REMARK 1 REMARK 1 REFERENCE 1 REMARK 1 AUTH U.SCHULZE-GAHMEN,J.M.RINI,J.AREVALO,E.A.STURA, REMARK 1 AUTH 2 J.H.KENTEN,I.A.WILSON REMARK 1 TITL PRELIMINARY CRYSTALLOGRAPHIC DATA, PRIMARY REMARK 1 TITL 2 SEQUENCE, AND BINDING DATA FOR AN ANTI-PEPTIDE FAB REMARK 1 TITL 3 AND ITS COMPLEX WITH A SYNTHETIC PEPTIDE FROM REMARK 1 TITL 4 INFLUENZA VIRUS HEMAGGLUTININ REMARK 1 REF J.BIOL.CHEM. V. 263 17100 1988 REMARK 1 REFN ISSN 0021-9258 REMARK 2 REMARK 2 RESOLUTION. 3.10 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : X-PLOR REMARK 3 AUTHORS : BRUNGER REMARK 3 REMARK 3 DATA USED IN REFINEMENT. REMARK 3 RESOLUTION RANGE HIGH (ANGSTROMS) : 3.10 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 8.00 REMARK 3 DATA CUTOFF (SIGMA(F)) : 2.000 REMARK 3 DATA CUTOFF HIGH (ABS(F)) : NULL REMARK 3 DATA CUTOFF LOW (ABS(F)) : NULL REMARK 3 COMPLETENESS (WORKING+TEST) (%) : NULL REMARK 3 NUMBER OF REFLECTIONS : NULL REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 CROSS-VALIDATION METHOD : NULL REMARK 3 FREE R VALUE TEST SET SELECTION : NULL REMARK 3 R VALUE (WORKING SET) : 0.220 REMARK 3 FREE R VALUE : NULL REMARK 3 FREE R VALUE TEST SET SIZE (%) : NULL REMARK 3 FREE R VALUE TEST SET COUNT : NULL REMARK 3 ESTIMATED ERROR OF FREE R VALUE : NULL REMARK 3 REMARK 3 FIT IN THE HIGHEST RESOLUTION BIN. REMARK 3 TOTAL NUMBER OF BINS USED : NULL REMARK 3 BIN RESOLUTION RANGE HIGH (A) : NULL REMARK 3 BIN RESOLUTION RANGE LOW (A) : NULL REMARK 3 BIN COMPLETENESS (WORKING+TEST) (%) : NULL REMARK 3 REFLECTIONS IN BIN (WORKING SET) : NULL REMARK 3 BIN R VALUE (WORKING SET) : NULL REMARK 3 BIN FREE R VALUE : NULL REMARK 3 BIN FREE R VALUE TEST SET SIZE (%) : NULL REMARK 3 BIN FREE R VALUE TEST SET COUNT : NULL REMARK 3 ESTIMATED ERROR OF BIN FREE R VALUE : NULL REMARK 3 REMARK 3 NUMBER OF NON-HYDROGEN ATOMS USED IN REFINEMENT. REMARK 3 PROTEIN ATOMS : 3410 REMARK 3 NUCLEIC ACID ATOMS : 0 REMARK 3 HETEROGEN ATOMS : 0 REMARK 3 SOLVENT ATOMS : 22 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) : NULL REMARK 3 B22 (A**2) : NULL REMARK 3 B33 (A**2) : NULL REMARK 3 B12 (A**2) : NULL REMARK 3 B13 (A**2) : NULL REMARK 3 B23 (A**2) : NULL REMARK 3 REMARK 3 ESTIMATED COORDINATE ERROR. REMARK 3 ESD FROM LUZZATI PLOT (A) : NULL REMARK 3 ESD FROM SIGMAA (A) : NULL REMARK 3 LOW RESOLUTION CUTOFF (A) : NULL REMARK 3 REMARK 3 CROSS-VALIDATED ESTIMATED COORDINATE ERROR. REMARK 3 ESD FROM C-V LUZZATI PLOT (A) : NULL REMARK 3 ESD FROM C-V SIGMAA (A) : NULL REMARK 3 REMARK 3 RMS DEVIATIONS FROM IDEAL VALUES. REMARK 3 BOND LENGTHS (A) : 0.019 REMARK 3 BOND ANGLES (DEGREES) : 3.90 REMARK 3 DIHEDRAL ANGLES (DEGREES) : NULL REMARK 3 IMPROPER ANGLES (DEGREES) : NULL REMARK 3 REMARK 3 ISOTROPIC THERMAL MODEL : NULL REMARK 3 REMARK 3 ISOTROPIC THERMAL