data_31032 ####################### # Entry information # ####################### save_entry_information _Entry.Sf_category entry_information _Entry.Sf_framecode entry_information _Entry.ID 31032 _Entry.Title ; NMR Solution Structure of C-terminally amidated, Full-length Human Galanin ; _Entry.Type macromolecule _Entry.Version_type original _Entry.Submission_date 2022-06-30 _Entry.Accession_date 2022-06-30 _Entry.Last_release_date 2022-07-07 _Entry.Original_release_date 2022-07-07 _Entry.Origination author _Entry.Format_name . _Entry.NMR_STAR_version 3.2.14.0 _Entry.NMR_STAR_dict_location . _Entry.Original_NMR_STAR_version 3.1 _Entry.Experimental_method NMR _Entry.Experimental_method_subtype 'SOLUTION NMR' _Entry.Source_data_format . _Entry.Source_data_format_version . _Entry.Generated_software_name . _Entry.Generated_software_version . _Entry.Generated_software_ID . _Entry.Generated_software_label . _Entry.Generated_date . _Entry.DOI . _Entry.UUID . _Entry.Related_coordinate_file_name . _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 R. Wilkinson R. E. . . 31032 2 K. Kraichely K. N. . . 31032 3 L. Buchanan L. E. . . 31032 4 S. Parnham S. . . . 31032 5 M. Giuliano M. W. . . 31032 stop_ loop_ _Struct_keywords.Keywords _Struct_keywords.Text _Struct_keywords.Entry_ID neuropeptide . 31032 synthetic . 31032 stop_ loop_ _Data_set.Type _Data_set.Count _Data_set.Entry_ID assigned_chemical_shifts 1 31032 spectral_peak_list 1 31032 stop_ loop_ _Datum.Type _Datum.Count _Datum.Entry_ID '1H chemical shifts' 194 31032 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 2 . . 2022-10-31 2022-06-30 update BMRB 'update entry citation' 31032 1 . . 2022-08-17 2022-06-30 original author 'original release' 31032 stop_ loop_ _Related_entries.Database_name _Related_entries.Database_accession_code _Related_entries.Relationship _Related_entries.Entry_ID PDB 8DJ4 'BMRB Entry Tracking System' 31032 stop_ save_ ############### # Citations # ############### save_citation_1 _Citation.Sf_category citations _Citation.Sf_framecode citation_1 _Citation.Entry_ID 31032 _Citation.ID 1 _Citation.Name . _Citation.Class 'entry citation' _Citation.CAS_abstract_code . _Citation.MEDLINE_UI_code . _Citation.PubMed_ID 35994823 _Citation.DOI . _Citation.Full_citation . _Citation.Title ; The neuropeptide galanin adopts an irregular secondary structure ; _Citation.Status published _Citation.Type journal _Citation.Journal_abbrev 'Biochem. Biophys. Res. Commun.' _Citation.Journal_name_full 'Biochemical and biophysical research communications' _Citation.Journal_volume 626 _Citation.Journal_issue . _Citation.Journal_ASTM . _Citation.Journal_ISSN 1090-2104 _Citation.Journal_CSD 0353 _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 121 _Citation.Page_last 128 _Citation.Year 2022 _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 R. Wilkinson R. E. . . 31032 1 2 K. Kraichely K. N. . . 31032 1 3 C. Hendy C. M. . . 31032 1 4 L. Buchanan L. E. . . 31032 1 5 S. Parnham S. . . . 31032 1 6 M. Giuliano M. W. . . 31032 1 stop_ save_ ############################################# # Molecular system (assembly) description # ############################################# save_assembly _Assembly.Sf_category assembly _Assembly.Sf_framecode assembly _Assembly.Entry_ID 31032 _Assembly.ID 1 _Assembly.Name Galanin _Assembly.BMRB_code . _Assembly.Number_of_components . _Assembly.Organic_ligands . _Assembly.Metal_ions . _Assembly.Non_standard_bonds . _Assembly.Ambiguous_conformational_states . _Assembly.Ambiguous_chem_comp_sites . _Assembly.Molecules_in_chemical_exchange . _Assembly.Paramagnetic no _Assembly.Thiol_state . _Assembly.Molecular_mass . _Assembly.Enzyme_commission_number . _Assembly.Details . _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 unit_1 1 $entity_1 A A yes . . . . . . 31032 1 stop_ save_ #################################### # Biological polymers and ligands # #################################### save_entity_1 _Entity.Sf_category entity _Entity.Sf_framecode entity_1 _Entity.Entry_ID 31032 _Entity.ID 1 _Entity.BMRB_code . _Entity.Name entity_1 _Entity.Type polymer _Entity.Polymer_common_type . _Entity.Polymer_type polypeptide(L) _Entity.Polymer_type_details . _Entity.Polymer_strand_ID A _Entity.Polymer_seq_one_letter_code_can . _Entity.Polymer_seq_one_letter_code ; GWTLNSAGYLLGPHAVGNHR SFSDKNGLTSX ; _Entity.Target_identifier . _Entity.Polymer_author_defined_seq . _Entity.Polymer_author_seq_details . _Entity.Ambiguous_conformational_states . _Entity.Ambiguous_chem_comp_sites . _Entity.Nstd_monomer yes _Entity.Nstd_chirality . _Entity.Nstd_linkage no _Entity.Nonpolymer_comp_ID . _Entity.Nonpolymer_comp_label . _Entity.Number_of_monomers 31 _Entity.Number_of_nonpolymer_components . _Entity.Paramagnetic no _Entity.Thiol_state 'not present' _Entity.Src_method syn _Entity.Parent_entity_ID 1 _Entity.Fragment . _Entity.Mutation . _Entity.EC_number . _Entity.Calc_isoelectric_point . _Entity.Formula_weight 3159.454 _Entity.Formula_weight_exptl . _Entity.Formula_weight_exptl_meth . _Entity.Details . _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 . GLY . 31032 1 2 . TRP . 31032 1 3 . THR . 31032 1 4 . LEU . 31032 1 5 . ASN . 31032 1 6 . SER . 31032 1 7 . ALA . 31032 1 8 . GLY . 31032 1 9 . TYR . 31032 1 10 . LEU . 31032 1 11 . LEU . 31032 1 12 . GLY . 31032 1 13 . PRO . 31032 1 14 . HIS . 31032 1 15 . ALA . 31032 1 16 . VAL . 31032 1 17 . GLY . 31032 1 18 . ASN . 31032 1 19 . HIS . 31032 1 20 . ARG . 31032 1 21 . SER . 31032 1 22 . PHE . 31032 1 23 . SER . 31032 1 24 . ASP . 31032 1 25 . LYS . 31032 1 26 . ASN . 31032 1 27 . GLY . 31032 1 28 . LEU . 31032 1 29 . THR . 31032 1 30 . SER . 31032 1 31 . NH2 . 31032 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 . GLY 1 1 31032 1 . TRP 2 2 31032 1 . THR 3 3 31032 1 . LEU 4 4 31032 1 . ASN 5 5 31032 1 . SER 6 6 31032 1 . ALA 7 7 31032 1 . GLY 8 8 31032 1 . TYR 9 9 31032 1 . LEU 10 10 31032 1 . LEU 11 11 31032 1 . GLY 12 12 31032 1 . PRO 13 13 31032 1 . HIS 14 14 31032 1 . ALA 15 15 31032 1 . VAL 16 16 31032 1 . GLY 17 17 31032 1 . ASN 18 18 31032 1 . HIS 19 19 31032 1 . ARG 20 20 31032 1 . SER 21 21 31032 1 . PHE 22 22 31032 1 . SER 23 23 31032 1 . ASP 24 24 31032 1 . LYS 25 25 31032 1 . ASN 26 26 31032 1 . GLY 27 27 31032 1 . LEU 28 28 31032 1 . THR 29 29 31032 1 . SER 30 30 31032 1 . NH2 31 31 31032 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 31032 _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 $entity_1 . 