data_26511 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Anisotropic rotational diffusion of perdeuterated HIV protease from 15N NMR relaxation measurements at two magnetic fields ; _BMRB_accession_number 26511 _BMRB_flat_file_name bmr26511.str _Entry_type original _Submission_date 2015-02-17 _Accession_date 2015-02-17 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Tjandra Nico . . 2 Wingfield Paul . . 3 Stahl Stephen . . 4 Bax Ad . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count heteronucl_NOE 1 T1_relaxation 2 T2_relaxation 2 S2_parameters 6 stop_ loop_ _Data_type _Data_type_count "T1 relaxation values" 156 "T2 relaxation values" 156 "order parameters" 462 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2015-02-24 original author . stop_ _Original_release_date 2015-02-24 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Anisotropic rotational diffusion of perdeuterated HIV protease from 15N NMR relaxation measurements at two magnetic fields' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 8953218 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Tjandra Nico . . 2 Wingfield Paul . . 3 Stahl Stephen . . 4 Bax Ad . . stop_ _Journal_abbreviation 'J. Biomol. NMR' _Journal_volume 8 _Journal_issue 3 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 273 _Page_last 284 _Year 1996 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'HIV-1 protease' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'protease, 1' $protease 'protease, 2' $protease 'DMP323, 1' $entity_DMP 'DMP323, 2' $entity_DMP stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_protease _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common protease _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 97 _Mol_residue_sequence ; PQVTLWQRPLVTIKIGGQLK EALLDTGADDTVLEEMSLGR WKKMIGGIGGFIKVRQYDQI LIEIAGHKAIGTVLVGPTPV NIIGRNLLTQIGATLNF ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 PRO 2 2 GLN 3 3 VAL 4 4 THR 5 5 LEU 6 6 TRP 7 7 GLN 8 8 ARG 9 9 PRO 10 10 LEU 11 11 VAL 12 12 THR 13 13 ILE 14 14 LYS 15 15 ILE 16 16 GLY 17 17 GLY 18 18 GLN 19 19 LEU 20 20 LYS 21 21 GLU 22 22 ALA 23 23 LEU 24 24 LEU 25 25 ASP 26 26 THR 27 27 GLY 28 28 ALA 29 29 ASP 30 30 ASP 31 31 THR 32 32 VAL 33 33 LEU 34 34 GLU 35 35 GLU 36 36 MET 37 37 SER 38 38 LEU 39 40 GLY 40 41 ARG 41 42 TRP 42 43 LYS 43 45 LYS 44 46 MET 45 47 ILE 46 48 GLY 47 49 GLY 48 50 ILE 49 51 GLY 50 52 GLY 51 53 PHE 52 54 ILE 53 55 LYS 54 56 VAL 55 57 ARG 56 58 GLN 57 59 TYR 58 60 ASP 59 61 GLN 60 62 ILE 61 63 LEU 62 64 ILE 63 65 GLU 64 66 ILE 65 67 ALA 66 68 GLY 67 69 HIS 68 70 LYS 69 71 ALA 70 72 ILE 71 73 GLY 72 74 THR 73 75 VAL 74 76 LEU 75 77 VAL 76 78 GLY 77 79 PRO 78 80 THR 79 81 PRO 80 82 VAL 81 83 ASN 82 84 ILE 83 85 ILE 84 86 GLY 85 87 ARG 86 88 ASN 87 89 LEU 88 90 LEU 89 91 THR 90 92 GLN 91 93 ILE 92 94 GLY 93 95 ALA 94 96 THR 95 97 LEU 96 98 ASN 97 99 PHE stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-04-08 loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value PDB 1BVE "Hiv-1 Protease-Dmp323 Complex In Solution, Nmr, 28 Structures" 101.03 99 96.94 96.94 3.44e-55 PDB 1BVG "Hiv-1 Protease-Dmp323 Complex In Solution, Nmr Minimized Average Structure" 101.03 99 96.94 96.94 3.44e-55 PDB 1DMP "Structure Of Hiv-1 Protease Complex" 101.03 99 96.94 96.94 7.62e-55 PDB 1HVH "Nonpeptide Cyclic Cyanoguanidines As Hiv Protease Inhibitors" 102.06 99 96.97 96.97 3.34e-56 PDB 1HVR "Rational Design Of Potent, Bioavailable, Nonpeptide Cyclic Ureas As Hiv Protease Inhibitors" 102.06 99 96.97 96.97 7.17e-56 PDB 1HWR "Molecular Recognition Of Cyclic Urea Hiv Protease Inhibitors" 101.03 99 96.94 96.94 3.44e-55 PDB 1QBR "Hiv-1 Protease Inhibitors Wiih Low Nanomolar Potency" 102.06 99 96.97 96.97 3.34e-56 PDB 1QBS "Hiv-1 Protease Inhibitors Wiih Low Nanomolar Potency" 102.06 99 96.97 96.97 7.17e-56 PDB 1QBT "Hiv-1 Protease Inhibitors Wiih Low Nanomolar Potency" 102.06 99 96.97 96.97 3.34e-56 PDB 1QBU "Hiv-1 Protease Inhibitors Wiih Low Nanomolar Potency" 102.06 99 96.97 96.97 3.34e-56 PDB 3MIM "X-Ray Snapshot Of Hiv-1 Protease In Action: Observation Of Tetrahedral Intermediate And Its Sihb With Catalytic Aspartate" 102.06 104 96.97 96.97 3.60e-56 stop_ save_ ############# # Ligands # ############# save_DMP _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common [4-R-(-4-ALPHA,5-ALPHA,6-BETA,7-BETA)]-HEXAHYDRO-5,6-BIS(HYDROXY)-[1,3-BIS([4-HYDROXYMETHYL-PHENYL]METHYL)-4,7-BIS(PHENYLMETHYL)]-2H-1,3-DIAZEPINONE _BMRB_code DMP _PDB_code DMP _Molecular_mass 566.687 _Mol_charge 0 _Mol_paramagnetic . _Mol_aromatic yes _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C1 C1 C . 0 . ? C3 C3 C . 0 . ? C4 C4 C . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? C20 C20 C . 0 . ? C21 C21 C . 0 . ? C22 C22 C . 0 . ? C23 C23 C . 0 . ? C24 C24 C . 0 . ? C25 C25 C . 0 . ? C26 C26 C . 0 . ? C27 C27 C . 0 . ? C30 C30 C . 0 . ? C31 C31 C . 0 . ? C32 C32 C . 0 . ? C33 C33 C . 0 . ? C34 C34 C . 0 . ? C35 C35 C . 0 . ? C36 C36 C . 0 . ? C60 C60 C . 0 . ? C61 C61 C . 0 . ? C62 C62 C . 0 . ? C63 C63 C . 0 . ? C64 C64 C . 0 . ? C65 C65 C . 0 . ? C66 C66 C . 0 . ? C70 C70 C . 0 . ? C71 C71 C . 0 . ? C72 C72 C . 0 . ? C73 C73 C . 0 . ? C74 C74 C . 0 . ? C75 C75 C . 0 . ? C76 C76 C . 0 . ? C77 C77 C . 0 . ? N2 N2 N . 0 . ? N7 N7 N . 0 . ? O1 O1 O . 0 . ? O4 O4 O . 0 . ? O5 O5 O . 0 . ? O27 O27 O . 0 . ? O77 O77 O . 0 . ? H3 H3 H . 0 . ? H4 H4 H . 0 . ? H5 H5 H . 0 . ? H6 H6 H . 0 . ? H201 H201 H . 0 . ? H202 H202 H . 0 . ? H22 H22 H . 0 . ? H23 H23 H . 0 . ? H25 H25 H . 0 . ? H26 H26 H . 0 . ? H271 H271 H . 0 . ? H272 H272 H . 