FACTOR RESTRAINTS. RMS SIGMA REMARK 3 MAIN-CHAIN BOND (A**2) : NULL ; NULL REMARK 3 MAIN-CHAIN ANGLE (A**2) : NULL ; NULL REMARK 3 SIDE-CHAIN BOND (A**2) : NULL ; NULL REMARK 3 SIDE-CHAIN ANGLE (A**2) : NULL ; NULL REMARK 3 REMARK 3 NCS MODEL : NULL REMARK 3 REMARK 3 NCS RESTRAINTS. RMS SIGMA/WEIGHT REMARK 3 GROUP 1 POSITIONAL (A) : NULL ; NULL REMARK 3 GROUP 1 B-FACTOR (A**2) : NULL ; NULL REMARK 3 REMARK 3 PARAMETER FILE 1 : NULL REMARK 3 TOPOLOGY FILE 1 : NULL REMARK 3 REMARK 3 OTHER REFINEMENT REMARKS: NULL REMARK 4 REMARK 4 1HIN COMPLIES WITH FORMAT V. 3.15, 01-DEC-08 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY BNL. 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 : NULL REMARK 200 NUMBER OF CRYSTALS USED : NULL REMARK 200 REMARK 200 SYNCHROTRON (Y/N) : NULL REMARK 200 RADIATION SOURCE : NULL REMARK 200 BEAMLINE : NULL REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : NULL REMARK 200 WAVELENGTH OR RANGE (A) : NULL REMARK 200 MONOCHROMATOR : NULL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : NULL REMARK 200 DETECTOR MANUFACTURER : NULL REMARK 200 INTENSITY-INTEGRATION SOFTWARE : NULL REMARK 200 DATA SCALING SOFTWARE : NULL REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : NULL REMARK 200 RESOLUTION RANGE HIGH (A) : NULL REMARK 200 RESOLUTION RANGE LOW (A) : NULL 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) : NULL 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: NULL REMARK 200 METHOD USED TO DETERMINE THE STRUCTURE: NULL REMARK 200 SOFTWARE USED: X-PLOR REMARK 200 STARTING MODEL: NULL REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 54.10 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 2.68 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 36.70000 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 APPLY THE FOLLOWING TO CHAINS: L, H, P 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 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: COVALENT BOND LENGTHS REMARK 500 REMARK 500 THE STEREOCHEMICAL PARAMETERS OF THE FOLLOWING RESIDUES REMARK 500 HAVE VALUES WHICH DEVIATE FROM EXPECTED VALUES BY MORE REMARK 500 THAN 6*RMSD (M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN REMARK 500 IDENTIFIER; SSEQ=SEQUENCE NUMBER; I=INSERTION CODE). REMARK 500 REMARK 500 STANDARD TABLE: REMARK 500 FORMAT: (10X,I3,1X,2(A3,1X,A1,I4,A1,1X,A4,3X),1X,F6.3) REMARK 500 REMARK 500 EXPECTED VALUES PROTEIN: ENGH AND HUBER, 1999 REMARK 500 EXPECTED VALUES NUCLEIC ACID: CLOWNEY ET AL 1996 REMARK 500 REMARK 500 M RES CSSEQI ATM1 RES CSSEQI ATM2 DEVIATION REMARK 500 HIS L 189 NE2 HIS L 189 CD2 -0.074 REMARK 500 GLU H 100 CD GLU H 100 OE2 -0.076 REMARK 500 HIS H 212 NE2 HIS H 212 CD2 -0.076 REMARK 500 REMARK 500 REMARK: NULL REMARK 