data_26677 ####################### # Entry information # ####################### save_entry_information _Entry.Sf_category entry_information _Entry.Sf_framecode entry_information _Entry.ID 26677 _Entry.Title ; 1H, 13C, and 15N Chemical Shift Assignments for redox-stable cyclic peptide inhibitors of SPSB2-iNOS interaction - CP2 ; _Entry.Type macromolecule _Entry.Version_type original _Entry.Submission_date 2015-10-03 _Entry.Accession_date 2015-10-03 _Entry.Last_release_date 2016-09-09 _Entry.Original_release_date 2016-09-09 _Entry.Origination author _Entry.NMR_STAR_version 3.1.2.6 _Entry.Original_NMR_STAR_version 3.1 _Entry.Experimental_method NMR _Entry.Experimental_method_subtype solution _Entry.Details . _Entry.BMRB_internal_directory_name . loop_ _Entry_author.Ordinal _Entry_author.Given_name _Entry_author.Family_name _Entry_author.First_initial _Entry_author.Middle_initials _Entry_author.Family_title _Entry_author.ORCID _Entry_author.Entry_ID 1 'Beow Keat' Yap . . . . 26677 2 Raymond Norton . . . . 26677 stop_ loop_ _Data_set.Type _Data_set.Count _Data_set.Entry_ID assigned_chemical_shifts 1 26677 stop_ loop_ _Datum.Type _Datum.Count _Datum.Entry_ID '13C chemical shifts' 22 26677 '15N chemical shifts' 11 26677 '1H chemical shifts' 47 26677 stop_ loop_ _Release.Release_number _Release.Format_type _Release.Format_version _Release.Date _Release.Submission_date _Release.Type _Release.Author _Release.Detail _Release.Entry_ID 1 . . 2016-09-09 . original BMRB . 26677 stop_ loop_ _Related_entries.Database_name _Related_entries.Database_accession_code _Related_entries.Relationship _Related_entries.Entry_ID BMRB 26676 CP1 26677 stop_ save_ ############### # Citations # ############### save_entry_citation _Citation.Sf_category citations _Citation.Sf_framecode entry_citation _Citation.Entry_ID 26677 _Citation.ID 1 _Citation.Class 'entry citation' _Citation.CAS_abstract_code . _Citation.MEDLINE_UI_code . _Citation.DOI . _Citation.PubMed_ID 26921848 _Citation.Full_citation . _Citation.Title ; Redox-stable cyclic peptide inhibitors of the SPSB2-iNOS interaction ; _Citation.Status published _Citation.Type journal _Citation.Journal_abbrev 'FEBS Lett.' _Citation.Journal_name_full . _Citation.Journal_volume 590 _Citation.Journal_issue 6 _Citation.Journal_ASTM . _Citation.Journal_ISSN . _Citation.Journal_CSD . _Citation.Book_title . _Citation.Book_chapter_title . _Citation.Book_volume . _Citation.Book_series . _Citation.Book_publisher . _Citation.Book_publisher_city . _Citation.Book_ISBN . _Citation.Conference_title . _Citation.Conference_site . _Citation.Conference_state_province . _Citation.Conference_country . _Citation.Conference_start_date . _Citation.Conference_end_date . _Citation.Conference_abstract_number . _Citation.Thesis_institution . _Citation.Thesis_institution_city . _Citation.Thesis_institution_country . _Citation.WWW_URL . _Citation.Page_first 696 _Citation.Page_last 704 _Citation.Year 2016 _Citation.Details . loop_ _Citation_author.Ordinal _Citation_author.Given_name _Citation_author.Family_name _Citation_author.First_initial _Citation_author.Middle_initials _Citation_author.Family_title _Citation_author.ORCID _Citation_author.Entry_ID _Citation_author.Citation_ID 1 'Beow Keat' Yap . . . . 26677 1 2 J. Harjani . R. . . 26677 1 3 E. Leung . W. . . 26677 1 4 S. Nicholson . E. . . 26677 1 5 M. Scanlon . J. . . 26677 1 6 D. Chalmers . K. . . 26677 1 7 P. Thompson . E. . . 26677 1 8 J. Baell . B. . . 26677 1 9 Raymond Norton . . . . 