0 . ? H301 H301 H . 0 . ? H302 H302 H . 0 . ? H32 H32 H . 0 . ? H33 H33 H . 0 . ? H34 H34 H . 0 . ? H35 H35 H . 0 . ? H36 H36 H . 0 . ? H601 H601 H . 0 . ? H602 H602 H . 0 . ? H62 H62 H . 0 . ? H63 H63 H . 0 . ? H64 H64 H . 0 . ? H65 H65 H . 0 . ? H66 H66 H . 0 . ? H701 H701 H . 0 . ? H702 H702 H . 0 . ? H72 H72 H . 0 . ? H73 H73 H . 0 . ? H75 H75 H . 0 . ? H76 H76 H . 0 . ? H771 H771 H . 0 . ? H772 H772 H . 0 . ? HO4 HO4 H . 0 . ? HO5 HO5 H . 0 . ? HO27 HO27 H . 0 . ? HO77 HO77 H . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING C1 N2 ? ? SING C1 N7 ? ? DOUB C1 O1 ? ? SING C3 C4 ? ? SING C3 C30 ? ? SING C3 N2 ? ? SING C3 H3 ? ? SING C4 C5 ? ? SING C4 O4 ? ? SING C4 H4 ? ? SING C5 C6 ? ? SING C5 O5 ? ? SING C5 H5 ? ? SING C6 C60 ? ? SING C6 N7 ? ? SING C6 H6 ? ? SING C20 C21 ? ? SING C20 N2 ? ? SING C20 H201 ? ? SING C20 H202 ? ? DOUB C21 C22 ? ? SING C21 C26 ? ? SING C22 C23 ? ? SING C22 H22 ? ? DOUB C23 C24 ? ? SING C23 H23 ? ? SING C24 C25 ? ? SING C24 C27 ? ? DOUB C25 C26 ? ? SING C25 H25 ? ? SING C26 H26 ? ? SING C27 O27 ? ? SING C27 H271 ? ? SING C27 H272 ? ? SING C30 C31 ? ? SING C30 H301 ? ? SING C30 H302 ? ? DOUB C31 C32 ? ? SING C31 C36 ? ? SING C32 C33 ? ? SING C32 H32 ? ? DOUB C33 C34 ? ? SING C33 H33 ? ? SING C34 C35 ? ? SING C34 H34 ? ? DOUB C35 C36 ? ? SING C35 H35 ? ? SING C36 H36 ? ? SING C60 C61 ? ? SING C60 H601 ? ? SING C60 H602 ? ? DOUB C61 C62 ? ? SING C61 C66 ? ? SING C62 C63 ? ? SING C62 H62 ? ? DOUB C63 C64 ? ? SING C63 H63 ? ? SING C64 C65 ? ? SING C64 H64 ? ? DOUB C65 C66 ? ? SING C65 H65 ? ? SING C66 H66 ? ? SING C70 C71 ? ? SING C70 N7 ? ? SING C70 H701 ? ? SING C70 H702 ? ? DOUB C71 C72 ? ? SING C71 C76 ? ? SING C72 C73 ? ? SING C72 H72 ? ? DOUB C73 C74 ? ? SING C73 H73 ? ? SING C74 C75 ? ? SING C74 C77 ? ? DOUB C75 C76 ? ? SING C75 H75 ? ? SING C76 H76 ? ? SING C77 O77 ? ? SING C77 H771 ? ? SING C77 H772 ? ? SING O4 HO4 ? ? SING O5 HO5 ? ? SING O27 HO27 ? ? SING O77 HO77 ? ? stop_ _Mol_thiol_state . _Sequence_homology_query_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $protease HIV-1 11676 . . . . $entity_DMP . . . . . . stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $protease 'recombinant technology' . . . . . $entity_DMP 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $protease 1.5 mM '[U-100% 15N; >85% 2H]' $entity_DMP 1.5 mM 'natural abundance' 'sodium acetate' 50 mM 'natural abundance' H2O 95 % 'natural abundance' D2O 5 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task collection 'data analysis' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AMX _Field_strength 360 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AMX _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_15N-{1H}_NOE_3 _Saveframe_category NMR_applied_experiment _Experiment_name '15N-{1H} NOE' _Sample_label $sample_1 save_ save_15N-{1H}_NOE_4 _Saveframe_category NMR_applied_experiment _Experiment_name '15N-{1H} NOE' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 300 . K pH 5.2 . pH pressure 1 . atm stop_ save_ save_heteronuclear_T1_list_1 _Saveframe_category T1_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 360 _T1_coherence_type S(+,-) _T1_value_units s _Mol_system_component_name 'protease, 1' _Text_data_format . _Text_data . loop_ _T1_ID _Residue_seq_code _Residue_label _Atom_name _T1_value _T1_value_error 1 2 GLN N 0.511 . 2 3 VAL N 0.483 . 3 7 GLN N 0.470 . 4 8 ARG N 0.447 . 5 10 LEU N 0.476 . 6 11 VAL N 0.442 . 7 12 THR N 0.460 . 8 13 ILE N 0.428 . 9 14 LYS N 0.421 . 10 15 ILE N 0.412 . 11 16 GLY N 0.436 . 12 17 GLY N 0.444 . 13 18 GLN N 0.442 . 14 19 LEU N 0.447 . 15 20 LYS N 0.448 . 16 21 GLU N 0.474 . 17 22 ALA N 0.424 . 18 24 LEU N 0.424 . 19 25 ASP N 0.486 . 20 26 THR N 0.426 . 21 27 GLY N 0.396 . 22 28 ALA N 0.422 . 23 29 ASP N 0.455 . 24 30 ASP N 0.516 . 25 32 VAL N 0.439 . 26 33 LEU N 0.433 . 27 34 GLU N 0.416 . 28 35 GLU N 0.506 . 29 36 MET N 0.435 . 30 37 SER N 0.470 . 31 38 LEU N 0.539 . 32 39 GLY N 0.593 . 33 40 ARG N 0.511 . 34 41 TRP N 0.524 . 35 42 LYS N 0.454 . 36 43 LYS N 0.445 . 37 44 MET N 0.450 . 38 46 GLY N 0.451 . 39 47 GLY N 0.456 . 40 48 ILE N 0.456 . 41 50 GLY N 0.460 . 42 51 PHE N 0.496 . 43 53 LYS N 0.470 . 44 54 VAL N 0.423 . 45 55 ARG N 0.425 . 46 56 GLN N 0.433 . 47 57 TYR N 0.473 . 48 58 ASP N 0.497 . 49 59 GLN N 0.480 . 50 61 LEU N 0.471 . 51 62 ILE N 0.420 . 52 63 GLU N 0.428 . 53 64 ILE N 0.445 . 54 65 ALA N 0.423 . 55 66 GLY N 0.444 . 56 68 LYS N 0.488 . 57 69 ALA N 0.455 . 58 72 THR N 0.461 . 59 73 VAL N 0.461 . 60 74 LEU N 0.450 . 61 75 VAL N 0.452 . 62 76 GLY N 0.412 . 63 80 VAL N 0.417 . 64 81 ASN N 0.440 . 65 82 ILE N 0.451 . 66 83 ILE N 0.457 . 67 84 GLY N 0.482 . 68 85 ARG N 0.431 . 69 86 ASN N 0.419 . 70 87 LEU N 0.446 . 71 88 LEU N 0.430 . 72 89 THR N 0.427 . 73 90 GLN N 0.467 . 74 91 ILE N 0.465 . 75 92 GLY N 0.447 . 76 93 ALA N 0.459 . 77 94 THR N 0.423 . 78 97 PHE N 0.429 . stop_ save_ save_heteronuclear_T1_list_2 _Saveframe_category T1_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _T1_coherence_type S(+,-) _T1_value_units s _Mol_system_component_name 'protease, 1' _Text_data_format . _Text_data . loop_ _T1_ID _Residue_seq_code _Residue_label _Atom_name _T1_value _T1_value_error 1 2 GLN N 0.962 . 2 3 VAL N 0.846 . 3 7 GLN N 0.905 . 4 8 ARG N 0.888 . 5 10 LEU N 1.010 . 6 11 VAL N 0.879 . 7 12 THR N 0.911 . 8 13 ILE N 0.859 . 9 14 LYS N 0.878 . 10 15 ILE N 0.821 . 11 16 GLY N 0.845 . 12 17 GLY N 0.864 . 13 18 GLN N 0.873 . 14 19 LEU N 0.893 . 15 20 LYS N 0.901 . 16 21 GLU N 0.955 . 17 22 ALA N 0.845 . 18 24 LEU N 0.857 . 19 25 ASP N 1.030 . 