9606 organism . 'Homo sapiens' human . . Eukaryota Metazoa Homo sapiens . . . . . . . . . . . . . 31032 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 31032 _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 $entity_1 . 'chemical synthesis' . . . . . . . . . . . . . . . . 31032 1 stop_ save_ ################################# # Polymer residues and ligands # ################################# save_chem_comp_NH2 _Chem_comp.Sf_category chem_comp _Chem_comp.Sf_framecode chem_comp_NH2 _Chem_comp.Entry_ID 31032 _Chem_comp.ID NH2 _Chem_comp.Provenance PDB _Chem_comp.Name 'AMINO GROUP' _Chem_comp.Type NON-POLYMER _Chem_comp.BMRB_code NH2 _Chem_comp.PDB_code NH2 _Chem_comp.Ambiguous_flag yes _Chem_comp.Initial_date 2020-07-10 _Chem_comp.Modified_date 2020-07-10 _Chem_comp.Release_status REL _Chem_comp.Replaced_by . _Chem_comp.Replaces . _Chem_comp.One_letter_code . _Chem_comp.Three_letter_code NH2 _Chem_comp.Number_atoms_all 3 _Chem_comp.Number_atoms_nh 1 _Chem_comp.Atom_nomenclature_source . _Chem_comp.PubChem_code . _Chem_comp.Subcomponent_list . _Chem_comp.InChI_code InChI=1/H3N/h1H3 _Chem_comp.Mon_nstd_flag no _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 'H2 N' _Chem_comp.Formula_weight 16.023 _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 'OpenEye OEToolkits' _Chem_comp.Ideal_coordinates_missing_flag no _Chem_comp.Model_coordinates_db_code 2FLY _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 InChI=1/H3N/h1H3 InChI InChI 1.02b 31032 NH2 N SMILES ACDLabs 10.04 31032 NH2 QGZKDVFQNNGYKY-UHFFFAOYAF InChIKey InChI 1.02b 31032 NH2 [NH2] SMILES CACTVS 3.341 31032 NH2 [NH2] SMILES 'OpenEye OEToolkits' 1.5.0 31032 NH2 [NH2] SMILES_CANONICAL CACTVS 3.341 31032 NH2 [NH2] SMILES_CANONICAL 'OpenEye OEToolkits' 1.5.0 31032 NH2 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 ammonia 'SYSTEMATIC NAME' ACDLabs 10.04 31032 NH2 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 N N . . . . 10.091 . 8.978 . -7.810 . 0.000 0.000 0.000 1 . 31032 NH2 HN1 HN1 HN1 1HN . H . . N 0 . . . 1 N N . . . . 9.517 . 8.769 . -7.044 . -0.385 -0.545 -0.771 2 . 31032 NH2 HN2 HN2 HN2 2HN . H . . N 0 . . . 1 N N . . . . 10.323 . 9.890 . -8.082 . 1.020 0.000 0.000 3 . 31032 NH2 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 HN1 N N 1 . 31032 NH2 2 . SING N HN2 N N 2 . 31032 NH2 stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Sample.Sf_category sample _Sample.Sf_framecode sample_1 _Sample.Entry_ID 31032 _Sample.ID 1 _Sample.Name . _Sample.Type 'lyophilized powder' _Sample.Sub_type . _Sample.Details '0.5 mM hGal(1-30)NH2, 4.14 mM [U-2H] sodium acetate, 5.86 mM [U-2H] acetic acid, 95% H2O/5% D2O' _Sample.Aggregate_sample_number . _Sample.Solvent_system '95% H2O/5% 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 hGal(1-30)NH2 'natural abundance' . . 1 $entity_1 . . 0.5 . . mM . . . . 31032 1 2 'sodium acetate' [U-2H] . . . . . . 4.14 . . mM . . . . 31032 1 3 'acetic acid' [U-2H] . . . . . . 5.86 . . mM . . . . 31032 1 stop_ save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Sample_condition_list.Sf_category sample_conditions _Sample_condition_list.Sf_framecode sample_conditions_1 _Sample_condition_list.Entry_ID 31032 _Sample_condition_list.ID 1 _Sample_condition_list.Name . _Sample_condition_list.Details 'sample was dissolved in 10 mM sodium acetate-d3/acetic acid-d4 buffer at pH 4.6; no additional additives were present.' 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 4.6 0.02 pH 31032 1 pressure 1 . atm 31032 1 temperature 298 . K 31032 1 stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Software.Sf_category software _Software.Sf_framecode software_1 _Software.Entry_ID 31032 _Software.ID 1 _Software.Type . _Software.Name CNS _Software.Version . _Software.DOI . _Software.Details . loop_ _Vendor.Name _Vendor.Address _Vendor.Electronic_address _Vendor.Entry_ID _Vendor.Software_ID 'Brunger A. T. et.al.' . . 31032 1 'Brunger, Adams, Clore, Gros, Nilges and Read' . . 31032 1 stop_ loop_ _Task.Task _Task.Software_module _Task.Entry_ID _Task.Software_ID refinement . 31032 1 'structure calculation' . 31032 1 stop_ save_ save_software_2 _Software.Sf_category software _Software.Sf_framecode software_2 _Software.Entry_ID 31032 _Software.ID 2 _Software.Type . _Software.Name 'MestreLab (Mnova / MestReNova / MestReC)' _Software.Version . _Software.DOI . _Software.Details . loop_ _Vendor.Name _Vendor.Address _Vendor.Electronic_address _Vendor.Entry_ID _Vendor.Software_ID MestreLab . . 31032 2 stop_ loop_ _Task.Task _Task.Software_module _Task.Entry_ID _Task.Software_ID 'chemical shift assignment' . 31032 2 'peak picking' . 31032 2 stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _NMR_spectrometer.Sf_category NMR_spectrometer _NMR_spectrometer.Sf_framecode NMR_spectrometer_1 _NMR_spectrometer.Entry_ID 31032 _NMR_spectrometer.ID 1 _NMR_spectrometer.Name . _NMR_spectrometer.Details 'TCI H-C/N-D Cryoprobe' _NMR_spectrometer.Manufacturer Bruker _NMR_spectrometer.Model 'AVANCE III' _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 31032 _NMR_spectrometer_list.ID 1 _NMR_spectrometer_list.Name . 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 NMR_spectrometer_1 Bruker 'AVANCE III' . 600 . . . 