26677 1 stop_ save_ ############################################# # Molecular system (assembly) description # ############################################# save_assembly _Assembly.Sf_category assembly _Assembly.Sf_framecode assembly _Assembly.Entry_ID 26677 _Assembly.ID 1 _Assembly.Name CP2 _Assembly.BMRB_code . _Assembly.Number_of_components 1 _Assembly.Organic_ligands . _Assembly.Metal_ions . _Assembly.Non_standard_bonds yes _Assembly.Ambiguous_conformational_states . _Assembly.Ambiguous_chem_comp_sites . _Assembly.Molecules_in_chemical_exchange . _Assembly.Paramagnetic no _Assembly.Thiol_state . _Assembly.Molecular_mass 827.55 _Assembly.Enzyme_commission_number . _Assembly.Details 'Cyclic peptide c[WDINNNbA]' _Assembly.DB_query_date . _Assembly.DB_query_revised_last_date . loop_ _Entity_assembly.ID _Entity_assembly.Entity_assembly_name _Entity_assembly.Entity_ID _Entity_assembly.Entity_label _Entity_assembly.Asym_ID _Entity_assembly.PDB_chain_ID _Entity_assembly.Experimental_data_reported _Entity_assembly.Physical_state _Entity_assembly.Conformational_isomer _Entity_assembly.Chemical_exchange_state _Entity_assembly.Magnetic_equivalence_group_code _Entity_assembly.Role _Entity_assembly.Details _Entity_assembly.Entry_ID _Entity_assembly.Assembly_ID 1 WDINNNX 1 $WDINNNX A . yes native no no . . . 26677 1 stop_ loop_ _Bond.ID _Bond.Type _Bond.Value_order _Bond.Assembly_atom_ID_1 _Bond.Entity_assembly_ID_1 _Bond.Entity_assembly_name_1 _Bond.Entity_ID_1 _Bond.Comp_ID_1 _Bond.Comp_index_ID_1 _Bond.Seq_ID_1 _Bond.Atom_ID_1 _Bond.Assembly_atom_ID_2 _Bond.Entity_assembly_ID_2 _Bond.Entity_assembly_name_2 _Bond.Entity_ID_2 _Bond.Comp_ID_2 _Bond.Comp_index_ID_2 _Bond.Seq_ID_2 _Bond.Atom_ID_2 _Bond.Auth_entity_assembly_ID_1 _Bond.Auth_entity_assembly_name_1 _Bond.Auth_seq_ID_1 _Bond.Auth_comp_ID_1 _Bond.Auth_atom_ID_1 _Bond.Auth_entity_assembly_ID_2 _Bond.Auth_entity_assembly_name_2 _Bond.Auth_seq_ID_2 _Bond.Auth_comp_ID_2 _Bond.Auth_atom_ID_2 _Bond.Entry_ID _Bond.Assembly_ID 1 peptide single . 1 . 1 BAL 7 7 C . 1 . 1 TRP 1 1 N . BAL na na C . WDINNN 1 Trp N 26677 1 2 peptide single . 1 . 1 BAL 7 7 N . 1 . 1 ASN 6 6 C . BAL na na N . WDINNN 6 Asn C 26677 1 stop_ save_ #################################### # Biological polymers and ligands # #################################### save_WDINNNX _Entity.Sf_category entity _Entity.Sf_framecode WDINNNX _Entity.Entry_ID 26677 _Entity.ID 1 _Entity.BMRB_code . _Entity.Name WDINNNX _Entity.Type polymer _Entity.Polymer_common_type . _Entity.Polymer_type polypeptide(L) _Entity.Polymer_type_details . _Entity.Polymer_strand_ID . _Entity.Polymer_seq_one_letter_code_can . _Entity.Polymer_seq_one_letter_code ; WDINNNX ; _Entity.Target_identifier . _Entity.Polymer_author_defined_seq ; 1, W 2, D 3, I 4, N 5, N 6, N 7, BAL ; _Entity.Polymer_author_seq_details . _Entity.Ambiguous_conformational_states no _Entity.Ambiguous_chem_comp_sites no _Entity.Nstd_monomer no _Entity.Nstd_chirality no _Entity.Nstd_linkage no _Entity.Nonpolymer_comp_ID . _Entity.Nonpolymer_comp_label . _Entity.Number_of_monomers 7 _Entity.Number_of_nonpolymer_components . _Entity.Paramagnetic no _Entity.Thiol_state 'not present' _Entity.Src_method . _Entity.Parent_entity_ID . _Entity.Fragment . _Entity.Mutation . _Entity.EC_number . _Entity.Calc_isoelectric_point . _Entity.Formula_weight . _Entity.Formula_weight_exptl . _Entity.Formula_weight_exptl_meth . _Entity.Details 'BAL is residue number 7 of CP2' _Entity.DB_query_date . _Entity.DB_query_revised_last_date . loop_ _Entity_comp_index.ID _Entity_comp_index.Auth_seq_ID _Entity_comp_index.Comp_ID _Entity_comp_index.Comp_label _Entity_comp_index.Entry_ID _Entity_comp_index.Entity_ID 1 . TRP . 26677 1 2 . ASP . 26677 1 3 . ILE . 26677 1 4 . ASN . 26677 1 5 . ASN . 26677 1 6 . ASN . 26677 1 7 . BAL . 26677 1 stop_ loop_ _Entity_poly_seq.Hetero _Entity_poly_seq.Mon_ID _Entity_poly_seq.Num _Entity_poly_seq.Comp_index_ID _Entity_poly_seq.Entry_ID _Entity_poly_seq.Entity_ID . TRP 1 1 26677 1 . ASP 2 2 26677 1 . ILE 3 3 26677 1 . ASN 4 4 26677 1 . ASN 5 5 26677 1 . ASN 6 6 26677 1 . BAL 7 7 26677 1 stop_ save_ #################### # Natural source # #################### save_natural_source _Entity_natural_src_list.Sf_category natural_source _Entity_natural_src_list.Sf_framecode natural_source _Entity_natural_src_list.Entry_ID 26677 _Entity_natural_src_list.ID 1 loop_ _Entity_natural_src.ID _Entity_natural_src.Entity_ID _Entity_natural_src.Entity_label _Entity_natural_src.Entity_chimera_segment_ID _Entity_natural_src.NCBI_taxonomy_ID _Entity_natural_src.Type _Entity_natural_src.Common _Entity_natural_src.Organism_name_scientific _Entity_natural_src.Organism_name_common _Entity_natural_src.Organism_acronym _Entity_natural_src.ICTVdb_decimal_code _Entity_natural_src.Superkingdom _Entity_natural_src.Kingdom _Entity_natural_src.Genus _Entity_natural_src.Species _Entity_natural_src.Strain _Entity_natural_src.Variant _Entity_natural_src.Organ _Entity_natural_src.Tissue _Entity_natural_src.Tissue_fraction _Entity_natural_src.Cell_line _Entity_natural_src.Cell_type _Entity_natural_src.ATCC_number _Entity_natural_src.Organelle _Entity_natural_src.Secretion _Entity_natural_src.Plasmid _Entity_natural_src.Gene_mnemonic _Entity_natural_src.Details _Entity_natural_src.Entry_ID _Entity_natural_src.Entity_natural_src_list_ID 1 1 $WDINNNX . . 'not applicable' . . . . . . . . . . . . . . . . . . . . . 'Synthesized by Fmoc-based solid phase peptide synthesis' 26677 1 stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Entity_experimental_src_list.Sf_category experimental_source _Entity_experimental_src_list.Sf_framecode experimental_source _Entity_experimental_src_list.Entry_ID 26677 _Entity_experimental_src_list.ID 1 loop_ _Entity_experimental_src.ID _Entity_experimental_src.Entity_ID _Entity_experimental_src.Entity_label _Entity_experimental_src.Entity_chimera_segment_ID _Entity_experimental_src.Production_method _Entity_experimental_src.Host_org_scientific_name _Entity_experimental_src.Host_org_name_common _Entity_experimental_src.Host_org_details _Entity_experimental_src.Host_org_NCBI_taxonomy_ID _Entity_experimental_src.Host_org_genus _Entity_experimental_src.Host_org_species _Entity_experimental_src.Host_org_strain _Entity_experimental_src.Host_org_variant _Entity_experimental_src.Host_org_ATCC_number _Entity_experimental_src.Vector_type _Entity_experimental_src.PDBview_host_org_vector_name _Entity_experimental_src.PDBview_plasmid_name _Entity_experimental_src.Vector_name _Entity_experimental_src.Vector_details _Entity_experimental_src.Vendor_name _Entity_experimental_src.Details _Entity_experimental_src.Entry_ID _Entity_experimental_src.Entity_experimental_src_list_ID 1 1 $WDINNNX . 'chemical synthesis' . . . . . . . . . . . . . . . . 26677 1 stop_ save_ ################################# # Polymer residues and ligands # ################################# save_chem_comp_BAL _Chem_comp.Sf_category chem_comp _Chem_comp.Sf_framecode chem_comp_BAL _Chem_comp.Entry_ID 26677 _Chem_comp.ID BAL _Chem_comp.Provenance PDB _Chem_comp.Name BETA-ALANINE _Chem_comp.Type PEPTIDE-LIKE _Chem_comp.BMRB_code BAL _Chem_comp.PDB_code BAL _Chem_comp.Ambiguous_flag no _Chem_comp.Initial_date 2012-11-20 _Chem_comp.Modified_date 2012-11-20 _Chem_comp.Release_status REL _Chem_comp.Replaced_by . _Chem_comp.Replaces . _Chem_comp.One_letter_code . _Chem_comp.Three_letter_code BAL _Chem_comp.Number_atoms_all 13 _Chem_comp.Number_atoms_nh 6 _Chem_comp.PubChem_code . _Chem_comp.Subcomponent_list . _Chem_comp.InChI_code InChI=1S/C3H7NO2/c4-2-1-3(5)6/h1-2,4H2,(H,5,6) _Chem_comp.Mon_nstd_flag . _Chem_comp.Mon_nstd_class . _Chem_comp.Mon_nstd_details . _Chem_comp.Mon_nstd_parent . _Chem_comp.Mon_nstd_parent_comp_ID . _Chem_comp.Std_deriv_one_letter_code . _Chem_comp.Std_deriv_three_letter_code . _Chem_comp.Std_deriv_BMRB_code . _Chem_comp.Std_deriv_PDB_code . _Chem_comp.Std_deriv_chem_comp_name . _Chem_comp.Synonyms . _Chem_comp.Formal_charge 0 _Chem_comp.Paramagnetic . _Chem_comp.Aromatic no _Chem_comp.Formula 'C3 H7 N O2' _Chem_comp.Formula_weight 89.093 _Chem_comp.Formula_mono_iso_wt_nat . _Chem_comp.Formula_mono_iso_wt_13C . _Chem_comp.Formula_mono_iso_wt_15N . _Chem_comp.Formula_mono_iso_wt_13C_15N . _Chem_comp.Image_file_name . _Chem_comp.Image_file_format . _Chem_comp.Topo_file_name . _Chem_comp.Topo_file_format . _Chem_comp.Struct_file_name . _Chem_comp.Struct_file_format . _Chem_comp.Stereochem_param_file_name . _Chem_comp.Stereochem_param_file_format . _Chem_comp.Model_details . _Chem_comp.Model_erf . _Chem_comp.Model_source . _Chem_comp.Model_coordinates_details . _Chem_comp.Model_coordinates_missing_flag