REMARK 2 REMARK 2 RESOLUTION. 2.25 ANGSTROMS. REMARK 3 REMARK 3 REFINEMENT. REMARK 3 PROGRAM : PHENIX (PHENIX.REFINE: 1.8_1069) 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) : 2.25 REMARK 3 RESOLUTION RANGE LOW (ANGSTROMS) : 40.37 REMARK 3 MIN(FOBS/SIGMA_FOBS) : 0.000 REMARK 3 COMPLETENESS FOR RANGE (%) : 99.7 REMARK 3 NUMBER OF REFLECTIONS : 43167 REMARK 3 REMARK 3 FIT TO DATA USED IN REFINEMENT. REMARK 3 R VALUE (WORKING + TEST SET) : 0.174 REMARK 3 R VALUE (WORKING SET) : 0.172 REMARK 3 FREE R VALUE : 0.203 REMARK 3 FREE R VALUE TEST SET SIZE (%) : 5.030 REMARK 3 FREE R VALUE TEST SET COUNT : 2173 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 40.3720 - 5.6661 0.98 2624 143 0.1741 0.2012 REMARK 3 2 5.6661 - 4.4992 0.99 2576 132 0.1415 0.1654 REMARK 3 3 4.4992 - 3.9310 1.00 2598 122 0.1423 0.1710 REMARK 3 4 3.9310 - 3.5719 0.99 2555 144 0.1649 0.1704 REMARK 3 5 3.5719 - 3.3160 1.00 2586 111 0.1806 0.2144 REMARK 3 6 3.3160 - 3.1205 1.00 2556 145 0.1819 0.2304 REMARK 3 7 3.1205 - 2.9643 1.00 2563 120 0.1795 0.2251 REMARK 3 8 2.9643 - 2.8353 1.00 2549 156 0.1817 0.2149 REMARK 3 9 2.8353 - 2.7262 1.00 2541 137 0.1792 0.2184 REMARK 3 10 2.7262 - 2.6321 1.00 2567 143 0.1883 0.2142 REMARK 3 11 2.6321 - 2.5498 1.00 2544 137 0.2003 0.2417 REMARK 3 12 2.5498 - 2.4770 1.00 2525 155 0.2018 0.2572 REMARK 3 13 2.4770 - 2.4118 1.00 2584 118 0.2081 0.2280 REMARK 3 14 2.4118 - 2.3529 1.00 2558 122 0.2100 0.2375 REMARK 3 15 2.3529 - 2.2995 1.00 2542 149 0.2163 0.2606 REMARK 3 16 2.2995 - 2.2510 1.00 2526 139 0.2360 0.2676 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 : 0.80 REMARK 3 K_SOL : NULL REMARK 3 B_SOL : NULL REMARK 3 REMARK 3 ERROR ESTIMATES. REMARK 3 COORDINATE ERROR (MAXIMUM-LIKELIHOOD BASED) : 0.200 REMARK 3 PHASE ERROR (DEGREES, MAXIMUM-LIKELIHOOD BASED) : 20.140 REMARK 3 REMARK 3 B VALUES. REMARK 3 FROM WILSON PLOT (A**2) : 42.03 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 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 : 0.008 3299 REMARK 3 ANGLE : 1.136 4508 REMARK 3 CHIRALITY : 0.075 518 REMARK 3 PLANARITY : 0.005 572 REMARK 3 DIHEDRAL : 13.442 1161 REMARK 3 REMARK 3 TLS DETAILS REMARK 3 NUMBER OF TLS GROUPS : 7 REMARK 3 TLS GROUP : 1 REMARK 3 SELECTION: chain 'L' and (resseq 5:91) REMARK 3 ORIGIN FOR THE GROUP (A): 0.1523 -60.1726 -8.1799 REMARK 3 T TENSOR REMARK 3 T11: 0.3739 T22: 0.9965 REMARK 3 T33: 0.5401 T12: -0.0463 REMARK 3 T13: 0.0232 T23: -0.0950 REMARK 3 L TENSOR REMARK 3 L11: 7.2190 L22: 3.6265 REMARK 3 L33: 4.7821 L12: -1.7727 REMARK 3 L13: 2.0239 L23: -1.1765 REMARK 3 S TENSOR