data_25820 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR structure of Peptide PG-992 in DPC micelles ; _BMRB_accession_number 25820 _BMRB_flat_file_name bmr25820.str _Entry_type original _Submission_date 2015-12-14 _Accession_date 2015-12-14 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Carotenuto Alfonso . . 2 Merlino Francesco . . 3 Chai Minying . . 4 Brancaccio Diego . . 5 Yousif 'Ali Munaim' . . 6 Novellino Ettore . . 7 Hruby 'Victor J' . . 8 Grieco Paolo . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 78 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2016-07-22 update BMRB 'update entry citation' 2015-12-14 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 25813 'Peptide PG-989 in DPC micelles' 25814 'Peptide PG-990 in DPC micelles' stop_ _Original_release_date 2015-12-14 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Discovery of Novel Potent and Selective Agonists at the Melanocortin3 Receptor ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 26599352 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Carotenuto Alfonso . . 2 Merlino Francesco . . 3 Chai Minying . . 4 Brancaccio Diego . . 5 Yousif 'Ali Munaim' . . 6 Novellino Ettore . . 7 Hruby 'Victor J' . . 8 Grieco Paolo . . stop_ _Journal_abbreviation 'J. Med. Chem.' _Journal_volume 58 _Journal_issue 24 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 9773 _Page_last 9778 _Year 2015 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Peptide PG-990' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label PG-992 $PG-992 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_PG-992 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common PG-992 _Molecular_mass 1322.594 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 10 _Mol_residue_sequence ; XXDWPXRWKX ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 3 ACE 2 4 NLE 3 5 ASP 4 6 TRP 5 7 PRO 6 8 4J2 7 9 ARG 8 10 TRP 9 11 LYS 10 12 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_NLE _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common NORLEUCINE _BMRB_code NLE _PDB_code NLE _Standard_residue_derivative . _Molecular_mass 131.173 _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 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? CE CE C . 0 . ? H H H . 0 . ? HN2 HN2 H . 0 . ? HA HA H . 0 . ? HXT HXT H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HD2 HD2 H . 0 . ? HD3 HD3 H . 0 . ? HE1 HE1 H . 0 . ? HE2 HE2 H . 0 . ? HE3 HE3 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 CA ? ? SING N H ? ? SING N HN2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? SING CD CE ? ? SING CD HD2 ? ? SING CD HD3 ? ? SING CE HE1 ? ? SING CE HE2 ? ? SING CE HE3 ? ? stop_ save_ save_chem_comp_4J2 _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common '(2R)-2-amino-3-(naphthalen-2-yl)propanoic acid' _BMRB_code 4J2 _PDB_code 4J2 _Standard_residue_derivative . _Molecular_mass 215.248 _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 . ? CA CA C . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD1 CD1 C . 0 . ? CD2 CD2 C . 0 . ? CE1 CE1 C . 0 . ? CZ1 CZ1 C . 0 . ? CZ2 CZ2 C . 0 . ? CZ3 CZ3 C . 0 . ? CE2 CE2 C . 0 . ? CE3 CE3 C . 0 . ? CE4 CE4 C . 0 . ? HE1 HE1 H . 0 . ? HE3 HE3 H . 0 . ? HE4 HE4 H . 0 . ? C C C . 0 . ? O O O . 0 . ? H H H . 0 . ? H1 H1 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB1 HB1 H . 0 . ? HD1 HD1 H . 0 . ? HD2 HD2 H . 0 . ? HZ2 HZ2 H . 0 . ? HZ23 HZ23 H . 0 . ? OXT OXT O . 0 . ? HXT HXT 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 CA ? ? SING CA CB ? ? SING CA C ? ? SING CB CG ? ? DOUB CG CD1 ? ? SING CG CD2 ? ? SING CD1 CE1 ? ? DOUB CD2 CE2 ? ? DOUB CE1 CZ1 ? ? SING CE1 HE1 ? ? SING CZ1 CZ2 ? ? SING CZ1 CE2 ? ? DOUB CZ2 CZ3 ? ? SING CZ3 CE4 ? ? SING CE2 CE3 ? ? DOUB CE3 CE4 ? ? SING CE3 HE3 ? ? SING CE4 HE4 ? ? DOUB C O ? ? SING N H ? ? SING N H1 ? ? SING CA HA ? ? SING CB HB2 ? ? SING CB HB1 ? ? SING CD1 HD1 ? ? SING CD2 HD2 ? ? SING CZ2 HZ2 ? ? SING CZ3 HZ23 ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ 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_ save_chem_comp_ACE _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'ACETYL GROUP' _BMRB_code ACE _PDB_code ACE _Standard_residue_derivative . _Molecular_mass 44.053 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C C C . 