no _Chem_comp.Ideal_coordinates_details Corina _Chem_comp.Ideal_coordinates_missing_flag no _Chem_comp.Model_coordinates_db_code 1MCE _Chem_comp.Processing_site RCSB _Chem_comp.Vendor . _Chem_comp.Vendor_product_code . _Chem_comp.Details . _Chem_comp.DB_query_date . _Chem_comp.DB_last_query_revised_last_date . loop_ _Chem_comp_descriptor.Descriptor _Chem_comp_descriptor.Type _Chem_comp_descriptor.Program _Chem_comp_descriptor.Program_version _Chem_comp_descriptor.Entry_ID _Chem_comp_descriptor.Comp_ID C(CN)C(=O)O SMILES 'OpenEye OEToolkits' 1.7.0 26677 BAL C(CN)C(=O)O SMILES_CANONICAL 'OpenEye OEToolkits' 1.7.0 26677 BAL InChI=1S/C3H7NO2/c4-2-1-3(5)6/h1-2,4H2,(H,5,6) InChI InChI 1.03 26677 BAL NCCC(O)=O SMILES CACTVS 3.370 26677 BAL NCCC(O)=O SMILES_CANONICAL CACTVS 3.370 26677 BAL O=C(O)CCN SMILES ACDLabs 12.01 26677 BAL UCMIRNVEIXFBKS-UHFFFAOYSA-N InChIKey InChI 1.03 26677 BAL stop_ loop_ _Chem_comp_identifier.Identifier _Chem_comp_identifier.Type _Chem_comp_identifier.Program _Chem_comp_identifier.Program_version _Chem_comp_identifier.Entry_ID _Chem_comp_identifier.Comp_ID '3-azanylpropanoic acid' 'SYSTEMATIC NAME' 'OpenEye OEToolkits' 1.7.0 26677 BAL beta-alanine 'SYSTEMATIC NAME' ACDLabs 12.01 26677 BAL stop_ loop_ _Chem_comp_atom.Atom_ID _Chem_comp_atom.BMRB_code _Chem_comp_atom.PDB_atom_ID _Chem_comp_atom.Alt_atom_ID _Chem_comp_atom.Auth_atom_ID _Chem_comp_atom.Type_symbol _Chem_comp_atom.Isotope_number _Chem_comp_atom.Chirality _Chem_comp_atom.Stereo_config _Chem_comp_atom.Charge _Chem_comp_atom.Partial_charge _Chem_comp_atom.Oxidation_number _Chem_comp_atom.Unpaired_electron_number _Chem_comp_atom.Align _Chem_comp_atom.Aromatic_flag _Chem_comp_atom.Leaving_atom_flag _Chem_comp_atom.Substruct_code _Chem_comp_atom.Ionizable _Chem_comp_atom.Drawing_2D_coord_x _Chem_comp_atom.Drawing_2D_coord_y _Chem_comp_atom.Model_Cartn_x _Chem_comp_atom.Model_Cartn_x_esd _Chem_comp_atom.Model_Cartn_y _Chem_comp_atom.Model_Cartn_y_esd _Chem_comp_atom.Model_Cartn_z _Chem_comp_atom.Model_Cartn_z_esd _Chem_comp_atom.Model_Cartn_x_ideal _Chem_comp_atom.Model_Cartn_y_ideal _Chem_comp_atom.Model_Cartn_z_ideal _Chem_comp_atom.PDBX_ordinal _Chem_comp_atom.Details _Chem_comp_atom.Entry_ID _Chem_comp_atom.Comp_ID N N N N . N . . N 0 . . . 1 no no . . . . 25.745 . -29.140 . 82.521 . 2.716 -0.247 -0.035 1 . 26677 BAL CB CB CB CB . C . . N 0 . . . 1 no no . . . . 26.010 . -30.369 . 81.740 . 1.400 0.405 -0.014 2 . 26677 BAL CA CA CA CA . C . . N 0 . . . 1 no no . . . . 24.667 . -30.987 . 81.251 . 0.302 -0.661 -0.022 3 . 26677 BAL C C C C . C . . N 0 . . . 1 no no . . . . 23.931 . -30.239 . 80.158 . -1.048 0.008 0.000 4 . 26677 BAL O O O O . O . . N 0 . . . 1 no no . . . . 24.209 . -29.153 . 79.662 . -1.124 1.214 0.020 5 . 26677 BAL OXT OXT OXT OXT . O . . N 0 . . . 1 no yes . . . . 23.529 . -31.208 . 79.500 . -2.165 -0.735 -0.003 6 . 26677 BAL H H H HN1 . H . . N 0 . . . 1 no no . . . . 26.611 . -28.749 . 82.832 . 3.458 0.436 -0.031 7 . 26677 BAL H2 H2 H2 HN2 . H . . N 0 . . . 1 no yes . . . . 25.267 . -28.476 . 81.946 . 2.813 -0.891 0.735 8 . 26677 BAL HB3 HB3 HB3 HB1 . H . . N 0 . . . 1 no no . . . . 26.634 . -30.119 . 80.869 . 1.310 1.013 0.887 9 . 26677 BAL HB2 HB2 HB2 HB2 . H . . N 0 . . . 1 no no . . . . 26.536 . -31.097 . 82.375 . 1.295 1.041 -0.893 10 . 26677 BAL HA1 HA1 HA1 HA1 . H . . N 0 . . . 1 no no . . . . 24.895 . -31.990 . 80.860 . 0.392 -1.268 -0.923 11 . 26677 BAL HA2 HA2 HA2 HA2 . H . . N 0 . . . 1 no no . . . . 23.996 . -31.032 . 82.121 . 0.407 -1.297 0.857 12 . 26677 BAL HXT HXT HXT HXT . H . . N 0 . . . 1 no yes . . . . 23.477 . -30.969 . 78.582 . -3.008 -0.261 0.012 13 . 26677 BAL stop_ loop_ _Chem_comp_bond.ID _Chem_comp_bond.Type _Chem_comp_bond.Value_order _Chem_comp_bond.Atom_ID_1 _Chem_comp_bond.Atom_ID_2 _Chem_comp_bond.Aromatic_flag _Chem_comp_bond.Stereo_config _Chem_comp_bond.Ordinal _Chem_comp_bond.Details _Chem_comp_bond.Entry_ID _Chem_comp_bond.Comp_ID 1 . SING N CB no N 1 . 26677 BAL 2 . SING N H no N 2 . 26677 BAL 3 . SING N H2 no N 3 . 26677 BAL 4 . SING CB CA no N 4 . 