data_27756 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Assigned 1H NMR Chemical Shifts for endomorphin-1 in 10 mM phosphate pH 7.0 ; _BMRB_accession_number 27756 _BMRB_flat_file_name bmr27756.str _Entry_type original _Submission_date 2019-01-16 _Accession_date 2019-01-16 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'Assigned NMR resonances from combined 2D 1H-1H COSY, TOCSY, and ROESY data' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Alexandra Schwartz C. . 2 Michael Giuliano W. . 3 Parnham Stuart . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 3 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 84 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2020-01-17 original BMRB . stop_ _Original_release_date 2019-01-16 save_ ############################# # Citation for this entry # ############################# save_In_Preparation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Sequential and Environmental Dependence of Conformation in a Small Opioid Peptide ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 31538782 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Schwartz Alexandra C. . 2 Jay Dashiell W. . 3 Parnham Stuart . . 4 Giuliano Michael W. . stop_ _Journal_abbreviation 'J. Org. Chem.' _Journal_volume 84 _Journal_issue 21 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 13299 _Page_last 13312 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Endomorphin-1 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label Endomorphin-1 $EM-1 stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_EM-1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common EM-1 _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 5 _Mol_residue_sequence ; YPWFX ; loop_ _Residue_seq_code _Residue_label 1 TYR 2 PRO 3 TRP 4 PHE 5 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'AMINO GROUP' _BMRB_code NH2 _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 H . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING N HN1 ? ? SING N HN2 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $EM-1 . . . . . . 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 _Details $EM-1 'chemical synthesis' . . . . . ; Peptide was accessed via Fmoc solid-phase peptide synthesis using piperidine/DMF deprotection conditions and HCTU/Cl-HOBt/NMM amino acid activation conditions. ; stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_ACS-I-020A _Saveframe_category sample _Sample_type solution _Details 'Endomorphin-1 in aqueous buffer' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $EM-1 2 mM 'natural abundance' D2O 10 '% v/v' '99.8% D incorporation' 'sodium phosphate' 10 mM 'natural abundance' H2O 90 '% v/v' 'natural abundance' stop_ save_ save_ACS-I-020A_-_lipids_-_major_conf _Saveframe_category sample _Sample_type solution _Details 'Endomorphin-1 in aqueous buffer with 15 wt% deuterated bicelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $EM-1 2 mM 'natural abundance' D2O 10 '% v/v' '99.8% D incorporation' 'sodium phosphate' 10 mM 'natural abundance' 'DMPC-d54/DHPC-d22 bicelles (q=0.5)' 15 'wt %' 'DMPC-d54 ; DHPC-d22' H2O 90 '% v/v' 'natural abundance' stop_ save_ save_ACS-I-020A_-_lipids_-_minor_conf _Saveframe_category sample _Sample_type solution _Details 'Endomorphin-1 in aqueous buffer with 15 wt% deuterated bicelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $EM-1 2 mM 'natural abundance' D2O 10 '% v/v' '99.8% D incorporation' 'sodium phosphate' 10 mM 'natural abundance' 'DMPC-d54/DHPC-d22 bicelles (q=0.5)' 15 'wt %' 'DMPC-d54 ; DHPC-d22' H2O 90 '% v/v' 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_Mestrenova _Saveframe_category software _Name Mestrenova _Version 12.02-20910 loop_ _Vendor _Address _Electronic_address 'Mestrelab Research S.L.' . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model 'Avance II' _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $ACS-I-020A save_ save_2D_1H-1H_COSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H COSY' _Sample_label $ACS-I-020A save_ save_2D_1H-1H_ROESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H ROESY' _Sample_label $ACS-I-020A save_ save_1D_1H_acquisition_4 _Saveframe_category NMR_applied_experiment _Experiment_name '1D 1H acquisition' _Sample_label $ACS-I-020A save_ save_2D_1H-1H_TOCSY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $ACS-I-020A_-_lipids_-_major_conf save_ save_2D_1H-1H_COSY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H COSY' _Sample_label $ACS-I-020A_-_lipids_-_major_conf save_ save_2D_1H-1H_NOESY_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $ACS-I-020A_-_lipids_-_major_conf save_ save_1D_1H_acquisition_8 _Saveframe_category NMR_applied_experiment _Experiment_name '1D 1H acquisition' _Sample_label $ACS-I-020A_-_lipids_-_major_conf save_ save_2D_1H-1H_TOCSY_9 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $ACS-I-020A_-_lipids_-_minor_conf save_ save_2D_1H-1H_COSY_10 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H COSY' _Sample_label $ACS-I-020A_-_lipids_-_minor_conf save_ save_2D_1H-1H_NOESY_11 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $ACS-I-020A_-_lipids_-_minor_conf save_ save_1D_1H_acquisition_12 _Saveframe_category NMR_applied_experiment _Experiment_name '1D 1H acquisition' _Sample_label $ACS-I-020A_-_lipids_-_minor_conf save_ ####################### # Sample conditions # ####################### save_sample_conditions_ACS-I-020A _Saveframe_category sample_conditions _Details ; 10% D2O, 90% H2O 2 mM peptide (endomorphin-1) 10 mM phosphate buffer pH 7.0 298K ; loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.012 . M pH 7.0 . pH pressure 1 . atm temperature 298 . K stop_ save_ save_sample_conditions_ACS-I-020A-lipids-major_conf _Saveframe_category sample_conditions _Details ; 10% D2O, 90% H2O 2 mM peptide (endomorphin-1) 10 mM phosphate buffer pH 7.0 15 wt % DMPC-d54/DHPC-d22 bicelles ; q = 0.5 298K ; loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7.0 . pH pressure 1 . atm temperature 298 . K stop_ save_ save_sample_conditions_ACS-I-020A-lipids-minor_conf _Saveframe_category sample_conditions _Details ; 10% D2O, 90% H2O 2 mM peptide (endomorphin-1) 10 mM phosphate buffer pH 7.0 15 wt % DMPC-d54/DHPC-d22 bicelles ; q = 0.5 298K ; loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7.0 . pH pressure 1 . atm temperature 298 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _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 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $Mestrenova stop_ loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-1H COSY' '2D 1H-1H ROESY' '1D 1H acquisition' stop_ loop_ _Sample_label $ACS-I-020A stop_ _Sample_conditions_label $sample_conditions_ACS-I-020A _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name