15 REMARK 465 LYS P 16 REMARK 465 LEU P 17 REMARK 465 VAL P 18 REMARK 465 PHE P 19 REMARK 465 PHE P 20 REMARK 465 ALA P 21 REMARK 465 GLU P 22 REMARK 465 ASP P 23 REMARK 465 VAL P 24 REMARK 465 GLY P 25 REMARK 465 SER P 26 REMARK 465 ASN P 27 REMARK 465 LYS P 28 REMARK 465 GLY P 29 REMARK 465 ALA P 30 REMARK 465 ILE P 31 REMARK 465 ILE P 32 REMARK 465 GLY P 33 REMARK 465 LEU P 34 REMARK 465 MET P 35 REMARK 465 VAL P 36 REMARK 465 GLY P 37 REMARK 465 GLY P 38 REMARK 465 VAL P 39 REMARK 465 VAL P 40 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 SER H 15 -16.77 91.89 REMARK 500 ASP H 57 -0.54 85.68 REMARK 500 LYS H 66 -143.37 52.21 REMARK 500 ASP H 180 -3.13 74.10 REMARK 500 VAL L 56 -50.68 75.33 REMARK 500 REMARK 500 REMARK: NULL REMARK 900 REMARK 900 RELATED ENTRIES REMARK 900 RELATED ID: 3IFL RELATED DB: PDB REMARK 900 X-RAY STRUCTURE OF AMYLOID BETA PEPTIDE:ANTIBODY (ABETA1-7: REMARK 900 12A11) COMPLEX REMARK 900 RELATED ID: 3IFO RELATED DB: PDB REMARK 900 X-RAY STRUCTURE OF AMYLOID BETA PEPTIDE:ANTIBODY (ABETA1-7: REMARK 900 10D5) COMPLEX REMARK 900 RELATED ID: 3IFP RELATED DB: PDB REMARK 900 X-RAY STRUCTURE OF AMYLOID BETA PEPTIDE:ANTIBODY (ABETA1-7: REMARK 900 12B4) COMPLEX