31032 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 31032 _Experiment_list.ID 1 _Experiment_list.Details ; The authors state the following regarding the geometric deviations with this ensemble: With most of the hydrogen bonds in the N-terminus of the peptide bifurcated, or even more, they are confident that the ensemble represents the time-averaged structure of a peptide that is rapidly interconverting turns of alpha, 310-, and pi-helix. Their shift assignments were largely unambiguous and can be found in BMRB entry 31032. The "irregular helix restraints" used (and described in the manuscript and its references) were employed to allow the ensemble to sample multiple arrangements during simulated annealing. By definition, this ensemble existing as an average will display a significant degree of geometric irregularity, particularly with regard the backbone and sidechain outliers as compared to statistical norms. Further, the clashscore level is quite high. This appears to be a consequence of the very high density of ROE-derived distance restraints in the N-terminus of the peptide, which were maximally relaxed to account for any uncertainty in their measurement throughout several rounds of validation and re-calculation. Tight sidechain packing and compression seems to be the dictated outcome of our data. Much of their study is concerned with compact hydrophobic packing in this sequence - this full-length peptide is indeed much more rigid across the stretch of residues it shares with fragment peptides described in entries 7S3O, 7S3Q, and 7S3R. Together with the compactness of the region of the sequence, the clashes appear to be a consequence of several averaged, coiling, helical conformers all existing on the NMR timescale. This is discussed at further length in the citation affiliated with this deposition ; loop_ _Experiment.ID _Experiment.Name _Experiment.Raw_data_flag _Experiment.NUS_flag _Experiment.Interleaved_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.Details _Experiment.Entry_ID _Experiment.Experiment_list_ID 1 '1H 1D NMR Spectrum' no . . . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 1 $NMR_spectrometer_1 . . . . . . . . . . . . . . . . . 31032 1 2 '2D 1H-1H COSY' no . . . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 1 $NMR_spectrometer_1 . . . . . . . . . . . . . . . . . 31032 1 3 '2D 1H-1H TOCSY' no . . . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 1 $NMR_spectrometer_1 . . . . . . . . . . . . . . . . . 31032 1 4 '2D 1H-1H ROESY' no . . . . . . . . . . . . 1 $sample_1 isotropic . . 1 $sample_conditions_1 . . . 1 $NMR_spectrometer_1 . . . . . . . . . . . . . . . . . 31032 1 stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_shift_reference_1 _Chem_shift_reference.Sf_category chem_shift_reference _Chem_shift_reference.Sf_framecode chem_shift_reference_1 _Chem_shift_reference.Entry_ID 31032 _Chem_shift_reference.ID 1 _Chem_shift_reference.Name . _Chem_shift_reference.Details ; Spectra were referenced to DSS methyl protons at 0.00ppm, this also reproducibly placed the water residual resonance at approximately 4.78 ppm. ; 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 H 1 DSS 'methyl protons' . . . . ppm 0.000 internal direct 1.0 . . . . . 31032 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_chemical_shifts_1 _Assigned_chem_shift_list.Sf_category assigned_chemical_shifts _Assigned_chem_shift_list.Sf_framecode assigned_chemical_shifts_1 _Assigned_chem_shift_list.Entry_ID 31032 _Assigned_chem_shift_list.ID 1 _Assigned_chem_shift_list.Name . _Assigned_chem_shift_list.Sample_condition_list_ID 1 _Assigned_chem_shift_list.Sample_condition_list_label $sample_conditions_1 _Assigned_chem_shift_list.Chem_shift_reference_ID 1 _Assigned_chem_shift_list.Chem_shift_reference_label $chem_shift_reference_1 _Assigned_chem_shift_list.Chem_shift_1H_err 0.01 _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 '1H 1D NMR Spectrum' . . . 31032 1 2 '2D 1H-1H COSY' . . . 31032 1 3 '2D 1H-1H TOCSY' . . . 31032 1 4 '2D 1H-1H ROESY' . . . 31032 1 stop_ loop_ _Atom_chem_shift.ID _Atom_chem_shift.Assembly_atom_ID _Atom_chem_shift.Entity_assembly_ID _Atom_chem_shift.Entity_assembly_asym_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.Ambiguity_set_ID _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 GLY HA2 H 1 3.79 0.01 . 2 . . . . A 1 GLY HA2 . 31032 1 2 . 1 . 1 1 1 GLY HA3 H 1 3.79 0.01 . 2 . . . . A 1 GLY HA3 . 31032 1 3 . 1 . 1 2 2 TRP H H 1 8.54 0.01 . 1 . . . . A 2 TRP H . 31032 1 4 . 1 . 1 2 2 TRP HA H 1 4.74 0.01 . 1 . . . . A 2 TRP HA . 31032 1 5 . 1 . 1 2 2 TRP HB2 H 1 3.27 0.01 . 1 . . . . A 2 TRP HB2 . 31032 1 6 . 1 . 1 2 2 TRP HB3 H 1 3.22 0.01 . 1 . . . . A 2 TRP HB3 . 31032 1 7 . 1 . 1 2 2 TRP HD1 H 1 7.24 0.01 . 1 . . . . A 2 TRP HD1 . 31032 1 8 . 1 . 1 2 2 TRP HE1 H 1 10.01 0.01 . 1 . . . . A 2 TRP HE1 . 31032 1 9 . 1 . 1 2 2 TRP HE3 H 1 7.59 0.01 . 1 . . . . A 2 TRP HE3 . 31032 1 10 . 1 . 1 2 2 TRP HZ2 H 1 7.47 0.01 . 1 . . . . A 2 TRP HZ2 . 31032 1 11 . 1 . 1 2 2 TRP HZ3 H 1 7.13 0.01 . 1 . . . . A 2 TRP HZ3 . 31032 1 12 . 1 . 1 2 2 TRP HH2 H 1 7.21 0.01 . 1 . . . . A 2 TRP HH2 . 31032 1 13 . 1 . 1 3 3 THR H H 1 8.01 0.01 . 1 . . . . A 3 THR H . 31032 1 14 . 1 . 1 3 3 THR HA H 1 4.24 0.01 . 1 . . . . A 3 THR HA . 31032 1 15 . 1 . 1 3 3 THR HB H 1 4.08 0.01 . 1 . . . . A 3 THR HB . 31032 1 16 . 1 . 1 3 3 THR HG21 H 1 1.09 0.01 . 1 . . . . A 3 THR HG21 . 31032 1 17 . 1 . 1 3 3 THR HG22 H 1 1.09 0.01 . 1 . . . . A 3 THR HG22 . 31032 1 18 . 1 . 1 3 3 THR HG23 H 1 1.09 0.01 . 1 . . . . A 3 THR HG23 . 31032 1 19 . 1 . 1 4 4 LEU H H 1 8.15 0.01 . 1 . . . . A 4 LEU H . 31032 1 20 . 1 . 1 4 4 LEU HA H 1 4.15 0.01 . 1 . . . . A 4 LEU HA . 31032 1 21 . 1 . 1 4 4 LEU HB2 H 1 1.55 0.01 . 4 . . . . A 4 LEU HB2 . 31032 1 22 . 1 . 1 4 4 LEU HB3 H 1 1.55 0.01 . 4 . . . . A 4 LEU HB3 . 31032 1 23 . 1 . 1 4 4 LEU HG H 1 1.55 0.01 . 4 . . . . A 4 LEU HG . 31032 1 24 . 1 . 1 4 4 LEU HD11 H 1 0.87 0.01 . 1 . . . . A 4 LEU HD11 . 31032 1 25 . 1 . 1 4 4 LEU HD12 H 1 0.87 0.01 . 1 . . . . A 4 LEU HD12 . 31032 1 26 . 1 . 1 4 4 LEU HD13 H 1 0.87 0.01 . 1 . . . . A 4 LEU HD13 . 31032 1 27 . 1 . 1 4 4 LEU HD21 H 1 0.91 0.01 . 1 . . . . A 4 LEU HD21 . 31032 1 28 . 1 . 1 4 4 LEU HD22 H 1 0.91 0.01 . 1 . . . . A 4 LEU HD22 . 31032 1 29 . 1 . 1 4 4 LEU HD23 H 1 0.91 0.01 . 1 . . . . A 4 LEU HD23 . 31032 1 30 . 1 . 1 5 5 ASN H H 1 8.37 0.01 . 1 . . . . A 5 ASN H . 31032 1 31 . 1 . 1 5 5 ASN HA H 1 4.66 0.01 . 1 . . . . A 5 ASN HA . 31032 1 32 . 1 . 1 5 5 ASN HB2 H 1 2.84 0.01 . 1 . . . . A 5 ASN HB2 . 31032 1 33 . 1 . 1 5 5 ASN HB3 H 1 2.78 0.01 . 1 . . . . A 5 ASN HB3 . 31032 1 34 . 