data_20004 ####################### # Entry information # ####################### save_entry_information _Entry.Sf_category entry_information _Entry.Sf_framecode entry_information _Entry.ID 20004 _Entry.Title ; NMR Solution Structure of Leucine-Enkephlain in DMPC+CHAPS (1:4) bicelles in 90% H2O/10% D2O of pH 6.6 at 298K ; _Entry.Type 'small molecule structure' _Entry.Version_type original _Entry.Submission_date 2007-12-27 _Entry.Accession_date 2007-12-27 _Entry.Last_release_date . _Entry.Original_release_date . _Entry.Origination author _Entry.NMR_STAR_version 3.1.1.61 _Entry.Original_NMR_STAR_version 3.0.8.111 _Entry.Experimental_method NMR _Entry.Experimental_method_subtype solution _Entry.Details ; NMR Solution Structure of Leucine-Enkephlain in DMPC+CHAPS (1:4) bicelles in 90% H2O/10% D2O of pH 6.6 at 298K ; _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.Entry_ID 1 Chaitali Mukhopadhyay . . . 20004 2 Anindita Gayen . . . 20004 stop_ loop_ _Entry_src.ID _Entry_src.Project_name _Entry_src.Organization_full_name _Entry_src.Organization_initials _Entry_src.Entry_ID 1 . 'Department of Chemistry, University of Calcutta, India' . 20004 stop_ loop_ _Struct_keywords.Keywords _Struct_keywords.Text _Struct_keywords.Entry_ID peptide . 20004 stop_ loop_ _Data_set.Type _Data_set.Count _Data_set.Entry_ID assigned_chemical_shifts 1 20004 stop_ loop_ _Datum.Type _Datum.Count _Datum.Entry_ID '13C chemical shifts' 24 20004 '1H chemical shifts' 28 20004 'coupling constants' 2 20004 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 3 . . 2012-06-28 2007-12-27 update BMRB 'coordinate file not annotated' 20004 2 . . 2011-03-22 2007-12-27 update BMRB 'update the coupling constant, etc' 20004 1 . . 2008-05-27 2007-12-27 original author 'original release' 20004 stop_ loop_ _Related_entries.Database_name _Related_entries.Database_accession_code _Related_entries.Relationship _Related_entries.Entry_ID BMRB 20003 'NMR solution structure of Leucine-enkephalin in' 20004 BMRB 20005 'NMR solution structure of Leucine-enkephalin in isotropic DMPC+CHAPS+GM1 (1:4:0.3) bicelles' 20004 stop_ save_ ############### # Citations # ############### save_entry_citation _Citation.Sf_category citations _Citation.Sf_framecode entry_citation _Citation.Entry_ID 20004 _Citation.ID 1 _Citation.Class 'entry citation' _Citation.CAS_abstract_code . _Citation.MEDLINE_UI_code . _Citation.DOI . _Citation.PubMed_ID 18412380 _Citation.Full_citation . _Citation.Title 'Evidence for Effect of GM1 on Opioid Peptide Conformation: NMR Study on Leucine Enkephalin in Ganglioside-Containing Isotropic Phospholipid Bicelles' _Citation.Status published _Citation.Type journal _Citation.Journal_abbrev Langmuir _Citation.Journal_name_full . _Citation.Journal_volume 24 _Citation.Journal_issue 10 _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 5422 _Citation.Page_last 5432 _Citation.Year 2008 _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.Entry_ID _Citation_author.Citation_ID 1 Anindita Gayen . . . 20004 1 2 Chaitali Mukhopadhyay . . . 20004 1 stop_ save_ ############################################# # Molecular system (assembly) description # ############################################# save_assembly _Assembly.Sf_category assembly _Assembly.Sf_framecode assembly _Assembly.Entry_ID 20004 _Assembly.ID 1 _Assembly.Name Leu-enkephalin _Assembly.BMRB_code . _Assembly.Number_of_components 1 _Assembly.Organic_ligands . _Assembly.Metal_ions . _Assembly.Non_standard_bonds no _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 na _Assembly.Details na _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 Leu-enkephalin 1 $Leu-Enkephalin A . yes N/A no no . . . 