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: COVALENT BOND ANGLES REMARK 500 REMARK 500 THE STEREOCHEMICAL PARAMETERS OF THE FOLLOWING RESIDUES REMARK 500 HAVE VALUES WHICH DEVIATE FROM EXPECTED VALUES BY MORE REMARK 500 THAN 6*RMSD (M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN REMARK 500 IDENTIFIER; SSEQ=SEQUENCE NUMBER; I=INSERTION CODE). REMARK 500 REMARK 500 STANDARD TABLE: REMARK 500 FORMAT: (10X,I3,1X,A3,1X,A1,I4,A1,3(1X,A4,2X),12X,F5.1) REMARK 500 REMARK 500 EXPECTED VALUES PROTEIN: ENGH AND HUBER, 1999 REMARK 500 EXPECTED VALUES NUCLEIC ACID: CLOWNEY ET AL 1996 REMARK 500 REMARK 500 M RES CSSEQI ATM1 ATM2 ATM3 REMARK 500 MET L 4 CG - SD - CE ANGL. DEV. = -9.7 DEGREES REMARK 500 CYS L 23 CA - CB - SG ANGL. DEV. = 7.1 DEGREES REMARK 500 SER L 25 N - CA - CB ANGL. DEV. = -9.8 DEGREES REMARK 500 TRP L 35 CD1 - CG - CD2 ANGL. DEV. = 5.3 DEGREES REMARK 500 LYS L 45 CA - CB - CG ANGL. DEV. = 17.6 DEGREES REMARK 500 TRP L 50 CD1 - CG - CD2 ANGL. DEV. = 7.1 DEGREES REMARK 500 TRP L 50 CG - CD1 - NE1 ANGL. DEV. = -7.1 DEGREES REMARK 500 TRP L 50 CE2 - CD2 - CG ANGL. DEV. = -6.3 DEGREES REMARK 500 SER L 52 N - CA - CB ANGL. DEV. = -9.9 DEGREES REMARK 500 THR L 69 N - CA - CB ANGL. DEV. = -13.4 DEGREES REMARK 500 LEU L 106 CA - CB - CG ANGL. DEV. = 17.2 DEGREES REMARK 500 CYS L 134 CA - CB - SG ANGL. DEV. = 8.5 DEGREES REMARK 500 ASN L 145 OD1 - CG - ND2 ANGL. DEV. = -13.9 DEGREES REMARK 500 ASN L 145 CB - CG - ND2 ANGL. DEV. = 16.1 DEGREES REMARK 500 TRP L 148 CD1 - CG - CD2 ANGL. DEV. = 6.7 DEGREES REMARK 500 TRP L 148 CE2 - CD2 - CG ANGL. DEV. = -6.3 DEGREES REMARK 500 TRP L 163 CD1 - CG - CD2 ANGL. DEV. = 6.1 DEGREES REMARK 500 TYR L 173 CB - CG - CD1 ANGL. DEV. = -3.8 DEGREES REMARK 500 MET L 175 CG - SD - CE ANGL. DEV. = -14.1 DEGREES REMARK 500 TYR L 192 CB - CG - CD1 ANGL. DEV. = -4.0 DEGREES REMARK 500 CYS L 194 CA - CB - SG ANGL. DEV. = 9.9 DEGREES REMARK 500 SER L 208 CA - CB - OG ANGL. DEV. = 17.0 DEGREES REMARK 500 ARG L 211 NE - CZ - NH1 ANGL. DEV. = 6.4 DEGREES REMARK 500 ARG L 211 NE - CZ - NH2 ANGL. DEV. = -3.7 DEGREES REMARK 500 TYR H 32 CB - CG - CD2 ANGL. DEV. = 4.1 DEGREES REMARK 500 TYR H 32 CB - CG - CD1 ANGL. DEV. = -5.9 DEGREES REMARK 500 MET H 34 CG - SD - CE ANGL. DEV. = -10.0 DEGREES REMARK 500 TRP H 36 CD1 - CG - CD2 ANGL. DEV. = 5.3 DEGREES REMARK 500 ARG H 44 NE - CZ - NH2 ANGL. DEV. = -3.5 DEGREES REMARK 500 TRP H 47 CD1 - CG - CD2 ANGL. DEV. = 6.0 DEGREES REMARK 500 TRP H 47 CE2 - CD2 - CG ANGL. DEV. = -5.3 DEGREES REMARK 500 TYR H 59 CB - CG - CD1 ANGL. DEV. = -5.5 DEGREES REMARK 500 ARG H 71 NE - CZ - NH2 ANGL. DEV. = -3.2 DEGREES REMARK 500 TYR H 91 CB - CG - CD1 ANGL. DEV. = -4.1 DEGREES REMARK 500 ARG H 94 NE - CZ - NH1 ANGL. DEV. = -3.8 DEGREES REMARK 500 ARG H 95 CD - NE - CZ ANGL. DEV. = -12.3 DEGREES REMARK 500 ARG H 95 NH1 - CZ - NH2 ANGL. DEV. = -7.4 DEGREES REMARK 500 ARG H 97 NE - CZ - NH1 ANGL. DEV. = 6.2 DEGREES REMARK 500 ARG H 97 NE - CZ - NH2 ANGL. DEV. = -4.0 DEGREES REMARK 500 TYR H 102 CB - CG - CD2 ANGL. DEV. = -5.9 DEGREES REMARK 500 TRP H 103 CD1 - CG - CD2 ANGL. DEV. = 5.5 DEGREES REMARK 500 TRP H 103 CE2 - CD2 - CG ANGL. DEV. = -4.9 DEGREES REMARK 500 TYR H 122 CB - CG - CD2 ANGL. DEV. = -5.1 DEGREES REMARK 500 VAL H 127 CA - C - N ANGL. DEV. = -13.6 DEGREES REMARK 500 CYS H 142 CA - CB - SG ANGL. DEV. = 11.2 DEGREES REMARK 500 TRP H 157 CD1 - CG - CD2 ANGL. DEV. = 7.8 DEGREES REMARK 500 TRP H 157 CG - CD1 - NE1 ANGL. DEV. = -6.3 DEGREES REMARK 500 TRP H 157 CE2 - CD2 - CG ANGL. DEV. = -6.1 DEGREES REMARK 500 LEU H 178 CA - CB - CG ANGL. DEV. = 18.3 DEGREES REMARK 500 GLN H 179 CA - CB - CG ANGL. DEV. = 15.4 DEGREES REMARK 500 REMARK 500 THIS ENTRY HAS 57 ANGLE DEVIATIONS. 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 THR L 14 -148.39 -88.10 REMARK 500 GLN L 29 45.62 95.46 REMARK 500 LEU L 47 -80.89 -98.40 REMARK 500 ALA L 51 -38.61 70.19 REMARK 500 ASP L 60 -6.52 -48.91 REMARK 500 PRO L 141 -172.93 -66.22 REMARK 500 ASP L 143 99.74 -66.97 REMARK 500 GLN L 156 -46.08 -132.80 REMARK 500 ARG L 188 30.81 -91.35 REMARK 500 ASN L 190 -71.20 -133.44 REMARK 500 SER L 201 94.95 -54.00 REMARK 500 PHE L 209 -141.51 -108.52 REMARK 500 ASN L 210 129.20 170.19 REMARK 500 SER H 30 -18.47 -43.48 REMARK 500 ALA H 49 148.06 -170.78 REMARK 500 TYR H 56 103.51 -49.54 REMARK 500 SER H 82B 79.21 47.48 REMARK 500 GLU H 100 85.49 79.62 REMARK 500 ASN H 100A 44.44 -166.59 REMARK 500 GLN H 105 53.72 -110.16 REMARK 500 CYS H 128 93.68 28.49 REMARK 500 THR H 133 -91.46 -82.10 REMARK 500 SER H 137 -169.56 -115.26 REMARK 500 PRO H 149 -99.12 -78.97 REMARK 500 ASN H 162 53.08 39.86 REMARK 500 GLN H 179 -126.37 -77.83 REMARK 500 SER H 180 71.16 -53.23 REMARK 500 ASP H 183 25.61 34.17 REMARK 500 SER H 195 -96.56 9.26 REMARK 500 SER H 196 -41.33 -22.64 REMARK 500 PRO H 227 -86.77 -79.23 REMARK 500 REMARK 500 REMARK: NULL REMARK 500 REMARK 500 GEOMETRY AND STEREOCHEMISTRY REMARK 500 SUBTOPIC: PLANAR GROUPS REMARK 500 REMARK 500 PLANAR GROUPS IN THE FOLLOWING RESIDUES HAVE A TOTAL REMARK 500 RMS DISTANCE OF ALL ATOMS FROM THE BEST-FIT PLANE REMARK 500 BY MORE THAN AN EXPECTED VALUE OF 6*RMSD, WITH AN REMARK 500 RMSD 0.02 ANGSTROMS, OR AT LEAST ONE ATOM HAS REMARK 500 AN RMSD GREATER THAN THIS VALUE REMARK 500 (M=MODEL NUMBER; RES=RESIDUE NAME; C=CHAIN IDENTIFIER; REMARK 500 SSEQ=SEQUENCE NUMBER; I=INSERTION CODE). REMARK 500 REMARK 500 M RES CSSEQI RMS TYPE REMARK 500 TYR L 32 0.07 SIDE_CHAIN REMARK 500 TYR L 86 0.08 SIDE_CHAIN REMARK 500 ARG H 95 0.29 SIDE_CHAIN REMARK 500 REMARK 500 REMARK: NULL