data_20003 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR Structure of Leucine-Enkephalin in Water ; _BMRB_accession_number 20003 _BMRB_flat_file_name bmr20003.str _Entry_type original _Submission_date 2007-12-27 _Accession_date 2007-12-27 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'NMR Structure of Leucine-Enkephalin in WATER' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Mukhopadhyay Chaitali . . 2 Gayen Anindita . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 24 "13C chemical shifts" 24 "coupling constants" 2 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2012-06-28 update BMRB 'coordinate file not annotated' 2011-03-22 update BMRB 'update the coupling constant, etc' 2008-06-11 update BMRB 'update the shift table, etc' 2008-05-27 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 20004 'NMR Structure of Leucine-Enkephalin in DMPC/CHAPS bicelle' 20005 'NMR Structure of Leucine-Enkephalin in DMPC/CHAPS/GM1' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _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 _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 18412380 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Gayen Anindita . . 2 Mukhopadhyay Chaitali . . stop_ _Journal_abbreviation Langmuir _Journal_volume 24 _Journal_issue 10 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 5422 _Page_last 5432 _Year 2008 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Leu-enkephalin _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label Leu-enkephalin $Leu-enkephalin stop_ _System_molecular_weight . _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_Leu-enkephalin _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common Leu-enkephalin _Molecular_mass 555.62 _Mol_thiol_state 'not present' loop_ _Biological_function 'Endogenous opioid neurotransmitter/neuromodulator' stop_ _Details 'Moleculer formula C28H37N5O7 xC2H4O2 yH2O' ############################## # Polymer residue sequence # ############################## _Residue_count 5 _Mol_residue_sequence YGGFL loop_ _Residue_seq_code _Residue_label 1 TYR 2 GLY 3 GLY 4 PHE 5 LEU stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $Leu-enkephalin Human 9606 Eukaryota Metazoa Homo sapiens stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $Leu-enkephalin 'recombinant technology' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_leucine_enkephalin _Saveframe_category sample _Sample_type solution _Details 'Lyophilized powder from Sigma-Aldrich dissolved in 90% H2O/10% D2O of pH 6.6 at 298K' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $Leu-enkephalin 4-5 mM 'natural abundance' H2O 90 % . D2O 10 % . stop_ save_ ############################ # Computer software used # ############################ save_xwinnmr _Saveframe_category software _Name xwinnmr _Version 3.75 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . Goddard . . 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task collection 'data analysis' refinement stop_ _Details 'Bruker Topspin' save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $leucine_enkephalin save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $leucine_enkephalin save_ save_2D_DQF-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $leucine_enkephalin save_ save_2D_1H-13C_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $leucine_enkephalin save_ ####################### # Sample conditions # ####################### save_solution_in_90%_H2O_10%_D2O_pH_6.6_298K _Saveframe_category sample_conditions _Details 'lyophillizd powder fron Sigma-Aldrich in 90%H20/10%D20 of pH 6.6' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 298 . K pH 6.6 . pH stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_TSP _Saveframe_category chemical_shift_reference _Details . loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio TSP H 1 'methly protons' ppm 0 external direct . . . 1.0 TSP C 13 'methly carbons' ppm 0 external direct . . . 1.0 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_water _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $xwinnmr stop_ loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $leucine_enkephalin stop_ _Sample_conditions_label $solution_in_90%_H2O_10%_D2O_pH_6.6_298K _Chem_shift_reference_set_label $TSP _Mol_system_component_name Leu-enkephalin _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 1 1 TYR HA H 4.233 0.01 1 2 1 1 TYR HB2 H 3.123 0.01 1 3 1 1 TYR HD1 H 7.15 0.01 3 4 1 1 TYR HE1 H 6.86 0.01 3 5 1 1 TYR C C 170.734 0.01 1 6 1 1 TYR CA C 54.14 0.01 1 7 1 1 TYR CB C 36.55 0.01 1 8 1 1 TYR CD1 C 130.809 0.01 3 9 1 1 TYR CE1 C 115.792 0.01 3 10 1 1 TYR CG C 127.089 0.01 1 11 1 1 TYR CZ C 155.069 0.01 1 12 2 2 GLY H H 8.57 0.01 1 13 2 2 GLY HA2 H 3.84 0.01 2 14 2 2 GLY HA3 H 3.91 0.01 2 15 2 2 GLY C C 171.209 0.01 1 16 2 2 GLY CA C 42.43 0.01 1 17 3 3 GLY H H 7.988 0.01 1 18 3 3 GLY HA2 H 3.83 0.01 2 19 3 3 GLY HA3 H 3.92 0.01 2 20 3 3 GLY C C 171.209 0.01 1 21 3 3 GLY CA C 42.133 0.01 1 22 4 4 PHE H H 7.988 0.01 1 23 4 4 PHE HA H 4.65 0.01 1 24 4 4 PHE HB2 H 3.18 0.01 3 25 4 4 PHE HB3 H 2.97 0.01 1 26 4 4 PHE HD1 H 7.266 0.01 3 27 4 4 PHE HE1 H 7.293 0.01 3 28 4 4 PHE HZ H 7.332 0.01 1 29 4 4 PHE C C 172.062 0.01 1 30 4 4 PHE CA C 54.79 0.01 1 31 4 4 PHE CB C 36.95 0.01 1 32 4 4 PHE CD1 C 129.387 0.01 3 33 4 4 PHE CE1 C 128.971 0.01 3 34 4 4 PHE CG C 136.543 0.01 1 35 4 4 PHE CZ C 128.547 0.01 1 36 5 5 LEU H H 7.901 0.01 1 37 5 5 LEU HA H 4.173 0.01 1 38 5 5 LEU HB2 H 1.575 0.01 1 39 5 5 LEU HB3 H 1.575 0.01 1 40 5 5 LEU HD1 H 0.8439 0.01 2 41 5 5 LEU HD2 H 0.8704 0.01 2 42 5 5 LEU HG H 1.575 0.01 1 43 5 5 LEU C C 179.463 0.01 1 44 5 5 LEU CA C 54.78 0.01 1 45 5 5 LEU CB C 40.875 0.01 1 46 5 5 LEU CD1 C 21.05 0.01 2 47 5 5 LEU CD2 C 22.38 0.01 2 48 5 5 LEU CG C 24.528 0.01 1 stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Saveframe_category coupling_constants _Details . loop_ _Software_label $xwinnmr stop_ loop_ _Experiment_label '2D DQF-COSY' stop_ _Sample_conditions_label $solution_in_90%_H2O_10%_D2O_pH_6.6_298K _Spectrometer_frequency_1H 500 _Mol_system_component_name Leu-enkephalin _Text_data_format . _Text_data . loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 4 PHE H 4 PHE HA 9.0 . . 0.2 2 3JHNHA 5 LEU H 5 LEU HA 8.0 . . 0.2 stop_ save_ save_constraint_statistics _Saveframe_category constraint_statistics _Text_data_format . _Text_data . _NOE_interproton_distance_evaluation . _NOE_pseudoatom_corrections . _Details . save_