1 . 1 5 5 ASN HD21 H 1 6.91 0.01 . 1 . . . . A 5 ASN HD21 . 31032 1 35 . 1 . 1 5 5 ASN HD22 H 1 7.63 0.01 . 1 . . . . A 5 ASN HD22 . 31032 1 36 . 1 . 1 6 6 SER H H 1 8.20 0.01 . 1 . . . . A 6 SER H . 31032 1 37 . 1 . 1 6 6 SER HA H 1 4.40 0.01 . 1 . . . . A 6 SER HA . 31032 1 38 . 1 . 1 6 6 SER HB2 H 1 3.85 0.01 . 2 . . . . A 6 SER HB2 . 31032 1 39 . 1 . 1 6 6 SER HB3 H 1 3.85 0.01 . 2 . . . . A 6 SER HB3 . 31032 1 40 . 1 . 1 7 7 ALA H H 1 8.27 0.01 . 1 . . . . A 7 ALA H . 31032 1 41 . 1 . 1 7 7 ALA HA H 1 4.28 0.01 . 1 . . . . A 7 ALA HA . 31032 1 42 . 1 . 1 7 7 ALA HB1 H 1 1.37 0.01 . 1 . . . . A 7 ALA HB1 . 31032 1 43 . 1 . 1 7 7 ALA HB2 H 1 1.37 0.01 . 1 . . . . A 7 ALA HB2 . 31032 1 44 . 1 . 1 7 7 ALA HB3 H 1 1.37 0.01 . 1 . . . . A 7 ALA HB3 . 31032 1 45 . 1 . 1 8 8 GLY H H 1 8.21 0.01 . 1 . . . . A 8 GLY H . 31032 1 46 . 1 . 1 8 8 GLY HA2 H 1 3.82 0.01 . 2 . . . . A 8 GLY HA2 . 31032 1 47 . 1 . 1 8 8 GLY HA3 H 1 3.82 0.01 . 2 . . . . A 8 GLY HA3 . 31032 1 48 . 1 . 1 9 9 TYR H H 1 7.86 0.01 . 1 . . . . A 9 TYR H . 31032 1 49 . 1 . 1 9 9 TYR HA H 1 4.51 0.01 . 1 . . . . A 9 TYR HA . 31032 1 50 . 1 . 1 9 9 TYR HB2 H 1 2.99 0.01 . 2 . . . . A 9 TYR HB2 . 31032 1 51 . 1 . 1 9 9 TYR HB3 H 1 2.99 0.01 . 2 . . . . A 9 TYR HB3 . 31032 1 52 . 1 . 1 9 9 TYR HD1 H 1 7.08 0.01 . 3 . . . . A 9 TYR HD1 . 31032 1 53 . 1 . 1 9 9 TYR HD2 H 1 7.08 0.01 . 3 . . . . A 9 TYR HD2 . 31032 1 54 . 1 . 1 9 9 TYR HE1 H 1 6.79 0.01 . 3 . . . . A 9 TYR HE1 . 31032 1 55 . 1 . 1 9 9 TYR HE2 H 1 6.79 0.01 . 3 . . . . A 9 TYR HE2 . 31032 1 56 . 1 . 1 10 10 LEU H H 1 8.06 0.01 . 1 . . . . A 10 LEU H . 31032 1 57 . 1 . 1 10 10 LEU HA H 1 4.26 0.01 . 1 . . . . A 10 LEU HA . 31032 1 58 . 1 . 1 10 10 LEU HB2 H 1 1.51 0.01 . 2 . . . . A 10 LEU HB2 . 31032 1 59 . 1 . 1 10 10 LEU HB3 H 1 1.51 0.01 . 2 . . . . A 10 LEU HB3 . 31032 1 60 . 1 . 1 10 10 LEU HG H 1 1.44 0.01 . 1 . . . . A 10 LEU HG . 31032 1 61 . 1 . 1 10 10 LEU HD11 H 1 0.81 0.01 . 1 . . . . A 10 LEU HD11 . 31032 1 62 . 1 . 1 10 10 LEU HD12 H 1 0.81 0.01 . 1 . . . . A 10 LEU HD12 . 31032 1 63 . 1 . 1 10 10 LEU HD13 H 1 0.81 0.01 . 1 . . . . A 10 LEU HD13 . 31032 1 64 . 1 . 1 10 10 LEU HD21 H 1 0.86 0.01 . 1 . . . . A 10 LEU HD21 . 31032 1 65 . 1 . 1 10 10 LEU HD22 H 1 0.86 0.01 . 1 . . . . A 10 LEU HD22 . 31032 1 66 . 1 . 1 10 10 LEU HD23 H 1 0.86 0.01 . 1 . . . . A 10 LEU HD23 . 31032 1 67 . 1 . 1 11 11 LEU H H 1 7.94 0.01 . 1 . . . . A 11 LEU H . 31032 1 68 . 1 . 1 11 11 LEU HA H 1 4.38 0.01 . 1 . . . . A 11 LEU HA . 31032 1 69 . 1 . 1 11 11 LEU HB2 H 1 1.60 0.01 . 4 . . . . A 11 LEU HB2 . 31032 1 70 . 1 . 1 11 11 LEU HB3 H 1 1.60 0.01 . 4 . . . . A 11 LEU HB3 . 31032 1 71 . 1 . 1 11 11 LEU HG H 1 1.60 0.01 . 4 . . . . A 11 LEU HG . 31032 1 72 . 1 . 1 11 11 LEU HD11 H 1 0.86 0.01 . 1 . . . . A 11 LEU HD11 . 31032 1 73 . 1 . 1 11 11 LEU HD12 H 1 0.86 0.01 . 1 . . . . A 11 LEU HD12 . 31032 1 74 . 1 . 1 11 11 LEU HD13 H 1 0.86 0.01 . 1 . . . . A 11 LEU HD13 . 31032 1 75 . 1 . 1 11 11 LEU HD21 H 1 0.91 0.01 . 1 . . . . A 11 LEU HD21 . 31032 1 76 . 1 . 1 11 11 LEU HD22 H 1 0.91 0.01 . 1 . . . . A 11 LEU HD22 . 31032 1 77 . 1 . 1 11 11 LEU HD23 H 1 0.91 0.01 . 1 . . . . A 11 LEU HD23 . 31032 1 78 . 1 . 1 12 12 GLY H H 1 8.08 0.01 . 1 . . . . A 12 GLY H . 31032 1 79 . 1 . 1 12 12 GLY HA2 H 1 4.04 0.01 . 2 . . . . A 12 GLY HA2 . 31032 1 80 . 1 . 1 12 12 GLY HA3 H 1 4.04 0.01 . 2 . . . . A 12 GLY HA3 . 31032 1 81 . 1 . 1 13 13 PRO HA H 1 4.34 0.01 . 1 . . . . A 13 PRO HA . 31032 1 82 . 1 . 1 13 13 PRO HB2 H 1 2.20 0.01 . 1 . . . . A 13 PRO HB2 . 31032 1 83 . 1 . 1 13 13 PRO HB3 H 1 1.77 0.01 . 1 . . . . A 13 PRO HB3 . 31032 1 84 . 1 . 1 13 13 PRO HG2 H 1 1.97 0.01 . 1 . . . . A 13 PRO HG2 . 31032 1 85 . 1 . 1 13 13 PRO HG3 H 1 1.87 0.01 . 1 . . . . A 13 PRO HG3 . 31032 1 86 . 1 . 1 13 13 PRO HD2 H 1 3.57 0.01 . 2 . . . . A 13 PRO HD2 . 31032 1 87 . 1 . 1 13 13 PRO HD3 H 1 3.57 0.01 . 2 . . . . A 13 PRO HD3 . 31032 1 88 . 1 . 1 14 14 HIS H H 1 8.54 0.01 . 1 . . . . A 14 HIS H . 31032 1 89 . 1 . 1 14 14 HIS HA H 1 4.68 0.01 . 1 . . . . A 14 HIS HA . 31032 1 90 . 1 . 1 14 14 HIS HB2 H 1 3.27 0.01 . 1 . . . . A 14 HIS HB2 . 31032 1 91 . 1 . 1 14 14 HIS HB3 H 1 3.14 0.01 . 1 . . . . A 14 HIS HB3 . 31032 1 92 . 1 . 1 14 14 HIS HD2 H 1 7.25 0.01 . 1 . . . . A 14 HIS HD2 . 31032 1 93 . 1 . 1 14 14 HIS HE1 H 1 8.53 0.01 . 1 . . . . A 14 HIS HE1 . 31032 1 94 . 1 . 1 15 15 ALA H H 1 8.13 0.01 . 1 . . . . A 15 ALA H . 31032 1 95 . 1 . 1 15 15 ALA HA H 1 4.32 0.01 . 1 . . . . A 15 ALA HA . 31032 1 96 . 1 . 1 15 15 ALA HB1 H 1 1.35 0.01 . 1 . . . . A 15 ALA HB1 . 31032 1 97 . 1 . 1 15 15 ALA HB2 H 1 1.35 0.01 . 1 . . . . A 15 ALA HB2 . 31032 1 98 . 1 . 1 15 15 ALA HB3 H 1 1.35 0.01 . 1 . . . . A 15 ALA HB3 . 31032 1 99 . 1 . 1 16 16 VAL H H 1 8.19 0.01 . 1 . . . . A 16 VAL H . 31032 1 100 . 1 . 1 16 16 VAL HA H 1 4.13 0.01 . 1 . . . . A 16 VAL HA . 31032 1 101 . 1 . 1 16 16 VAL HB H 1 2.08 0.01 . 1 . . . . A 16 VAL HB . 31032 1 102 . 1 . 1 16 16 VAL HG11 H 1 0.94 0.01 . 2 . . . . A 16 VAL HG11 . 31032 1 103 . 1 . 1 16 16 VAL HG12 H 1 0.94 0.01 . 2 . . . . A 16 VAL HG12 . 31032 1 104 . 1 . 1 16 16 VAL HG13 H 1 0.94 0.01 . 2 . . . . A 16 VAL HG13 . 31032 1 105 . 1 . 1 16 16 VAL HG21 H 1 0.94 0.01 . 2 . . . . A 16 VAL HG21 . 31032 1 106 . 1 . 1 16 16 VAL HG22 H 1 0.94 0.01 . 2 . . . . A 16 VAL HG22 . 31032 1 107 . 1 . 1 16 16 VAL HG23 H 1 0.94 0.01 . 2 . . . . A 16 VAL HG23 . 31032 1 108 . 1 . 1 17 17 GLY H H 1 8.44 0.01 . 1 . . . . A 17 GLY H . 31032 1 109 . 1 . 1 17 17 GLY HA2 H 1 3.93 0.01 . 2 . . . . A 17 GLY HA2 . 31032 1 110 . 1 . 1 17 17 GLY HA3 H 1 3.93 0.01 . 2 . . . . A 17 GLY HA3 . 31032 1 111 . 1 . 1 18 18 ASN H H 1 8.29 0.01 . 1 . . . . A 18 ASN H . 31032 1 112 . 1 . 1 18 18 ASN HA H 1 4.65 0.01 . 1 . . . . A 18 ASN HA . 31032 1 113 . 1 . 1 18 18 ASN HB2 H 1 2.74 0.01 . 2 . . . . A 18 ASN HB2 . 31032 1 114 . 1 . 1 18 18 ASN HB3 H 1 2.74 0.01 . 2 . . . . A 18 ASN HB3 . 31032 1 115 . 1 . 1 18 18 ASN HD21 H 1 6.89 0.01 . 1 . . . . A 18 ASN HD21 . 31032 1 116 . 1 . 1 18 18 ASN HD22 H 1 7.56 0.01 . 1 . . . . A 18 ASN HD22 . 31032 1 117 . 1 . 1 19 19 HIS H H 1 8.51 0.01 . 1 . . . . A 19 HIS H . 31032 1 118 . 1 . 1 19 19 HIS HA H 1 4.66 0.01 . 1 . . . . A 19 HIS HA . 31032 1 119 . 1 . 1 19 19 HIS HB2 H 1 3.26 0.01 . 1 . . . . A 19 HIS HB2 . 31032 1 120 . 1 . 1 19 19 HIS HB3 H 1 3.16 0.01 . 1 . . . . A 19 HIS HB3 . 31032 1 121 . 1 . 1 19 19 HIS HD2 H 1 7.23 0.01 . 1 . . . . A 19 HIS HD2 . 31032 1 122 . 1 . 1 19 19 HIS HE1 H 1 8.52 0.01 . 1 . . . . A 19 HIS HE1 . 31032 1 123 . 1 . 1 20 20 ARG H H 1 8.34 0.01 . 1 . . . . A 20 ARG H . 31032 1 124 . 1 . 1 20 20 ARG HA H 1 4.32 0.01 . 1 . . . . A 20 ARG HA . 31032 1 125 . 1 . 1 20 20 ARG HB2 H 1 1.75 0.01 . 1 . . . . A 20 ARG HB2 . 31032 1 126 . 1 . 1 20 20 ARG HB3 H 1 1.70 0.01 . 1 . . . . A 20 ARG HB3 . 31032 1 127 . 1 . 1 20 20 ARG HG2 H 1 1.54 0.01 . 2 . . . . A 20 ARG HG2 . 31032 1 128 . 1 . 1 20 20 ARG HG3 H 1 1.54 0.01 . 2 . . . . A 20 ARG HG3 . 31032 1 129 . 1 . 1 20 20 ARG HD2 H 1 3.14 0.01 . 2 . . . . A 20 ARG HD2 . 31032 1 130 . 1 . 1 20 20 ARG HD3 H 1 3.14 0.01 . 2 . . . . A 20 ARG HD3 . 31032 1 131 . 1 . 1 20 20 ARG HE H 1 7.14 0.01 . 1 . . . . A 20 ARG HE . 31032 1 132 . 1 . 1 21 21 SER H H 1 8.40 0.01 . 1 . . . . A 21 SER H . 31032 1 133 . 1 . 1 21 21 SER HA H 1 4.43 0.01 . 1 . . . . A 21 SER HA . 31032 1 134 . 1 . 1 21 21 SER HB2 H 1 3.81 0.01 . 2 . . . . A 21 SER HB2 . 31032 1 135 . 1 . 1 21 21 SER HB3 H 1 3.81 0.01 . 2 . . . . A 21 SER HB3 . 31032 1 136 . 1 . 1 22 22 PHE H H 1 8.36 0.01 . 1 . . . . A 22 PHE H . 31032 1 137 . 1 . 1 22 22 PHE HA H 1 4.64 0.01 . 1 . . . . A 22 PHE HA . 31032 1 138 . 1 . 1 22 22 PHE HB2 H 1 3.15 0.01 . 1 . . . . A 22 PHE HB2 . 31032 1 139 . 1 . 1 22 22 PHE HB3 H 1 3.03 0.01 . 1 . . . . A 22 PHE HB3 . 31032 1 140 . 1 . 1 22 22 PHE HD1 H 1 7.24 0.01 . 3 . . . . A 22 PHE HD1 . 31032 1 141 . 1 . 1 22 22 PHE HD2 H 1 7.24 0.01 . 3 . . . . A 22 PHE HD2 . 31032 1 142 . 1 . 1 22 22 PHE HE1 H 1 7.33 0.01 . 3 . . . . A 22 PHE HE1 . 31032 1 143 . 1 . 1 22 22 PHE HE2 H 1 7.33 0.01 . 3 . . . . A 22 PHE HE2 . 31032 1 144 . 1 . 1 22 22 PHE HZ H 1 7.27 0.01 . 1 . . . . A 22 PHE HZ . 31032 1 145 . 1 . 1 23 23 SER H H 1 8.20 0.01 . 1 . . . . A 23 SER H . 31032 1 146 . 1 . 1 23 23 SER HA H 1 4.41 0.01 . 1 . . . . A 23 SER HA . 31032 1 147 . 1 . 1 23 23 SER HB2 H 1 3.84 0.01 . 2 . . . . A 23 SER HB2 . 31032 1 148 . 1 . 1 23 23 SER HB3 H 1 3.84 0.01 . 2 . . . . A 23 SER HB3 . 31032 1 149 . 1 . 1 24 24 ASP H H 1 8.25 0.01 . 1 . . . . A 24 ASP H . 31032 1 150 . 1 . 1 24 24 ASP HA H 1 4.57 0.01 . 1 . . . . A 24 ASP HA . 31032 1 151 . 1 . 1 24 24 ASP HB2 H 1 2.71 0.01 . 2 . . . . A 24 ASP HB2 . 31032 1 152 . 1 . 1 24 24 ASP HB3 H 1 2.71 0.01 . 2 . . . . A 24 ASP HB3 . 31032 1 153 . 1 . 1 25 25 LYS H H 1 8.29 0.01 . 1 . . . . A 25 LYS H . 31032 1 154 . 1 . 1 25 25 LYS HA H 1 4.28 0.01 . 1 . . . . A 25 LYS HA . 31032 1 155 . 1 . 1 25 25 LYS HB2 H 1 1.85 0.01 . 1 . . . . A 25 LYS HB2 . 31032 1 156 . 1 . 1 25 25 LYS HB3 H 1 1.76 0.01 . 1 . . . . A 25 LYS HB3 . 31032 1 157 . 1 . 1 25 25 LYS HG2 H 1 1.41 0.01 . 2 . . . . A 25 LYS HG2 . 31032 1 158 . 1 . 1 25 25 LYS HG3 H 1 1.41 0.01 . 2 . . . . A 25 LYS HG3 . 31032 1 159 . 1 . 1 25 25 LYS HD2 H 1 1.66 0.01 . 2 . . . . A 25 LYS HD2 . 31032 1 160 . 1 . 1 25 25 LYS HD3 H 1 1.66 0.01 . 2 . . . . A 25 LYS HD3 . 31032 1 161 . 1 . 1 25 25 LYS HE2 H 1 2.97 0.01 . 2 . . . . A 25 LYS HE2 . 31032 1 162 . 1 . 1 25 25 LYS HE3 H 1 2.97 0.01 . 2 . . . . A 25 LYS HE3 . 31032 1 163 . 1 . 1 26 26 ASN H H 1 8.38 0.01 . 1 . . . . A 26 ASN H . 31032 1 164 . 1 . 1 26 26 ASN HA H 1 4.68 0.01 . 1 . . . . A 26 ASN HA . 31032 1 165 . 1 . 1 26 26 ASN HB2 H 1 2.82 0.01 . 2 . . . . A 26 ASN HB2 . 31032 1 166 . 1 . 1 26 26 ASN HB3 H 1 2.82 0.01 . 2 . . . . A 26 ASN HB3 . 31032 1 167 . 1 . 1 26 26 ASN HD21 H 1 6.89 0.01 . 1 . . . . A 26 ASN HD21 . 31032 1 168 . 1 . 1 26 26 ASN HD22 H 1 7.56 0.01 . 1 . . . . A 26 ASN HD22 . 31032 1 169 . 1 . 1 27 27 GLY H H 1 8.29 0.01 . 1 . . . . A 27 GLY H . 31032 1 170 . 1 . 1 27 27 GLY HA2 H 1 3.94 0.01 . 2 . . . . A 27 GLY HA2 . 31032 1 171 . 1 . 1 27 27 GLY HA3 H 1 3.94 0.01 . 2 . . . . A 27 GLY HA3 . 31032 1 172 . 1 . 1 28 28 LEU H H 1 8.14 0.01 . 1 . . . . A 28 LEU H . 31032 1 173 . 1 . 1 28 28 LEU HA H 1 4.41 0.01 . 1 . . . . A 28 LEU HA . 31032 1 174 . 1 . 1 28 28 LEU HB2 H 1 1.62 0.01 . 4 . . . . A 28 LEU HB2 . 31032 1 175 . 1 . 1 28 28 LEU HB3 H 1 1.62 0.01 . 4 . . . . A 28 LEU HB3 . 31032 1 176 . 1 . 1 28 28 LEU HG H 1 1.62 0.01 . 4 . . . . A 28 LEU HG . 31032 1 177 . 1 . 1 28 28 LEU HD11 H 1 0.87 0.01 . 1 . . . . A 28 LEU HD11 . 31032 1 178 . 1 . 1 28 28 LEU HD12 H 1 0.87 0.01 . 1 . . . . A 28 LEU HD12 . 31032 1 179 . 1 . 1 28 28 LEU HD13 H 1 0.87 0.01 . 1 . . . . A 28 LEU HD13 . 31032 1 180 . 1 . 1 28 28 LEU HD21 H 1 0.92 0.01 . 1 . . . . A 28 LEU HD21 . 31032 1 181 . 1 . 1 28 28 LEU HD22 H 1 0.92 0.01 . 1 . . . . A 28 LEU HD22 . 31032 1 182 . 1 . 1 28 28 LEU HD23 H 1 0.92 0.01 . 1 . . . . A 28 LEU HD23 . 31032 1 183 . 1 . 1 29 29 THR H H 1 8.19 0.01 . 1 . . . . A 29 THR H . 31032 1 184 . 1 . 1 29 29 THR HA H 1 4.41 0.01 . 1 . . . . A 29 THR HA . 31032 1 185 . 1 . 1 29 29 THR HB H 1 4.28 0.01 . 1 . . . . A 29 THR HB . 31032 1 186 . 1 . 1 29 29 THR HG21 H 1 1.20 0.01 . 1 . . . . A 29 THR HG21 . 31032 1 187 . 1 . 1 29 29 THR HG22 H 1 1.20 0.01 . 1 . . . . A 29 THR HG22 . 31032 1 188 . 1 . 1 29 29 THR HG23 H 1 1.20 0.01 . 1 . . . . A 29 THR HG23 . 31032 1 189 . 1 . 1 30 30 SER H H 1 8.20 0.01 . 1 . . . . A 30 SER H . 31032 1 190 . 1 . 1 30 30 SER HA H 1 4.33 0.01 . 1 . . . . A 30 SER HA . 31032 1 191 . 1 . 1 30 30 SER HB2 H 1 3.83 0.01 . 2 . . . . A 30 SER HB2 . 31032 1 192 . 1 . 1 30 30 SER HB3 H 1 3.83 0.01 . 2 . . . . A 30 SER HB3 . 31032 1 193 . 1 . 1 31 31 NH2 HN1 H 1 7.58 0.01 . 1 . . . . A 31 NH2 HN1 . 31032 1 194 . 1 . 1 31 31 NH2 HN2 H 1 7.16 0.01 . 1 . . . . A 31 NH2 HN2 . 