REMARK 3 S11: -0.0828 S12: 1.0343 S13: -0.3626 REMARK 3 S21: -0.2616 S22: -0.1147 S23: 0.0134 REMARK 3 S31: -0.3871 S32: 0.0919 S33: 0.1687 REMARK 3 TLS GROUP : 2 REMARK 3 SELECTION: chain 'L' and (resseq 92:130) REMARK 3 ORIGIN FOR THE GROUP (A): -23.6934 -59.1450 -7.1496 REMARK 3 T TENSOR REMARK 3 T11: 0.3962 T22: 0.5455 REMARK 3 T33: 0.4678 T12: 0.1401 REMARK 3 T13: -0.0044 T23: -0.0709 REMARK 3 L TENSOR REMARK 3 L11: 4.1407 L22: 0.5920 REMARK 3 L33: 1.5968 L12: 0.9936 REMARK 3 L13: 2.0459 L23: 0.0403 REMARK 3 S TENSOR REMARK 3 S11: 0.0329 S12: 0.4048 S13: 0.1164 REMARK 3 S21: 0.0824 S22: 0.0719 S23: -0.1701 REMARK 3 S31: -0.1712 S32: 0.4125 S33: -0.0692 REMARK 3 TLS GROUP : 3 REMARK 3 SELECTION: chain 'L' and (resseq 131:211) REMARK 3 ORIGIN FOR THE GROUP (A): -38.4871 -56.5726 -12.8195 REMARK 3 T TENSOR REMARK 3 T11: 0.3473 T22: 0.4461 REMARK 3 T33: 0.3125 T12: 0.1541 REMARK 3 T13: -0.0322 T23: -0.0178 REMARK 3 L TENSOR REMARK 3 L11: 1.5241 L22: 3.0099 REMARK 3 L33: 5.3079 L12: 1.2117 REMARK 3 L13: 0.1918 L23: -0.1383 REMARK 3 S TENSOR REMARK 3 S11: 0.0034 S12: 0.0244 S13: 0.1983 REMARK 3 S21: -0.0358 S22: 0.0396 S23: -0.0076 REMARK 3 S31: -0.5621 S32: -0.0905 S33: -0.0160 REMARK 3 TLS GROUP : 4 REMARK 3 SELECTION: chain 'H' and (resseq 2:52) REMARK 3 ORIGIN FOR THE GROUP (A): -8.9097 -60.5973 13.1263 REMARK 3 T TENSOR REMARK 3 T11: 0.3838 T22: 0.9217 REMARK 3 T33: 0.5582 T12: -0.0186 REMARK 3 T13: 0.0033 T23: 0.0923 REMARK 3 L TENSOR REMARK 3 L11: 5.9559 L22: 3.8128 REMARK 3 L33: 2.9728 L12: -1.7470 REMARK 3 L13: -0.2036 L23: 0.0521 REMARK 3 S TENSOR REMARK 3 S11: -0.0795 S12: -0.7106 S13: -0.3935 REMARK 3 S21: 0.0814 S22: -0.2175 S23: -0.0759 REMARK 3 S31: -0.1529 S32: 0.5228 S33: 0.2813 REMARK 3 TLS GROUP : 5 REMARK 3 SELECTION: chain 'H' and (resseq 53:121) REMARK 3 ORIGIN FOR THE GROUP (A): -4.9833 -59.1028 14.1752 REMARK 3 T TENSOR REMARK 3 T11: 0.4281 T22: 1.0027 REMARK 3 T33: 0.5252 T12: -0.0526 REMARK 3 T13: -0.0321 T23: 0.0206 REMARK 3 L TENSOR REMARK 3 L11: 7.0407 L22: 1.1232 REMARK 3 L33: 0.6278 L12: -1.9199 REMARK 3 L13: -0.4631 L23: 0.3035 REMARK 3 S TENSOR REMARK 3 S11: -0.1234 S12: -1.2828 S13: -0.0037 REMARK 3 S21: 0.2804 S22: 0.1328 S23: -0.2061 REMARK 3 S31: -0.2876 S32: 0.5687 S33: 0.0139 REMARK 3 TLS GROUP : 6 REMARK 3 SELECTION: chain 'H' and (resseq 122:187) REMARK 3 ORIGIN FOR THE GROUP (A): -33.9979 -64.3803 -0.1957 REMARK 3 T TENSOR REMARK 3 T11: 0.3263 T22: 0.4610 REMARK 3 T33: 0.3622 T12: 0.1342 REMARK 3 T13: -0.0118 T23: 0.0036 REMARK 3 L TENSOR REMARK 3 L11: 3.3095 L22: 1.9628 REMARK 3 L33: 4.5590 