26677 BAL 5 . SING CB HB3 no N 5 . 26677 BAL 6 . SING CB HB2 no N 6 . 26677 BAL 7 . SING CA C no N 7 . 26677 BAL 8 . SING CA HA1 no N 8 . 26677 BAL 9 . SING CA HA2 no N 9 . 26677 BAL 10 . DOUB C O no N 10 . 26677 BAL 11 . SING C OXT no N 11 . 26677 BAL 12 . SING OXT HXT no N 12 . 26677 BAL stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Sample.Sf_category sample _Sample.Sf_framecode sample_1 _Sample.Entry_ID 26677 _Sample.ID 1 _Sample.Type solution _Sample.Sub_type . _Sample.Details . _Sample.Aggregate_sample_number . _Sample.Solvent_system '90% H2O/10% D2O' _Sample.Preparation_date . _Sample.Preparation_expiration_date . _Sample.Polycrystallization_protocol . _Sample.Single_crystal_protocol . _Sample.Crystal_grow_apparatus . _Sample.Crystal_grow_atmosphere . _Sample.Crystal_grow_details . _Sample.Crystal_grow_method . _Sample.Crystal_grow_method_cit_ID . _Sample.Crystal_grow_pH . _Sample.Crystal_grow_pH_range . _Sample.Crystal_grow_pressure . _Sample.Crystal_grow_pressure_esd . _Sample.Crystal_grow_seeding . _Sample.Crystal_grow_seeding_cit_ID . _Sample.Crystal_grow_temp . _Sample.Crystal_grow_temp_details . _Sample.Crystal_grow_temp_esd . _Sample.Crystal_grow_time . _Sample.Oriented_sample_prep_protocol . _Sample.Lyophilization_cryo_protectant . _Sample.Storage_protocol . loop_ _Sample_component.ID _Sample_component.Mol_common_name _Sample_component.Isotopic_labeling _Sample_component.Assembly_ID _Sample_component.Assembly_label _Sample_component.Entity_ID _Sample_component.Entity_label _Sample_component.Product_ID _Sample_component.Type _Sample_component.Concentration_val _Sample_component.Concentration_val_min _Sample_component.Concentration_val_max _Sample_component.Concentration_val_units _Sample_component.Concentration_val_err _Sample_component.Vendor _Sample_component.Vendor_product_name _Sample_component.Vendor_product_code _Sample_component.Entry_ID _Sample_component.Sample_ID 1 CP2 'natural abundance' . . 1 $WDINNNX . . 1.9 . . mM . . . . 26677 1 stop_ save_ ####################### # Sample conditions # ####################### save_sample_conditions_H2O _Sample_condition_list.Sf_category sample_conditions _Sample_condition_list.Sf_framecode sample_conditions_H2O _Sample_condition_list.Entry_ID 26677 _Sample_condition_list.ID 1 _Sample_condition_list.Details . loop_ _Sample_condition_variable.Type _Sample_condition_variable.Val _Sample_condition_variable.Val_err _Sample_condition_variable.Val_units _Sample_condition_variable.Entry_ID _Sample_condition_variable.Sample_condition_list_ID pH 4.8 . pH 26677 1 temperature 298 . K 26677 1 stop_ save_ save_sample_conditions_D2O _Sample_condition_list.Sf_category sample_conditions _Sample_condition_list.Sf_framecode sample_conditions_D2O _Sample_condition_list.Entry_ID 26677 _Sample_condition_list.ID 2 _Sample_condition_list.Details . loop_ _Sample_condition_variable.Type _Sample_condition_variable.Val _Sample_condition_variable.Val_err _Sample_condition_variable.Val_units _Sample_condition_variable.Entry_ID _Sample_condition_variable.Sample_condition_list_ID pH* 4.8 . pH* 26677 2 temperature 298 . K 26677 2 stop_ save_ ############################ # Computer software used # ############################ save_CcpNmr_Analysis _Software.Sf_category software _Software.Sf_framecode CcpNmr_Analysis _Software.Entry_ID 26677 _Software.ID 1 _Software.Name CcpNmr_Analysis _Software.Version 2.1.5 _Software.Details . loop_ _Vendor.Name _Vendor.Address _Vendor.Electronic_address _Vendor.Entry_ID _Vendor.Software_ID CCPN . . 26677 1 stop_ loop_ _Task.Task _Task.Entry_ID _Task.Software_ID 'chemical shift assignment' 26677 1 stop_ save_ save_TOPSPIN _Software.Sf_category software _Software.Sf_framecode TOPSPIN _Software.Entry_ID 26677 _Software.ID 2 _Software.Name TOPSPIN _Software.Version 3.2 _Software.Details . loop_ _Vendor.Name _Vendor.Address _Vendor.Electronic_address _Vendor.Entry_ID _Vendor.Software_ID 'Bruker Biospin' . . 