20 26 THR N 0.923 . 21 27 GLY N 0.785 . 22 28 ALA N 0.824 . 23 29 ASP N 0.915 . 24 30 ASP N 1.030 . 25 32 VAL N 0.892 . 26 33 LEU N 0.890 . 27 34 GLU N 0.840 . 28 35 GLU N 1.040 . 29 36 MET N 0.886 . 30 37 SER N 0.937 . 31 38 LEU N 1.030 . 32 39 GLY N 1.090 . 33 40 ARG N 0.983 . 34 41 TRP N 0.996 . 35 42 LYS N 0.888 . 36 43 LYS N 0.887 . 37 44 MET N 0.895 . 38 46 GLY N 0.918 . 39 47 GLY N 0.938 . 40 48 ILE N 0.950 . 41 50 GLY N 0.898 . 42 51 PHE N 0.976 . 43 53 LYS N 0.961 . 44 54 VAL N 0.864 . 45 55 ARG N 0.901 . 46 56 GLN N 0.871 . 47 57 TYR N 0.961 . 48 58 ASP N 1.030 . 49 59 GLN N 0.991 . 50 61 LEU N 0.963 . 51 62 ILE N 0.821 . 52 63 GLU N 0.866 . 53 64 ILE N 0.936 . 54 65 ALA N 0.842 . 55 66 GLY N 0.908 . 56 68 LYS N 0.960 . 57 69 ALA N 0.897 . 58 72 THR N 0.932 . 59 73 VAL N 0.966 . 60 74 LEU N 0.956 . 61 75 VAL N 0.948 . 62 76 GLY N 0.847 . 63 80 VAL N 0.835 . 64 81 ASN N 0.867 . 65 82 ILE N 0.886 . 66 83 ILE N 0.905 . 67 84 GLY N 1.010 . 68 85 ARG N 0.898 . 69 86 ASN N 0.865 . 70 87 LEU N 0.950 . 71 88 LEU N 0.888 . 72 89 THR N 0.800 . 73 90 GLN N 0.850 . 74 91 ILE N 0.903 . 75 92 GLY N 0.873 . 76 93 ALA N 0.917 . 77 94 THR N 0.867 . 78 97 PHE N 0.890 . stop_ save_ save_heteronuclear_T2_list_1 _Saveframe_category T2_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 360 _T2_coherence_type S(+,-) _T2_value_units s _Mol_system_component_name 'protease, 1' _Text_data_format . _Text_data . loop_ _T2_ID _Residue_seq_code _Residue_label _Atom_name _T2_value _T2_value_error _Rex_value _Rex_error 1 2 GLN N 0.1080 . . . 2 3 VAL N 0.0924 . . . 3 7 GLN N 0.0925 . . . 4 8 ARG N 0.0985 . . . 5 10 LEU N 0.0884 . . . 6 11 VAL N 0.0908 . . . 7 12 THR N 0.0907 . . . 8 13 ILE N 0.0878 . . . 9 14 LYS N 0.0893 . . . 10 15 ILE N 0.0852 . . . 11 16 GLY N 0.0908 . . . 12 17 GLY N 0.0963 . . . 13 18 GLN N 0.0955 . . . 14 19 LEU N 0.0895 . . . 15 20 LYS N 0.0886 . . . 16 21 GLU N 0.0978 . . . 17 22 ALA N 0.0879 . . . 18 24 LEU N 0.0906 . . . 19 25 ASP N 0.0746 . . . 20 26 THR N 0.0759 . . . 21 27 GLY N 0.0830 . . . 22 28 ALA N 0.0864 . . . 23 29 ASP N 0.0920 . . . 24 30 ASP N 0.0915 . . . 25 32 VAL N 0.0816 . . . 26 33 LEU N 0.0827 . . . 27 34 GLU N 0.0899 . . . 28 35 GLU N 0.0847 . . . 29 36 MET N 0.0935 . . . 30 37 SER N 0.1020 . . . 31 38 LEU N 0.1230 . . . 32 39 GLY N 0.1190 . . . 33 40 ARG N 0.1050 . . . 34 41 TRP N 0.1010 . . . 35 42 LYS N 0.0846 . . . 36 43 LYS N 0.0964 . . . 37 44 MET N 0.0974 . . . 38 46 GLY N 0.0965 . . . 39 47 GLY N 0.0914 . . . 40 48 ILE N 0.0814 . . . 41 50 GLY N 0.0959 . . . 42 51 PHE N 0.0951 . . . 43 53 LYS N 0.1010 . . . 44 54 VAL N 0.0902 . . . 45 55 ARG N 0.0886 . . . 46 56 GLN N 0.0863 . . . 47 57 TYR N 0.0761 . . . 48 58 ASP N 0.0869 . . . 49 59 GLN N 0.0838 . . . 50 61 LEU N 0.0824 . . . 51 62 ILE N 0.0876 . . . 52 63 GLU N 0.0856 . . . 53 64 ILE N 0.0890 . . . 54 65 ALA N 0.0928 . . . 55 66 GLY N 0.0998 . . . 56 68 LYS N 0.0938 . . . 57 69 ALA N 0.0943 . . . 58 72 THR N 0.0870 . . . 59 73 VAL N 0.0787 . . . 60 74 LEU N 0.0782 . . . 61 75 VAL N 0.0860 . . . 62 76 GLY N 0.0847 . . . 63 80 VAL N 0.0877 . . . 64 81 ASN N 0.0941 . . . 65 82 ILE N 0.0814 . . . 66 83 ILE N 0.0795 . . . 67 84 GLY N 0.0781 . . . 68 85 ARG N 0.0793 . . . 69 86 ASN N 0.0841 . . . 70 87 LEU N 0.0840 . . . 71 88 LEU N 0.0845 . . . 72 89 THR N 0.0809 . . . 73 90 GLN N 0.0953 . . . 74 91 ILE N 0.0851 . . . 75 92 GLY N 0.0897 . . . 76 93 ALA N 0.0799 . . . 77 94 THR N 0.0892 . . . 78 97 PHE N 0.0885 . . . stop_ save_ save_heteronuclear_T2_list_2 _Saveframe_category T2_relaxation _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _T2_coherence_type S(+,-) _T2_value_units s _Mol_system_component_name 'protease, 1' _Text_data_format . _Text_data . loop_ _T2_ID _Residue_seq_code _Residue_label _Atom_name _T2_value _T2_value_error _Rex_value _Rex_error 1 2 GLN N 0.0971 . . . 2 3 VAL N 0.0759 . . . 3 7 GLN N 0.0804 . . . 4 8 ARG N 0.0793 . . . 5 10 LEU N 0.0789 . . . 6 11 VAL N 0.0765 . . . 7 12 THR N 0.0806 . . . 8 13 ILE N 0.0775 . . . 9 14 LYS N 0.0768 . . . 10 15 ILE N 0.0777 . . . 11 16 GLY N 0.0802 . . . 12 17 GLY N 0.0818 . . . 13 18 GLN N 0.0815 . . . 14 19 LEU N 0.0801 . . . 15 20 LYS N 0.0808 . . . 16 21 GLU N 0.0837 . . . 17 22 ALA N 0.0784 . . . 18 24 LEU N 0.0766 . . . 19 25 ASP N 0.0628 . . . 20 26 THR N 0.0751 . . . 21 27 GLY N 0.0726 . . . 22 28 ALA N 0.0751 . . . 23 29 ASP N 0.0779 . . . 24 30 ASP N 0.0823 . . . 25 32 VAL N 0.0828 . . . 26 33 LEU N 0.0752 . . . 27 34 GLU N 0.0771 . . . 28 35 GLU N 0.0756 . . . 29 36 MET N 0.0810 . . . 30 37 SER N 0.0872 . . . 31 38 LEU N 0.1050 . . . 32 39 GLY N 0.1120 . . . 33 40 ARG N 0.0953 . . . 34 41 TRP N 0.0847 . . . 35 42 LYS N 0.0746 . . . 36 43 LYS N 0.0832 . . . 37 44 MET N 0.0857 . . . 38 46 GLY N 0.0815 . . . 39 47 GLY N 0.0772 . . . 40 48 ILE N 0.0573 . . . 41 50 GLY N 0.0802 . . . 42 51 PHE N 0.0848 . . . 43 53 LYS N 0.0869 . . . 44 54 VAL N 0.0784 . . . 45 55 ARG N 0.0776 . . . 46 56 GLN N 0.0769 . . . 47 57 TYR N 0.0678 . . . 48 58 ASP N 0.0771 . . . 49 59 GLN N 0.0750 . . . 50 61 LEU N 0.0716 . . . 51 62 ILE N 0.0775 . . . 52 63 GLU N 0.0796 . . . 53 64 ILE N 0.0804 . . . 54 65 ALA N 0.0803 . . . 55 66 GLY N 0.0817 . . . 56 68 LYS N 0.0862 . . . 57 69 ALA N 0.0867 . . . 58 72 THR N 0.0766 . . . 59 73 VAL N 0.0659 . . . 60 74 LEU N 0.0689 . . . 61 75 VAL N 0.0779 . . . 62 76 GLY N 0.0739 . . . 63 80 VAL N 0.0768 . . . 64 81 ASN N 0.0820 . . . 65 82 ILE N 0.0747 . . . 66 83 ILE N 0.0738 . . . 67 84 GLY N 0.0672 . . . 68 85 ARG N 0.0678 . . . 69 86 ASN N 0.0716 . . . 70 87 LEU N 0.0702 . . . 71 88 LEU N 0.0713 . . . 