20004 1 stop_ save_ #################################### # Biological polymers and ligands # #################################### save_Leu-Enkephalin _Entity.Sf_category entity _Entity.Sf_framecode Leu-Enkephalin _Entity.Entry_ID 20004 _Entity.ID 1 _Entity.BMRB_code . _Entity.Name Leu-Enkephalin _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 YGGFL _Entity.Target_identifier . _Entity.Polymer_author_defined_seq 'TYR 1 GLY 2 GLY 3 PHE 4 LEU 5' _Entity.Polymer_author_seq_details 'TYROSINE 1 GLYCINE 2 GLYCINE 3 PHENYLALANINE 4 LEUCINE 5' _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 5 _Entity.Number_of_nonpolymer_components . _Entity.Paramagnetic no _Entity.Thiol_state 'not present' _Entity.Src_method . _Entity.Parent_entity_ID . _Entity.Fragment na _Entity.Mutation na _Entity.EC_number na _Entity.Calc_isoelectric_point . _Entity.Formula_weight 555.62 _Entity.Formula_weight_exptl . _Entity.Formula_weight_exptl_meth . _Entity.Details 'Formula C28H37N5O7 xC2H4O2 yH2O' _Entity.DB_query_date . _Entity.DB_query_revised_last_date . loop_ _Entity_db_link.Ordinal _Entity_db_link.Author_supplied _Entity_db_link.Database_code _Entity_db_link.Accession_code _Entity_db_link.Entry_mol_code _Entity_db_link.Entry_mol_name _Entity_db_link.Entry_experimental_method _Entity_db_link.Entry_structure_resolution _Entity_db_link.Entry_relation_type _Entity_db_link.Entry_details _Entity_db_link.Chimera_segment_ID _Entity_db_link.Seq_query_to_submitted_percent _Entity_db_link.Seq_subject_length _Entity_db_link.Seq_identity _Entity_db_link.Seq_positive _Entity_db_link.Seq_homology_expectation_val _Entity_db_link.Seq_align_begin _Entity_db_link.Seq_align_end _Entity_db_link.Seq_difference_details _Entity_db_link.Seq_alignment_details _Entity_db_link.Entry_ID _Entity_db_link.Entity_ID . . PDB 1LND . Leu-enkephalin . . . . . . . . . . . . . . 20004 1 stop_ loop_ _Entity_biological_function.Biological_function _Entity_biological_function.Entry_ID _Entity_biological_function.Entity_ID 'Endogenous opioid neurotransmitter/neuromodulator' 20004 1 stop_ 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 . TYR . 20004 1 2 . GLY . 20004 1 3 . GLY . 20004 1 4 . PHE . 20004 1 5 . LEU . 20004 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 . TYR 1 1 20004 1 . GLY 2 2 20004 1 . GLY 3 3 20004 1 . PHE 4 4 20004 1 . LEU 5 5 20004 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 20004 _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.Subvariant _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.Cellular_location _Entity_natural_src.Fragment _Entity_natural_src.Fraction _Entity_natural_src.Secretion _Entity_natural_src.Plasmid _Entity_natural_src.Plasmid_details _Entity_natural_src.Gene_mnemonic _Entity_natural_src.Dev_stage _Entity_natural_src.Details _Entity_natural_src.Citation_ID _Entity_natural_src.Citation_label _Entity_natural_src.Entry_ID _Entity_natural_src.Entity_natural_src_list_ID 1 1 $Leu-Enkephalin . 9606 organism . . Human . . Eukaryota Metazoa Homo sapiens . . . . . . . . . . . . . . . . . . . . . 