26677 2 stop_ loop_ _Task.Task _Task.Entry_ID _Task.Software_ID collection 26677 2 stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_AV600 _NMR_spectrometer.Sf_category NMR_spectrometer _NMR_spectrometer.Sf_framecode AV600 _NMR_spectrometer.Entry_ID 26677 _NMR_spectrometer.ID 1 _NMR_spectrometer.Details . _NMR_spectrometer.Manufacturer Bruker _NMR_spectrometer.Model Avance _NMR_spectrometer.Serial_number . _NMR_spectrometer.Field_strength 600 save_ save_NMR_spectrometer_list _NMR_spectrometer_list.Sf_category NMR_spectrometer_list _NMR_spectrometer_list.Sf_framecode NMR_spectrometer_list _NMR_spectrometer_list.Entry_ID 26677 _NMR_spectrometer_list.ID 1 loop_ _NMR_spectrometer_view.ID _NMR_spectrometer_view.Name _NMR_spectrometer_view.Manufacturer _NMR_spectrometer_view.Model _NMR_spectrometer_view.Serial_number _NMR_spectrometer_view.Field_strength _NMR_spectrometer_view.Details _NMR_spectrometer_view.Citation_ID _NMR_spectrometer_view.Citation_label _NMR_spectrometer_view.Entry_ID _NMR_spectrometer_view.NMR_spectrometer_list_ID 1 AV600 Bruker Avance . 600 . . . 26677 1 stop_ save_ ############################# # NMR applied experiments # ############################# save_experiment_list _Experiment_list.Sf_category experiment_list _Experiment_list.Sf_framecode experiment_list _Experiment_list.Entry_ID 26677 _Experiment_list.ID 1 _Experiment_list.Details . loop_ _Experiment.ID _Experiment.Name _Experiment.Raw_data_flag _Experiment.NMR_spec_expt_ID _Experiment.NMR_spec_expt_label _Experiment.MS_expt_ID _Experiment.MS_expt_label _Experiment.SAXS_expt_ID _Experiment.SAXS_expt_label _Experiment.FRET_expt_ID _Experiment.FRET_expt_label _Experiment.EMR_expt_ID _Experiment.EMR_expt_label _Experiment.Sample_ID _Experiment.Sample_label _Experiment.Sample_state _Experiment.Sample_volume _Experiment.Sample_volume_units _Experiment.Sample_condition_list_ID _Experiment.Sample_condition_list_label _Experiment.Sample_spinning_rate _Experiment.Sample_angle _Experiment.NMR_tube_type _Experiment.NMR_spectrometer_ID _Experiment.NMR_spectrometer_label _Experiment.NMR_spectrometer_probe_ID _Experiment.NMR_spectrometer_probe_label _Experiment.NMR_spectral_processing_ID _Experiment.NMR_spectral_processing_label _Experiment.Mass_spectrometer_ID _Experiment.Mass_spectrometer_label _Experiment.Xray_instrument_ID _Experiment.Xray_instrument_label _Experiment.Fluorescence_instrument_ID _Experiment.Fluorescence_instrument_label _Experiment.EMR_instrument_ID _Experiment.EMR_instrument_label _Experiment.Chromatographic_system_ID _Experiment.Chromatographic_system_label _Experiment.Chromatographic_column_ID _Experiment.Chromatographic_column_label _Experiment.Entry_ID _Experiment.Experiment_list_ID 1 '2D 1H-1H TOCSY' no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_H2O . . . 1 $AV600 . . . . . . . . . . . . . . . . 26677 1 2 '2D 1H-1H ROESY' no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_H2O . . . 1 $AV600 . . . . . . . . . . . . . . . . 26677 1 3 '2D DQF-COSY' no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_H2O . . . 1 $AV600 . . . . . . . . . . . . . . . . 26677 1 4 '2D 1H-15N HSQC' no . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_H2O . . . 1 $AV600 . . . . . . . . . . . . . . . . 26677 1 5 '2D 1H-13C HSQC' no . . . . . . . . . . 1 $sample_1 isotropic . . 2 $sample_conditions_D2O . . . 1 $AV600 . . . . . . . . . . . . . . . . 26677 1 stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _Chem_shift_reference.Sf_category chem_shift_reference _Chem_shift_reference.Sf_framecode chemical_shift_reference_1 _Chem_shift_reference.Entry_ID 26677 _Chem_shift_reference.ID 1 _Chem_shift_reference.Details . loop_ _Chem_shift_ref.Atom_type _Chem_shift_ref.Atom_isotope_number _Chem_shift_ref.Mol_common_name _Chem_shift_ref.Atom_group _Chem_shift_ref.Concentration_val _Chem_shift_ref.Concentration_units _Chem_shift_ref.Solvent _Chem_shift_ref.Rank _Chem_shift_ref.Chem_shift_units _Chem_shift_ref.Chem_shift_val _Chem_shift_ref.Ref_method _Chem_shift_ref.Ref_type _Chem_shift_ref.Indirect_shift_ratio _Chem_shift_ref.External_ref_loc _Chem_shift_ref.External_ref_sample_geometry _Chem_shift_ref.External_ref_axis _Chem_shift_ref.Ref_correction_type _Chem_shift_ref.Correction_val _Chem_shift_ref.Entry_ID _Chem_shift_ref.Chem_shift_reference_ID C 13 DSS 'methyl protons' . . . . ppm 0.00 na indirect 0.251449530 . . . . . 