31032 1 stop_ save_ ######################### # Spectral peak lists # ######################### save_spectral_peak_list_1 _Spectral_peak_list.Sf_category spectral_peak_list _Spectral_peak_list.Sf_framecode spectral_peak_list_1 _Spectral_peak_list.Entry_ID 31032 _Spectral_peak_list.ID 1 _Spectral_peak_list.Name . _Spectral_peak_list.Sample_ID 1 _Spectral_peak_list.Sample_label $sample_1 _Spectral_peak_list.Sample_condition_list_ID 1 _Spectral_peak_list.Sample_condition_list_label $sample_conditions_1 _Spectral_peak_list.Chem_shift_reference_ID 1 _Spectral_peak_list.Chem_shift_reference_label $chem_shift_reference_1 _Spectral_peak_list.Experiment_ID 3 _Spectral_peak_list.Experiment_name '2D 1H-1H TOCSY' _Spectral_peak_list.Experiment_class . _Spectral_peak_list.Experiment_type . _Spectral_peak_list.Number_of_spectral_dimensions 2 _Spectral_peak_list.Chemical_shift_list . _Spectral_peak_list.Assigned_chem_shift_list_ID 1 _Spectral_peak_list.Assigned_chem_shift_list_label $assigned_chemical_shifts_1 _Spectral_peak_list.Details ; Chemical shifts were measured from chosen TOCSY peaks, assigned from an overlay of 1H-1H 2D COSY, TOCSY, and ROESY spectra using sequential procedures. The TOCSY peaks gave the most accurate shift measurements. ; _Spectral_peak_list.Text_data_format text _Spectral_peak_list.Text_data ; Notes on peak picking and annotation: "1) Chemical shifts were calculated only from non-ROE peaks, using TOCSY maxima and in cases of overlap, the centerpoint of a phase-sensitve COSY crosspeak" "2) Diastereotopic protons and methyl groups were annotate such that the more upfield of the pair was labeled 1 and the more downfield labeled 2.E If superimposed and not resolvable in the f2 dimension, then the group was labeled 12.E e.g. For leucine methyl groups, resolved: HD1 and HD2.E For leucine beta protons, not resolved - HB12." 3) Peaks that were solely chosen from the ROESY spectrum are indicated with (ROE) in parentheses.E No ROE peaks that also included a TOCSY peak were used to generate the NMR ensemble or any of the associated restraints.E f2 (ppm) f1 (ppm) Annotation 1 10.09 7.47 Trp(2)NH1-H7 (ROE) 2 10.09 7.24 Trp(2)NH1-H2 3 10.09 8.21 unassigned 4 8.55 3.79 Trp(2)HN-Gly(1)HA12 (ROE) 5 8.54 3.25 Trp(2)HN-HB12 6 8.54 4.74 Trp(2)HN-HA 7 8.54 4.34 His(14)HN-Pro(13)HA (ROE) 8 8.54 4.7 HIs(14)HN-HA 9 8.54 3.13 His(14)HN-HB1 10 8.54 3.28 His(14)HN-HB2 11 8.54 3.57 His(14)HN-Pro(13)HD12 (ROE) 12 8.54 1.78 His(14)HN-Pro(13)HB1 (ROE) 13 8.53 7.25 His(14)H2-H4 14 8.52 7.24 His(19)H2-H4 15 8.51 4.66 His(19)HN-HA 16 8.51 3.16 His(19)HN-HB1 17 8.51 2.75 His(19)HN-Asn(18)HB12 (ROE) 18 8.51 3.25 His(19)HN-HB2 19 8.46 1.34 Gly(17)HN-Ala(15)HB (ROE) 20 8.45 4.12 Gly(17)HN-Val(16)HA (ROE) 21 8.45 3.92 Gly(17)HN-HA12 22 8.45 0.94 Gly(17HN)-Val(16)HG12 (ROE) 23 8.45 2.09 Gly(17)HN-Val(16)HB (ROE) 24 8.4 3.8 Ser(21)HN-HB 25 8.4 1.54 Ser(21)HN-Arg(20)HG12 (ROE) 26 8.4 3.15 Ser(21)HN-Arg(20)HD12 (ROE) 27 8.4 1.74 Ser(21)HN-Arg(20)HB12 (ROE) 28 8.4 4.32 Ser(21)HN-Arg(20)HA (ROE) 29 8.4 4.44 Ser(21)HN-HA 30 8.38 4.68 Asn(26)HN-HA 31 8.38 2.81 Asn(26)HN-HB12 32 8.36 0.9 Asn(5)HN-Leu(4)HD12 (ROE) 33 8.36 7.24 Asn(5)HN-Trp(2)H2 (ROE) 34 8.36 4.44 Phe(22)HN-Ser(21)HA (ROE) 35 8.36 4.66 Asn(5)HN-HA 36 8.36 4.16 Asn(5)HN-Leu(4)HA (ROE) 37 8.36 3.81 Phe(22)HN-Ser(21)HB 38 8.36 4.65 Phe(22)HN-HA 39 8.36 2.79 Asn(5)HN-HB12 40 8.36 3.03 Phe(22)HN-HB1 41 8.36 3.15 Phe(22)HN-HB2 42 8.34 4.32 Arg(20)NH-HA 43 8.34 4.63 Arg(20)NH-His(19)HA (ROE) 44 8.34 1.72 Arg(20)NH-HB12 45 8.34 1.54 Arg(20)NH-HG12 46 8.34 3.15 Arg(20)NH-HD12 47 8.29 4.64 Asn(18)HN-HA 48 8.29 4.58 Lys(25)HN-Asp(24)HA (ROE) 49 8.29 1.81 Lys(25)HN-HB12 50 8.29 2.73 Asn(18)HN-HB12 51 8.29 3.94 Gly(27)HN-HA12 52 8.29 1.67 Lys(25)HN-HD12 53 8.29 1.4 Lys(25)HN-HG12 54 8.29 4.27 Lys(25)HN-HA 55 8.28 2.99 Lys(25)HN-HE12 56 8.27 0.94 Gly(17)HN-Val(16)HG12 (ROE) 57 8.27 2.09 Val(16)HB-Asn(18)HN (ROE) 58 8.27 4.28 Ala(7)HN-HA 59 8.26 1.37 Ala(7)HN-HB 60 8.26 3.15 unassigned 61 8.26 3.03 unassigned 62 8.24 2.72 Asp(24)HN-HB12 63 8.24 4.58 Asp(24)HN-HA 64 8.21 7.85 Gly(8)HN-Tyr(9)HN (ROE) 65 8.21 3.81 Gly(8)HN-HA12 66 8.21 2.77 Asn(5)HB12-Ser(6)HN (ROE) 67 8.2 3.85 Ser(6)/ (30)HN-HB 68 8.2 4.4 Ser(6)HN-HA 69 8.2 4.63 Ser(23)HN-Phe(22)HA (ROE) 70 8.2 4.39 Ser(23)HN-HA 71 8.2 3.84 Ser(23)HN-HB 72 8.2 3.15 Ser(23)HN-Phe(22)HB2 (ROE) 73 8.2 3.03 Ser(23)HN-Phe(22)HB1 (ROE) 74 8.2 1.2 Thr(29)HN-HG 75 8.2 1.36 Ser(6)HN-Ala(7)HB or Val(16)HN to Ala(15)HB (ROE) 76 8.2 7.58 Val(16)HN-Asn(18)NH2 (ROE) 77 8.2 10.09 unassigned 78 8.19 4.29 Thr(29)HN-HB 79 8.19 4.41 Thr(29)HN-HA 80 8.19 3.26 Val(16)HN-His(14)HB2 (ROE) 81 8.19 2.09 Val(16)HN-HB 82 8.19 0.94 Val(16)HN-HG12 83 8.18 4.13 Val(16)HN-HA 84 8.15 4.14 Leu(4)HN-HA 85 8.15 4.24 Leu(4)HN-Thr(3)HA (ROE) 86 8.15 1.57 Leu(4)HN-HB12/ HG 87 8.15 0.89 Leu(4)HN-HD12 88 8.15 1.1 Leu(4)HN-Thr(3)HG (ROE) 89 8.14 2.78 Leu(4)HN-Asn(5)HB12 (ROE) 90 8.14 3.93 Leu(28)HN-Gly(27)HA12 (ROE) 91 8.14 0.9 Leu(28)HN-HD12 92 8.14 1.6 Leu(28)HN-HB12/ HG 93 8.14 4.32 Ala(15)HN-HA 94 8.14 4.4 Leu(28)HN-HA 95 8.13 3.12 Ala(15)HN-His(14)HB1 (ROE) 96 8.13 1.35 Ala(15)HN-HB 97 8.13 4.67 Ala(15)HN-His(14)HA (ROE) 98 8.13 3.26 Ala(15)HN-His(14)HB2 (ROE) 99 8.08 4.37 Gly(12)HN-Leu(11)HA (ROE) 100 8.08 3.54 Gly(12)HN-Pro(13)HD12 (ROE) 101 8.07 4.04 Gly(12)HN-HA12 102 8.06 2.99 Leu(10)HN-Tyr(9)HB12 (ROE) 103 8.06 4.25 Leu(10)HN-HA 104 8.06 4.5 Leu(10)HN-Tyr(9)HA (ROE) 105 8.06 3.84 Leu(10)HN-Gly(8)HA12 (ROE) 106 8.06 0.85 Leu(10)HN-HD12 107 8.06 1.53 Leu(10)HN-HB12/ HG 108 8.01 4.68 Thr(3)HN-Trp(2)HA (ROE) 109 8.01 4.08 Thr(3)HN-HB 110 8.01 3.25 Thr(3)HN-Trp(2)HB12 (ROE) 111 8.01 4.24 Thr(3)HN-HA 112 8.01 1.1 Thr(3)HN-HG 113 8.01 3.81 Thr(3)HN-Gly(8)HA12 (ROE) 114 7.94 4.37 Leu(11)HN-HA 115 7.94 4.25 Leu(11)HN-Leu(10)HA (ROE) 116 7.94 4.08 Leu(11)HN-Thr(3)HB (ROE) 117 7.94 1.61 Leu(11)HN-HB12/ HG 118 7.94 1.5 Leu(11)HN-Leu(10)HB12/ HG (ROE) 119 7.94 0.87 Leu(11)HN_HD12 120 7.94 3.83 Leu(11)HN-Gly(8)HA12 (ROE) 121 7.94 3 Leu(11)HN-Tyr(9)HB12 (ROE) 122 7.86 4.29 Tyr(9)HN-Ala(7)HA (ROE) 123 7.86 8.21 Tyr(9)HN-Gly(8)HN (ROE) 124 7.86 1.38 Tyr(9)HN-Ala(7)HB (ROE) 125 7.86 2.98 Tyr(9)HN-HB12 126 7.86 4.51 Tyr(9)HN-HA 127 7.86 3.83 Tyr(9)HN-Gly(8)HA12 (ROE) 128 7.86 7.07 Tyr(9)H26-HN (intraROE) 129 7.64 2.8 Asn(5)NH2-HB12 (intraROE) 130 7.64 4.42 Asn(5)HN2-Ser(6)HA (ROE) 131 7.64 6.91 Asn(5)NH2-NH1 132 7.59 4.07 Trp(2)H4-Thr(3)HB (ROE) 133 7.59 7.46 Trp(2)H4-H7 134 7.58 3.26 Trp(2)H4-HB12 (ROE) 135 7.58 4.24 Trp(2)H4-Thr(3)HA (ROE) 