L12: 1.2891 REMARK 3 L13: 2.0560 L23: 1.3812 REMARK 3 S TENSOR REMARK 3 S11: -0.0868 S12: 0.1944 S13: 0.2327 REMARK 3 S21: -0.1862 S22: -0.0837 S23: 0.1661 REMARK 3 S31: -0.1749 S32: 0.1691 S33: 0.1888 REMARK 3 TLS GROUP : 7 REMARK 3 SELECTION: chain 'H' and (resseq 188:223) REMARK 3 ORIGIN FOR THE GROUP (A): -35.8621 -73.1688 1.0375 REMARK 3 T TENSOR REMARK 3 T11: 0.3853 T22: 0.4425 REMARK 3 T33: 0.3935 T12: 0.1372 REMARK 3 T13: 0.0016 T23: -0.0223 REMARK 3 L TENSOR REMARK 3 L11: 3.8701 L22: 1.5924 REMARK 3 L33: 4.1827 L12: 0.4682 REMARK 3 L13: 1.7061 L23: 0.4203 REMARK 3 S TENSOR REMARK 3 S11: 0.1827 S12: -0.1115 S13: -0.4689 REMARK 3 S21: 0.2425 S22: -0.2228 S23: 0.2381 REMARK 3 S31: 0.7444 S32: -0.1383 S33: -0.0246 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 4GSD COMPLIES WITH FORMAT V. 3.30, 13-JUL-11 REMARK 100 REMARK 100 THIS ENTRY HAS BEEN PROCESSED BY RCSB ON 20-SEP-12. REMARK 100 THE RCSB ID CODE IS RCSB074575. REMARK 200 REMARK 200 EXPERIMENTAL DETAILS REMARK 200 EXPERIMENT TYPE : X-RAY DIFFRACTION REMARK 200 DATE OF DATA COLLECTION : 07-AUG-11 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 : APS REMARK 200 BEAMLINE : 21-ID-G REMARK 200 X-RAY GENERATOR MODEL : NULL REMARK 200 MONOCHROMATIC OR LAUE (M/L) : M REMARK 200 WAVELENGTH OR RANGE (A) : 0.97856 REMARK 200 MONOCHROMATOR : NULL REMARK 200 OPTICS : NULL REMARK 200 REMARK 200 DETECTOR TYPE : CCD REMARK 200 DETECTOR MANUFACTURER : MARMOSAIC 300 MM CCD REMARK 200 INTENSITY-INTEGRATION SOFTWARE : HKL-2000 REMARK 200 DATA SCALING SOFTWARE : HKL-2000 REMARK 200 REMARK 200 NUMBER OF UNIQUE REFLECTIONS : 43198 REMARK 200 RESOLUTION RANGE HIGH (A) : 2.250 REMARK 200 RESOLUTION RANGE LOW (A) : 50.000 REMARK 200 REJECTION CRITERIA (SIGMA(I)) : 0.000 REMARK 200 REMARK 200 OVERALL. REMARK 200 COMPLETENESS FOR RANGE (%) : 99.7 REMARK 200 DATA REDUNDANCY : 4.400 REMARK 200 R MERGE (I) : 0.06000 REMARK 200 R SYM (I) : NULL REMARK 200 FOR THE DATA SET : 18.3000 REMARK 200 REMARK 200 IN THE HIGHEST RESOLUTION SHELL. REMARK 200 HIGHEST RESOLUTION SHELL, RANGE HIGH (A) : 2.25 REMARK 200 HIGHEST RESOLUTION SHELL, RANGE LOW (A) : 2.33 REMARK 200 COMPLETENESS FOR SHELL (%) : 100.0 REMARK 200 DATA REDUNDANCY IN SHELL : 4.40 REMARK 200 R MERGE FOR SHELL (I) : 0.57100 REMARK 200 R SYM FOR SHELL (I) : NULL REMARK 200 FOR SHELL : 2.600 REMARK 200 REMARK 200 DIFFRACTION PROTOCOL: SINGLE WAVELENGTH REMARK 200 METHOD USED TO DETERMINE THE STRUCTURE: MOLECULAR REPLACEMENT REMARK 200 SOFTWARE USED: MOLREP REMARK 200 STARTING MODEL: 1FGW REMARK 200 REMARK 200 REMARK: NULL REMARK 280 