26677 1 H 1 DSS 'methyl protons' . . . . ppm 0.00 internal direct 1.000000000 . . . . . 26677 1 N 15 DSS 'methyl protons' . . . . ppm 0.00 na indirect 0.101329118 . . . . . 26677 1 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chem_shift_list_1 _Assigned_chem_shift_list.Sf_category assigned_chemical_shifts _Assigned_chem_shift_list.Sf_framecode assigned_chem_shift_list_1 _Assigned_chem_shift_list.Entry_ID 26677 _Assigned_chem_shift_list.ID 1 _Assigned_chem_shift_list.Sample_condition_list_ID 1 _Assigned_chem_shift_list.Sample_condition_list_label $sample_conditions_H2O _Assigned_chem_shift_list.Chem_shift_reference_ID 1 _Assigned_chem_shift_list.Chem_shift_reference_label $chemical_shift_reference_1 _Assigned_chem_shift_list.Chem_shift_1H_err . _Assigned_chem_shift_list.Chem_shift_13C_err . _Assigned_chem_shift_list.Chem_shift_15N_err . _Assigned_chem_shift_list.Chem_shift_31P_err . _Assigned_chem_shift_list.Chem_shift_2H_err . _Assigned_chem_shift_list.Chem_shift_19F_err . _Assigned_chem_shift_list.Error_derivation_method . _Assigned_chem_shift_list.Details . _Assigned_chem_shift_list.Text_data_format . _Assigned_chem_shift_list.Text_data . loop_ _Chem_shift_experiment.Experiment_ID _Chem_shift_experiment.Experiment_name _Chem_shift_experiment.Sample_ID _Chem_shift_experiment.Sample_label _Chem_shift_experiment.Sample_state _Chem_shift_experiment.Entry_ID _Chem_shift_experiment.Assigned_chem_shift_list_ID 1 '2D 1H-1H TOCSY' . . . 26677 1 2 '2D 1H-1H ROESY' . . . 26677 1 3 '2D DQF-COSY' . . . 26677 1 4 '2D 1H-15N HSQC' . . . 26677 1 5 '2D 1H-13C HSQC' . . . 26677 1 stop_ loop_ _Atom_chem_shift.ID _Atom_chem_shift.Assembly_atom_ID _Atom_chem_shift.Entity_assembly_ID _Atom_chem_shift.Entity_ID _Atom_chem_shift.Comp_index_ID _Atom_chem_shift.Seq_ID _Atom_chem_shift.Comp_ID _Atom_chem_shift.Atom_ID _Atom_chem_shift.Atom_type _Atom_chem_shift.Atom_isotope_number _Atom_chem_shift.Val _Atom_chem_shift.Val_err _Atom_chem_shift.Assign_fig_of_merit _Atom_chem_shift.Ambiguity_code _Atom_chem_shift.Occupancy _Atom_chem_shift.Resonance_ID _Atom_chem_shift.Auth_entity_assembly_ID _Atom_chem_shift.Auth_asym_ID _Atom_chem_shift.Auth_seq_ID _Atom_chem_shift.Auth_comp_ID _Atom_chem_shift.Auth_atom_ID _Atom_chem_shift.Details _Atom_chem_shift.Entry_ID _Atom_chem_shift.Assigned_chem_shift_list_ID 1 . 1 1 1 1 TRP H H 1 8.106 0.001 . 1 . . . . 1 TRP H . 26677 1 2 . 1 1 1 1 TRP HA H 1 4.703 0.010 . 1 . . . . 1 TRP HA . 26677 1 3 . 1 1 1 1 TRP HB2 H 1 3.263 0.005 . 2 . . . . 1 TRP HB2 . 26677 1 4 . 1 1 1 1 TRP HB3 H 1 3.361 0.007 . 2 . . . . 1 TRP HB3 . 26677 1 5 . 1 1 1 1 TRP HD1 H 1 7.279 0.005 . 1 . . . . 1 TRP HD1 . 26677 1 6 . 1 1 1 1 TRP HE1 H 1 10.120 0.001 . 1 . . . . 1 TRP HE1 . 26677 1 7 . 1 1 1 1 TRP HE3 H 1 7.659 0.007 . 1 . . . . 1 TRP HE3 . 26677 1 8 . 1 1 1 1 TRP HZ2 H 1 7.507 0.007 . 1 . . . . 1 TRP HZ2 . 26677 1 9 . 1 1 1 1 TRP HZ3 H 1 7.185 0.007 . 1 . . . . 1 TRP HZ3 . 26677 1 10 . 1 1 1 1 TRP HH2 H 1 7.255 0.007 . 1 . . . . 1 TRP HH2 . 26677 1 11 . 1 1 1 1 TRP CA C 13 55.180 0.000 . 1 . . . . 1 TRP CA . 26677 1 12 . 1 1 1 1 TRP CB C 13 26.477 0.002 . 1 . . . . 1 TRP CB . 26677 1 13 . 1 1 1 1 TRP CD1 C 13 124.426 0.000 . 1 . . . . 1 TRP CD1 . 26677 1 14 . 1 1 1 1 TRP CE3 C 13 118.402 0.000 . 1 . . . . 1 TRP CE3 . 26677 1 15 . 1 1 1 1 TRP CZ2 C 13 111.983 0.000 . 1 . . . . 1 TRP CZ2 . 26677 1 16 . 1 1 1 1 TRP CZ3 C 13 119.449 0.000 . 1 . . . . 1 TRP CZ3 . 26677 1 17 . 1 1 1 1 TRP CH2 C 13 122.063 0.000 . 1 . . . . 1 TRP CH2 . 26677 1 18 . 1 1 1 1 TRP N N 15 125.716 0.000 . 1 . . . . 1 TRP N . 26677 1 19 . 1 1 1 1 TRP NE1 N 15 129.249 0.000 . 1 . . . . 1 TRP NE1 . 26677 1 20 . 1 1 2 2 ASP H H 1 8.133 0.006 . 1 . . . . 2 ASP H . 26677 1 21 . 1 1 2 2 ASP HA H 1 4.652 0.006 . 1 . . . . 2 ASP HA . 26677 1 22 . 1 1 2 2 ASP HB3 H 1 2.650 0.004 . 