20004 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 20004 _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_subvariant _Entity_experimental_src.Host_org_organ _Entity_experimental_src.Host_org_tissue _Entity_experimental_src.Host_org_tissue_fraction _Entity_experimental_src.Host_org_cell_line _Entity_experimental_src.Host_org_cell_type _Entity_experimental_src.Host_org_cellular_location _Entity_experimental_src.Host_org_organelle _Entity_experimental_src.Host_org_gene _Entity_experimental_src.Host_org_culture_collection _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.Host_org_dev_stage _Entity_experimental_src.Details _Entity_experimental_src.Citation_ID _Entity_experimental_src.Citation_label _Entity_experimental_src.Entry_ID _Entity_experimental_src.Entity_experimental_src_list_ID 1 1 $Leu-Enkephalin . 'recombinant technology' . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20004 1 stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_Leu-Enkephalin_in_isotropic_DMPC+CHAPS_(1:4)_bicelles_with_peptide:lipid_1:13 _Sample.Sf_category sample _Sample.Sf_framecode Leu-Enkephalin_in_isotropic_DMPC+CHAPS_(1:4)_bicelles_with_peptide:lipid_1:13 _Sample.Entry_ID 20004 _Sample.ID 1 _Sample.Type bicelle _Sample.Sub_type . _Sample.Details ; Lyophilized powder from Sigma-Aldrich dissolved in isotropic DMPC+CHAPS(1:4) bicelles in 90%H2O/10% D2O (pH 6.6 at 298 K) with peptide:lipid 1:13 ; _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 Leu-Enkephalin 'natural abundance' . . 1 $Leu-Enkephalin . . 4-5 . . mM . . . . 20004 1 2 DMPC+CHAPS 'natural abundance' . . . . . . 4 . . '% w/v' . . . . 20004 1 stop_ save_ ####################### # Sample conditions # ####################### save_bicelles _Sample_condition_list.Sf_category sample_conditions _Sample_condition_list.Sf_framecode bicelles _Sample_condition_list.Entry_ID 20004 _Sample_condition_list.ID 1 _Sample_condition_list.Details ; isotropic bicellar DMPC+CHAPS 1:4 solution in 90% H2O/10% D2O pH 6.6 at 298K ; 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 6.6 . na 20004 1 temperature 298 . K 20004 1 stop_ save_ ############################ # Computer software used # ############################ save_xwinnmr _Software.Sf_category software _Software.Sf_framecode xwinnmr _Software.Entry_ID 20004 _Software.ID 1 _Software.Name xwinnmr _Software.Version 3.75 _Software.Details 'Bruker Topspin' loop_ _Vendor.Name _Vendor.Address _Vendor.Electronic_address _Vendor.Entry_ID _Vendor.Software_ID 'Bruker Biospin' . . 20004 1 Goddard . . 20004 1 'Schwieters, Kuszewski, Tjandra and Clore' . . 20004 1 stop_ loop_ _Task.Task _Task.Entry_ID _Task.Software_ID collection 20004 1 'data analysis' 20004 1 refinement 20004 1 stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _NMR_spectrometer.Sf_category NMR_spectrometer _NMR_spectrometer.Sf_framecode spectrometer_1 _NMR_spectrometer.Entry_ID 20004 _NMR_spectrometer.ID 1 _NMR_spectrometer.Details 'Bruker Topspin' _NMR_spectrometer.Manufacturer Bruker _NMR_spectrometer.Model DRX _NMR_spectrometer.Serial_number . _NMR_spectrometer.Field_strength 500 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 20004 _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 spectrometer_1 Bruker DRX . 500 'Bruker Topspin' . . 20004 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 20004 _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 $Leu-Enkephalin_in_isotropic_DMPC+CHAPS_(1:4)_bicelles_with_peptide:lipid_1:13 isotropic . . 1 $bicelles . . . 1 $spectrometer_1 . . . . . . . . . . . . . . . . 20004 1 2 '2D 1H-1H NOESY' no . . . . . . . . . . 