REMARK 280 CRYSTAL REMARK 280 SOLVENT CONTENT, VS (%): 75.09 REMARK 280 MATTHEWS COEFFICIENT, VM (ANGSTROMS**3/DA): 4.94 REMARK 280 REMARK 280 CRYSTALLIZATION CONDITIONS: 24% PEG 1500 AND 20% GLYCEROL, 21 MG/ REMARK 280 ML PROTEIN, PH 7.5, VAPOR DIFFUSION, TEMPERATURE 298K REMARK 290 REMARK 290 CRYSTALLOGRAPHIC SYMMETRY REMARK 290 SYMMETRY OPERATORS FOR SPACE GROUP: P 61 REMARK 290 REMARK 290 SYMOP SYMMETRY REMARK 290 NNNMMM OPERATOR REMARK 290 1555 X,Y,Z REMARK 290 2555 -Y,X-Y,Z+1/3 REMARK 290 3555 -X+Y,-X,Z+2/3 REMARK 290 4555 -X,-Y,Z+1/2 REMARK 290 5555 Y,-X+Y,Z+5/6 REMARK 290 6555 X-Y,X,Z+1/6 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 -0.500000 -0.866025 0.000000 0.00000 REMARK 290 SMTRY2 2 0.866025 -0.500000 0.000000 0.00000 REMARK 290 SMTRY3 2 0.000000 0.000000 1.000000 23.50567 REMARK 290 SMTRY1 3 -0.500000 0.866025 0.000000 0.00000 REMARK 290 SMTRY2 3 -0.866025 -0.500000 0.000000 0.00000 REMARK 290 SMTRY3 3 0.000000 0.000000 1.000000 47.01133 REMARK 290 SMTRY1 4 -1.000000 0.000000 0.000000 0.00000 REMARK 290 SMTRY2 4 0.000000 -1.000000 0.000000 0.00000 REMARK 290 SMTRY3 4 0.000000 0.000000 1.000000 35.25850 REMARK 290 SMTRY1 5 0.500000 0.866025 0.000000 0.00000 REMARK 290 SMTRY2 5 -0.866025 0.500000 0.000000 0.00000 REMARK 290 SMTRY3 5 0.000000 0.000000 1.000000 58.76417 REMARK 290 SMTRY1 6 0.500000 -0.866025 0.000000 0.00000 REMARK 290 SMTRY2 6 0.866025 0.500000 0.000000 0.00000 REMARK 290 SMTRY3 6 0.000000 0.000000 1.000000 11.75283 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: 3240 ANGSTROM**2 REMARK 350 SURFACE AREA OF THE COMPLEX: 19590 ANGSTROM**2 REMARK 350 CHANGE IN SOLVENT FREE ENERGY: -25.0 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 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 SER L 2 REMARK 465 TYR L 3 REMARK 465 GLU L 4 REMARK 465 CYS L 212 REMARK 465 SER L 213 REMARK 465 GLU H 1 REMARK 465 LYS H 224 REMARK 465 SER H 225 REMARK 465 CYS H 226 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 L 382 O HOH H 384 1.86 REMARK 500 O HOH H 383 O HOH H 386 1.93 REMARK 500 O HOH L 377 O HOH H 386 1.95 REMARK 500 O HOH L 337 O HOH L 338 1.96 REMARK 500 OD1 ASP H 111 O HOH H 372 2.04 REMARK 500 O HOH L 368 O HOH L 371 2.05 REMARK 500 OG SER H 198 O HOH H 336 2.05 REMARK 500 NZ LYS H 127 O HOH H 342 2.10 REMARK 500 O HOH L 352 O HOH L 384 2.11 REMARK 500 OG SER L 65 O HOH L 351 2.16 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 L 51 -38.07 70.60 REMARK 500 ARG L 108 36.85 -86.09 REMARK 500 SER H 15 -3.28 73.45 REMARK 500 SER H 30 2.92 -69.51 REMARK 500 REMARK 500 REMARK: NULL