1 . . . . 2 ASP HB3 . 26677 1 23 . 1 1 2 2 ASP CA C 13 50.829 0.000 . 1 . . . . 2 ASP CA . 26677 1 24 . 1 1 2 2 ASP CB C 13 38.954 0.000 . 1 . . . . 2 ASP CB . 26677 1 25 . 1 1 2 2 ASP N N 15 119.487 0.000 . 1 . . . . 2 ASP N . 26677 1 26 . 1 1 3 3 ILE H H 1 8.250 0.005 . 1 . . . . 3 ILE H . 26677 1 27 . 1 1 3 3 ILE HA H 1 4.057 0.004 . 1 . . . . 3 ILE HA . 26677 1 28 . 1 1 3 3 ILE HB H 1 1.905 0.006 . 1 . . . . 3 ILE HB . 26677 1 29 . 1 1 3 3 ILE HG12 H 1 1.246 0.011 . 2 . . . . 3 ILE HG12 . 26677 1 30 . 1 1 3 3 ILE HG13 H 1 1.439 0.011 . 2 . . . . 3 ILE HG13 . 26677 1 31 . 1 1 3 3 ILE HG21 H 1 0.933 0.010 . 1 . . . . 3 ILE HG21 . 26677 1 32 . 1 1 3 3 ILE HG22 H 1 0.933 0.010 . 1 . . . . 3 ILE HG22 . 26677 1 33 . 1 1 3 3 ILE HG23 H 1 0.933 0.010 . 1 . . . . 3 ILE HG23 . 26677 1 34 . 1 1 3 3 ILE HD11 H 1 0.900 0.006 . 1 . . . . 3 ILE HD11 . 26677 1 35 . 1 1 3 3 ILE HD12 H 1 0.900 0.006 . 1 . . . . 3 ILE HD12 . 26677 1 36 . 1 1 3 3 ILE HD13 H 1 0.900 0.006 . 1 . . . . 3 ILE HD13 . 26677 1 37 . 1 1 3 3 ILE CA C 13 60.308 0.000 . 1 . . . . 3 ILE CA . 26677 1 38 . 1 1 3 3 ILE CB C 13 35.780 0.000 . 1 . . . . 3 ILE CB . 26677 1 39 . 1 1 3 3 ILE CG1 C 13 24.890 0.006 . 1 . . . . 3 ILE CG1 . 26677 1 40 . 1 1 3 3 ILE CG2 C 13 14.802 0.000 . 1 . . . . 3 ILE CG2 . 26677 1 41 . 1 1 3 3 ILE CD1 C 13 10.893 0.000 . 1 . . . . 3 ILE CD1 . 26677 1 42 . 1 1 3 3 ILE N N 15 119.799 0.000 . 1 . . . . 3 ILE N . 26677 1 43 . 1 1 4 4 ASN H H 1 8.186 0.004 . 1 . . . . 4 ASN H . 26677 1 44 . 1 1 4 4 ASN HA H 1 4.676 0.010 . 1 . . . . 4 ASN HA . 26677 1 45 . 1 1 4 4 ASN HB2 H 1 2.757 0.004 . 2 . . . . 4 ASN HB2 . 26677 1 46 . 1 1 4 4 ASN HB3 H 1 2.870 0.012 . 2 . . . . 4 ASN HB3 . 26677 1 47 . 1 1 4 4 ASN HD21 H 1 6.927 0.001 . 1 . . . . 4 ASN HD21 . 26677 1 48 . 1 1 4 4 ASN HD22 H 1 7.715 0.001 . 1 . . . . 4 ASN HD22 . 26677 1 49 . 1 1 4 4 ASN CA C 13 51.215 0.000 . 1 . . . . 4 ASN CA . 26677 1 50 . 1 1 4 4 ASN CB C 13 35.930 0.003 . 1 . . . . 4 ASN CB . 26677 1 51 . 1 1 4 4 ASN N N 15 118.232 0.000 . 1 . . . . 4 ASN N . 26677 1 52 . 1 1 4 4 ASN ND2 N 15 113.708 0.008 . 1 . . . . 4 ASN ND2 . 26677 1 53 . 1 1 5 5 ASN H H 1 8.011 0.005 . 1 . . . . 5 ASN H . 26677 1 54 . 1 1 5 5 ASN HA H 1 4.601 0.005 . 1 . . . . 5 ASN HA . 26677 1 55 . 1 1 5 5 ASN HB2 H 1 2.671 0.007 . 2 . . . . 5 ASN HB2 . 26677 1 56 . 1 1 5 5 ASN HB3 H 1 2.838 0.004 . 2 . . . . 5 ASN HB3 . 26677 1 57 . 1 1 5 5 ASN HD21 H 1 6.735 0.001 . 1 . . . . 5 ASN HD21 . 26677 1 58 . 1 1 5 5 ASN HD22 H 1 7.656 0.003 . 1 . . . . 5 ASN HD22 . 26677 1 59 . 1 1 5 5 ASN CA C 13 51.044 0.000 . 1 . . . . 5 ASN CA . 26677 1 60 . 1 1 5 5 ASN CB C 13 35.768 0.014 . 1 . . . . 5 ASN CB . 26677 1 61 . 1 1 5 5 ASN N N 15 115.738 0.000 . 1 . . . . 5 ASN N . 26677 1 62 . 1 1 5 5 ASN ND2 N 15 113.218 0.017 . 1 . . . . 5 ASN ND2 . 26677 1 63 . 1 1 6 6 ASN H H 1 8.304 0.002 . 1 . . . . 6 ASN H . 26677 1 64 . 1 1 6 6 ASN HA H 1 4.564 0.006 . 1 . . . . 6 ASN HA . 26677 1 65 . 1 1 6 6 ASN HB2 H 1 2.660 0.001 . 2 . . . . 6 ASN HB2 . 26677 1 66 . 1 1 6 6 ASN HB3 H 1 2.795 0.004 . 2 . . . . 6 ASN HB3 . 26677 1 67 . 1 1 6 6 ASN HD21 H 1 6.809 0.001 . 1 . . . . 6 ASN HD21 . 26677 1 68 . 1 1 6 6 ASN HD22 H 1 7.580 0.000 . 1 . . . . 6 ASN HD22 . 26677 1 69 . 1 1 6 6 ASN CA C 13 51.353 0.000 . 1 . . . . 6 ASN CA . 26677 1 70 . 1 1 6 6 ASN CB C 13 35.902 0.000 . 1 . . . . 6 ASN CB . 26677 1 71 . 1 1 6 6 ASN N N 15 117.565 0.000 . 1 . . . . 6 ASN N . 26677 1 72 . 1 1 6 6 ASN ND2 N 15 112.642 0.006 . 1 . . . . 6 ASN ND2 . 26677 1 73 . 1 1 7 7 BAL H H 1 7.901 0.002 . 1 . . . . 7 BAL H . 26677 1 74 . 1 1 7 7 BAL HA1 H 1 2.431 0.007 . 2 . . . . 7 BAL HA1 . 26677 1 75 . 1 1 7 7 BAL HA2 H 1 2.292 0.009 . 2 . . . . 7 BAL HA2 . 26677 1 76 . 1 1 7 7 BAL HB2 H 1 3.481 0.004 . 2 . . . . 7 BAL HB2 . 26677 1 77 . 1 1 7 7 BAL HB3 H 1 3.317 0.005 . 2 . . . . 7 BAL HB3 . 26677 1 78 . 1 1 7 7 BAL CA C 13 34.968 0.005 . 1 . . . . 7 BAL CA . 26677 1 79 . 1 1 7 7 BAL CB C 13 35.920 0.005 . 1 . . . . 7 BAL CB . 26677 1 80 . 1 1 7 7 BAL N N 15 116.672 0.000 . 1 . . . . 7 BAL N . 26677 1 stop_ save_