1 $Leu-Enkephalin_in_isotropic_DMPC+CHAPS_(1:4)_bicelles_with_peptide:lipid_1:13 isotropic . . 1 $bicelles . . . 1 $spectrometer_1 . . . . . . . . . . . . . . . . 20004 1 3 '2D DQF-COSY' no . . . . . . . . . . 1 $Leu-Enkephalin_in_isotropic_DMPC+CHAPS_(1:4)_bicelles_with_peptide:lipid_1:13 isotropic . . 1 $bicelles . . . 1 $spectrometer_1 . . . . . . . . . . . . . . . . 20004 1 4 '2D 1H-13C HSQC' no . . . . . . . . . . 1 $Leu-Enkephalin_in_isotropic_DMPC+CHAPS_(1:4)_bicelles_with_peptide:lipid_1:13 isotropic . . 1 $bicelles . . . 1 $spectrometer_1 . . . . . . . . . . . . . . . . 20004 1 stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_TSP _Chem_shift_reference.Sf_category chem_shift_reference _Chem_shift_reference.Sf_framecode TSP _Chem_shift_reference.Entry_ID 20004 _Chem_shift_reference.ID 1 _Chem_shift_reference.Details 'TSP as reference' 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.Indirect_shift_ratio_cit_ID _Chem_shift_ref.Indirect_shift_ratio_cit_label _Chem_shift_ref.Ref_correction_type _Chem_shift_ref.Correction_val _Chem_shift_ref.Correction_val_cit_ID _Chem_shift_ref.Correction_val_cit_label _Chem_shift_ref.Entry_ID _Chem_shift_ref.Chem_shift_reference_ID C 13 TSP 'methyl carbons' . . . . ppm 0 external direct . . . . . . . . . . 20004 1 H 1 TSP 'methyl protons' . . . . ppm 0 external direct . . . . . . . . . . 20004 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_chemicalshift_dmpcbicelle _Assigned_chem_shift_list.Sf_category assigned_chemical_shifts _Assigned_chem_shift_list.Sf_framecode chemicalshift_dmpcbicelle _Assigned_chem_shift_list.Entry_ID 20004 _Assigned_chem_shift_list.ID 1 _Assigned_chem_shift_list.Sample_condition_list_ID 1 _Assigned_chem_shift_list.Sample_condition_list_label $bicelles _Assigned_chem_shift_list.Chem_shift_reference_ID 1 _Assigned_chem_shift_list.Chem_shift_reference_label $TSP _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' . . . 20004 1 4 '2D 1H-13C HSQC' . . . 20004 1 stop_ loop_ _Chem_shift_software.Software_ID _Chem_shift_software.Software_label _Chem_shift_software.Method_ID _Chem_shift_software.Method_label _Chem_shift_software.Entry_ID _Chem_shift_software.Assigned_chem_shift_list_ID 1 $xwinnmr . . 20004 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 TYR HA H 1 4.228 0.01 . 1 . . . . 1 TYR HA . 20004 1 2 . 1 1 1 1 TYR HB2 H 1 3.125 0.01 . 1 . . . . 1 TYR HB2 . 20004 1 3 . 1 1 1 1 TYR HD1 H 1 7.153 0.01 . 3 . . . . 1 TYR HD1 . 20004 1 4 . 1 1 1 1 TYR HE1 H 1 6.851 0.01 . 3 . . . . 1 TYR HE1 . 20004 1 5 . 1 1 1 1 TYR C C 13 170.803 0.01 . 1 . . . . 1 TYR C . 20004 1 6 . 1 1 1 1 TYR CA C 13 54.8 0.01 . 1 . . . . 1 TYR CA . 20004 1 7 . 1 1 1 1 TYR CB C 13 37.11 0.01 . 1 . . . . 1 TYR CB . 20004 1 8 . 1 1 1 1 TYR CD1 C 13 130.83 0.01 . 3 . . . . 1 TYR CD1 . 20004 1 9 . 1 1 1 1 TYR CE1 C 13 115.85 0.01 . 3 . . . . 1 TYR CE1 . 20004 1 10 . 1 1 1 1 TYR CG C 13 127.045 0.01 . 1 . . . . 1 TYR CG . 20004 1 11 . 1 1 1 1 TYR CZ C 13 155.19 0.01 . 1 . . . . 1 TYR CZ . 20004 1 12 . 1 1 2 2 GLY H H 1 8.575 0.01 . 1 . . . . 2 GLY H . 20004 1 13 . 1 1 2 2 GLY HA2 H 1 3.84 0.01 . 2 . . . . 2 GLY HA2 . 20004 1 14 . 1 1 2 2 GLY HA3 H 1 3.9 0.01 . 2 . . . . 2 GLY HA3 . 20004 1 15 . 1 1 2 2 GLY C C 13 171.246 0.01 . 1 . . . . 2 GLY C . 20004 1 16 . 1 1 2 2 GLY CA C 13 42.47 0.01 . 1 . . . . 2 GLY CA . 20004 1 17 . 1 1 3 3 GLY H H 1 8.001 0.01 . 1 . . . . 3 GLY H . 20004 1 18 . 1 1 3 3 GLY HA2 H 1 3.83 0.01 . 2 . . . . 