136 7.58 7.19 Trp(2)H4-H6 137 7.58 7.14 Trp((2)H4-H5 138 7.57 3.86 Trp(2)H4-Ser(6)HB12 (ROE) 139 7.57 4.43 Trp(2)H4-Ser(6)HA (ROE) 140 7.57 8.18 Asn(18)NH2-Val(16)HN (ROE) 141 7.56 6.88 Asn(26)NH2-NH1 142 7.56 6.88 Asn(18)NH2-NH1 143 7.56 2.82 Asn(26)NH2-HB12 (intraROE) 144 7.55 2.72 Asn(18)NH2-HB12 (intraROE) 145 7.47 7.59 Trp(2)H7-H4 146 7.47 0.89 Trp(2)H7-Leu(4)HD12 (ROE) 147 7.47 7.19 Trp(2)H7-H6 148 7.47 7.13 Trp(2)H7-H5 149 7.46 4.16 Trp(2)H7-Leu(4)HA (ROE) 150 7.46 10.09 Trp(2)H7-NH1 (ROE) 151 7.33 7.23 Phe(22)H35-H26 152 7.33 4.42 Phe(22)H35-Ser(23)HA (ROE) 153 7.33 2.75 Phe(24)H35-Asp(24)HB12 (ROE) 154 7.33 7.27 Phe(22)H35-H4 155 7.33 3.15 Phe(22)H35-HB2 (ROE) 156 7.33 3.03 Phe(22)H35-HB1 (intraROE) 157 7.32 3.8 Phe(22)H35-Ser(21)HB12 (ROE) 158 7.28 2.74 Phe(22)H4-Asp(24)HB12 (ROE) 159 7.27 7.33 Phe(22)H4-H35 (intraROE) 160 7.27 3.03 Phe(22)H4-HB1 (intraROE) 161 7.27 3.16 Phe(22)H4-HB2 (intraROE) 162 7.26 8.53 His(14)H4-H2 163 7.26 1.76 His(14)H4-Pro(13)HB1 (ROE) 164 7.26 3.27 His(14)H4-HB2 165 7.26 3.15 His(14)H4-HB1 166 7.25 8.25 unassigned 167 7.25 2.71 Phe(22)H26-Asp(24)HB12 (ROE) 168 7.24 4.42 Phe(22)H26-Ser(23)HA (ROE) 169 7.24 3.8 Phe(22)H26-Ser(21)HB12 (ROE) 170 7.24 3.03 Phe(22)H26-HB1 (intraROE) 171 7.24 3.16 Phe(22)H26-HB2 (intraROE) 172 7.24 0.89 Trp(2)H2-Leu(4)HD12 (ROE) 173 7.24 4.15 Trp(2)H2-Leu(4)HA (ROE) 174 7.24 7.33 Phe(22)H26-H35 175 7.24 10.1 Trp(2)H2-NH1 176 7.23 8.52 His(19)H4-H2 177 7.23 3.16 His(19)H4-HB1 178 7.23 3.26 His(19)H4-HB2 179 7.23 3.26 Trp(2)H2-HB12 180 7.23 1.54 Trp(2)H2/ His(19)H4-Arg(20)HG12 or Leu(4)HB12/ HG 181 7.22 7.48 Trp(2)H6-H7 182 7.22 7.59 Trp(2)H6-H4 183 7.21 7.13 Trp(2)H6-H5 184 7.14 3.12 Arg(20)NHE-HD12 185 7.14 1.54 Arg(20)NHE-HG12 186 7.14 1.73 Arg(20)NH2-HB12 187 7.13 7.24 Trp(2)H5-H6 188 7.13 7.46 Trp(2)H5-H7 189 7.13 7.59 Trp(2)H5-H4 190 7.13 0.9 Trp(2)H5-Leu(4)HD12 (ROE) 191 7.12 4.15 Trp(2)H5-Leu(4)HA (ROE) 192 7.07 4.28 Tyr(9)H26-Ala(7)HA (ROE) 193 7.07 4.5 Tyr(9)H26-HA (intraROE) 194 7.07 3.83 Tyr(9)H26-Gly(8)HA12 (ROE) 195 7.07 6.78 Tyr(9)H26-H35 196 7.07 4.15 Tyr(9)H26-Leu(4)HA (ROE) 197 7.06 0.85 Tyr(9)H26-Leu(10)HD12 (ROE) 198 7.06 1.37 Tyr(9)H26-Ala(7)HB (ROE) 199 7.06 3 Tyr(9)H26-HB12 (intraROE) 200 7.06 7.87 Tyr(9)H26-HN (intraROE) 201 6.91 2.8 Asn(5)NH1-HB12 (intraROE) 202 6.91 7.61 Asn(5)NH1-NH2 203 6.89 7.56 Asn(26)NH1-NH2 204 6.89 7.56 Asn(18)NH1-NH2 205 6.89 2.82 Asn(26)NH1-HB12 (intraROE) 206 6.88 2.73 Asn(18)NH1-HB12 (intraROE) 207 6.8 4.5 Tyr(9)H35-HA (intraROE) 208 6.8 3.01 Tyr(9)H35-HB12 (intraROE) 209 6.79 1.57 Tyr(9)H35-Leu(11)HB12/ HG (ROE) 210 6.79 1.37 Tyr(9)H35-Ala(7)HB (ROE) 211 6.79 7.08 Tyr(9)H35-H26 212 6.79 0.86 Tyr(9)H35-Leu(10)HD12 (ROE) 213 4.68 8.38 Asn(26)HA-HN 214 4.67 2.82 Asn(26)HA-HB12 215 4.59 8.25 Asp(24)HA-HN 216 4.51 7.86 Tyr(9)HA-HN 217 4.51 8.06 Tyr(9)HA-Leu(10)HN (ROE) 218 4.51 7.07 Tyr(9)HA-H26 (intraROE) 219 4.5 3 Tyr(9)HA-HB12 220 4.43 8.39 Ser(21)HA-HN 221 4.43 3.82 Ser(21)HA-HB 222 4.43 3.84 Ser(6)HA-HB12 223 4.43 7.57 Ser(6)HA-Trp(2)H4 (ROE) 224 4.42 1.63 Leu(28)HA-HB12/ HG 225 4.42 3.84 Ser(23)HA-HB 226 4.42 0.9 Leu(28)HA-HD12 227 4.42 8.19 Ser(23)HA-HN 228 4.42 8.19 Thr(29)HA-HN 229 4.41 8.2 Ser(6)HA-HN 230 4.4 1.22 Thr(29)HA-HG 231 4.4 0.89 Leu(28)HA-HD12 232 4.39 1.61 Leu(28)HA-HB12/ HG 233 4.38 1.61 Leu(11)HA-HB12/ HG 234 4.38 8.07 Leu(11)HA-Gly(12)HA12 (ROE) 235 4.38 7.95 Leu(11)HA-HN 236 4.37 0.88 Leu(11)HA-HD12 237 4.36 2.19 Pro(13)HA-HB2 238 4.35 8.53 Pro(13)HA-His(14)HN (ROE) 239 4.35 1.97 Pro(13)HA-HG2 240 4.35 1.86 Pro(13)HA-HG1 241 4.35 1.76 Pro(13)HA-HB1 242 4.35 3.59 Pro(13)HA-HD12 243 4.33 3.84 Ser(30)HA-HB12 244 4.33 1.35 Ala(15)HA-HB 245 4.33 8.2 Ser(30)HA-HN 246 4.33 1.72 Arg(20)HA-HB12 247 4.32 3.14 Arg(20)HA-HD12 248 4.32 8.35 Arg(20)HA-HN 249 4.29 1.37 Ala(7)HA-HB 250 4.29 6.8 Ala(7)HA-Tyr(9)H35 (ROE) 251 4.29 2.95 Lys(25)HA-HE12 252 4.28 7.07 Ala(7)HA-Tyr(9)H26 (ROE) 253 4.28 1.2 Thr(29)HB-HG 254 4.28 1.65 Lys(25)HA-HD12 255 4.28 8.27 Ala(7)HA-HN 256 4.28 1.41 Lys(25)HA-HG12 257 4.28 1.75 Lys(25)HA-HB12 258 4.27 8.27 Lys(25)HA-HN 259 4.27 8.2 Thr(29)HB-HN 260 4.27 8.06 Leu(10)HA-HN 261 4.26 1.52 Leu(10)HA-HB12/ HG 262 4.26 0.83 Leu(10)HA-HD12 263 4.25 7.58 Thr(3)HA-Trp(2)H4 (ROE) 264 4.24 8.01 Thr(3)HA-HN 265 4.24 8.14 Thr(3)HA-Leu(4)HN (ROE) 266 4.24 4.08 Thr(3)HA-HB 267 4.24 1.09 Thr(3)HA-HG 268 4.16 8.37 Leu(4)HA-Asn(5)HN (ROE) 269 4.16 0.9 Leu(4)HA-HD12 270 4.16 1.53 Leu(4)HA-HB12/ HG 271 4.16 7.07 Leu(4)HA-Tyr(9)H26 (ROE) 272 4.16 7.24 Leu(4)HA-Trp(2)H2 (ROE) 273 4.16 7.46 Leu(4)HA-Trp(2)H7 (ROE) 274 4.15 8.14 Leu(4)HA-HN 275 4.14 1.35 Val(16)HA-Ala(15)HB (ROE) 276 4.14 0.94 Val(16)HA-HG12 277 4.14 2.07 Val(16)HA-HB 278 4.13 8.45 Val(16)HA-Gly(17)HN (ROE) 279 4.13 8.19 Val(16)HA-HN 280 4.08 4.24 Thr(3)HB-HA 281 4.08 8.01 Thr(3)HB-HN 282 4.08 1.09 Thr(3)HB-HG 283 4.05 0.8 Thr(3)HB-Leu(10)HD12 (ROE) 284 4.04 8.08 Gly(12)HA12-HN 285 4.04 3.56 Gly(12)HA12-Pro(13)HD12) (ROE) 286 3.94 8.14 Gly(27)HA12-Leu(28)HN (ROE) 287 3.94 8.29 Gly(27)HA12-HN 288 3.93 8.43 Gly(17)HA12-HN 289 3.93 0.93 Gly(17)HA12-Val(16)HG12 (ROE) 290 3.86 7.57 Ser(6)HB12-Trp(2)H4 (ROE) 291 3.84 8.06 Gly(8)HA12-Leu(10)HN (ROE) 292 3.84 7.87 Gly(8)HA12-Tyr(9)HN (ROE) 293 3.84 4.42 Ser(23)HB-HA 294 3.83 8.2 Ser(23)HB-HN 295 3.83 8.2 Gly(8)HA12-HN 296 3.83 7.07 Gly(8)HA12-Tyr(9)H26 (ROE) 297 3.83 8.2 Ser(6)/ (30)HB-HN 298 3.83 4.33 Ser(30)HB12-HA 299 3.83 4.4 Ser(6)HB12-HA 300 3.8 4.43 Ser(21)HB-HA 301 3.8 7.25 Ser(21)HB12-Phe(22)H26 (ROE) 302 3.8 8.39 Ser(21)HB-HN 303 3.78 8.55 Gly(1)HA12-Trp(2)HN (ROE) 304 3.57 1.98 Pro(13)HD12-HG2 305 3.57 1.87 Pro(13)HD12-HG1 306 3.57 4.04 Pro(13)HD12-Gly(12)HA12 (ROE) 307 3.57 2.2 Pro(13)HD12-HB2 308 3.57 1.78 Pro(13)HD12-HB1 309 3.57 4.34 Pro(13)HD12-HA 310 3.28 8.54 His(14)HB2-HN 311 3.27 7.23 HIs(14)HB2-H4 312 3.27 7.59 Trp(2)HB2-H4 (ROE) 313 3.27 8.15 Trp(2)HB2-Leu(4)HN (ROE) 314 3.27 8.53 Trp(2)HB2-HN 315 3.27 8.02 Trp(2)HB2-Thr(3)HN (ROE) 316 3.27 7.24 Trp(2)HB2-H2 317 3.26 7.24 His(19)HB2-H4 318 3.25 4.66 His(19)HB2-HA 319 3.22 7.24 Trp(2)HB1-H2 320 3.22 8.53 Trp(2)HB1-HN 321 3.21 7.59 Trp(2)HB1-H4 (ROE) 322 3.21 8.01 Trp(2)HB1-Thr(3)HN (ROE) 