72 89 THR N 0.0743 . . . 73 90 GLN N 0.0774 . . . 74 91 ILE N 0.0767 . . . 75 92 GLY N 0.0771 . . . 76 93 ALA N 0.0698 . . . 77 94 THR N 0.0743 . . . 78 97 PHE N 0.0781 . . . stop_ save_ save_heteronuclear_noe_list_1 _Saveframe_category heteronuclear_NOE _Details . loop_ _Experiment_label '15N-{1H} NOE' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 600 _Mol_system_component_name 'protease, 1' _Atom_one_atom_name N _Atom_two_atom_name H _Heteronuclear_NOE_value_type 'peak height' _NOE_reference_value 1 _NOE_reference_description . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 2 GLN 0.600 . 3 VAL 0.645 . 7 GLN 0.696 . 8 ARG 0.776 . 10 LEU 0.766 . 11 VAL 0.741 . 12 THR 0.716 . 13 ILE 0.740 . 14 LYS 0.764 . 15 ILE 0.800 . 16 GLY 0.752 . 17 GLY 0.734 . 18 GLN 0.689 . 19 LEU 0.787 . 20 LYS 0.761 . 21 GLU 0.680 . 22 ALA 0.773 . 24 LEU 0.801 . 25 ASP 0.800 . 26 THR 0.813 . 27 GLY 0.799 . 28 ALA 0.792 . 29 ASP 0.753 . 30 ASP 0.670 . 32 VAL 0.806 . 33 LEU 0.805 . 34 GLU 0.783 . 35 GLU 0.716 . 36 MET 0.712 . 37 SER 0.687 . 38 LEU 0.571 . 39 GLY 0.310 . 40 ARG 0.569 . 41 TRP 0.603 . 42 LYS 0.754 . 43 LYS 0.732 . 44 MET 0.682 . 46 GLY 0.747 . 47 GLY 0.800 . 48 ILE 0.822 . 50 GLY 0.747 . 51 PHE 0.746 . 53 LYS 0.650 . 54 VAL 0.725 . 55 ARG 0.788 . 56 GLN 0.950 . 57 TYR 0.780 . 58 ASP 0.714 . 59 GLN 0.731 . 61 LEU 0.778 . 62 ILE 0.759 . 63 GLU 0.765 . 64 ILE 0.762 . 65 ALA 0.715 . 66 GLY 0.733 . 68 LYS 0.675 . 69 ALA 0.673 . 72 THR 0.743 . 73 VAL 0.798 . 74 LEU 0.813 . 75 VAL 0.790 . 76 GLY 0.804 . 80 VAL 0.755 . 81 ASN 0.769 . 82 ILE 0.783 . 83 ILE 0.785 . 84 GLY 0.789 . 85 ARG 0.825 . 86 ASN 0.802 . 87 LEU 0.747 . 88 LEU 0.860 . 89 THR 0.869 . 90 GLN 0.757 . 91 ILE 0.738 . 92 GLY 0.809 . 93 ALA 0.788 . 97 PHE 0.765 . stop_ save_ save_order_parameter_list_1 _Saveframe_category S2_parameters _Details ; Order parameter (S2) and Tau e values derived from the 360 MHz relaxation data, and relaxation values predicted for these S2 and Tau e values, using the constrained asymmetric diffusion tensor with Tau c equal to 10.97 ns, and the simple Lipari-Szabo description for internal motion. Residues D25, E35, I50, Y59, V75, L76, and G86 yield a poor fit due to the presence of exchange broadening; residues Q2, V3, L38, G40, R41 and W42 require fitting with the extended Lipari-Szabo model because of intermediate time scale internal motions (Clore et al., 1990b). ; _Sample_conditions_label $sample_conditions_1 _Mol_system_component_name 'protease, 1' _Tau_e_value_units ps _Tau_s_value_units . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Atom_name _Model_fit _S2_value _S2_value_fit_error _Tau_e_value _Tau_e_value_fit_error _S2f_value _S2f_value_fit_error _S2s_value _S2s_value_fit_error _Tau_s_value _Tau_s_value_fit_error _S2H_value _S2H_value_fit_error _S2N_value _S2N_value_fit_error 2 GLN N . 0.68 . 28 . . . . . . . . . . . 3 VAL N . 0.73 . 22 . . . . . . . . . . . 7 GLN N . 0.76 . 23 . . . . . . . . . . . 8 ARG N . 0.80 . 12 . . . . . . . . . . . 10 LEU N . 0.77 . 11 . . . . . . . . . . . 11 VAL N . 0.78 . 18 . . . . . . . . . . . 12 THR N . 0.79 . 23 . . . . . . . . . . . 13 ILE N . 0.81 . 22 . . . . . . . . . . . 14 LYS N . 0.81 . 16 . . . . . . . . . . . 15 ILE N . 0.83 . 8 . . . . . . . . . . . 16 GLY N . 0.80 . 18 . . . . . . . . . . . 17 GLY N . 0.83 . 23 . . . . . . . . . . . 18 GLN N . 0.78 . 29 . . . . . . . . . . . 19 LEU N . 0.83 . 9 . . . . . . . . . . . 20 LYS N . 0.78 . 13 . . . . . . . . . . . 21 GLU N . 0.76 . 26 . . . . . . . . . . . 22 ALA N . 0.82 . 15 . . . . . . . . . . . 24 LEU N . 0.82 . 8 . . . . . . . . . . . 25 ASP N . 0.80 . 6 . . . . . . . . . . . 26 THR N . 0.86 . 5 . . . . . . . . . . . 27 GLY N . 0.92 . 19 . . . . . . . . . . . 28 ALA N . 0.84 . 11 . . . . . . . . . . . 29 ASP N . 0.80 . 17 . . . . . . . . . . . 31 THR N . 0.74 . 23 . . . . . . . . . . . 32 VAL N . 0.83 . 6 . . . . . . . . . . . 33 LEU N . 0.83 . 7 . . . . . . . . . . . 34 GLU N . 0.83 . 13 . . . . . . . . . . . 35 GLU N . 0.78 . 20 . . . . . . . . . . . 36 MET N . 0.80 . 27 . . . . . . . . . . . 37 SER N . 0.74 . 23 . . . . . . . . . . . 38 LEU N . 0.62 . 25 . . . . . . . . . . . 39 GLY N . 0.56 . 43 . . . . . . . . . . . 40 ARG N . 0.68 . 32 . . . . . . . . . . . 41 TRP N . 0.68 . 27 . . . . . . . . . . . 42 LYS N . 0.79 . 15 . . . . . . . . . . . 43 LYS N . 0.75 . 17 . . . . . . . . . . . 44 MET N . 0.77 . 28 . . . . . . . . . . . 46 GLY N . 0.78 . 17 . . . . . . . . . . . 47 GLY N . 0.77 . 5 . . . . . . . . . . . 48 ILE N . 0.85 . 1 . . . . . . . . . . . 50 GLY N . 0.75 . 14 . . . . . . . . . . . 51 PHE N . 0.74 . 13 . . . . . . . . . . . 53 LYS N . 0.75 . 31 . . . . . . . . . . . 54 VAL N . 0.80 . 24 . . . . . . . . . . . 55 ARG N . 0.81 . 10 . . . . . . . . . . . 56 GLN N . 0.87 . 12 . . . . . . . . . . . 57 TYR N . 0.80 . 10 . . . . . . . . . . . 58 ASP N . 0.77 . 20 . . . . . . . . . . . 59 GLN N . 0.80 . 20 . . . . . . . . . . . 61 LEU N . 0.83 . 13 . . . . . . . . . . . 62 ILE N . 0.81 . 17 . . . . . . . . . . . 63 GLU N . 0.81 . 15 . . . . . . . . . . . 64 ILE N . 0.78 . 14 . . . . . . . . . . . 66 GLY N . 0.81 . 28 . . . . . . . . . . . 68 LYS N . 0.74 . 24 . . . . . . . . . . . 69 ALA N . 0.75 . 27 . . . . . . . . . . . 72 THR N . 0.82 . 20 . . . . . . . . . . . 73 VAL N . 0.82 . 8 . . . . . . . . . . . 74 LEU N . 0.85 . 5 . . . . . . . . . . . 75 VAL N . 0.80 . 8 . . . . . . . . . . . 76 GLY N . 0.84 . 7 . . . . . . . . . . . 80 VAL N . 0.83 . 21 . . . . . . . . . . . 81 ASN N . 0.81 . 14 . . . . . . . . . . . 82 ILE N . 0.81 . 11 . . . . . . . . . . . 