3 GLY HA2 . 20004 1 19 . 1 1 3 3 GLY HA3 H 1 3.9 0.01 . 2 . . . . 3 GLY HA3 . 20004 1 20 . 1 1 3 3 GLY C C 13 171.246 0.01 . 1 . . . . 3 GLY C . 20004 1 21 . 1 1 3 3 GLY CA C 13 42.19 0.01 . 1 . . . . 3 GLY CA . 20004 1 22 . 1 1 4 4 PHE H H 1 8.001 0.01 . 1 . . . . 4 PHE H . 20004 1 23 . 1 1 4 4 PHE HA H 1 4.64 0.01 . 1 . . . . 4 PHE HA . 20004 1 24 . 1 1 4 4 PHE HB2 H 1 3.171 0.01 . 3 . . . . 4 PHE HB2 . 20004 1 25 . 1 1 4 4 PHE HB3 H 1 2.97 0.01 . 1 . . . . 4 PHE HB3 . 20004 1 26 . 1 1 4 4 PHE HD1 H 1 7.245 0.01 . 3 . . . . 4 PHE HD1 . 20004 1 27 . 1 1 4 4 PHE HE1 H 1 7.334 0.01 . 3 . . . . 4 PHE HE1 . 20004 1 28 . 1 1 4 4 PHE HZ H 1 7.284 0.01 . 1 . . . . 4 PHE HZ . 20004 1 29 . 1 1 4 4 PHE C C 13 171.953 0.01 . 1 . . . . 4 PHE C . 20004 1 30 . 1 1 4 4 PHE CA C 13 54.88 0.01 . 1 . . . . 4 PHE CA . 20004 1 31 . 1 1 4 4 PHE CB C 13 37.27 0.01 . 1 . . . . 4 PHE CB . 20004 1 32 . 1 1 4 4 PHE CD1 C 13 129.342 0.01 . 3 . . . . 4 PHE CD1 . 20004 1 33 . 1 1 4 4 PHE CE1 C 13 129.071 0.01 . 3 . . . . 4 PHE CE1 . 20004 1 34 . 1 1 4 4 PHE CG C 13 136.722 0.01 . 1 . . . . 4 PHE CG . 20004 1 35 . 1 1 4 4 PHE CZ C 13 128.714 0.01 . 1 . . . . 4 PHE CZ . 20004 1 36 . 1 1 5 5 LEU H H 1 7.869 0.01 . 1 . . . . 5 LEU H . 20004 1 37 . 1 1 5 5 LEU HA H 1 4.17 0.01 . 1 . . . . 5 LEU HA . 20004 1 38 . 1 1 5 5 LEU HB2 H 1 1.545 0.01 . 1 . . . . 5 LEU HB . 20004 1 39 . 1 1 5 5 LEU HB3 H 1 1.545 0.01 . 1 . . . . 5 LEU HB . 20004 1 40 . 1 1 5 5 LEU HD11 H 1 0.8419 0.01 . 2 . . . . 5 LEU HD1 . 20004 1 41 . 1 1 5 5 LEU HD12 H 1 0.8419 0.01 . 2 . . . . 5 LEU HD1 . 20004 1 42 . 1 1 5 5 LEU HD13 H 1 0.8419 0.01 . 2 . . . . 5 LEU HD1 . 20004 1 43 . 1 1 5 5 LEU HD21 H 1 0.8664 0.01 . 2 . . . . 5 LEU HD2 . 20004 1 44 . 1 1 5 5 LEU HD22 H 1 0.8664 0.01 . 2 . . . . 5 LEU HD2 . 20004 1 45 . 1 1 5 5 LEU HD23 H 1 0.8664 0.01 . 2 . . . . 5 LEU HD2 . 20004 1 46 . 1 1 5 5 LEU HG H 1 1.54 0.01 . 1 . . . . 5 LEU HG . 20004 1 47 . 1 1 5 5 LEU C C 13 179.309 0.01 . 1 . . . . 5 LEU C . 20004 1 48 . 1 1 5 5 LEU CA C 13 55.02 0.01 . 1 . . . . 5 LEU CA . 20004 1 49 . 1 1 5 5 LEU CB C 13 41.27 0.01 . 1 . . . . 5 LEU CB . 20004 1 50 . 1 1 5 5 LEU CD1 C 13 21.06 0.01 . 2 . . . . 5 LEU CD1 . 20004 1 51 . 1 1 5 5 LEU CD2 C 13 22.36 0.01 . 2 . . . . 5 LEU CD2 . 20004 1 52 . 1 1 5 5 LEU CG C 13 24.555 0.01 . 1 . . . . 5 LEU CG . 20004 1 stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Coupling_constant_list.Sf_category coupling_constants _Coupling_constant_list.Sf_framecode coupling_constant_list_1 _Coupling_constant_list.Entry_ID 20004 _Coupling_constant_list.ID 1 _Coupling_constant_list.Sample_condition_list_ID 1 _Coupling_constant_list.Sample_condition_list_label $bicelles _Coupling_constant_list.Spectrometer_frequency_1H 500 _Coupling_constant_list.Details 'extracted from DQF-COSY in isotropic bicellar medium of DMPC:CHAPS 1:4' _Coupling_constant_list.Text_data_format . _Coupling_constant_list.Text_data . loop_ _Coupling_constant_experiment.Experiment_ID _Coupling_constant_experiment.Experiment_name _Coupling_constant_experiment.Sample_ID _Coupling_constant_experiment.Sample_label _Coupling_constant_experiment.Sample_state _Coupling_constant_experiment.Entry_ID _Coupling_constant_experiment.Coupling_constant_list_ID 3 '2D DQF-COSY' . . . 20004 1 stop_ loop_ _Coupling_constant_software.Software_ID _Coupling_constant_software.Software_label _Coupling_constant_software.Method_ID _Coupling_constant_software.Method_label _Coupling_constant_software.Entry_ID _Coupling_constant_software.Coupling_constant_list_ID 1 $xwinnmr . . 