323 3.21 2.77 Trp(2)HB1-Asn(5)HB1 (ROE) 324 3.16 7.24 His(19)HB1-H4 325 3.15 8.21 Phe(22)HB2-Ser(23)HN (ROE) 326 3.15 8.36 Phe(22)HB2-HN 327 3.15 7.24 Phe(22)HB2-H26 (intraROE) 328 3.14 4.65 His(19)HB1-HA 329 3.14 4.64 Phe(22)HB2-HA 330 3.14 7.15 Arg(20)HD12-NHE 331 3.14 1.73 Arg(20)HD12-HB12 332 3.14 4.32 Arg(20)HD12-HA 333 3.14 1.54 Arg(20)HD12-HG12 334 3.14 8.34 Arg(20)HD12-HN 335 3.13 7.25 His(14)HB1-H4 336 3.13 8.54 His(14)HB1-HN 337 3.04 7.24 Phe(22)HB1-H26 (intraROE) 338 3.04 8.36 Phe(22)HB1-HN 339 3.03 4.64 Phe(22)HB1-HA 340 3.01 4.5 Tyr(9)HB2-HA 341 3.01 7.07 Tyr(9)HB2-H26 (intraROE) 342 3.01 8.06 Tyr(9)HB2-Leu(10)HN (ROE) 343 3.01 7.86 Try(9)HB2-HN 344 2.97 1.79 Lys(25)HE12-HB12 345 2.97 4.27 Lys(25)HE12-HA 346 2.97 1.66 Lys(25)HE12-HD12 347 2.97 8.29 Lys(25)HE12-HN 348 2.97 1.41 Lys(25)HE12-HG12 349 2.96 7.07 Tyr(9)HB1-H26 (intraROE) 350 2.96 7.86 Tyr(9)HB1-HN 351 2.96 4.5 Tyr(9)HB1-HA 352 2.95 8.03 Tyr(9)HB1-Leu(10)HN (ROE) 353 2.85 7.64 Asn(5)HB2-NH2 (intraROE) 354 2.84 8.38 Asn(5)HB2-HN 355 2.84 6.92 Asn(5)HB2-NH1 (intraROE) 356 2.84 4.66 Asn(5)HB2-HA 357 2.83 8.28 Asn(26)HB12-Gly(27)HN (ROE) 358 2.82 8.38 Asn(26)HB12-HN 359 2.81 4.67 Asn(26)HB12-HA 360 2.8 6.9 Asn(26)HB12-NH1 (intraROE) 361 2.8 7.56 Asn(26)HB12-NH2 (IntraROE) 362 2.78 4.67 Asn(5)HB1-HA 363 2.78 8.21 Asn(5)HB1-Ser(6)HN (ROE) 364 2.78 8.36 Asn(5)HB1-HN 365 2.78 3.21 Asn(5)HB1-Trp(2)HB1 (ROE) 366 2.78 7.64 Asn(5)HB1-NH2 (intraROE) 367 2.78 6.92 Asn(5)HB1-NH1 (intraROE) 368 2.75 4.65 Asn(18)HB12-HA 369 2.75 8.52 Asn(18)HB12-His(19)HN (ROE) 370 2.75 8.29 Asn(18)HB12-HN 371 2.73 7.56 Asn(18)HB12-NH2 (intraROE) 372 2.73 6.9 Asn(18)HB12-NH1 (intraROE) 373 2.71 8.25 Asp(24)HB12-HN 374 2.71 4.55 Asp(24)HB12-HA 375 2.71 7.28 Asp(24)HB12-Phe(22)H4 (ROE) 376 2.2 1.78 Pro(13)HB2-HB1 377 2.2 1.97 Pro(13)HB2-HG2 378 2.2 1.87 Pro(13)HB2-HG11 379 2.2 4.34 Pro(13)HB2-HA 380 2.2 3.57 Pro(13)HB2-HD12 381 2.09 0.94 Val(16)HB-HG12 382 2.08 8.44 Val(16)HB-Gly(17)HN (ROE) 383 2.08 8.17 Val(16)HB-HN 384 2.08 4.12 Val(16)HB-HA 385 1.97 2.2 Pro(13)HG2-HB2 386 1.97 4.35 Pro(13)HG2-HA 387 1.97 3.57 Pro(13)HG2-HD12 388 1.87 3.57 Pro(13)HG1-HD12 389 1.87 8.54 Pro(13)HG1-His(14)HN (H2) (ROE) 390 1.87 4.3 Pro(13)HG1-HA 391 1.86 2.2 Pro(13)HG1-HB2 392 1.86 2.97 Lys(25)HB2-HE12 393 1.85 4.33 Lys(25)HB2-HA 394 1.85 8.28 Lys(25)HB2-HN 395 1.81 7.15 Arg(20)HB12-NHE 396 1.78 2.2 Pro(13)HB1-HB2 397 1.77 8.54 Pro(13)HB1-His(14)HN (H2) (ROE) 398 1.77 4.34 Pro(13)HB1-HA 399 1.77 3.57 Pro(13)HB1-HD12 400 1.76 4.28 Lys(25)HB1-HA 401 1.76 7.27 Pro(13)HB1-His(14)H4 (ROE) 402 1.76 2.97 Lys(25)HB1-HE12 403 1.76 1.41 Lys(25)HB1-HG12 404 1.75 8.4 Arg(20)HB2-Ser(21)HB (ROE) 405 1.75 8.34 Arg(20)HB2-HN 406 1.75 3.14 Arg(20)HB2-HD12 407 1.75 1.52 Arg(20)HB2-HG12 408 1.75 8.28 Lys(25)HB1-HN 409 1.75 4.32 Arg(20)HB2-HA 410 1.7 8.4 Arg(20)HB1-Ser(21)HB1 (ROE) 411 1.7 1.52 Arg(20)HB1-HG12 412 1.7 8.34 Arg(20)HB1-HN 413 1.7 3.15 Arg(20)HB1-HD12 414 1.7 4.32 Arg(20)HB1-HA 415 1.66 2.97 Lys(25)HD12-HE12 416 1.66 4.29 Lys(25)HD12-HA 417 1.65 4.42 Leu(28)HB12/ HG-HA (multiple shifts overlapping) 418 1.65 8.29 Lys(25)HD12-HN 419 1.65 1.41 Lys(25)HD12-HG12 420 1.64 4.4 Leu(28)HB12/ HG-HA 421 1.6 4.39 Leu(11)HB12/ HG-HA 422 1.59 7.93 Leu(11)HB12/ HG-HN 423 1.55 1.74 Arg(20)HG12-HB12 424 1.55 8.4 Arg(20)HG12-Ser(21)HN (ROE) 425 1.55 8.33 Arg(20)HG12-HN 426 1.54 4.14 Leu(4)HB12/ HG 427 1.54 3.14 Arg(20)HG12-HD12 428 1.54 6.78 Leu(11)HB12/ HG-Tyr(9)H35 (ROE) 429 1.54 4.32 Arg(20)HG12-HA 430 1.54 8.14 Leu(4)HB12/ HG-HN 431 1.54 7.14 Arg(20)HG12-NHE 432 1.51 7.93 Leu(10)HB12-Leu(11)HN (ROE) 433 1.51 4.26 Leu(10)HB12-HA 434 1.51 8.06 Leu(10)HB12-HN 435 1.44 8.06 Leu(10)HG-HN 436 1.44 4.26 Leu(10)HG-HA 437 1.43 7.07 Leu(10)HG-Tyr(9)H26 (ROE) 438 1.41 1.64 Lys(25)HG12-HD12 439 1.41 4.28 Lys(25)HG12-HA 440 1.41 1.75 Lys(25)HG12-HB1 441 1.41 2.98 Lys(25)HG12-HE12 442 1.4 8.29 Lys(25)HG12-HN 443 1.37 4.28 Ala(7)HB-HA 444 1.37 7.07 Ala(7)HB-Tyr(9)H26 (ROE) 445 1.37 7.86 Ala(7)HB-Tyr(9)HN (ROE) 446 1.37 6.78 Ala(7)HB-Tyr(9)H35 (ROE) 447 1.37 8.27 Ala(7)HB-HN 448 1.35 4.14 Ala(15)HB-Val(16)HA (ROE) 449 1.35 8.13 Ala(15)HB-HN 450 1.35 4.31 Ala(15)HB-HA 451 1.35 8.46 Ala(15)HB-Gly(17)HN (ROE) 452 1.2 4.42 Thr(29)HG-HA 453 1.19 4.27 Thr(29)HG-HB 454 1.19 8.19 Thr(29)HG-HN 455 1.1 8.36 Thr(3)HG-Asn(5)HN (ROE) 456 1.09 8.17 Thr(3)HG-Leu(4)HN (ROE) 457 1.09 4.08 Thr(3)HG-HB 458 1.09 8.01 Thr(3)HG-HN 459 1.09 4.24 Thr(3)HG-HA 460 0.94 3.93 Val(16)HG12-Gly(17)HA12 (ROE) 461 0.94 8.45 Val(16)HG12-Gly(17)HN (ROE) 462 0.94 2.08 Val(16)HG12-HB 463 0.94 8.19 Val(16)HG12-HN 464 0.94 4.13 Val(16)HG12-HA 465 0.92 7.24 Leu(4)HD2-Trp(2)H2 (ROE) 466 0.92 4.42 Leu(28)HD2-HA 467 0.92 8.36 Leu(4)HD2-Asn(5)HN (ROE) 468 0.91 8.15 Leu(4)HD2-HN 469 0.91 4.14 Leu(4)HD2-HA 470 0.91 4.4 Leu(11)HD2-HA 471 0.9 7.86 Leu(11)HD2-Tyr(9)HN (ROE) 472 0.9 7.94 Leu(11)HD2-HN 473 0.87 8.36 Leu(4)HD1-Asn(5)HN (ROE) 474 0.87 4.42 Leu(28)HD1-HA 475 0.87 8.16 Leu(4)HD1-HN 476 0.86 4.14 Leu(4)HD1-HA 477 0.86 7.24 Leu(4)HD1-Trp(2)H2 (ROE) 478 0.86 4.4 Leu(11)HD1-HA 479 0.86 6.8 Leu(10)HD2-Tyr(9)H35 (ROE) 480 0.86 8.06 Leu(10)HD2-HN 481 0.85 7.08 Leu(10)HD2-Tyr(9)H26 (ROE) 482 0.85 7.93 Leu(11)HD1-HN 483 0.85 4.27 Leu(10)HD2-HA 484 0.85 7.86 Leu(11)HD1/ Leu(10)HD2-Tyr9)HN (ROE) 485 0.81 4.26 Leu(10)HD1-HA 486 0.8 4.08 Leu(10)HD1-Thr(3)HB (ROE) 487 0.8 7.07 Leu(10)HD1-Tyr(9)H26 (ROE) 488 0.8 6.8 Leu(10)HD1-Tyr(9)H35 (ROE) 489 0.8 8.06 Leu(10)HD1-HN ; loop_ _Spectral_dim.ID _Spectral_dim.Axis_code _Spectral_dim.Spectrometer_frequency _Spectral_dim.Atom_type _Spectral_dim.Atom_isotope_number _Spectral_dim.Spectral_region _Spectral_dim.Magnetization_linkage_ID _Spectral_dim.Under_sampling_type _Spectral_dim.Sweep_width _Spectral_dim.Sweep_width_units _Spectral_dim.Value_first_point _Spectral_dim.Absolute_peak_positions _Spectral_dim.Acquisition _Spectral_dim.Center_frequency_offset _Spectral_dim.Encoding_code _Spectral_dim.Encoded_reduced_dimension_ID _Spectral_dim.Entry_ID _Spectral_dim.Spectral_peak_list_ID 1 . . H 1 H . 'not observed' 8403.4 Hz . . . 4.78 . . 31032 1 2 . . H 1 H . 'not observed' 8403.4 Hz . . . 4.78 . . 31032 1 stop_ save_