83 ILE N . 0.81 . 10 . . . . . . . . . . . 84 GLY N . 0.82 . 9 . . . . . . . . . . . 85 ARG N . 0.88 . 2 . . . . . . . . . . . 86 ASN N . 0.85 . 9 . . . . . . . . . . . 87 LEU N . 0.82 . 20 . . . . . . . . . . . 88 LEU N . 0.84 . 1 . . . . . . . . . . . 89 THR N . 0.86 . 1 . . . . . . . . . . . 90 GLN N . 0.76 . 13 . . . . . . . . . . . 91 ILE N . 0.79 . 18 . . . . . . . . . . . 92 GLY N . 0.80 . 5 . . . . . . . . . . . 93 ALA N . 0.83 . 10 . . . . . . . . . . . 94 THR N . 0.83 . 11 . . . . . . . . . . . 97 PHE N . 0.81 . 15 . . . . . . . . . . . stop_ save_ save_order_parameter_list_2 _Saveframe_category S2_parameters _Details ; Order parameter (S2) and Tau e values derived from the 600 MHz relaxation data, and relaxation values predicted for these S2 and Tau e values, using the constrained asymmetric diffusion tensor with Tau c equal to 10.82 ns, and the simple Lipari-Szabo description for internal motion. Residues D25, E35, I50, Y59, V75, L76, and G86 yield a poor fit due to the presence of exchange broadening; residues Q2, V3, L38, G40, R41 and W42 require fitting with the extended Lipari-Szabo model because of intermediate time scale internal motions (Clore et al., 1990b). ; _Sample_conditions_label $sample_conditions_1 _Mol_system_component_name 'protease, 1' _Tau_e_value_units ps _Tau_s_value_units . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Atom_name _Model_fit _S2_value _S2_value_fit_error _Tau_e_value _Tau_e_value_fit_error _S2f_value _S2f_value_fit_error _S2s_value _S2s_value_fit_error _Tau_s_value _Tau_s_value_fit_error _S2H_value _S2H_value_fit_error _S2N_value _S2N_value_fit_error 2 GLN N . 0.71 . 34 . . . . . . . . . . . 3 VAL N . 0.83 . 41 . . . . . . . . . . . 7 GLN N . 0.81 . 32 . . . . . . . . . . . 8 ARG N . 0.84 . 17 . . . . . . . . . . . 10 LEU N . 0.76 . 10 . . . . . . . . . . . 11 VAL N . 0.81 . 22 . . . . . . . . . . . 12 THR N . 0.82 . 28 . . . . . . . . . . . 13 ILE N . 0.83 . 26 . . . . . . . . . . . 14 LYS N . 0.82 . 16 . . . . . . . . . . . 15 ILE N . 0.85 . 12 . . . . . . . . . . . 16 GLY N . 0.84 . 25 . . . . . . . . . . . 17 GLY N . 0.86 . 34 . . . . . . . . . . . 18 GLN N . 0.81 . 35 . . . . . . . . . . . 19 LEU N . 0.83 . 12 . . . . . . . . . . . 20 LYS N . 0.79 . 15 . . . . . . . . . . . 21 GLU N . 0.78 . 29 . . . . . . . . . . . 22 ALA N . 0.85 . 20 . . . . . . . . . . . 24 LEU N . 0.86 . 11 . . . . . . . . . . . 25 ASP N . 0.81 . 4 . . . . . . . . . . . 26 THR N . 0.82 . 4 . . . . . . . . . . . 27 GLY N . 0.96 . 43 . . . . . . . . . . . 28 ALA N . 0.88 . 18 . . . . . . . . . . . 29 ASP N . 0.83 . 21 . . . . . . . . . . . 31 THR N . 0.76 . 27 . . . . . . . . . . . 32 VAL N . 0.85 . 8 . . . . . . . . . . . 33 LEU N . 0.84 . 8 . . . . . . . . . . . 34 GLU N . 0.86 . 18 . . . . . . . . . . . 35 GLU N . 0.79 . 21 . . . . . . . . . . . 36 MET N . 0.81 . 28 . . . . . . . . . . . 37 SER N . 0.76 . 26 . . . . . . . . . . . 38 LEU N . 0.66 . 30 . . . . . . . . . . . 39 GLY N . 0.58 . 47 . . . . . . . . . . . 40 ARG N . 0.71 . 38 . . . . . . . . . . . 41 TRP N . 0.72 . 33 . . . . . . . . . . . 42 LYS N . 0.83 . 21 . . . . . . . . . . . 43 LYS N . 0.78 . 21 . . . . . . . . . . . 44 MET N . 0.79 . 33 . . . . . . . . . . . 46 GLY N . 0.80 . 19 . . . . . . . . . . . 47 GLY N . 0.79 . 5 . . . . . . . . . . . 48 ILE N . 0.93 . 1 . . . . . . . . . . . 50 GLY N . 0.80 . 19 . . . . . . . . . . . 51 PHE N . 0.77 . 15 . . . . . . . . . . . 53 LYS N . 0.75 . 31 . . . . . . . . . . . 54 VAL N . 0.81 . 26 . . . . . . . . . . . 55 ARG N . 0.80 . 9 . . . . . . . . . . . 56 GLN N . 0.89 . 16 . . . . . . . . . . . 57 TYR N . 0.82 . 11 . . . . . . . . . . . 58 ASP N . 0.78 . 22 . . . . . . . . . . . 59 GLN N . 0.81 . 22 . . . . . . . . . . . 61 LEU N . 0.86 . 17 . . . . . . . . . . . 62 ILE N . 0.85 . 25 . . . . . . . . . . . 63 GLU N . 0.82 . 18 . . . . . . . . . . . 64 ILE N . 0.77 . 13 . . . . . . . . . . . 66 GLY N . 0.83 . 34 . . . . . . . . . . . 68 LYS N . 0.76 . 28 . . . . . . . . . . . 69 ALA N . 0.77 . 32 . . . . . . . . . . . 72 THR N . 0.84 . 23 . . . . . . . . . . . 73 VAL N . 0.84 . 9 . . . . . . . . . . . 74 LEU N . 0.85 . 4 . . . . . . . . . . . 75 VAL N . 0.79 . 8 . . . . . . . . . . . 76 GLY N . 0.85 . 9 . . . . . . . . . . . 80 VAL N . 0.85 . 25 . . . . . . . . . . . 81 ASN N . 0.85 . 20 . . . . . . . . . . . 82 ILE N . 0.84 . 16 . . . . . . . . . . . 83 ILE N . 0.83 . 14 . . . . . . . . . . . 84 GLY N . 0.83 . 9 . . . . . . . . . . . 85 ARG N . 0.90 . 2 . . . . . . . . . . . 86 ASN N . 0.87 . 10 . . . . . . . . . . . 87 LEU N . 0.82 . 20 . . . . . . . . . . . 88 LEU N . 0.87 . 1 . . . . . . . . . . . 89 THR N . 0.92 . 1 . . . . . . . . . . . 90 GLN N . 0.86 . 26 . . . . . . . . . . . 91 ILE N . 0.83 . 24 . . . . . . . . . . . 92 GLY N . 0.85 . 7 . . . . . . . . . . . 93 ALA N . 0.86 . 13 . . . . . . . . . . . 94 THR N . 0.85 . 12 . . . . . . . . . . . 97 PHE N . 0.81 . 15 . . . . . . . . . . . stop_ save_ save_order_parameter_list_3 _Saveframe_category S2_parameters _Details ; Order parameter (S2) and Tau e values derived from the 360 MHz relaxation data, and relaxation values predicted for these S2 and Tau e values, using the constrained asymmetric diffusion tensor with Tau c equal to 10.81 ns, and the simple Lipari-Szabo description for internal motion. Residues D25, E35, I50, Y59, V75, L76, and G86 yield a poor fit due to the presence of exchange broadening; residues Q2, V3, L38, G40, R41 and W42 require fitting with the extended Lipari-Szabo model because of intermediate time scale internal motions (Clore et al., 1990b). ; _Sample_conditions_label $sample_conditions_1 _Mol_system_component_name 'protease, 1' _Tau_e_value_units ps _Tau_s_value_units . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Atom_name _Model_fit _S2_value _S2_value_fit_error _Tau_e_value _Tau_e_value_fit_error _S2f_value _S2f_value_fit_error _S2s_value _S2s_value_fit_error _Tau_s_value _Tau_s_value_fit_error _S2H_value _S2H_value_fit_error _S2N_value _S2N_value_fit_error 2 GLN N . 0.67 . 27 . . . . . . . . . . . 3 VAL N . 0.73 . 22 . . . . . . . . . . . 7 GLN N . 0.76 . 23 . . . . . . . . . . . 8 ARG N . 0.79 . 11 . . . . . . . . . . . 10 LEU N . 0.77 . 11 . . . . . . . . . . . 11 VAL N . 0.79 . 17 . . . . . . . . . . . 12 THR N . 0.79 . 23 . . . . . . . . . . . 13 ILE N . 0.80 . 21 . . . . . . . . . . . 14 LYS N . 0.81 . 16 . . . . . . . . . . . 15 ILE N . 0.82 . 8 . . . . . . . . . . . 16 GLY N . 0.80 . 17 . . . . . . . . . . . 17 GLY N . 0.81 . 22 . . . . . . . . . . . 18 GLN N . 0.77 . 28 . . . . . . . . . . . 19 LEU N . 0.81 . 9 . . . . . . . . . . . 20 LYS N . 0.77 . 13 . . . . . . . . . . . 21 GLU N . 0.76 . 26 . . . . . . . . . . . 22 ALA N . 0.82 . 14 . . . . . . . . . . . 24 LEU N . 0.82 . 8 . . . . . . . . . . . 25 ASP N . 0.79 . 5 . . . . . . . . . . . 26 THR N . 0.86 . 4 . . . . . . . . . . . 27 GLY N . 0.92 . 18 . . . . . . . . . . . 28 ALA N . 0.83 . 10 . . . . . . . . . . . 29 ASP N . 0.79 . 16 . . . . . . . . . . . 31 THR N . 0.74 . 23 . . . . . . . . . . . 32 VAL N . 0.83 . 6 . . . . . . . . . . . 33 LEU N . 0.83 . 6 . . . . . . . . . . . 34 GLU N . 0.83 . 13 . . . . . . . . . . . 35 GLU N . 0.78 . 20 . . . . . . . . . . . 36 MET N . 0.79 . 25 . . . . . . . . . . . 37 SER N . 0.74 . 23 . . . . . . . . . . . 38 LEU N . 0.62 . 25 . . . . . . . . . . . 39 GLY N . 0.56 . 43 . . . . . . . . . . . 40 ARG N . 0.68 . 32 . . . . . . . . . . . 41 TRP N . 0.67 . 27 . . . . . . . . . . . 42 LYS N . 0.79 . 15 . . . . . . . . . . . 43 LYS N . 0.75 . 17 . . . . . . . . . . . 44 MET N . 0.77 . 28 . . . . . . . . . . . 46 GLY N . 0.78 . 16 . . . . . . . . . . . 47 GLY N . 0.76 . 5 . . . . . . . . . . . 48 ILE N . 0.84 . 1 . . . . . . . . . . . 50 GLY N . 0.75 . 14 . . . . . . . . . . . 51 PHE N . 0.73 . 12 . . . . . . . . . . . 53 LYS N . 0.84 . 29 . . . . . . . . . . . 54 VAL N . 0.80 . 24 . . . . . . . . . . . 55 ARG N . 0.81 . 10 . . . . . . . . . . . 56 GLN N . 0.86 . 11 . . . . . . . . . . . 57 TYR N . 0.79 . 9 . . . . . . . . . . . 58 ASP N . 0.77 . 20 . . . . . . . . . . . 59 GLN N . 0.80 . 20 . . . . . . . . . . . 61 LEU N . 0.83 . 13 . . . . . . . . . . . 62 ILE N . 0.81 . 17 . . . . . . . . . . . 63 GLU N . 0.81 . 15 . . . . . . . . . . . 64 ILE N . 0.78 . 13 . . . . . . . . . . . 66 GLY N . 0.80 . 27 . . . . . . . . . . . 68 LYS N . 0.84 . 24 . . . . . . . . . . . 69 ALA N . 0.84 . 26 . . . . . . . . . . . 72 THR N . 0.81 . 19 . . . . . . . . . . . 73 VAL N . 0.82 . 7 . . . . . . . . . . . 74 LEU N . 0.84 . 4 . . . . . . . . . . . 75 VAL N . 0.79 . 8 . . . . . . . . . . . 76 GLY N . 0.84 . 7 . . . . . . . . . . . 80 VAL N . 0.83 . 20 . . . . . . . . . . . 81 ASN N . 0.81 . 14 . . . . . . . . . . . 82 ILE N . 0.80 . 10 . . . . . . . . . . . 83 ILE N . 0.80 . 9 . . . . . . . . . . . 84 GLY N . 0.82 . 9 . . . . . . . . . . . 85 ARG N . 0.88 . 1 . . . . . . . . . . . 86 ASN N . 0.84 . 8 . . . . . . . . . . . 87 LEU N . 0.81 . 19 . . . . . . . . . . . 88 LEU N . 0.84 . 1 . . . . . . . . . . . 89 THR N . 0.85 . 1 . . . . . . . . . . . 90 GLN N . 0.76 . 13 . . . . . . . . . . . 91 ILE N . 0.78 . 17 . . . . . . . . . . . 92 GLY N . 0.80 . 4 . . . . . . . . . . . 93 ALA N . 0.83 . 9 . . . . . . . . . . . 94 THR N . 0.82 . 11 . . . . . . . . . . . 97 PHE N . 0.81 . 15 . . . . . . . . . . . stop_ save_ save_order_parameter_list_4 _Saveframe_category S2_parameters _Details ; Order parameter (S2) and Tau e values derived from the 600 MHz relaxation data, and relaxation values predicted for these S2 and Tau e values, using the constrained asymmetric diffusion tensor with Tau c equal to 10.59 ns, and the simple Lipari-Szabo description for internal motion. Residues D25, E35, I50, Y59, V75, L76, and G86 yield a poor fit due to the presence of exchange broadening; residues Q2, V3, L38, G40, R41 and W42 require fitting with the extended Lipari-Szabo model because of intermediate time scale internal motions (Clore et al., 1990b). ; _Sample_conditions_label $sample_conditions_1 _Mol_system_component_name 'protease, 1' _Tau_e_value_units ps _Tau_s_value_units . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Atom_name _Model_fit _S2_value _S2_value_fit_error _Tau_e_value _Tau_e_value_fit_error _S2f_value _S2f_value_fit_error _S2s_value _S2s_value_fit_error _Tau_s_value _Tau_s_value_fit_error _S2H_value _S2H_value_fit_error _S2N_value _S2N_value_fit_error 2 GLN N . 0.71 . 34 . . . . . . . . . . . 3 VAL N . 0.83 . 40 . . . . . . . . . . . 7 GLN N . 0.80 . 30 . . . . . . . . . . . 8 ARG N . 0.84 . 15 . . . . . . . . . . . 10 LEU N . 0.75 . 8 . . . . . . . . . . . 11 VAL N . 0.81 . 21 . . . . . . . . . . . 12 THR N . 0.81 . 27 . . . . . . . . . . . 13 ILE N . 0.82 . 24 . . . . . . . . . . . 14 LYS N . 0.81 . 15 . . . . . . . . . . . 15 ILE N . 0.85 . 10 . . . . . . . . . . . 16 GLY N . 0.84 . 24 . . . . . . . . . . . 17 GLY N . 0.85 . 32 . . . . . . . . . . . 18 GLN N . 0.80 . 33 . . . . . . . . . . . 19 LEU N . 0.83 . 11 . . . . . . . . . . . 20 LYS N . 0.78 . 15 . . . . . . . . . . . 21 GLU N . 0.78 . 28 . . . . . . . . . . . 22 ALA N . 0.84 . 19 . . . . . . . . . . . 24 LEU N . 0.85 . 11 . . . . . . . . . . . 