20004 1 stop_ loop_ _Coupling_constant.ID _Coupling_constant.Code _Coupling_constant.Assembly_atom_ID_1 _Coupling_constant.Entity_assembly_ID_1 _Coupling_constant.Entity_ID_1 _Coupling_constant.Comp_index_ID_1 _Coupling_constant.Seq_ID_1 _Coupling_constant.Comp_ID_1 _Coupling_constant.Atom_ID_1 _Coupling_constant.Atom_type_1 _Coupling_constant.Atom_isotope_number_1 _Coupling_constant.Ambiguity_code_1 _Coupling_constant.Assembly_atom_ID_2 _Coupling_constant.Entity_assembly_ID_2 _Coupling_constant.Entity_ID_2 _Coupling_constant.Comp_index_ID_2 _Coupling_constant.Seq_ID_2 _Coupling_constant.Comp_ID_2 _Coupling_constant.Atom_ID_2 _Coupling_constant.Atom_type_2 _Coupling_constant.Atom_isotope_number_2 _Coupling_constant.Ambiguity_code_2 _Coupling_constant.Val _Coupling_constant.Val_min _Coupling_constant.Val_max _Coupling_constant.Val_err _Coupling_constant.Resonance_ID_1 _Coupling_constant.Resonance_ID_2 _Coupling_constant.Auth_entity_assembly_ID_1 _Coupling_constant.Auth_seq_ID_1 _Coupling_constant.Auth_comp_ID_1 _Coupling_constant.Auth_atom_ID_1 _Coupling_constant.Auth_entity_assembly_ID_2 _Coupling_constant.Auth_seq_ID_2 _Coupling_constant.Auth_comp_ID_2 _Coupling_constant.Auth_atom_ID_2 _Coupling_constant.Details _Coupling_constant.Entry_ID _Coupling_constant.Coupling_constant_list_ID 1 3JHNHA . 1 1 4 4 PHE H H 1 . . 1 1 4 4 PHE HA H 1 . 9.0 . . 0.2 . . 1 4 PHE H 1 4 PHE HA . 20004 1 2 3JHNHA . 1 1 5 5 LEU H H 1 . . 1 1 5 5 LEU HA H 1 . 8.0 . . 0.2 . . 1 5 LEU H 1 5 LEU HA . 20004 1 stop_ save_ ############################## # Structure determinations # ############################## ########################## # Conformer statistics # ########################## save_conformer_statistics _Conformer_stat_list.Sf_category conformer_statistics _Conformer_stat_list.Sf_framecode conformer_statistics _Conformer_stat_list.Entry_ID 20004 _Conformer_stat_list.ID 1 _Conformer_stat_list.Text_data_format . _Conformer_stat_list.Text_data . _Conformer_stat_list.Original_conformer_stats_file_ID . _Conformer_stat_list.Conf_family_coord_set_ID 1 _Conformer_stat_list.Conf_family_coord_set_label $ensemble_coordinates _Conformer_stat_list.Representative_conformer_ID . _Conformer_stat_list.Representative_conformer_label . _Conformer_stat_list.Conformer_calculated_total_num 250 _Conformer_stat_list.Conformer_submitted_total_num 90 _Conformer_stat_list.Conformer_selection_criteria 'structures with the least restraint violations' _Conformer_stat_list.Representative_conformer 1 _Conformer_stat_list.Rep_conformer_selection_criteria 'closest to the average' _Conformer_stat_list.Statistical_struct_param_details . _Conformer_stat_list.Details . save_ ##################################### # Conformer family coordinate set # ##################################### save_ensemble_coordinates _Conformer_family_coord_set.Sf_category conformer_family_coord_set _Conformer_family_coord_set.Sf_framecode ensemble_coordinates _Conformer_family_coord_set.Entry_ID 20004 _Conformer_family_coord_set.ID 1 _Conformer_family_coord_set.File_name . _Conformer_family_coord_set.Constraints_PDB_file_ID . _Conformer_family_coord_set.PDB_accession_code . _Conformer_family_coord_set.Sample_condition_list_ID 1 _Conformer_family_coord_set.Sample_condition_list_label $bicelles _Conformer_family_coord_set.Atom_site_uncertainty_desc . _Conformer_family_coord_set.Atom_site_ordered_flag_desc . _Conformer_family_coord_set.Details . loop_ _Conformer_family_refinement.Refine_method _Conformer_family_refinement.Refine_details _Conformer_family_refinement.Software_ID _Conformer_family_refinement.Software_label _Conformer_family_refinement.Entry_ID _Conformer_family_refinement.Conformer_family_coord_set_ID 'simulated annealing' ; Distance restraints were obtained from the combination of NOESY and ROESY experiments (tmix= 300ms) for enkephalin in water, PC and GM1 containing PC bicelles. Backbone torsion angle constants extracted from DQF-COSY were used for two residues Phe4 and Leu5. Two hundred and fifty structures were generated from the random starting conformation using the standard simulated annealing protocol (anneal.py)of XPLOR-NIH.The highest temperature that was achieved during the SA (simulated annealing) protocol was 3000 K, and the final lowest temperature that was achieved, was 12.5 K. A repel constant of 1.2 was used. The top structures from the SA were further refined using the refinement protocol of XPLOR-NIH (refine.py). Several rounds of structure calculations were carried out, and depending on the NOE violations, the distance constraints were adjusted. ; . . 20004 1 stop_ loop_ _Conformer_family_coord_set_expt.Experiment_ID _Conformer_family_coord_set_expt.Experiment_name _Conformer_family_coord_set_expt.Sample_ID _Conformer_family_coord_set_expt.Sample_label _Conformer_family_coord_set_expt.Sample_state _Conformer_family_coord_set_expt.Entry_ID _Conformer_family_coord_set_expt.Conformer_family_coord_set_ID . . 1 $Leu-Enkephalin_in_isotropic_DMPC+CHAPS_(1:4)_bicelles_with_peptide:lipid_1:13 . 20004 1 stop_ save_ ########################### # Constraint Statistics # ########################### save_constraint_statistics _Constraint_stat_list.Sf_category constraint_statistics _Constraint_stat_list.Sf_framecode constraint_statistics _Constraint_stat_list.Entry_ID 20004 _Constraint_stat_list.ID 1 _Constraint_stat_list.Details . _Constraint_stat_list.Text_data_format . _Constraint_stat_list.Text_data . _Constraint_stat_list.Stats_not_available . _Constraint_stat_list.NOE_interproton_dist_evaluation . _Constraint_stat_list.NOE_pseudoatom_corrections . _Constraint_stat_list.NOE_dist_averaging_method r-6 _Constraint_stat_list.ROE_interproton_dist_evaluation . _Constraint_stat_list.ROE_pseudoatom_corrections . _Constraint_stat_list.ROE_dist_averaging_method . _Constraint_stat_list.NOE_tot_num 34 _Constraint_stat_list.RDC_tot_num . _Constraint_stat_list.Dihedral_angle_tot_num 2 _Constraint_stat_list.Protein_dihedral_angle_tot_num 2 _Constraint_stat_list.NA_dihedral_angle_tot_num . _Constraint_stat_list.NOE_intraresidue_tot_num 16 _Constraint_stat_list.NOE_sequential_tot_num 16 _Constraint_stat_list.NOE_medium_range_tot_num 2 _Constraint_stat_list.NOE_long_range_tot_num 0 _Constraint_stat_list.NOE_unique_tot_num . _Constraint_stat_list.NOE_intraresidue_unique_tot_num . _Constraint_stat_list.NOE_sequential_unique_tot_num . _Constraint_stat_list.NOE_medium_range_unique_tot_num . _Constraint_stat_list.NOE_long_range_unique_tot_num . _Constraint_stat_list.NOE_unamb_intramol_tot_num . _Constraint_stat_list.NOE_unamb_intermol_tot_num . _Constraint_stat_list.NOE_ambig_intramol_tot_num . _Constraint_stat_list.NOE_ambig_intermol_tot_num . _Constraint_stat_list.NOE_interentity_tot_num . _Constraint_stat_list.NOE_other_tot_num 0 _Constraint_stat_list.ROE_tot_num . _Constraint_stat_list.ROE_intraresidue_tot_num . _Constraint_stat_list.ROE_sequential_tot_num . _Constraint_stat_list.ROE_medium_range_tot_num . _Constraint_stat_list.ROE_long_range_tot_num . _Constraint_stat_list.ROE_unambig_intramol_tot_num . _Constraint_stat_list.ROE_unambig_intermol_tot_num . _Constraint_stat_list.ROE_ambig_intramol_tot_num . _Constraint_stat_list.ROE_ambig_intermol_tot_num . _Constraint_stat_list.ROE_other_tot_num . _Constraint_stat_list.RDC_HH_tot_num . _Constraint_stat_list.RDC_HNC_tot_num . _Constraint_stat_list.RDC_NH_tot_num . _Constraint_stat_list.RDC_CC_tot_num . _Constraint_stat_list.RDC_CN_i_1_tot_num . _Constraint_stat_list.RDC_CAHA_tot_num . _Constraint_stat_list.RDC_HNHA_tot_num . _Constraint_stat_list.RDC_HNHA_i_1_tot_num . _Constraint_stat_list.RDC_CAC_tot_num . _Constraint_stat_list.RDC_CAN_tot_num . _Constraint_stat_list.RDC_intraresidue_tot_num . _Constraint_stat_list.RDC_sequential_tot_num . _Constraint_stat_list.RDC_medium_range_tot_num . _Constraint_stat_list.RDC_long_range_tot_num . _Constraint_stat_list.RDC_other_tot_num . _Constraint_stat_list.RDC_unambig_intramol_tot_num . _Constraint_stat_list.RDC_unambig_intermol_tot_num . _Constraint_stat_list.RDC_ambig_intramol_tot_num . _Constraint_stat_list.RDC_ambig_intermol_tot_num . _Constraint_stat_list.RDC_intermol_tot_num . _Constraint_stat_list.Protein_phi_angle_tot_num 2 _Constraint_stat_list.Protein_psi_angle_tot_num 0 _Constraint_stat_list.Protein_chi_one_angle_tot_num 0 _Constraint_stat_list.Protein_other_angle_tot_num 0 _Constraint_stat_list.Protein_ambig_dihedral_tot_num 0 _Constraint_stat_list.Protein_other_tot_num . _Constraint_stat_list.NA_alpha_angle_tot_num . _Constraint_stat_list.NA_beta_angle_tot_num . _Constraint_stat_list.NA_gamma_angle_tot_num . _Constraint_stat_list.NA_delta_angle_tot_num . _Constraint_stat_list.NA_epsilon_angle_tot_num . _Constraint_stat_list.NA_chi_angle_tot_num . _Constraint_stat_list.NA_sugar_pucker_tot_num . _Constraint_stat_list.NA_other_angle_tot_num . _Constraint_stat_list.NA_amb_dihedral_angle_tot_num . _Constraint_stat_list.NA_other_tot_num . _Constraint_stat_list.H_bonds_constrained_tot_num . _Constraint_stat_list.Constr_def_H_bonds_tot_num . _Constraint_stat_list.SS_bonds_constrained_tot_num . _Constraint_stat_list.Constr_def_SS_bonds_tot_num . _Constraint_stat_list.Derived_coupling_const_tot_num . _Constraint_stat_list.Derived_CACB_chem_shift_tot_num . _Constraint_stat_list.Derived_1H_chem_shifts_tot_num . _Constraint_stat_list.Derived_photo_cidnps_tot_num . _Constraint_stat_list.Derived_paramag_relax_tot_num . _Constraint_stat_list.Assumed_distances_tot_num . _Constraint_stat_list.Assumed_angles_tot_num . _Constraint_stat_list.Constraints_per_residue_avg . _Constraint_stat_list.Constr_violations_per_residue_avg . _Constraint_stat_list.Dist_constr_violat_stat_calc_method . loop_ _Constraint_file.ID _Constraint_file.Constraint_filename _Constraint_file.Software_ID _Constraint_file.Software_label _Constraint_file.Software_name _Constraint_file.Block_ID _Constraint_file.Constraint_type _Constraint_file.Constraint_subtype _Constraint_file.Constraint_subsubtype _Constraint_file.Constraint_number _Constraint_file.Entry_ID _Constraint_file.Constraint_stat_list_ID 1 diheddmpclenk-tbl.txt . . XPLOR . 'protein dihedral angle' 'Not applicable' simple . 20004 1 2 noelenkdmpc-tbl.txt . . XPLOR . distance NOE simple . 20004 1 stop_ save_