0 . ? O O O . 0 . ? CH3 CH3 C . 0 . ? H H H . 0 . ? H1 H1 H . 0 . ? H2 H2 H . 0 . ? H3 H3 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 DOUB C O ? ? SING C CH3 ? ? SING C H ? ? SING CH3 H1 ? ? SING CH3 H2 ? ? SING CH3 H3 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $PG-992 enterobacteria 562 Bacteria . Escherichia coli 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 $PG-992 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type micelle _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $PG-992 2 mM 'natural abundance' DPC 200 mM [U-2H] H2O 90 % 'natural abundance' D2O 10 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_XEASY _Saveframe_category software _Name XEASY _Version . loop_ _Vendor _Address _Electronic_address 'Bartels et al.' . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_CYANA _Saveframe_category software _Name CYANA _Version . loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 700 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_DQF-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 10 . mM pH 5.5 . pH pressure 1 . atm temperature 298.0 . 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_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name PG-992 _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 3 1 ACE H1 H 1.912 0.000 . 2 3 1 ACE H2 H 1.912 0.000 . 3 3 1 ACE H3 H 1.912 0.000 . 4 4 2 NLE HA H 5.021 0.000 . 5 4 2 NLE HB2 H 1.521 0.000 . 6 4 2 NLE HB3 H 1.665 0.000 . 7 4 2 NLE HG2 H 0.636 0.000 . 8 4 2 NLE HG3 H 0.836 0.000 . 9 4 2 NLE HN H 7.977 0.000 . 10 4 2 NLE HD2 H 1.159 0.000 . 11 4 2 NLE HD3 H 1.159 0.000 . 12 4 2 NLE HE1 H 0.371 0.000 . 13 4 2 NLE HE2 H 0.371 0.000 . 14 4 2 NLE HE3 H 0.371 0.000 . 15 5 3 ASP H H 8.807 0.001 . 16 5 3 ASP HA H 5.506 0.000 . 17 5 3 ASP HB2 H 2.541 0.000 . 18 5 3 ASP HB3 H 2.933 0.000 . 19 6 4 TRP H H 7.928 0.000 . 20 6 4 TRP HA H 3.959 0.000 . 21 6 4 TRP HB2 H 3.063 0.000 . 22 6 4 TRP HB3 H 3.101 0.030 . 23 6 4 TRP HD1 H 6.975 0.001 . 24 6 4 TRP HE1 H 10.677 0.000 . 25 6 4 TRP HE3 H 6.253 0.001 . 26 6 4 TRP HZ2 H 7.420 0.000 . 27 6 4 TRP HZ3 H 6.661 0.000 . 28 6 4 TRP HH2 H 7.001 0.000 . 29 7 5 PRO HA H 2.715 0.001 . 30 7 5 PRO HB2 H 0.228 0.000 . 31 7 5 PRO HB3 H 1.628 0.000 . 32 7 5 PRO HG2 H 1.175 0.000 . 33 7 5 PRO HG3 H 1.615 0.000 . 34 7 5 PRO HD2 H 3.050 0.000 . 35 7 5 PRO HD3 H 3.311 0.000 . 36 8 6 4J2 HA H 4.844 0.000 . 37 8 6 4J2 HB2 H 2.832 0.000 . 38 8 6 4J2 HB3 H 3.059 0.000 . 39 8 6 4J2 HD1 H 7.115 0.001 . 40 8 6 4J2 HD2 H 7.382 0.002 . 41 8 6 4J2 HE1 H 7.553 0.000 . 42 8 6 4J2 HE3 H 7.924 0.000 . 43 8 6 4J2 HE4 H 7.592 0.000 . 44 8 6 4J2 HN H 8.868 0.000 . 45 8 6 4J2 HZ2 H 7.887 0.000 . 46 8 6 4J2 HZ3 H 7.507 0.000 . 47 9 7 ARG H H 8.308 0.000 . 48 9 7 ARG HA H 4.726 0.000 . 49 9 7 ARG HB2 H 1.674 0.000 . 50 9 7 ARG HB3 H 1.876 0.000 . 51 9 7 ARG HG2 H 1.455 0.000 . 52 9 7 ARG HG3 H 1.534 0.000 . 53 9 7 ARG HD2 H 3.157 0.000 . 54 9 7 ARG HD3 H 3.157 0.000 . 55 9 7 ARG HE H 7.151 0.000 . 56 10 8 TRP H H 9.085 0.000 . 57 10 8 TRP HA H 5.171 0.000 . 58 10 8 TRP HB2 H 3.148 0.000 . 59 10 8 TRP HB3 H 3.389 0.000 . 60 10 8 TRP HD1 H 7.299 0.000 . 61 10 8 TRP HE1 H 10.671 0.000 . 62 10 8 TRP HE3 H 7.697 0.001 . 63 10 8 TRP HZ2 H 7.498 0.000 . 64 10 8 TRP HZ3 H 6.962 0.001 . 65 10 8 TRP HH2 H 7.078 0.000 . 66 11 9 LYS H H 8.689 0.000 . 67 11 9 LYS HA H 4.176 0.000 . 68 11 9 LYS HB2 H 1.531 0.000 . 69 11 9 LYS HB3 H 1.745 0.000 . 70 11 9 LYS HG2 H 1.199 0.000 . 71 11 9 LYS HG3 H 1.307 0.000 . 72 11 9 LYS HD2 H 1.448 0.000 . 73 11 9 LYS HD3 H 1.448 0.000 . 74 11 9 LYS HE2 H 3.059 0.000 . 75 11 9 LYS HE3 H 3.384 0.000 . 76 11 9 LYS HZ H 7.881 0.000 . 77 12 10 NH2 HN1 H 6.497 0.000 . 78 12 10 NH2 HN2 H 7.128 0.000 . stop_ save_