25 ASP N . 0.80 . 2 . . . . . . . . . . . 26 THR N . 0.81 . 4 . . . . . . . . . . . 27 GLY N . 0.96 . 34 . . . . . . . . . . . 28 ALA N . 0.88 . 17 . . . . . . . . . . . 29 ASP N . 0.83 . 19 . . . . . . . . . . . 31 THR N . 0.76 . 27 . . . . . . . . . . . 32 VAL N . 0.85 . 6 . . . . . . . . . . . 33 LEU N . 0.83 . 8 . . . . . . . . . . . 34 GLU N . 0.85 . 17 . . . . . . . . . . . 35 GLU N . 0.79 . 20 . . . . . . . . . . . 36 MET N . 0.80 . 27 . . . . . . . . . . . 37 SER N . 7.60 . 26 . . . . . . . . . . . 38 LEU N . 0.65 . 30 . . . . . . . . . . . 39 GLY N . 0.58 . 47 . . . . . . . . . . . 40 ARG N . 0.70 . 36 . . . . . . . . . . . 41 TRP N . 0.72 . 33 . . . . . . . . . . . 42 LYS N . 0.83 . 20 . . . . . . . . . . . 43 LYS N . 0.77 . 20 . . . . . . . . . . . 44 MET N . 0.79 . 32 . . . . . . . . . . . 46 GLY N . 0.80 . 18 . . . . . . . . . . . 47 GLY N . 0.78 . 4 . . . . . . . . . . . 48 ILE N . 0.98 . 1 . . . . . . . . . . . 50 GLY N . 0.79 . 18 . . . . . . . . . . . 51 PHE N . 0.86 . 15 . . . . . . . . . . . 53 LYS N . 0.75 . 30 . . . . . . . . . . . 54 VAL N . 0.80 . 24 . . . . . . . . . . . 55 ARG N . 0.80 . 7 . . . . . . . . . . . 56 GLN N . 0.88 . 15 . . . . . . . . . . . 57 TYR N . 0.81 . 10 . . . . . . . . . . . 58 ASP N . 0.78 . 22 . . . . . . . . . . . 59 GLN N . 0.80 . 20 . . . . . . . . . . . 61 LEU N . 0.85 . 15 . . . . . . . . . . . 62 ILE N . 0.85 . 23 . . . . . . . . . . . 63 GLU N . 0.81 . 17 . . . . . . . . . . . 64 ILE N . 0.77 . 12 . . . . . . . . . . . 66 GLY N . 0.83 . 33 . . . . . . . . . . . 68 LYS N . 0.76 . 27 . . . . . . . . . . . 69 ALA N . 0.76 . 30 . . . . . . . . . . . 72 THR N . 0.83 . 21 . . . . . . . . . . . 73 VAL N . 0.84 . 7 . . . . . . . . . . . 74 LEU N . 0.84 . 3 . . . . . . . . . . . 75 VAL N . 0.79 . 7 . . . . . . . . . . . 76 GLY N . 0.85 . 6 . . . . . . . . . . . 80 VAL N . 0.85 . 23 . . . . . . . . . . . 81 ASN N . 0.84 . 19 . . . . . . . . . . . 82 ILE N . 0.84 . 15 . . . . . . . . . . . 83 ILE N . 0.83 . 13 . . . . . . . . . . . 84 GLY N . 0.83 . 7 . . . . . . . . . . . 85 ARG N . 0.89 . 1 . . . . . . . . . . . 86 ASN N . 0.86 . 8 . . . . . . . . . . . 87 LEU N . 0.82 . 18 . . . . . . . . . . . 88 LEU N . 0.87 . 1 . . . . . . . . . . . 89 THR N . 0.92 . 1 . . . . . . . . . . . 90 GLN N . 0.86 . 25 . . . . . . . . . . . 91 ILE N . 0.82 . 23 . . . . . . . . . . . 92 GLY N . 0.85 . 5 . . . . . . . . . . . 93 ALA N . 0.86 . 10 . . . . . . . . . . . 94 THR N . 0.85 . 9 . . . . . . . . . . . 97 PHE N . 0.81 . 14 . . . . . . . . . . . stop_ save_ save_order_parameter_list_5 _Saveframe_category S2_parameters _Details ; Order parameter (S2) and Tau e values derived from the 360 MHz relaxation data, and relaxation values predicted for these S2 and Tau e values, using the isotropic diffusion model and the simple Lipari-Szabo description for internal motion. Residues D25, E35, I50, Y59, V75, L76, and G86 yield a poor fit due to the presence of exchange broadening; residues Q2, V3, L38, G40, R41 and W42 require fitting with the extended Lipari-Szabo model because of intermediate time scale internal motions (Clore et al., 1990b). ; _Sample_conditions_label $sample_conditions_1 _Mol_system_component_name 'protease, 1' _Tau_e_value_units ps _Tau_s_value_units . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Atom_name _Model_fit _S2_value _S2_value_fit_error _Tau_e_value _Tau_e_value_fit_error _S2f_value _S2f_value_fit_error _S2s_value _S2s_value_fit_error _Tau_s_value _Tau_s_value_fit_error _S2H_value _S2H_value_fit_error _S2N_value _S2N_value_fit_error 2 GLN N . 0.68 . 44 . . . . . . . . . . . 3 VAL N . 0.75 . 29 . . . . . . . . . . . 7 GLN N . 0.77 . 29 . . . . . . . . . . . 8 ARG N . 0.8 . 1 . . . . . . . . . . . 10 LEU N . 0.78 . 1 . . . . . . . . . . . 11 VAL N . 0.81 . 17 . . . . . . . . . . . 12 THR N . 0.79 . 23 . . . . . . . . . . . 13 ILE N . 0.84 . 21 . . . . . . . . . . . 14 LYS N . 0.85 . 9 . . . . . . . . . . . 15 ILE N . 0.87 . 1 . . . . . . . . . . . 16 GLY N . 0.82 . 13 . . . . . . . . . . . 17 GLY N . 0.8 . 20 . . . . . . . . . . . 18 GLN N . 0.8 . 40 . . . . . . . . . . . 19 LEU N . 0.81 . 1 . . . . . . . . . . . 20 LYS N . 0.81 . 6 . . . . . . . . . . . 21 GLU N . 0.75 . 33 . . . . . . . . . . . 22 ALA N . 0.85 . 2 . . . . . . . . . . . 24 LEU N . 0.85 . 1 . . . . . . . . . . . 25 ASP N . 0.82 . 1 . . . . . . . . . . . 26 THR N . 0.88 . 1 . . . . . . . . . . . 27 GLY N . 0.91 . 1 . . . . . . . . . . . 28 ALA N . 0.86 . 1 . . . . . . . . . . . 29 ASP N . 0.8 . 8 . . . . . . . . . . . 31 THR N . 0.72 . 28 . . . . . . . . . . . 32 VAL N . 0.85 . 1 . . . . . . . . . . . 33 LEU N . 0.85 . 1 . . . . . . . . . . . 34 GLU N . 0.86 . 1 . . . . . . . . . . . 35 GLU N . 0.85 . 15 . . . . . . . . . . . 36 MET N . 0.81 . 32 . . . . . . . . . . . 37 SER N . 0.75 . 31 . . . . . . . . . . . 38 LEU N . 0.63 . 42 . . . . . . . . . . . 39 GLY N . 0.56 . 76 . . . . . . . . . . . 40 ARG N . 0.68 . 52 . . . . . . . . . . . 41 TRP N . 0.68 . 42 . . . . . . . . . . . 42 LYS N . 0.82 . 6 . . . . . . . . . . . 43 LYS N . 0.8 . 20 . . . . . . . . . . . 44 MET N . 0.78 . 39 . . . . . . . . . . . 46 GLY N . 0.79 . 13 . . . . . . . . . . . 47 GLY N . 0.8 . 1 . . . . . . . . . . . 48 ILE N . 0.83 . 1 . . . . . . . . . . . 50 GLY N . 0.78 . 11 . . . . . . . . . . . 51 PHE N . 0.74 . 7 . . . . . . . . . . . 53 LYS N . 0.74 . 42 . . . . . . . . . . . 54 VAL N . 0.84 . 31 . . . . . . . . . . . 55 ARG N . 0.85 . 1 . . . . . . . . . . . 56 GLN N . 0.84 . 1 . . . . . . . . . . . 57 TYR N . 0.83 . 1 . . . . . . . . . . . 58 ASP N . 0.76 . 