Endomorphin-1 _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 4.82 0.01 1 2 1 1 TYR HB2 H 2.57 0.01 1 3 1 1 TYR HB3 H 2.70 0.01 1 4 1 1 TYR HD1 H 7.06 0.01 3 5 1 1 TYR HD2 H 7.06 0.01 3 6 1 1 TYR HE1 H 6.82 0.01 3 7 1 1 TYR HE2 H 6.82 0.01 3 8 2 2 PRO HA H 4.41 0.01 1 9 2 2 PRO HB2 H 1.71 0.01 1 10 2 2 PRO HB3 H 2.13 0.01 1 11 2 2 PRO HG2 H 1.86 0.01 1 12 2 2 PRO HG3 H 1.91 0.01 1 13 2 2 PRO HD2 H 3.18 0.01 1 14 2 2 PRO HD3 H 3.62 0.01 1 15 3 3 TRP H H 7.72 0.01 1 16 3 3 TRP HA H 4.54 0.01 1 17 3 3 TRP HB2 H 3.23 0.01 2 18 3 3 TRP HB3 H 3.23 0.01 2 19 3 3 TRP HD1 H 7.14 0.01 1 20 3 3 TRP HE1 H 10.13 0.01 1 21 3 3 TRP HE3 H 7.63 0.01 1 22 3 3 TRP HZ2 H 7.37 0.01 1 23 3 3 TRP HZ3 H 7.20 0.01 1 24 3 3 TRP HH2 H 7.16 0.01 1 25 4 4 PHE H H 7.73 0.01 1 26 4 4 PHE HA H 4.50 0.01 1 27 4 4 PHE HB2 H 2.85 0.01 1 28 4 4 PHE HB3 H 2.95 0.01 1 29 4 4 PHE HD1 H 7.27 0.01 4 30 4 4 PHE HD2 H 7.27 0.01 4 31 4 4 PHE HE1 H 7.27 0.01 4 32 4 4 PHE HE2 H 7.27 0.01 4 33 4 4 PHE HZ H 7.27 0.01 4 stop_ save_ save_assigned_chem_shift_list_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $Mestrenova stop_ loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-1H COSY' '2D 1H-1H NOESY' '1D 1H acquisition' stop_ loop_ _Sample_label $ACS-I-020A_-_lipids_-_major_conf stop_ _Sample_conditions_label $sample_conditions_ACS-I-020A-lipids-major_conf _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name Endomorphin-1 _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 4.46 0.01 1 2 1 1 TYR HB2 H 2.70 0.01 1 3 1 1 TYR HB3 H 3.06 0.01 1 4 1 1 TYR HD1 H 7.00 0.01 3 5 1 1 TYR HD2 H 7.00 0.01 3 6 1 1 TYR HE1 H 6.78 0.01 3 7 1 1 TYR HE2 H 6.78 0.01 3 8 2 2 PRO HA H 4.49 0.01 1 9 2 2 PRO HB2 H 1.93 0.01 1 10 2 2 PRO HB3 H 2.13 0.01 1 11 2 2 PRO HG2 H 1.76 0.01 2 12 2 2 PRO HG3 H 1.76 0.01 2 13 2 2 PRO HD2 H 3.09 0.01 1 14 2 2 PRO HD3 H 3.63 0.01 1 15 3 3 TRP H H 7.81 0.01 1 16 3 3 TRP HA H 4.45 0.01 1 17 3 3 TRP HB2 H 3.09 0.01 2 18 3 3 TRP HB3 H 3.09 0.01 2 19 3 3 TRP HD1 H 7.28 0.01 1 20 3 3 TRP HE1 H 10.47 0.01 1 21 3 3 TRP HE3 H 7.56 0.01 1 22 3 3 TRP HZ2 H 7.40 0.01 1 23 3 3 TRP HZ3 H 7.00 0.01 1 24 3 3 TRP HH2 H 7.06 0.01 1 25 4 4 PHE H H 7.56 0.01 1 26 4 4 PHE HA H 4.61 0.01 1 27 4 4 PHE HB2 H 2.93 0.01 1 28 4 4 PHE HB3 H 3.10 0.01 1 29 4 4 PHE HD1 H 7.21 0.01 3 30 4 4 PHE HD2 H 7.21 0.01 3 31 4 4 PHE HE1 H 7.27 0.01 3 32 4 4 PHE HE2 H 7.27 0.01 3 33 4 4 PHE HZ H 7.15 0.01 1 34 5 5 NH2 HN1 H 7.22 0.01 1 35 5 5 NH2 HN2 H 7.77 0.01 1 stop_ save_ save_assigned_chem_shift_list_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $Mestrenova stop_ loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-1H COSY' '2D 1H-1H NOESY' '1D 1H acquisition' stop_ loop_ _Sample_label $ACS-I-020A_-_lipids_-_minor_conf stop_ _Sample_conditions_label $sample_conditions_ACS-I-020A-lipids-minor_conf _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name Endomorphin-1 _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 HB2 H 2.70 0.01 1 2 1 1 TYR HB3 H 2.95 0.01 1 3 1 1 TYR HD1 H 6.68 0.01 3 4 1 1 TYR HD2 H 6.68 0.01 3 5 1 1 TYR HE1 H 6.57 0.01 3 6 1 1 TYR HE2 H 6.57 0.01 3 7 3 3 TRP H H 8.03 0.01 1 8 3 3 TRP HA H 4.66 0.01 1 9 3 3 TRP HB2 H 3.03 0.01 2 10 3 3 TRP HB3 H 3.03 0.01 2 11 3 3 TRP HD1 H 7.33 0.01 1 12 3 3 TRP HE1 H 10.60 0.01 1 13 3 3 TRP HE3 H 7.62 0.01 1 14 3 3 TRP HZ2 H 7.57 0.01 1 15 3 3 TRP HZ3 H 7.16 0.01 1 16 3 3 TRP HH2 H 7.14 0.01 1 stop_ save_