17 . . . . . . . . . . . 59 GLN N . 0.79 . 13 . . . . . . . . . . . 61 LEU N . 0.8 . 1 . . . . . . . . . . . 62 ILE N . 0.86 . 10 . . . . . . . . . . . 63 GLU N . 0.85 . 5 . . . . . . . . . . . 64 ILE N . 0.82 . 5 . . . . . . . . . . . 66 GLY N . 0.83 . 36 . . . . . . . . . . . 68 LYS N . 0.74 . 32 . . . . . . . . . . . 69 ALA N . 0.78 . 42 . . . . . . . . . . . 72 THR N . 0.8 . 11 . . . . . . . . . . . 73 VAL N . 0.83 . 1 . . . . . . . . . . . 74 LEU N . 0.84 . 1 . . . . . . . . . . . 75 VAL N . 0.82 . 1 . . . . . . . . . . . 76 GLY N . 0.8 . 1 . . . . . . . . . . . 80 VAL N . 0.86 . 15 . . . . . . . . . . . 81 ASN N . 0.81 . 5 . . . . . . . . . . . 82 ILE N . 0.83 . 1 . . . . . . . . . . . 83 ILE N . 0.83 . 1 . . . . . . . . . . . 84 GLY N . 0.81 . 1 . . . . . . . . . . . 85 ARG N . 0.87 . 1 . . . . . . . . . . . 86 ASN N . 0.87 . 1 . . . . . . . . . . . 87 LEU N . 0.83 . 11 . . . . . . . . . . . 88 LEU N . 0.85 . 1 . . . . . . . . . . . 89 THR N . 0.87 . 1 . . . . . . . . . . . 90 GLN N . 0.77 . 7 . . . . . . . . . . . 91 ILE N . 0.8 . 13 . . . . . . . . . . . 92 GLY N . 0.81 . 1 . . . . . . . . . . . 93 ALA N . 0.83 . 1 . . . . . . . . . . . 94 THR N . 0.85 . 1 . . . . . . . . . . . 97 PHE N . 0.84 . 6 . . . . . . . . . . . stop_ save_ save_order_parameter_list_6 _Saveframe_category S2_parameters _Details ; Order parameter (S2) and Tau e values derived from the 600 MHz relaxation data, and relaxation values predicted for these S2 and Tau e values, using the isotropic diffusion model and the simple Lipari-Szabo description for internal motion. Residues D25, E35, I50, Y59, V75, L76, and G86 yield a poor fit due to the presence of exchange broadening; residues Q2, V3, L38, G40, R41 and W42 require fitting with the extended Lipari-Szabo model because of intermediate time scale internal motions (Clore et al., 1990b). ; _Sample_conditions_label $sample_conditions_1 _Mol_system_component_name 'protease, 1' _Tau_e_value_units ps _Tau_s_value_units . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Atom_name _Model_fit _S2_value _S2_value_fit_error _Tau_e_value _Tau_e_value_fit_error _S2f_value _S2f_value_fit_error _S2s_value _S2s_value_fit_error _Tau_s_value _Tau_s_value_fit_error _S2H_value _S2H_value_fit_error _S2N_value _S2N_value_fit_error 2 GLN N . 0.74 . 37 . . . . . . . . . . . 3 VAL N . 0.88 . 57 . . . . . . . . . . . 7 GLN N . 0.82 . 33 . . . . . . . . . . . 8 ARG N . 0.85 . 15 . . . . . . . . . . . 10 LEU N . 0.77 . 8 . . . . . . . . . . . 11 VAL N . 0.86 . 27 . . . . . . . . . . . 12 THR N . 0.82 . 27 . . . . . . . . . . . 13 ILE N . 0.87 . 32 . . . . . . . . . . . 14 LYS N . 0.86 . 20 . . . . . . . . . . . 15 ILE N . 0.91 . 18 . . . . . . . . . . . 16 GLY N . 0.88 . 31 . . . . . . . . . . . 17 GLY N . 0.86 . 32 . . . . . . . . . . . 18 GLN N . 0.84 . 41 . . . . . . . . . . . 19 LEU N . 0.85 . 11 . . . . . . . . . . . 20 LYS N . 0.84 . 18 . . . . . . . . . . . 21 GLU N . 0.78 . 28 . . . . . . . . . . . 22 ALA N . 0.89 . 24 . . . . . . . . . . . 24 LEU N . 0.89 . 10 . . . . . . . . . . . 25 ASP N . 0.84 . 1 . . . . . . . . . . . 26 THR N . 0.84 . 1 . . . . . . . . . . . 27 GLY N . 0.96 . 39 . . . . . . . . . . . 28 ALA N . 0.91 . 21 . . . . . . . . . . . 29 ASP N . 0.83 . 18 . . . . . . . . . . . 31 THR N . 0.74 . 22 . . . . . . . . . . . 32 VAL N . 0.87 . 3 . . . . . . . . . . . 33 LEU N . 0.87 . 4 . . . . . . . . . . . 34 GLU N . 0.89 . 21 . . . . . . . . . . . 35 GLU N . 0.77 . 15 . . . . . . . . . . . 36 MET N . 0.84 . 33 . . . . . . . . . . . 37 SER N . 0.79 . 29 . . . . . . . . . . . 38 LEU N . 0.69 . 33 . . . . . . . . . . . 39 GLY N . 0.61 . 50 . . . . . . . . . . . 40 ARG N . 0.73 . 40 . . . . . . . . . . . 41 TRP N . 0.74 . 35 . . . . . . . . . . . 42 LYS N . 0.86 . 21 . . . . . . . . . . . 43 LYS N . 0.84 . 27 . . . . . . . . . . . 44 MET N . 0.82 . 37 . . . . . . . . . . . 46 GLY N . 0.82 . 19 . . . . . . . . . . . 47 GLY N . 0.83 . 3 . . . . . . . . . . . 48 ILE N . 0.92 . 1 . . . . . . . . . . . 50 GLY N . 0.84 . 22 . . . . . . . . . . . 51 PHE N . 0.78 . 14 . . . . . . . . . . . 53 LYS N . 0.77 . 32 . . . . . . . . . . . 54 VAL N . 0.86 . 35 . . . . . . . . . . . 55 ARG N . 0.85 . 10 . . . . . . . . . . . 56 GLN N . 0.87 . 11 . . . . . . . . . . . 57 TYR N . 0.85 . 3 . . . . . . . . . . . 58 ASP N . 0.77 . 16 . . . . . . . . . . . 59 GLN N . 0.79 . 15 . . . . . . . . . . . 61 LEU N . 0.83 . 6 . . . . . . . . . . . 62 ILE N . 0.91 . 38 . . . . . . . . . . . 63 GLU N . 0.86 . 22 . . . . . . . . . . . 64 ILE N . 0.81 . 14 . . . . . . . . . . . 66 GLY N . 0.87 . 44 . . . . . . . . . . . 68 LYS N . 0.77 . 28 . . . . . . . . . . . 69 ALA N . 0.81 . 38 . . . . . . . . . . . 72 THR N . 0.82 . 18 . . . . . . . . . . . 73 VAL N . 0.86 . 1 . . . . . . . . . . . 74 LEU N . 0.85 . 1 . . . . . . . . . . . 75 VAL N . 0.82 . 5 . . . . . . . . . . . 76 GLY N . 0.9 . 10 . . . . . . . . . . . 80 VAL N . 0.9 . 35 . . . . . . . . . . . 81 ASN N . 0.86 . 21 . . . . . . . . . . . 82 ILE N . 0.87 . 12 . . . . . . . . . . . 83 ILE N . 0.86 . 9 . . . . . . . . . . . 84 GLY N . 0.82 . 1 . . . . . . . . . . . 85 ARG N . 0.89 . 1 . . . . . . . . . . . 86 ASN N . 0.9 . 5 . . . . . . . . . . . 87 LEU N . 0.84 . 15 . . . . . . . . . . . 88 LEU N . 0.89 . 1 . . . . . . . . . . . 89 THR N . 0.94 . 1 . . . . . . . . . . . 90 GLN N . 0.88 . 28 . . . . . . . . . . . 91 ILE N . 0.84 . 23 . . . . . . . . . . . 92 GLY N . 0.87 . 6 . . . . . . . . . . . 93 ALA N . 0.87 . 4 . . . . . . . . . . . 94 THR N . 0.88 . 14 . . . . . . . . . . . 97 PHE N . 0.85 . 18 . . . . . . . . . . . stop_ save_